Uddin Dissertation 2022

INVESTIGATION OF STRUCTURE-PROPERTY EFFECTS ON NANOINDENTATION
AND SMALL-SCALE MECHANICAL TESTING OF IRRADIATED ADDITIVELY
MANUFACTURED STAINLESS STEELS
Mohammad Jashim Uddin, B.S., M.S.
Dissertation Prepared for the Degree of
DOCTOR OF PHILOSOPHY
UNIVERSITY OF NORTH TEXAS
August 2022
APPROVED:
Hector R. Siller, Major Professor

Reza Mirshams, Co- Major Professor
Taeyul Theo Choi, Committee Member
Sheldon Shi, Committee Member
Bibhudutta Rout, Committee Member
Herman Shen, Chair of the Department of
Mechanical Engineering
Shengli Fu, Interim Dean of the College of
Engineering
Victor Prybutok, Dean of the Toulouse Graduate
School
Uddin, Mohammad Jashim. Investigation of Structure-Property Effects on
Nanoindentation and Small-Scale Mechanical Testing of Irradiated Additively Manufactured
Stainless Steels. Doctor of Philosophy (Mechanical and Energy Engineering), August 2022, 128
pp., 21 tables, 44 figures, 198 numbered references.
Additively manufactured (AM) 316L and 17-4PH stainless steel parts, concretely made by
laser powder bed fusion (L-PBF), are characterized and micro-mechanical properties of those
steels are analyzed. This study also explored and extended to proton irradiation and small-scale
mechanical testing of those materials, to investigate how irradiation affects microstructural
evolution and thus mechanical properties at the surface level, which could be detrimental in the
long term in nuclear applications. In-depth anisotropy analysis of L-PBF 316L stainless steel parts
with the variations of volumetric energy density, a combined study of nanoindentation with EBSD
(electron backscatter diffraction) mapping is shown to be an alternative methodology for enriching
qualification protocols. Each grain with a different crystallographic orientation was mapped
successfully by proper indentation properties. <122> and <111> oriented grains displayed higher
than average indentation modulus and hardness whereas, <001>, <101>, and <210> oriented
grains were found to be weaker in terms of indentation properties.
Based on an extensive nanoindentation study, L-PBF 17-4 PH stainless steels are found to
be very sensitive to high load rates and irradiation further escalates that sensitivity, especially after
a 0.25 s-1 strain rate. 3D porosity measurement via X-ray microscope ensures L-PBF stainless steel
parts are of more than 99.7% density and could be promising for many industrial applications.
High percentages of increment of nanohardness, maximum theoretical shear strength, and yield
strength were observed due to proton irradiation of 5 um damage depth on the surface of 17-4 PH
steel parts.
Small-scale mechanical testing of irradiated AM nuclear stainless steels such as 17-4 PH
was carried out and investigated by micro-compression of FIB fabricated pillars of different sizes
of diameter. Irradiated 17-4 PH materials have never been investigated by this kind of testing
procedure to asses the stress-strain characteristics of micro-scale volumes and to explore the
structure-property relationship. Both as-built and irradiated AM 17-4 PH micropillars exhibited
step-ups in the early stage of load-displacement curves with a varying number of slip bands
intermittently formed throughout the pillar volume while compressed by the uniaxial load. As for
the radiation-damaged zone, micropillars displayed lesser slip bands compared to as-built parts as
irradiation damage creates an obstacle to dislocations movement and hence hardening. It requires
higher loads to initiate plastic deformation as dislocation must overcome irradiation-induced
obstacles for the slip to occur and localization of strain without increasing the load for a certain
amount of time during the test. Proton irradiation effects on the compressive mechanical properties
of AM 17-4 PH stainless steel parts depending on the volumetric energy density (VED) used
during the parts’ fabrication process. On as-built parts, compressive yield strength varied from
107.27 MPa to 150.70 MPa and it was in the range of 133.43 MPa to 244.57 MPa under irradiated
conditions. All 2 μm pillars were fabricated as their height falls within the radiation damage depth
of 5 μm. It was expected to generate the highest yield strength and tensile strength due to the
radiation hardening effect as discussed earlier. Yield and tensile strength were found to be the
highest as expected as of 244.57 MPa and 375.08 MPa in irradiated 17-4 PH sample 1 (VED =
54.76 J/mm3). Samples with lower VED exhibited better micro-mechanical compressive responses
than higher VED AM 17-4 PH parts in both as-built and irradiated conditions.
Copyright 2022
by
Mohammad Jashim Uddin
ii
ACKNOWLEDGEMENTS
From the very start to the very end of my Ph.D. program in Mechanical Engineering at the
University of North Texas, I am so blessed to meet and work with so many outstanding professors,
colleagues, and friends. I would like to thank Dr. Hector Siller for being my thesis major professor
as well as to give me a chance to work in his research group where I received his continuous
guidance and mentorship throughout my research and dissertation. Additionally, I am so grateful
for his countless hours of reflecting, reading, and providing ideas for the resolution of problems
throughout the entire process and without his guidance, I would not be able to come this far. I
would also like to thank Dr. Reza Mirshams for being my co-major professor and to provide
continuous support and advice in every step of my study.
I would like to give special thanks to Dr. Taeyul Choi and Dr. Sheldon Shi, for being part
of my dissertation committee and to provide their valuable input and expertise throughout the
process. I convey special thanks to Dr. Teresa Golden and Dr. Bibhudutta Raut for their
collaboration, support, and helpful discussions.
I dedicate this dissertation to my family specially my parents Md. Majibar Rahman and
Momtaz Begum who encouraged and supported me. I also dedicate this dissertation to my lovely
wife Sabiha Tul Jannat for her unconditional inspiration, love, and support throughout the process.
iii
TABLE OF CONTENTS
Page
ACKNOWLEDGEMENTS ........................................................................................................... iii
LIST OF TABLES ......................................................................................................................... vi
LIST OF FIGURES ..................................................................................................................... viii
CHAPTER 1. INTRODUCTION ................................................................................................... 1

1.1 Additive Manufacturing .......................................................................................... 1
1.2 Radiation-Resistant Alloys Manufacturing by Laser Powder Bed Fusion (L-PBF)
................................................................................................................................. 8
1.3 Laser Powder Bed Fusion of 316L and 17-4 PH Stainless Steels ........................ 10
1.4 Thesis Objectives .................................................................................................. 13
1.5 Scientific Justification of the Research ................................................................. 17
1.6 Hypothesis............................................................................................................. 23
1.7 What’s Inside this Dissertation ............................................................................. 24
CHAPTER 2. MATERIALS AND EXPERIMENTAL PROCEDURES .................................... 25

2.1 Methodology ......................................................................................................... 25
2.2 Materials ............................................................................................................... 30
2.3 Process Parameters................................................................................................ 31
2.4 Sample Preparation ............................................................................................... 33
2.5 Proton Irradiation .................................................................................................. 34
2.6 Nanoindentation .................................................................................................... 36
2.7 Strain-rate Sensitivity of 17-4 PH Stainless Steels ............................................... 37
2.8 Small-scale Mechanical Testing ........................................................................... 40
2.9 X-ray Diffraction (XRD) and Electron Backscattered Diffraction (EBSD)
Microstructural Characterization .......................................................................... 41
2.10 Porosity Analysis .................................................................................................. 43
2.11 Fabrication of Micropillars by Focused Ion Beam (FIB) ..................................... 44
CHAPTER 3. RESULTS AND DISCUSSIONS.......................................................................... 45

3.1 Nanoindentation and Electron Backscatter Diffraction Mapping in Laser Powder
Bed Fusion of Stainless Steel 316L ...................................................................... 45
3.1.1 Energy Dispersive X-ray Spectroscopy (EDS) ......................................... 46
iv
3.1.2 Nanoindentation Results ........................................................................... 46
3.1.3 Grain Morphology and Microstructures ................................................... 49
3.1.4 Electron Backscattered Diffraction (EBSD) Maps ................................... 54
3.1.5 Validation of the Indentation Results ....................................................... 61
3.1.6 Misorientation Angle and Grain Size Estimation ..................................... 62
3.1.7 Conclusions on Nanoindentation, Anisotropy, and Mechanical Properties
................................................................................................................... 64
3.2 Effects of Proton Irradiation on Nanoindentation Strain-Rate Sensitivity and
Microstructural Properties in L-PBF 17-4 PH Stainless Steels ............................ 66
3.2.1 X-ray Diffraction (XRD) Analysis ........................................................... 67
3.2.2 Micro-Mechanical Properties by Nanoindentation ................................... 68
3.2.3 EBSD Microstructural Characterization ................................................... 73
3.2.4 Correlation of Martensite Fractions to Process Parameters of L-PBF 17-4
PH As-Built and Irradiated Stainless Steel Parts ...................................... 78
3.2.5 Porosity Analysis ...................................................................................... 81
3.2.6 Strain-Rate Sensitivity (SRS) and Effect of Proton Irradiation on the
Hardness .................................................................................................... 83
3.2.7 Maximum Shear and Yield Strength Approximation ............................... 86
3.2.8 Conclusions of Irradiation Effects on Mechanical Properties and
Microstructure ........................................................................................... 90
3.3 Small-Scale Mechanical Testing of Proton Irradiated L-PBF 17-4 PH Stainless
Steels ..................................................................................................................... 91
3.3.1 Micro-Compression Testing, Observation of Micropillar Fractures, and
Nanoindentation Response........................................................................ 91
3.3.2 Conclusions of Irradiation Effects on Small-Scale Mechanical Testing of
AM 17-4 PH Stainless Steel ................................................................... 102
CHAPTER 4. CONCLUSIONS AND FUTURE WORKS........................................................ 104
REFERENCES ........................................................................................................................... 110
v
LIST OF TABLES
Page
Table 1: A literature review on nanoindentation study of similar AM metallic alloys (MC =

microstructural characterization, OIP = Orientation based indentation properties, SSE =
indentation size effect, SSMT = small-scale mechanical test, SRS = strain-rate sensitivity, B =
Berkovich, S = Spherical, FT = Flat tip)....................................................................................... 18
Table 2: Literature review on small-scale mechanical testing of relevant metallic alloys (LP =
laser power, HD = hatch distance, LT = layer thickness, SS = scanning speed, SS = strain rate,
YS = yield strength, UTS = ultimate tensile strength) .................................................................. 21
Table 3: Elemental composition of LPW AISI 316L stainless steel powder particles ................. 30
Table 4: EOS elemental composition of L-PBF 17-4 PH powder particles and printed parts ..... 31
Table 5: L-PBF AISI 316L stainless steel manufacturing process parameters ............................ 32
Table 6: L-PBF process parameters for the fabrication of 17-4 PH stainless steel parts.............. 33
Table 7: XRM Scan parameters .................................................................................................... 44
Table 8: Elemental quantitative analysis of AISI 316L powder by energy dispersive spectroscopy
(EDS) ............................................................................................................................................ 46
Table 9: Analysis of variance (ANOVA) of the influence of volumetric energy density (VED) on
the indentation modulus (significance level, α =0.05) .................................................................. 47
Table 10: Analysis of variance (ANOVA) of the influence of volumetric energy density (VED)
on hardness values by nanoindentation (significance level, α =0.05) .......................................... 48
Table 11: Statistical One-way ANOVA of hardness data ............................................................ 70
Table 12: Statistical One-way ANOVA of indentation modulus data.......................................... 72
Table 13: Quantitative analysis of EBSD scans of as-built and irradiated L-PBF 17-4 PH
stainless steel parts ........................................................................................................................ 79
Table 14: Percentage of martensite phase according to experiment and Eq. 8 for L-PBF 17-4 PH
stainless steels from open literatures............................................................................................. 80
Table 15: Percentage of porosity determined by using different methods for L-PBF 17-4 PH
stainless steels extracted from open literature. ............................................................................. 82
Table 16: Strain-rate of L-PBF 17-4 PH stainless steel using different approaches .................... 85
Table 17: Maximum shear strength of as-built and irradiated L-PBF 17-4 PH steel parts at 0.01s-1
strain rate with loads associated with first displacement bursts. .................................................. 87
vi
Table 18: Yield strength of as-built and irradiated L-PBF 17-4 PH steel parts at 0.01s-1 strain
rate................................................................................................................................................. 88
Table 19: Ultimate tensile strength and yield strength determined from engineering stress-strain
curves of all the pillars in as-built and irradiated conditions. ..................................................... 100
Table 20: Comparison with other AM 17-4 PH stainless steel micropillar compression testing
literature (LP = laser power (Watts), HD = hatch distance (μm), LT = layer thickness (μm), SS =
scanning speed (mm/s), UTS = Ultimate tensile strength) ......................................................... 101
Table 21: Summary of major mechanical properties calculated from indentation and small-scale
mechanical testing (for 3 μm) methods on as-built and irradiated 17-4 PH stainless steels....... 107
vii
LIST OF FIGURES
Page
Figure 1: Schematic of laser powder bed fusion (L-PBF) process and parameters. ....................... 6
Figure 2: Summary of dissertation investigations from AM to small-scale mechanical testing.

....................................................................................................................................................... 14
Figure 3: Research map with the outline of this study.................................................................. 15
Figure 4: List of mechanical properties that are studied and analyzed in this research................ 23
Figure 5: Methodology of the proposal ........................................................................................ 26
Figure 6: Layer-by-layer micro-mechanical properties by small-scale mechanical testing ......... 29
Figure 7: Schematics of process parameters and scanning strategy for the fabrication of L-PBF
AISI 316L parts............................................................................................................................. 32
Figure 8: SRIM simulated (a) distribution of 1 MeV proton in the 17-4PH steel, (b) Vacancies
and displacements per atom (dpa) as a function of depth for a proton irradiation fluence of
1.0×1019 ions/cm2. ......................................................................................................................... 35
Figure 9: Nanoindentation experimental set-up for strain-rate sensitivity study on as-built and
irradiated L-PBF 17-4 PH stainless steel parts. ............................................................................ 37
Figure 10: Example of a load-displacement (P-h) curve of as-built L-PBF 17-4 PH part (VED =
61.11 J/mm3) at 0.1 s-1 strain-rate. ................................................................................................ 37
Figure 11: Micro-compression experimental set up (a) 10 um diameter flat indenter tip, (b) array
of micropillars in irradiated condition, and (c) array of micropillars in as-built condition of AM
17-4 PH stainless steel parts. ........................................................................................................ 41
Figure 12: Regression analysis (ANOVA) of nanoindentation hardness and modulus data with
various VED; (a) Interval plot of indentation modulus and (b) interval plot of hardness with a
confidence level of 95%................................................................................................................ 47
Figure 13: SEM images showing build direction (BD) and grain morphology of L-PBF AISI
316L parts with different volumetric energy density (VED); (a) and (b) VED = 45.24 J/mm3, (c)
and (d) VED = 50 J/mm3, (e) and (f) VED = 56.67 J/mm3. ......................................................... 49
Figure 14: SEM images showing planar and cellular dendritic grains with build direction (BD) of
L-PBF AISI 316L parts with volumetric energy density (VED)=50 J/mm3; (a) area of SEM scan,
(b) cellular dendritic structures with preferential 45o angle growth with pool boundary, and (c)
planar grains. ................................................................................................................................. 52
viii
Figure 15: Microstructures of L-PBF AISI 316L parts with different process parameters; (a)
VED = 50 J/mm3, (b) VED = 56.67 J/mm3. ................................................................................. 53
Figure 16: EBSD maps of L-PBF AISI 316L parts showing one of three nanoindentation regions
with the variation of volumetric energy density; (a) EBSD and IPF color map, (b) texture PF and
(c) texture IPF of parts (VED = 45.24 J/mm3), and (d) EBSD map, (e) texture, and (f) texture IPF
of parts (VED = 50 J/mm3). .......................................................................................................... 55
Figure 17: EBSD maps of L-PBF AISI 316L parts showing one of three nanoindentation regions
with the variation of volumetric energy density; (a) EBSD map, (b) texture PF and (c) texture
IPF of parts (VED = 56.67 J/mm3), and followed by (d) EBSD map and IPF color map, (e)
texture PF and (f) texture IPF of parts (VED = 66.67 J/mm3). ..................................................... 56
Figure 18: EBSD map of L-PBF AISI 316L parts showing one of three nanoindentation regions
with the variation of volumetric energy density; (a) EBSD map, (b) texture PF and (c) texture
IPF of parts (VED = 83.33 J/mm3), and (d) original image quality map of part with VED = 50
J/mm3, and (e) IPF color map. ...................................................................................................... 57
Figure 19: EBSD maps of all L-PBF AISI 316L parts marked as rectangles in Fig. 16, Fig. 17
and Fig. 18. All indents are labeled with indentation modulus (IM) and hardness (H) generated
by the nanoindentation experiment; (a) VED = 45.24 J/mm3, (b) VED = 50 J/mm3, (c) VED =
56.67 J/mm3, (d) VED = 66.67 J/mm3, (e) VED = 83.33 J/mm3, and (f) original Image Quality
(IQ) of part with VED = 66.67 J/mm3 and IPF color map............................................................ 58
Figure 20: (a) EBSD maps of conventionally manufactured AISI 316L stainless steel, (b) texture
PF, (c) texture IPF, (d) rectangular area with indent’s hardness (H) and indentation modulus
(IM), (e) original IQ, and, (f) IPF color map. ............................................................................... 60
Figure 21: Indentation modulus (IM) and hardness (H) within same crystallographic orientation
grains from EBSD maps of AISI 316L parts with (a) VED = 56.67 J/mm3 and (b) VED = 66.67
J/mm3. ........................................................................................................................................... 61
Figure 22: Effect of grain size and misorientation angle on indentation modulus and hardness
based on volumetric energy density (VED). ................................................................................. 63
Figure 23: X-ray diffraction measurements of L-PBF 17-4 PH as-built (AB) and irradiated (IR)
stainless steel parts. ....................................................................................................................... 67
Figure 24: Nanoindentation hardness plot against different strain rates (histogram) for as-built
and irradiated L-PBF (54.76 J/mm3 and 61.11 J/mm3) 17-4 PH steel parts. ................................ 69
Figure 25: Nanoindentation modulus plot against different strain rates (mean plot and standard
deviation as error) for (a) as-built and (b) irradiated L-PBF 54.76 J/mm3 and 61.11 J/mm3 17-4
PH steel parts. ............................................................................................................................... 71
Figure 26: EBSD scan of nanoindentation area (at 0.5 s-1 strain rate) of as-built L-PBF 17-4 PH
stainless steel part with VED = 54.76 J/mm3; (a) IPF map in the (X–Y) plane perpendicular to
ix
the build direction, (b) phase map, (c) texture pole figure, (d) inverse texture pole figure, and (e)
IPF color maps of phases. ............................................................................................................. 75
Figure 27: EBSD scan of nanoindentation area (at 1 s-1 strain rate) of irradiated L-PBF 17-4 PH
Figure 30: X-ray microscope scan of L-PBF 17-4 PH stainless steel including irradiated zone
(volumetric energy density of 54.76 J/mm3); (a) 3D scan volume (reconstructed), (b) single slice
(ImageJ), and (c) 3D reconstruction of all 2401 slices showing pores or voids within the scanned
volume........................................................................................................................................... 81
volume........................................................................................................................................... 82
Figure 32: Load-displacement curves (P-h) for as-built L-PBF 17-4 PH stainless steel in different
strain rates, (a) VED = 54.76 J/mm3 and (b) VED = 61.11 J/mm3. .............................................. 84
Figure 33: Load-displacement curves (P-h) for irradiated L-PBF 17-4 PH stainless steel in
different strain rates, (a) VED = 54.76 J/mm3 and (b) VED = 61.11 J/mm3. ............................... 84
Figure 34: Strain-rate sensitivity (SRS) determined by plotting the log-log scale of average
hardness and strain rate values and plots are drawn considering the density of the parts
(normalized); (a) SRS in as-built and (b) SRS in irradiated L-PBF 17-4 PH steels parts. ........... 85
Figure 35: (a) First displacement pop-ins in load-displacement curves for as-built and irradiated
L-PBF 17-4 PH stainless steel parts and (b) effect of irradiation on maximum shear strength at
0.1 s-1 strain rate nanoindentation tests. ........................................................................................ 87
Figure 36: Hardness-displacement curves of as-built and irradiated 54.76 J/mm3 17-4 PH
stainless steel parts in different strain rates................................................................................... 88
Figure 37: Summary of micro-mechanical properties, quantitative analysis of EBSD maps, and
maximum shear strength of as-built (AB) and irradiated (IR) L-PBF 17-4 PH stainless steel parts
(based on EBSD scans performed on 1 s-1 strain rate nanoindentation areas).............................. 89
x
Figure 38: Initial (top row) and after micro-compression (bottom row) micropillars of as-built
AM 17-4 PH stainless steels with the volumetric energy density of 54.76 J/mm3 (sample 1); (a1)
and (a2) 3 μm pillar, and (b1) and (b2) 5 μm pillar. ..................................................................... 92
Figure 39: Initial (top row) and after micro-compression (bottom row) micropillars of as-built
and (a2) 3 μm pillar, and (b1) and (b2) 5 μm pillar. ..................................................................... 93
Figure 40: Initial (top row) and after micro-compression (bottom row) micropillars of irradiated
and (a2) 2 μm pillar, (b1) and (b2) 3 μm pillar , and (c1) and (c2) 5 μm pillar. ........................... 93
Figure 41: Initial (top row) and after micro-compression (bottom row) micropillars of irradiated
and (a2) 2 μm pillar, (b1) and (b2) 3 μm pillar, and (c1) and (c2) 5 μm pillar. ............................ 94
Figure 42: Load-displacement curves of as-built and irradiated AM 17-4 PH stainless steel parts
with two different volumetric energy densities (sample 1 = VED of 54.76 J/mm3 and sample 2 =
VED of 61.11 J/mm3). .................................................................................................................. 96
Figure 43: Engineering stress-strain curves of sample 1 (VED = 54.76 J/mm3) with different
sizes of micropillars of L-PBF 17-4 PH stainless steels in (a) as-built condition, (b) irradiation
condition, and (c) comparison between as-built and irradiation conditions. ................................ 97
Figure 44: Engineering stress-strain curves of sample 2 (VED of 61.11 J/mm3) with different
sizes of micropillars of L-PBF 17-4 PH stainless steels in (a) as-built condition, (b) irradiation
condition., and (c) comparison between as-built and irradiation conditions. ............................... 98
xi
CHAPTER 1
INTRODUCTION
1.1 Additive Manufacturing*
Additive manufacturing (AM) techniques are the processes to fabricate a wide range of
structures and complex geometries from 3-D solid models. These processes are usually fabricating
successive layers of materials that are formed on top of each other and built on support structures.
This technology was developed by Charles Hull in 1986 as a process known as stereolithography
(SLA), which later evolved into processes such as powder bed fusion, fused deposition modeling
(FDM), inkjet printing, and contour crafting (CC), and so on. An additive manufacturing process
involves numerous methods, materials, and equipment [1]. The growing consensus of adapting the
additive manufacturing techniques over traditional techniques is attributed to several advantages
including fabrication of complex geometry with high precision, maximum material savings,
flexibility in design, and personal customization. A wide range of materials is becoming available
to be fabricated using AM processes as traditional processes are more time-consuming, difficult,
and costly. An optimized pattern of additive manufacturing parts is important to control flaw
sensitivity and anisotropic behavior [2]. Also, changes in the printing environment influence the
quality of finished products [3]. AM is capable of fabricating parts of various sizes from the micro-
to macro-scale.
The revolution of additive manufacturing technology happened recently a few decades ago.
Some advantages over traditional manufacturing processes established the additive manufacturing
process as a unique field of fabrication of hundreds of materials and the numbers are increasing
* The latter portion of this section is reproduced from E. Ramirez-Cedillo, M.J. Uddin, J.A. Sandoval-Robles, R.A.
Mirshams, L. Ruiz-Huerta, C.A. Rodriguez, H.R. Siller, Process planning of L-PBF of AISI 316L for improving
surface quality and relating part integrity with microstructural characteristics, Surf. Coatings Technol. 396 (2020)
125956. https://doi.org/10.1016/j.surfcoat.2020.125956, with permission from Elsevier.
1
day by day. Some of the advantages are rapid prototyping, improved speed of production, ability
to create complex parts without any difficulty, cost-effective even for lower production volume,
high strength fabricated alloys parts, improved carbon footprint i.e. less waste in the production
process, and less energy usage, the requirement of less space to operate. Many industries such as
aerospace (engine and turbine parts), automotive (exhausts, mirrors, seat belt hook, headlight
heatsink, tire rims), clothing (eye wear, sports shoes, helmet, rackets), construction (entire
building), electronics (circuits, parts, mobile phones, antennas, sensors), medical (prosthetics,
body parts as in reconstructive surgery), technology (laptop and tablet cases, motherboards,
robotics) are implementing additive manufacturing processes and that number is increasing rapidly
[4–11]. From its roots in prototypes, metal AM has rapidly become a core technology that has a
practical application in several different industries. Often described as belonging to a group known
as “disruptive technologies” metal AM has the capacity to completely revolutionize how things
are made. It’s not currently used in high volume, mass productions, but instead offers the most
value where precision engineering is vital or where customization and flexibility are key. Fuel
nozzles in the aerospace industry are a great example of how this technology is used in practice.
The new designs created with the use of metal AM techniques are five times more durable and
25% lighter.
Different additive manufacturing processes are described in the standard ISO-ASTM
52900. Among them, the process of interest in this dissertation is Laser powder bed fusion
technologies (L-PBF), which have been extensively used in recent years since machines are more
affordable and the process is in continuous improvement [12–14]. With the advances in the
development of more efficient systems and lasers, and in situ monitoring, the productivity of L-
PBF machines has increased. The Wohlers report presented that revenue from AM metal machines
2
grew 29.9% in 2018 to an estimated 947.8 US million dollars [15]. Early adoption in the academy
and industry has increased the research and development of final products significantly. In the
academic field, according to the SCOPUS database, from 1975 to 2019, a total of 5889 documents
were published about L-PBF. In the last years, 2016 (624 documents), 2017 (865 documents), and
2018 (1226 documents) have been published, increasing the scientific and industrial knowledge
around this technology, where China, Germany, and the US are the countries with more
contributions. Another growing market in AM is the production of the powder. Commercially
available alloys commonly used for casting/powder metallurgy have been introduced to L-PBF
with successful results. Significant growth of 41.9% in 2018 of the revenue of different types of
commercial alloys in a total of 260.2 US million dollars. However, some critical issues have been
limiting the advantages of AM with these available materials, such as balling of the material during
the process, defects produced due to the thermal history of the material (solidification cracking/hot
tearing), and others [16]. Hence, the development of new alloys that can be weldable avoiding the
cracking tendency, has contributed to the exponential growth in the research on this topic. Even
though it is a recent technology, and there is a curve of knowledge for early adopters, with the
right guidelines, workflow, documentation, and characterization, optimized parameters can be
obtained. Thereby machines can be running production as some industries have reported. AM
processes provide unique challenges not experienced in traditional manufacturing methods. Due
to the nature of many AM processes, it is difficult to control the thermal history of a component,
resulting in heterogeneous microstructures and defect distributions [17]. This can be a result of the
size of the component, variations in thickness, or the number of components. As microstructure
plays a significant role in the material behavior in extreme environments, whether it be mechanical
3
properties or other environmental effects, it is vital that this process be better understood and
controlled.
The advantages of AM processes have emerged and continue to prevail through ongoing
research efforts to understand and eliminate constraints that inhibited the use of this technology.
Design tools to assess life-cycle costs i.e., AM-oriented computer-aided design (CAD) systems
with more user-friendly and advanced simulation capabilities are some of the key aspects that need
to be realized [18]. A distinguished advantage of AM techniques is mass customization i.e., the
production of a series of personalized goods such that each product can be different while
maintaining a low price due to mass production. These processes are devoid of the added cost due
to mold making and tooling for a customized product. Therefore, mass production of a number of
identical parts can be as cost-effective as the same number of different personalized goods. The
change between different designs is straightforward with negligible added cost and no need for
special preparation. AM processes also have the potential for mass production of complex
geometries such as lattice structures, where the application of traditional methods of manufacturing
such as casting is not straightforward and require further time-consuming tooling and post-
processing. However, improvements in the fabrication speed and cost reduction must be resolved
through the improvement of machine design. Also, the high costs and time-consumption of the
AM processes remain to be major hurdles that inhibit mass production [19].
Nuclear Regulatory Commission is inspiring scientific communities to perform
investigations to the better understanding of the behavior of irradiated additively manufactured
(AM) materials, like austenitic stainless steels that are used in the Transformational Challenge
Reactor Program [20,21] and Generation IV nuclear reactors. Presently, there are significant
efforts in several fields for thermo-mechanical processing to treat the intrinsic change of
4
mechanical properties and microstructural changes in additively manufactured components prone
to degradation, such as the evaluation of stress-corrosion cracking susceptibility, porosity,
crystallography, thermal diffusivity, anisotropy, and chemical heterogeneity, considering that AM
processes could bring profits to the fabrication of complex components in nuclear reactors and
vessels [22–26]. To mitigate the chance of materials failure or damage during service, AM
radiation-resistant engineering alloys must withstand levels of temperature and radiation existing
in operational conditions; hence the study of microstructure and micro-mechanical properties upon
irradiation, is mandatory toward effective materials qualification.
The reliance on witness specimens and printed coupons to determine the results of process
parameters are time-consuming and costly, and typically covers low-temperature applications
(witness specimens are scarcely been used for creep or high-temperature cyclic testing). There is
a large need for better AM models that more accurately reflect actual thermal histories, as well as
the resulting variations in microstructures, to reduce the need for experimental optimization of
processing parameters. The testing of AM material so far has largely, if not entirely, been
performed with uniaxial testing. There is a need to expand this work to examine the effects of
multiaxial loading [27,28], particularly for AM components that have exhibited anisotropic
mechanical strengths [12]. While necessary for all testing, it is expected that multiaxial testing
would be of particular importance when considering elevated temperature failure mechanisms. For
energy applications, however, there is a need to understand and qualify the behavior of AM
materials at elevated temperatures. Long-term and time-dependent failure mechanisms such as
creep and creep-fatigue damage control the design of high-temperature structural components [29].
These failure mechanisms are connected to time-dependent properties, such as creep, thermal
aging, cyclic softening, etc., and not time-independent properties, such as yield stress and ultimate
5
tensile stress. There is a significant gap in understanding the effects of AM properties on the
corrosion of a material. For many advanced energy systems, the environments have become
increasingly complex (molten salt, liquid sodium, super critical water, and super critical CO2). For
the use of AM within these and other environments, there needs to be an increased understanding
of the corrosion behavior of AM materials.
Figure 1: Schematic of laser powder bed fusion (L-PBF) process and parameters.
Understanding the basics of the processing parameters and variables that are inherent to
the process is fundamental to generate workflow or process guidelines. Firstly, processing
parameters have different names and nomenclatures. Figure 1 represents a summary of the most
important and well-known processing variables and their equivalences for different machines.
Laser Power (P), Layer thickness (LT), laser scanning speed (vs), and hatch distance (HD) are
considered to be the most important parameters due to their impact on the integrity of the parts
(Figure 1) [30]. Commercial machines have different laser systems that can be programmed in
different forms: pulse width modulated (PWM) and continuous (CW). When a laser is working
6
either in PWM, it can provide processing parameters related to the pulse frequency, duration, and
peak power [31]. Since L-PBF is an AM process, where layers (n) are added continuously, process
parameters such as the initial and rotation angle of layers can have an impact on the distribution
of stresses in all directions [32].
In order to relate parameters with the mechanical, geometric, surface, and density
properties, the volumetric energy density has been widely adopted as an indicator to select the
optimum range of parameters. Eq. (1) is the representation of VED in terms of the previously
presented most influential parameters P (watts), vs (mm/s), LT (μm), and HD (μm).

𝑃𝑃
𝑉𝑉𝑉𝑉𝑉𝑉 = 𝑣𝑣𝑠𝑠 ×𝐿𝐿𝐿𝐿×𝐻𝐻𝐻𝐻
(Eq. 1)
Some authors discussed if VED is a good approximation for parameter synthesis, drawing
several concerns due to the lack of information about the material consideration in the VED
equation [33], the lack of understanding of the main characteristics of the laser [34]; and the
uncertainty in reproducibility and feasibility. Other authors made profound conclusions about why
VED is a thermodynamic quantity without capturing complex physical phenomena such as the
Marangoni flow, hydrodynamic instabilities, and the recoil pressure, which have a direct impact
on the consistency of the tracks [35]. Still, VED is widely used to summarize process parameters,
in addition to characterization techniques such as porosity analysis, density measurements, and
tensile and hardness tests.
In summary, this dissertation is a package of a new strain-rate sensitivity model,
correlations between process-driven microstructures and micro-mechanical properties, and small-
scale mechanical testing of as-built and proton irradiated stainless steel materials fabricated by the
additive manufacturing process. The package, wholeheartedly, would be crucial for the overall
7
integrity of alternative materials qualification protocol for nuclear intricate material parts’
applications.
1.2 Radiation-Resistant Alloys Manufacturing by Laser Powder Bed Fusion (L-PBF)
Nuclear energy is looking to AM, along with other advanced manufacturing techniques, to
provide design flexibility, reduce costs, and shorten timelines for the production of components
that make up a nuclear power plant [36]. While other methods for nuclear energy components,
such as powder metallurgy (specifically hot isostatic pressing), are more developed, AM is a fairly
new area of interest for nuclear energy. AM has the benefit of allowing for constant process
monitoring of each layer of material as it is manufactured, allowing for improved manufacturing
control and the collection of detailed information about the properties of the final component.
Another benefit of AM is the ability to transition materials more seamlessly (gradual transitions
and narrow fusion zones with minimized heat-affected zones) than traditional joining (brazing,
welding, or soldering) or to create functionally graded compositions, or even fully 3D patterned
phase, grain size, and composition-distributions aimed at optimizing the microstructure-properties
relationship [37]. Material transitions are particularly common in nuclear plants, as there are large
variations in pressures, temperatures, and radiation doses, resulting in the need to employ a variety
of materials. AM has been demonstrated to create graded compositions of many types of materials,
such as Inconel to steel, copper to steel, titanium alloys to steel, as well as titanium alloys to carbide
materials [37–41]. Modeling and simulation efforts have helped progress this work and increase
the feasibility of functionally graded compositions, and even 3D printed micro-composites [42,43].
Most reactor internals is not pressure-retaining components and do not fall within the
restrictions of the ASME BPV Code, therefore, AM work has progressed more significantly in the
area of actual application in nuclear power plants. There is interest in AM for reactor core internals,
8
including manufacturing of fuel, cladding, control elements, etc. Westinghouse was one of the first
to consider installing actual AM components into a reactor, choosing to install a thimble plugging
device made of AM 316L steel. Significant work is being performed within research and test
reactors to better understand the performance of AM components. Oak Ridge National Laboratory
has explored the use of AM to manufacture control elements for the High-Flux Isotope Reactor
(HFIR) [44,45] and Idaho National Laboratory has used AM capsules for tests inside the Advanced
Test Reactor. Similar to the structural components, the benefits from AM include the ability to
create complex designs, rapidly prototype, and transition between dissimilar materials. For some
exotic materials, such as those used in nuclear fuels, there are additional benefits, such as using
the AM energy source not only for manufacturing the structure of the fuel but also for reducing or
modifying the fuel composition, such as in the conversion of UF4 to U3Si2, an accident tolerant
fuel [46]. In this case, there are additional benefits, such as using less equipment for fuel fabrication
from cradle to fuel product, as well as less raw material input and minimizing the facility footprint.
It also has the potential to improve the economics, as traditional manufacturing routes would
include an additional step of converting the UF4 to uranium metal before the formation of U3Si2.
AM has found applications in other areas related to nuclear energy outside of the plant itself. One
such application is the use of AM in the reprocessing of spent fuel. Spent nuclear fuel is a
significant challenge for the nuclear energy industry. One method for overcoming this problem is
to recycle the spent fuel and use it again in reactors. AM has been demonstrated to manufacture
complex, fluid devices with internal channels, as well as a full array of 1.25-cm diameter rotor
centrifugal contactors for small-scale demonstrations of separation techniques aiming to remove
minor actinides from used nuclear fuel [47]. In this case, AM was used to simplify the fabrication
processes and reduce the level of needed materials and human effort.
9
1.3 Laser Powder Bed Fusion of 316L and 17-4 PH Stainless Steels*
316L stainless steel alloy is a member of the austenitic steels that were developed more
than three decades ago for fast-breeder reactor applications within the EU countries. AISI 316L
grade has both good weldability and machinability and in combination with high corrosion
resistance, it can be used in a wide range of applications. Based on its excellent properties the
SS316L steel was selected as the main structure retaining material for the Vacuum Vessel and
other systems in the International Thermo-Nuclear Experimental Reactor (ITER) [48]. Researchers
and engineers have performed many experiments to establish the properties of 316L stainless
steels and tested various fabrication and joining methods used for the manufacturing of designed
components for nuclear fusion applications [49–51]. The aim was to confirm the steel behavior
under tough and very critical working environments. One major problem encountered has been the
complex geometry of the ITER in-vessel components, like the first wall (FW) panel, which needs
assembly of different sub-components to achieve the final complex part. This process is both
difficult and costly and the assembled larger component has a higher risk to fail at the joints. An
example of the presently favored technique is to make separate sub-components and use hot
isostatic pressing (HIP) to press them together. This procedure, however, involves many steps;
machining of the sub-plates, assembling of these sub-plates, pre-welding the sub-plates by laser or
electron beam, HIP at elevated temperature, post-machining, and final heat treatments. With such
a complex procedure a flaw formed in any of the initial steps might generate failure in the final
* This section is reproduced from a combination of 2 sources, both used with permission from Elseiver: (1) M.J.
Uddin, E. Ramirez-Cedillo, R.A. Mirshams, H.R. Siller, Nanoindentation and electron backscatter diffraction
mapping in laser powder bed fusion of stainless steel 316L, Mater. Charact. 174 (2021) 111047,
https://doi.org/10.1016/j.matchar.2021.111047 and (2) M.J. Uddin, H.R. Siller, R.A. Mirshams, T.A. Byers, B.
Rout, Effects of proton irradiation on nanoindentation strain-rate sensitivity and microstructural properties in L-PBF
17–4 PH stainless steels, Mater. Sci. Eng. A. 837 (2022) 142719. https://doi.org/10.1016/j.msea.2022.142719.
10
component. Therefore, new manufacturing methods are highly demanded for future fusion reactor
construction components.
The first material of interest in this research, austenitic stainless steel with denomination
AISI 316L, is widely employed in marine engineering, potable water systems, food preparation
equipment, pharmaceutical manufacturing, and medical implants. Particularly, the applications of
additively manufactured parts via laser powder bed fusion (L-PBF) are constantly expanding in
medical, nuclear, chemical, food, petrochemical, architecture, and automotive fields very rapidly,
because of its exceptional corrosion resistance and superior biocompatibility [52–61]. Several
limitations are preventing the full exploitation of L-PBF of AISI 316L; some of them are due to
the anisotropy and the heterogeneity in microstructure and mechanical properties as reported in
recent studies [62–66]. Pores, impurities, and unmelted powder particles are responsible for this
behavior, but there is also the influence of the nature of the microstructure: columnar and cellular
grain microstructures are formed together, a complex cyclic thermal history that includes
directional heat extraction, repeated melting, and rapid solidification of powder particles on the
same layer [67]. Additionally, the grain size and shape variation in different fabrication planes
parallel and perpendicular to the build direction also contribute to the anisotropy in mechanical
properties [63]. Another group of researchers verified that AISI 316L parts fabricated by L-PBF
exhibit lower resistance to deformation along the building direction, and anisotropy in
microstructure and mechanical properties which can be eliminated after recrystallization [62]. It is
also reported that post-processing of AM parts, though currently very costly, is mandatory to
obtain optimum dynamic properties like fatigue resistance in comparison to conventionally
produced parts [68]. One key aspect to consider for obtaining enhanced mechanical properties is
the control of grain aspect ratio and orientation since it was found in this study that material with
11
a lower grain aspect ratio (equiaxed shape) showed significantly increased mechanical properties
(YS=583 MPa, TS=685 MPa) compared to parts with a higher grain aspect ratio (columnar shape)
(YS=521MPa, TS=617MPa). To sum up, the influencing factors in the anisotropy and
heterogeneity in the microstructure and mechanical properties involve crystallographic texture,
lack-of-fusion defects, grain morphology, phase transformation, heterogeneous recrystallization,
layer building, and microstructural coarsening.
Different research studies addressed the relationship between anisotropy and process
parameters in the L-PBF of AISI 316L. According to recent scientific work, the most influential
parameter is the laser power, which affects part’s density, residual stresses, and tensile mechanical
properties [68]. Regarding the impact in terms of microstructure, a group of researchers found
that laser power of 380 W resulted in a <001> crystallographic texture and lower strains with larger
grain size and higher laser power (950 W) resulted in a <011> crystallographic texture and higher
strains with more dislocation density, which eventually make the latter stronger and tougher [69].
In parallel, high laser power of 1 kW with narrow Gaussian power distribution resulted in the
formation of long columnar grains along the building direction with variation in mechanical
properties and microstructures, whereas, low laser power of 400 W resulted in a finer sub-grain
and randomly oriented columnar grains with an increase in hardness and tensile strength [70].
From these findings, it can be stated that power by itself does not describe properly a clear
relationship and that the use of energy density could be more appropriate for understanding the
microstructural evolution and its connection with the mechanical response.
The second nuclear alloy in this research study is 17-4 precipitation hardening (PH) steels
which are considered difficult to be manufactured via conventional machining processes due to
their high strength and high hardness properties. PH steels are well suited to be fabricated by laser
12
powder bed fusion (L-PBF) technique due to better weldability and austenitic/martensitic
microstructure [71]. Nuclear, aerospace, marine, naval, and chemical industries use PH steels for
components and intricate parts. One of the most popular and widely used PH steel alloys is 17-4
PH stainless steel, and in the specific case of L-PBF 17-4 PH steels, the findings demonstrate their
corrosion resistance, a relatively high mechanical strength, good resistance against radiation, and
favorable fatigue behavior [72–74]. However, microstructural analysis and mechanical properties
have been reported and discussed in limited literature. Additively manufactured alloys are suitable
for applications under severe radiation environments and the application usually narrows the
materials qualification processes. Materials used under those harsh conditions require a standard
level of mechanical strength and stability, especially at elevated temperatures along with
corrosion-prone surroundings [75]. Recently, a group of researchers investigated the neutron-
irradiated conventional 304L austenitic stainless steels at a microstructural scale but did not study
the effect of irradiation on micro-mechanical properties such as nanohardness and indentation
modulus [76]. Therefore, to mitigate the chance of materials failure or damage, L-PBF radiation-
resistant engineering alloys must withstand successfully that level of temperature and radiation;
hence the study of microstructure and micro-mechanical properties of L-PBF 17-4 PH stainless
steels upon ion irradiation, seems to be mandatory toward effective materials selection in nuclear
industries.
1.4 Thesis Objectives
Laser powder bed fusion (L-PBF) processes are associated with pores, impurities, and
unmelted powder particles that are generally accountable for inferior performance of parts in the
field of applications, but there is also the influence of the nature of the microstructures as columnar
and cellular grain microstructures are formed together at complex cyclic thermal history, which
13
includes directional heat extraction, repeated melting, and rapid solidification of powder particles
on the same layer. As a whole, the manipulating factors in the microstructure disturbing
mechanical response comprise of crystallographic texture, lack-of-fusion defects, grain
morphology, phase transformation, heterogeneous recrystallization, layer building, and
microstructural coarsening among others. The different qualification methods in AM materials,
schematized in Figure 2, rely on the use of standardized specimens at different orientations on the
powder bed, and with different configurations of process parameters like laser power, laser
scanning speeds, layer thicknesses, hatching distances, and others.
Figure 2: Summary of dissertation investigations from AM to small-scale mechanical testing.
These tests can capture most of the mechanical characteristics but are unable to discover intrinsic
material properties of irradiated materials at low surface depths. The use of nanoindentation
(Figure 2) becomes an alternative and is complementary to elucidating the effect of proton and
neutron irradiation on a change in mechanical properties, that ultimately would be detrimental in
14
the long term. With the use of witness specimens replicating those geometries used in nuclear
reactors, the use of nanoindentation mapping, tensile testing, creep-fatigue testing, and
proton/neutron irradiation on AM materials, the development of microstructurally informed
models could be created as digital threads to increase reliability which is the main objective of this
dissertation.
Figure 3: Research map with the outline of this study
Besides, the research on the fundamental science of alternative qualification processes for
additively manufactured materials at the surface level is limited. Concretely, studies of
nanoindentation response, small-scale mechanical testing i.e. micropillar micro-compression,
strain-rate sensitivity (SRS), and microstructural and micro-mechanical characterizations on AM
nuclear alloys such as 316L and 17-4 PH stainless steels are very limited. This dissertation
emphasizes those scarcely explored research fields at the sub-micron level on L-PBF radiation-
resistant stainless steels and claims to have a multi-scale approach. The objective is to experiment
15
micro-mechanical behavior on L-PBF alloys in terms of micro-mechanical properties such as
indentation hardness, compressive strength, shear strength, and other critical properties needed to
be qualified in parts that will be subjected to extreme operational conditions. Additionally, to study
the sensitivity of nanoindentation behavior to loading rate in sub-micron level in which load-
displacement curves in different strain rates will provide insights into whether the radiation-
resistant alloys are susceptible to an increase in loading rate. Furthermore, the implementation of
focused ion beam (FIB) milling to create flat nanoindenter tip and micropillars is proposed as a
method to create samples to assess the size effects at the micro and small scale but particularized
to AM irradiated materials [77–82]. The research map is shown in Figure 3.
Studying strain-rate sensitivity (SRS) would also be helpful to determine the maximum
shear stress from the nanoindentation curve which is an estimate of the theoretical shear strength
of L-PBF radiation-resistant stainless steels. A mechanistic relationship is thereby possible
between size effects and micro-mechanical properties. Micro-compression tests with a range of
micropillars (diameter of 2 μm to 5 μm) are proposed for minimizing the size effects on the
accuracy of nanoindentation and to study how to determine yield strength in terms of a power-law
relationship. A large array of nanoindentation batch experiments would validate the hardness
measurements. On the other hand, radiation effects on the L-PBF parts in terms of hardness,
microstructures, and micro-compressive strength via micropillars both on the surface and along
the damage profile depth would be beneficial to characterize them in depth. Besides, process
parameters such as laser power, hatch distance, and layer thickness play an important role in
determining the micro-mechanical properties and crystallographic microstructures. There are
available resources of research on mechanical properties by nanoindentation of L-PBF radiation-
resistant stainless steels. But, the fields of exploring size effects, minimizing those effects, layer-
16
by-layer micro-mechanical properties along with the height of parts [83], the study of strain-rate
sensitivity by increasing the loading rate on those alloys, are very limited, and studying those fields
would be a significant contribution to the scientific community.
1.5 Scientific Justification of the Research*
Firstly, in-depth analysis of the microstructure and mechanical properties of additively
manufactured metals are less reported especially for radiation-resistant stainless steels. To realize
the full design potential that additively manufactured alloys can offer, more precisely for load-
bearing structural components, it is very important to provide a thorough understanding of the
anisotropic and heterogeneous microstructure and mechanical properties that often occur within
L-PBF parts during the complex solidification process. This dissertation outlines 316L and 17-4
PH stainless steel parts and reviews literature on the anisotropy and heterogeneity in microstructure
and mechanical. It can be highlighted that the contributing factors to the anisotropy and
heterogeneity within metal L-PBF parts were either their unique microstructural features or
manufacturing deficiencies. The correlation will be drawn by implementing quantitative analysis
tools provided based on EBSD (Electron backscatter diffraction) patterns between the grain
orientations and indent’s modulus of elasticity and hardness values determined by
nanoindentation.
Indentation techniques such as nanoindentation have a long practice in characterizing
mechanical property changes due to exposure in a nuclear environment and allow access to more
data from an instrumented indentation test. The utilization of nanoindentation has received great
* This section is reproduced from M.J. Uddin, H.R. Siller, R.A. Mirshams, T.A. Byers, B. Rout, Effects of proton
irradiation on nanoindentation strain-rate sensitivity and microstructural properties in L-PBF 17–4 PH stainless
steels, Mater. Sci. Eng. A. 837 (2022) 142719. https://doi.org/10.1016/j.msea.2022.142719, with permission from
Elsevier.
17
attention in ion beam irradiated materials [84]. Application of indentation in cross-section (large
array of indents in an area) to assess the ion-beam irradiation-related property changes has been
growing rapidly. Continuous stiffness mode indentation (where a low amplitude oscillation,
typically, 2 nm at 50 Hz, is overlaid on the load curve), is increasingly used because of very
shallow ion-beam irradiation, and more complex material properties such as strain rate sensitivity
and creep properties can be measured. A comparative literature review on nanoindentation
properties of various additively manufactured metallic alloys is shown in Table 1:
Table 1: A literature review on nanoindentation study of similar AM metallic alloys (MC =

microstructural characterization, OIP = Orientation based indentation properties, SSE = indentation
size effect, SSMT = small-scale mechanical test, SRS = strain-rate sensitivity, B = Berkovich, S =
Spherical, FT = Flat tip)
Tip used and
Mechanical Properties
Author Alloy (H=Nanohardness, IM= OIP SSE SSMT Irradiation SRS
Indentation Modulus in
GPa)
JS Weaver
SS 316 L B, S, H=3.59
[85]
X Wang
Ti-6Al-4V B, IM=112-116, H =6
[86]
B, H=2.6, H= 3.1
X Sun [87] SS 316 L (Irradiated Helium √ √
bubble interface)
A
Ti-6Al-4V, B, IM=112-144, H=2.9-
Reichardt
SS 304L 5.1
[88]
NT
B, H=1.82±0.01,
Aboulkhair AlSi10Mg
H=1.52±0.02 (HT)
[89]
H Wang B, H=3.58-4.70,
Inconel 718 √
[90] IM=160-200
B
B, FT, H=3.27±0.25,
AlMangour SS 17-4 PH √
H=3.87-4.07 (HT)
[91]
Ali
B, H=2.0±0.19,
Behroozfar Cu alloy √
IM=128.2±10.9
[92]
B, H=2.92-3.89 (variable
D. Gu [93] Ti alloy
scan speed)
W
B, H=2.8±0.5,
Żórawski Ti alloy
IM=98.8±12.9
[94]
18
Tip used and
Mechanical Properties
Author Alloy (H=Nanohardness, IM= OIP SSE SSMT Irradiation SRS
Indentation Modulus in
GPa)
Nicola M.
AlSi10Mg B, H=2.25±0.02
Everitt [95]
M Munther B, H=2.98-3.65,
Inconel 718
[96] IM=155-218
J. S.
Weaver Inconel 625 B, H=~5.5 √
[83]
R Erick, M
B, H= 3.93Y±1.19, IM=
J Uddin SS 316 L √
191.05±22.92
[12]
B, H=3.55±0.15,
SS 316 L,
M J Uddin IM=184.85±11.93,
Conventional √ √
[97] Conv: H=3.60±0.05,
316L
IM=189.15±5.88
B, H=4.02±1.25,
IM=170±70.89 (as-
M J Uddin built), H=7.47±3.15,
SS 17-4 PH √ √ √
[14] IM=196.15±70.352
(Irradiated) @variable
strain rates (0.01-1 s-1)
B, FT, At 0.01 s-1:
H=3.28±0.14,
M J Uddin, IM=185.32±5.27 (as-
SS 17-4 PH √ √ √ √
2022 built), H=6.46±0.15,
IM=224.18±6.82
(Irradiated)
Secondly, the term ‘small-scale materials’ testing relates to mechanical test specimens with
dimensions that require focused ion beam (FIB) to fabricate micropillars, a nanoindenter with a
flat indenter tip to perform the micro-compression test, and lastly, SEM or FIB to observe the
fracture type. Typically, the size scale is in the order of tens of nanometers to tens of micrometers,
therefore covering the lower end of the mesoscale spectrum. Small-scale mechanical testing
techniques have a long history in nuclear material research due to the limitations posed by nuclear
facilities [98]. The limited space in reactors and the issue that metal structures are often radioactive,
in addition to the increasing need to obtain mechanical properties from ion beam irradiated
samples, require small specimen mechanical testing. Since the beginning of the nuclear age, the
19
question of material degradation in a nuclear environment being influenced by radiation has always
been a key issue. The reliability of materials in nuclear environments is a big issue, in civil as well
as defense-related applications. Today, for all nuclear reactor concepts proposed or in service, it is
the material issues that pose the greatest challenge. If no material is available or qualified to be
used in a nuclear environment, it is impossible to realize future concepts with greater demands on
material performance. Therefore, it is vital to assess the mechanical properties, microstructural
changes, and the status of materials at specific locations in a component such as an end cap welds,
fuel/clad interfaces, or rather small parts such as the spacer grits and all these parts go under very
high dose of irradiation. Unfortunately, achieving these high doses requires extremely long
irradiation times in reactors and naturally, there are only very few materials irradiated to such high
doses. In fact, in this dissertation L-PBF materials have been irradiated to doses little above 20 dpa
with a limited penetration depth and therefore drastically limits the amount of material available
to be investigated. Overall, the higher penetration depth on the L-PBF parts and bigger area take a
very long time to be irradiated. This limited penetration depth of the ions, which is one of the
drawbacks of utilizing ion beam irradiations, makes small-scale material investigations essential
and is one of the main driving forces to enhance and deploy techniques such as nanoindentation.
In addition, oftentimes the amount of available testing material is limited due to reactor space
limitations. Statistical certainty of the data is another issue leading to the fact that a smaller sample
volume in small-scale mechanical testing is advantageous to obtain more data points on a given
volume of material. A comparative study on small-scale mechanical testing on similar AM alloys
to 316L and 17-4 PH stainless steels is in Table 2.
All irradiation procedures benefit from small-scale material testing techniques regardless
if using reactor neutron or being the ion-beam source. The necessity to link testing with bulk
20
properties is a big concern in the field to extract bulk engineering data. Therefore, the development
of small-scale mechanical testing in combination with the microstructural investigation is of great
interest to the nuclear material community for both, material development and monitoring
applications, respectively. One of the main focuses of this dissertation regarding irradiation is to
evaluate yield stresses, since the more interesting parameters such as total or uniform elongation,
and work hardening rate are more difficult to capture. It has to be noted that irradiation does cause
a noticeable difference in failure mode, where a sudden localized failure of the micropillars could
be observed.
Table 2: Literature review on small-scale mechanical testing of relevant metallic alloys (LP = laser
power, HD = hatch distance, LT = layer thickness, SS = scanning speed, SS = strain rate, YS = yield
strength, UTS = ultimate tensile strength)
AM LP, HD, PD, UTS, Indentation

Author AR SR, s-1 YS, MPa
alloys LT, SS μm MPa properties
B
As-built 200, 110, 688.52±36.
AlMangour --- ---
17-4 PH 40, 750 31
[99]
As-built 4 1:3 0.0001
B
17-4 PH 200, 110, 1130 ±
AlMangour 914±12.73 ---
shot 40, 750 17.68
[91]
peened
As-built
197-451 --- ---
316L 400, 250,
C Shiau,
LT [x], 5 1:2 0.001
2022 [100]
Irradiated 12.7
476-588 --- ---
316L
Sinle
400, HD crytal:
X Wang, As-built
[x], LT 8 1:2 0.0031 408±18, --- ---
2021[101] 316L
[x], 17 Bi-crystal:
502
As-built 107.27- 213.58 -
√
17-4 PH 220-230, 150.70 286.40
M J Uddin, 1: 2-
120, 50, 2 to 5 0.01
2022 2.5
Irradiated 600-700 133.43- 212.75-
√
17-4 PH 244.57 375.08
21
Cross-section (at a certain area) indentation enables a more precise way of assessing
hardness versus dose. The indentation experiment on irradiated as well as the unirradiated area
within the same field of indents allows a direct comparison between an unirradiated and irradiated
L-PBF 316L and 17-4 PH stainless steel parts. It is known that irradiated materials lead to different
behavior and irradiation damage increases the strength of a polycrystalline material due to the
presence of small but strong and densely spaced radiation defects (a particular region on the
irradiated area), creating a new small internal material length scale [98]. However, once the sample
size is getting small compared to the length scales represented by grain structure or radiation
damage, they are no longer the limiting factors but rather the stress to create or propagate a
dislocation takes over, returning the material behavior to the unirradiated (quasi single crystal)
material. It is expected that the hardness values generated by nanoindentation would exhibit an
increment over the irradiated area compared to as-built area. The microstructural changes are also
expected on the surface area of irradiation as well as beneath the surface.
Thirdly, strain-rate sensitivities are to be determined by choosing high loading or test rate.
High-resolution property mapping and detailed statistical studies from a large array of indents by
nanoindentation help to confirm the qualification process aimed for nuclear applications of
additively manufactured 316L and 17-4 PH stainless steels. The quality and accuracy of results
largely depend on the quality, calibration, right newer indenter tip, and adequacy of the models
used for data evaluation as well as a well-known example is the increase of accuracy in the
determination of hardness and elastic modulus, which could be attained by calculating the contact
stiffness via a power-law approximation of unloading curve (Oliver & Pharr, 1992) instead of the
originally suggested linear approximation [102]. It is generally accepted that the values of SRS are
strongly size-dependent: for face-centered-cubic (FCC) metals, SRS normally increases with
22
decreasing grain sizes, whereas the opposite holds for body-center-cubic (BCC) structures.
1.6 Hypothesis
Structure-property relationship of additively manufactured (AM) alloys could affect the
mechanical properties of nuclear alloys used in nuclear applications. Nanoindentation and small-
scale mechanical tests could provide a comprehensive set of mechanical properties (as shown in
Figure 4) and evaluation methods for qualification purposes, and could help to accelerate AM
product reliability and process integrity.
Figure 4: List of mechanical properties that are studied and analyzed in this research
The following assumptions could be derived from this hypothesis:
• A modification of the process parameters of laser powder bed fusion in terms of the
use of different energy densities could induce a change in microstructural behavior and
orientation that would affect mechanical properties at the surface level.
• The use of small-scale mechanical testing techniques can afford the possibility of
measuring constitutive materials properties such as compressive strength, yield
strength, maximum shear strength, and studying intrinsic size effects in terms of
deformation behavior.
• Strain-rate sensitivity study of L-PBF radiation-resistant alloys such as 316L and 17-4
PH stainless steel could assist in characterizing the deformation mechanics of those
alloys before and after the irradiation.
23
• The use of small-scale mechanical test techniques in the characterization of L-PBF
radiation-resistant alloys could improve the accuracy of the evaluation of surface
mechanics.
The set of experimentation techniques could clarify and help to understand in a better way:
 Compressive yield strength with the correlation with indentation hardness and modulus
of elasticity.
 Irradiation affects the L-PBF materials (microstructure, micro-mechanical properties,

strength) and changes in deformation mechanics in the damaged surface and sub-
surface up to 5 µm depth.
1.7 What’s Inside this Dissertation
This dissertation includes an introduction of key areas of the research, experimental
procedures of material’s microstructural and mechanical properties’ characteristics, results and
discussion of each experimental section in detail with experimental data, images, and analysis of
data, and conclusion with probable future works that can be accomplished, and numbered
references of open journals or books or dissertations that are used in those studies.
24
CHAPTER 2
MATERIALS AND EXPERIMENTAL PROCEDURES
2.1 Methodology*
L-PBF processes are utilized to fabricate nuclear alloys such as 316L and 17-4 PH stainless
steels. After cutting by electrical discharge machining (EDM), the parts are prepared for material
characterization beginning with nanoindentation and proton irradiation. A 10 by 10 indents array
has been selected to increase the validity of the results. Five different strain rates have been chosen
for measuring SRM to study material’s deformation behavior with increasing loading rate. The
SRS would be calculated by plotting the log scale of both hardness values and different strain rates.
The same setup is being used after the irradiation process. Indented parts would then be observed
under FEI Quanta ESEM to study grain morphology, energy dispersive spectroscopy (EDS) for
elemental composition analysis, and X-ray diffraction patterns (XRD) are being achieved to
confirm the phases present on the parts by using Rigaku Ultima III. The indentation areas would
then be inspected and electron backscattered diffraction (EBSD) patterns are acquired by using
FEI Nova NanoSEM to study the microstructures, grain size distribution, grains crystallographic
orientations, and texture intensity. The overall methodology has been illustrated in Figure 5.
The parts with different process parameters would be placed on a pin mount in FIB (FEI
NOVA FIB/SEM) to fabricate micropillars for micro-compression testing. A very small current
would be used to eliminate the possibility of FIB damage on the micron-sized pillars. Pillars of
size ranging from 2 to 5 μm with an aspect ratio of 2- 2.5 would be milled very carefully and later
* Sections 2.1 to 2.4 are reproduced from a combination of 2 sources, both used with permission from Elseiver: (1)
M.J. Uddin, E. Ramirez-Cedillo, R.A. Mirshams, H.R. Siller, Nanoindentation and electron backscatter diffraction
mapping in laser powder bed fusion of stainless steel 316L, Mater. Charact. 174 (2021) 111047,
25
on those micropillars would be compressed by using a 10 μm flat indenter using MTS nanoindenter
and stress-strain curves such as shown in Figure 6 are being expected. The L-PBF stainless steel
parts are being proton irradiated up to 5 μm depth and on an approximate area of 3.5 mm X 4 mm.
Micropillars will be fabricated in the irradiated area with before mentioned parameters via FIB to
compare the mechanical properties with those micropillars in the unirradiated area. Layer-by-layer
mechanical properties and layer strength are possible to determine as depicted in Figure 5.
Figure 5: Methodology of the proposal
Additive manufacturing processes based on the local fusion of a powder bed (L-PBF) are
a valid alternative to conventional technologies and a growing number of industrial sectors are
currently relying on these processes for the production of different components of nuclear alloys
such as 316L and 17-4 PH stainless steels. With the advances in the development of more efficient
systems and lasers, the productivity of SLM machines has increased. Also, the development of
new alloys has contributed to the exponential growth in the research on this topic. To work with
26
this technology, there is a curve of knowledge that has to be considered, but with the right
guidelines, workflow, documentation, and characterization, machines can be running production
as some industries have been reported.
L-PBF stainless steels would be cut by EDM in order to minimize the temperature and
residual stress effect on the microstructures. Additively manufactured parts would be put in
bakelite and polished with silica carbide papers with grate sizes ranging from 240 to 1200,
followed by polishing in micro polishing clothes with Al2O3 powders of grain sizes ranging from
5 μm to .05 μm and lastly with 0.03 μm colloidal silica suspension. The polished scratch-free
samples would then be carefully dried with acetone and air blow gun. An MTS Nanoindenter®
XP equipped with TestWorks® software and continuous Stiffness Measurement (CSM)
technology would be used in nanoindentation. For assessing micro-mechanical properties,
nanoindentation would be performed on the top surface of the additively manufactured alloys with
10 x 10 indents with a standard Berkovich tip with a radius of 50 nm and φ and β angles of 65.3°
and 12.95°, respectively. Besides, the Berkovich indenter, a flat indenter (FIB milled) will also be
used for the micro-compression test of micro-pillars. The samples will be collocated on the stage
assembly of the MTS Nanoindenter® XP for the nanoindentation test. The important parameters
that will be used for nanoindentation testing are the strain rate of 5×10−2 s-1, Poisson's ratio of 0.3,
and surface approach velocity of 10 nm/s. The instrument will be calibrated before each batch test
using a standard fused silica specimen. In an array of 10×10 indents with a spacing of 50 µm in
‘x’ and ‘y’ directions. The machine would make indents consecutively by minimizing the traveling
distance of the indenter head. The indentation depth limit for each indent will be in the range of
800 to 1500 nm to make it easier to find the indents on NanoSEM and also to get a better EBSD
map. Average values will be determined based on the values of all the indents' hardness and
27
modulus of elasticity. Statistical analysis will also be performed on each part by analyzing the data
provided by the nanosuite software.
The intention of using sharp Berkovich in this proposal is to study strain-rate sensitivity
and determine the indentation modulus of elasticity and hardness. Though, spherical
nanoindentation has recently become a tool to generate an effective stress-strain response which
can be compared with a uniaxial true stress-strain response by means of conversion and can give
an approximation of uniaxial yield strength.
Strain-rate sensitivity studies will be performed by choosing five different strain rates from
slow to fast loading rates of 0.01, 0.05, 0.1, 0.5, and 1 s-1. In this way, by implementing a simple
power-law relationship, the values of SRS (m) will be determined and will be correlated with
micro-mechanical properties, phases, microstructures, and micro-compression testing. This way
as discussed in the literature review section, it is possible to determine maximum shear strength
from the SRS study and yield strength from micropillar micro-compression.
In this study, microstructures will be analyzed using an optical microscope as well as
NanoSEM after the nanoindentation, micro-tension, and micro-compression tests. An FEI Nova
NanoSEM 230 with EDAX Octane Elite EDS and Hikari Super EBSD detector with an operating
voltage of 20 kV would be used to obtain an EBSD map of the nanoindentation region. Electron
Backscatter Diffraction (EBSD) provides (2D) maps of crystal orientation from polished cross-
sections. The latest version (v8) OIM Analysis™ has reset the standard for EBSD data analysis
capability with the addition of new functionality such as Neighbor Pattern Averaging and
Reindexing (NPAR™) and other features which enables users to achieve new insight into
microstructural characterization. The samples will be mirror polished and tilted 70˚ angle in order
to increase the diffraction efficiency during the EBSD acquisition. TEAMTM EBSD analysis
28
system will be used for EBSD data acquisition and TSL OIM Version 8 software for data analysis.
Typical scan area, step size, and average Confidence Index (CI) of EBSD acquisition would be
determined by surface texture and polishing quality. The additively manufactured high-
performance alloy samples crystal structures will be studied and phases will be determined to input
on the EBSD NanoSEM software. The selected phase/phases on the OIM software contained the
information necessary to model the electron backscatter patter (EBSP) produced by the expected
phase in the alloy’s samples. The hardness and modulus of elasticity of each indent will be
identified from the nanoindentation data and effort will be given to find out any correlation
between different crystallographic planes and mechanical properties layer by layer. 3D porosity
map would be achieved by using X-ray microscopy (AMMPI facility). This will facilitate the
micro-compression testing assuming that bigger micropillars would have more porosity compared
to smaller micropillars.
Figure 6: Layer-by-layer micro-mechanical properties by small-scale mechanical testing
29
2.2 Materials
The material used for the experimentation is LPW’s gas atomized stainless steel AISI 316L
powder particles of sizes ranging from 15 μm to 45 μm. The elemental chemical microanalysis
was performed using energy dispersive X-ray spectroscopy (EDS) in an FEI Quanta 200
Environmental SEM and the results are presented in Table 3. This instrument is capable of running
a low vacuum and thus able to reduce charging on an insulating sample and allowing imaging
without applying a conductive coating. The analysis is included in the experimental results in
Section 3.1. A conventional round rod of AISI 316L stainless steel was purchased for addressing
the difference between additively manufactured and conventionally manufactured parts, in terms
of microstructure and small-scale mechanical response.
Table 3: Elemental composition of LPW AISI 316L stainless steel powder particles
Element Minimum Maximum
Symbol Name wt% wt%
C Carbon 0.03
Cr Chromium 17.5 18
Cu Copper 0.5
Fe Iron Balance
Mn Manganese 2
Mo Molybdenum 2.25 2.5
N Nitrogen 0.1
Ni Nickel 12.5 13
O Oxygen 0.1
P Phosphorous 0.025
S Sulfur 0.01
Si Silicon 0.75
For this study, stainless steel 17-4 PH powder was procured from EOS® which is a leading
provider of metallic powder for additive manufacturing. According to the vendor, the parts built
from the powder should have chemical composition corresponding to ASTM F899 and certain
30
anisotropy which can be eased by solution annealing. The chemical composition of the powders is
listed in Table 4. The particle size is ranging from 16 µm to 63 µm and the as-built part density is
7.77 g/cm3. The elemental chemical composition analysis has been performed by implementing
energy dispersive X-ray spectroscopy (EDS) in an FEI Quanta 200 Environmental SEM. The
instrument can run at a low vacuum and thus able to minimize charging on the insulating sample
and allow imaging without applying a conductive coating. The analysis is included as the
experimental results and presented in section 2.5.
Table 4: EOS elemental composition of L-PBF 17-4 PH powder particles and printed parts
EOS 17-4 PH SS powder EDS of 17-4 PH SS
Min (%wt) Max (%wt) parts
Chromium (Cr) 15 17.5 16.30

Nickel (Ni) 3 5 4.40
Copper (Cu) 3 5 3.97
Silicon (Si) - 1 0.78
Manganese (Mn) - 1 1.55
Phosphorus (P) - 0.04 NA
Sulfur (S) - 0.003 0.30
Carbon (C) - 0.07 NA
Niobium + Tantalum (Ta) 0.15 0.45 0.33
Iron (Fe) Balance Balance
2.3 Process Parameters
In L-PBF, scanning strategy, processed parameters, and micro-mechanical properties are
required to be studied together for the ease of understanding the laser processing of powder metal
materials. There are unchangeable laser characteristics such as wavelength, beam energy
distribution during the fabricating process, and beam spot diameter for the end-user. On the other
hand, there is a set of process parameters in the L-PBF process that can be modified such as laser
power (P), hatch distance (HD), scan velocity (vs), and layer thickness (LT) with proper selection
31
of scanning strategy. The laser scanning strategy has been an important factor in determining better
surface quality and reducing residual stress effects in L-PBF parts. ‘Quad Islands’ was chosen as
a divisional scanning strategy. The schematics and the scanning strategy are illustrated in Figure
7. An experimental design was made by taking into consideration the parameters previously
mentioned along with some constraints for the determination of processing parameters. The laser
power was used in the range of 150 to 190 watts with VED ranging from 45.24 J/mm3 to 83.33
J/mm3. The other process parameters are: hatch distance (HD) = 120 μm, layer thickness (LT) =
50 μm and scanning speeds (vs) = ranging from 300 mm/s to 700 mm/s (Table 5). These parameters
were pre-defined based on previous investigations and on the machine manufacturer’s
recommendations to deliver functional parts with enhanced levels of surface quality (areal surface
roughness (Sa) between 14.24 µm and 24.34 µm).
Figure 7: Schematics of process parameters and scanning strategy for the fabrication of L-PBF AISI
316L parts.
Table 5: L-PBF AISI 316L stainless steel manufacturing process parameters

Sample P, Power HD, Hatch LT, Layer vs, Scanning VED
Number (Watts) Distance (μm) Thickness (μm) Speed (mm/s) (J/mm3)
1 190 120 50 700 45.24
2 180 120 50 600 50
3 170 120 50 500 56.67
32
Sample P, Power HD, Hatch LT, Layer vs, Scanning VED
Number (Watts) Distance (μm) Thickness (μm) Speed (mm/s) (J/mm3)
4 160 120 50 400 66.67
5 150 120 50 300 83.33
The geometry of the AM 316L stainless steel parts was 5 mm × 15 mm (height × diameter)
and the parts were manufactured using a laser powder bed fusion system from Aconity 3D
(AconityMIDI), with a maximum building volume of 170 mm of diameter and 400 mm of vertical
displacement. The radiation source was a single-mode fiber laser with a maximum power of P = 1
KW, a wavelength of λ= 1070 nm, and a spot size (diameter) in the range of 80-500 µm.
AM As-built 17-4 PH stainless steel parts have been produced as a cylinder with a
dimension of 5 mm × 20 mm (height × diameter). The laser powers have been used at 220 watts
and 230 watts from which volumetric energy density (VED) is calculated to be 54.76 J/mm3 and
61.11 J/mm3. The process parameters for additive manufacturing are shown in Table 6. A single-
mode fiber laser is being used as the radiation source with a maximum power of P = 1 KW along
with the above-mentioned parameters.
Table 6: L-PBF process parameters for the fabrication of 17-4 PH stainless steel parts
Sample P, Power HD, Hatch LT, Layer vs, Scanning

VED (J/mm3)
Number (Watts) Distance (μm) Thickness (μm) Speed (mm/s)
1 230 120 50 700 54.76

2 220 120 50 600 61.11
2.4 Sample Preparation
Both L-PBF AISI 316L and 17-4 PH stainless steels samples were prepared for the material
characterization. The first step was to carefully cut from the steel disc base by conventional
Electrical Discharge Machining (EDM) in order to minimize the temperature, unanticipated phase
33
formation, strain, and residual stress effects on the microstructures and overall on the micro-
mechanical properties. The samples were mounted with resin mixtures after applying the release
agent to mounting cups and to acquire a mirror-like surface, the grinding operation was carried out
in the sequence of silicon carbide papers with increasing grit sizes starting from 180 and then 320,
400, 600, 800, and 1200. Then the mounted samples were polished on polishing wheels embedded
with a fine Rayon polishing pad using a liquid suspension of alumina (Al2O3) powder particles
very carefully so that previous scratches would be removed starting with 5 µm, 1 µm then 0.05
µm, and lastly, 0.03 µm to get the mirror finish. Additionally, 0.03 µm colloidal silica was used
for a better result in the characterization processes. In the next step, the polished sample’s surface
was laved using an ultrasonic cleaning process and utilized to remove any remaining metal
particulate, dirt, and silica particles on the polished samples. This process uses ultrasound to agitate
solvent (distilled water/alcohol/acetone). The samples of conventional AISI 316 stainless steel
were prepared by following the same above procedure.
2.5 Proton Irradiation*
Before the proton irradiation, the range of the proton and created vacancies were estimated
utilizing a well-known ion-solid simulation code Stopping Range of Ions in Matter [SRIM/TRIM]
[103]. A detailed calculation with a full damage cascade was chosen within the TRIM code. The
1.0 MeV proton irradiation in the L-PBF 17-4 PH stainless steel target simulations was performed
using 160,000 ions. The target composition was taken as Cr (16 atomic %), Co (4 atomic %), Ni
(4 atomic %), Si (0.5 atomic %), C (0.035 atomic %), and Fe (75.465 atomic %) with a density of
Elsevier.
34
7.77 g/cm3, which is equivalent to 8.44×1022 atoms/cm3. The target layer was kept at a thickness
of 8 µm to speed up the calculations. In the SRIM calculation, different displacement energies of
25eV for the metal target atoms (Cr, Co, Fe, and Ni), 15 eV for silicon, and 28 eV for carbon were
considered to estimate the damages. The distribution of protons as a function of depth is given in
Figure 8(a). This plot shows that the maximum impact lies at a depth range of ~6.6 µm. The
variation in the number of vacancies generated and the displacements per atom (dpa) with target
depth when irradiated with a fluence of 1.0×1019 ions/cm2 are given in Figure 8(b). At the mean
depth of the 1 MeV proton beam (a depth of ~6.6 µm corresponding to ~33×10-4 vacancies/Ao-ion
and ~39 dpa. The samples were irradiated with 1.0 MeV protons with a fluences 1.0×1019 ions/cm2
from a 3MV Pelletron accelerator (NEC-9SH) [104]. The beams were irradiated at a target area of
0.4 cm × 0.3 cm with a beam flux of 2.6×1014 ions/cm2-sec. The proton irradiation occurred at a
vacuum of 2×10-8 torr. The samples were mounted on a stainless-steel holder with silver paste.
During the irradiation, the target temperature was periodically measured using an IR camera and
found to reach up to 60 oC.
Figure 8: SRIM simulated (a) distribution of 1 MeV proton in the 17-4PH steel, (b) Vacancies and
displacements per atom (dpa) as a function of depth for a proton irradiation fluence of 1.0×1019
ions/cm2.
35
2.6 Nanoindentation
An MTS Nanoindenter® XP equipped with TestWorks® software and Continuous
Stiffness Measurement (CSM) technology has been utilized at room temperature for
nanoindentation to determine micro-scale mechanical properties (indentation modulus and
hardness), strain-rate sensitivity (SRS) investigation, and theoretical shear strength of as-built and
irradiated parts. For the SRS study, five different strain rates (0.01, 0.05, 0.1, 0.5, and 1 s-1) have
been selected in five different regions of as-built 17-4 PH parts and an additional two strain rates
(0.25, 0.75 s-1) have been added for irradiated parts (4mm × 4mm area with 5μm depth) and it is
shown schematically in Figure 9. As-built (unirradiated) and irradiated areas are examined using
all the strain rates mentioned above. An indentation depth of 1500 nm is selected and a total of
100 (10× 10 array) indents in five (5) different regions have been made on each sample in as-built
and irradiated areas with 50 μm of spacing between two consecutive indents. A Berkovich tip (50
nm radius with φ and β angles of 65.3° and 12.95° respectively) is employed. The CSM has been
engaged with an amplitude of 2 nm and a frequency of 45 Hz. The CSM allows the measurement
of depth-dependent properties of any metal in a single step and it involves applying a dynamic
load on top of the static load while loading. It also helps in unloading stiffness continuously
through the indentation depth, by overlaying small oscillations over the primary loading signal.
The required inputs on the nanoindentation batch operation are being the surface approach velocity
of 10 nm/s, strain rate of 0.01 s-1 to 1 s-1, and the Poisson's ratio of 0.3. The instrument has been
carefully calibrated for each batch of the nanoindentation using a standard sample. The equipment
generates the values of hardness and indentation modulus as a spreadsheet by using the Nanosuite
software. Nanoindentation experiment has been designed in such a way so that leads to locating
easily any indents under Nano-SEM for microstructural observation and could be labeled with
36
measured micro-mechanical properties with different crystallographic orientations.
Figure 9: Nanoindentation experimental set-up for strain-rate sensitivity study on as-built and
irradiated L-PBF 17-4 PH stainless steel parts.
2.7 Strain-rate Sensitivity of 17-4 PH Stainless Steels
One of the useful features of nanoindentation is the capability of generating load-
displacement curves using a variety of methods such as displacement and load control modes using
continuous stiffness measurement (CSM).
Figure 10: Example of a load-displacement (P-h) curve of as-built L-PBF 17-4 PH part (VED = 61.11
J/mm3) at 0.1 s-1 strain-rate.
37
The loading portion of the load-displacement curve (Figure 10) can be taken as a power-law
relationship (Eq. 2) and contact stiffness, S can be defined as the slope of the unloading portion of
the curve as in Eq. 3 [105].
P = Chk (Eq. 2)
where P = load, C = loading curvature, and k = an exponent ranging from 1.5 to 2
dPu
S= at h = hm (Eq. 3)
dh
where S = contact stiffness, Pu = unloading force, h = displacement into the surface and hm =
maximum displacement into the surface
Strain-rate sensitivity (SRS) studies are generally based on conventional methods by
instrumented indentation for macroscopic materials testing. For better understanding in detail, a
textbook by Caliard [106] can be referred to. SRS is usually denoted as ‘m’ and the value of ‘m’
can be directly calculated from the power-law relationship (Eq. 5) between plastic stress, σ, and
strain rate, ε [107]. For instrumented indentation processes such as nanoindentation experiments,
stress can be replaced with nano-hardness since the stress is directly proportional to hardness with
a constraint factor C* (Eq. 4). The hardness values are determined by nanoindentation and plotted
against different strain-rates (0.01 s-1, 0.05 s-1, 0.1 s-1, 0.5 s-1, and 1 s-1) in log scale.
E∝H
H
E= C∗
(Eq. 4)
where C* = constraint factor (depends on the elastic-plastic deformation behavior of the material)
∂lnσ ∂ ln H
Strain − rate sensitivity, m = ∂ ln ε̇ ≅ ∂ ln ε̇
∂ ln H2 −∂ ln H1
= (Eq. 5)
∂ ln ε2̇ − ∂ ln ε1̇
= slope of the logarithmic load − displacement curve
38
Nanoindentation load-displacement curves are used to determine maximum shear stresses
with different strain rates by using displacement bursts (initial sudden fluctuations in
displacements) [108,109]. Incipient plasticity and elastoplastic deformation behavior of materials
are easy to apprehend with the help of these curves [110,111]. These curves from the very small
amount of strain rate are also very important to analyze dislocation activity and are related to the
first nucleation of dislocations. First displacements bursts are more significant compared to very
low strain-rate and become less prominent with the increase in strain rates. First displacement
bursts are not dependent on strain rates [108]. Elastoplastic behavior can be predicted from these
bursts which are separated by elastic regions. To determine maximum shear stress (Eq. 6), load-
displacement curves with 0.01 s-1 are selected for both L-PBF 17-4 PH parts before and after the
proton irradiation and only initial portions of the curves are considered. Using the loads
corresponding to displacement bursts, reduced modulus of elasticity, and Berkovich tip radius,
maximum shear stress has been calculated. The modulus of elasticity of L-PBF 17-4 PH is chosen
from a recent study [112]. The reduced modulus of elasticity (Er) is determined according to Eq.
7. Hardness values determined by nanoindenter can be converted to Vickers hardness as per
empirical relationships given in Eq. 8 and the yield strength of as-built and irradiated 17-4 PH
stainless steel parts has been calculated according to Eq. 9 which is applicable for BCC structured
iron-chromium alloys [113,114]. Factor 3.06 was determined empirically, especially for ferritic/
martensitic alloys in Eq. 9 those hardness values are highly affected by irradiation which is true
for L-PBF 17-4 PH stainless steels [115].

1
6PEr 2 3
Τmax = 0.31 � π3R2 � (Eq. 6)
where P = load correscponds to first displacement burts, Er = reduced modulus of elasticity, and R
= Berkovich indenter tip radius = 50 nm
39
−1
1−vsa 2 1−vin 2
Er = � + � (Eq. 7)
Esa Ein
where vsa and vin = Poisson rations of the sample and Berkovich indenter, Esa and Ein = modulus
of elasticity of the sample and Berkovich indenter (1000 Gpa) respectively
𝐻𝐻𝑣𝑣 = 94.495 𝐻𝐻 (Eq. 8)
𝜎𝜎𝑦𝑦 = 3.06 𝐻𝐻𝑣𝑣 (Eq. 9)
kg
where Hv = Vickers hardness �mm2� , H = nanohardness (GPa), σy = yield strength (MPa)
2.8 Small-scale Mechanical Testing
Small-scale mechanical testing has been widely utilized right after the commercialization
of nanoindentation in the 1980s and uniaxial micro-compression testing was carried out in 2004
right after it was possible to fabricate precisely smaller geometries by the implementation of the
focused ion beam (FIB) which opened the window to investigate in micro and nano-level
mechanical properties [116]. In this process, the bulk material is used in as-fabricated conditions
to fabricate or mill micro-sized pillar structures into the material surface and a very low current is
used to avoid FIB induced near surface damages [117].
Layer-by-layer micro-mechanical properties determination would be useful to study the
strength of the L-PBF layer on the fabricated parts as well as define the size effects with the
sample’s dimensions. As of now, there are no studies available in the literature for L-PBF
radiation-resistant alloys such as 17-4 PH stainless steels. To fabricate the pillars, different beam
currents have been used in rough, fine, and very fine milling in different stages during micropillar
fabrications. All the pillars of size ranging from 2 μm to 5 μm are punched by a 10 μm flat conical
diamond indenter in MTS XP nanoindenter at a strain rate of 0.01 s-1 and 2 μm pillars are milled
only on irradiated regions of 17-4 PH steels so that the height of those pillars (~5 μm) falls within
40
the radiation damage depth of around 5 μm. The micropillars arrays in as-built and irradiated
damaged areas with flat indenter are shown in Figure 11.
Figure 11: Micro-compression experimental set up (a) 10 um diameter flat indenter tip, (b) array of
micropillars in irradiated condition, and (c) array of micropillars in as-built condition of AM 17-4
PH stainless steel parts.
2.9 X-ray Diffraction (XRD) and Electron Backscattered Diffraction (EBSD) Microstructural
Characterization*
SEM with electron backscattered diffraction (EBSD) has been a useful technique for the
measurement and understanding of material’s textures, phase identification, grain size, and
misorientation angle distribution. The crystallographic orientations related to phases/grains are
provided by the EBSD at a precise location, allowing them to be related with each indent and their
corresponding measurement of hardness and indentation modulus. This capability is helpful in
explaining anisotropy within the scan area with indents having different crystallographic
orientations.
An FEI Nova NanoSEM 230 with EDAX Octane Elite EDS and Hikari Super EBSD
detector with an operating voltage of 20 kV with suitable current, was employed to generate EBSD
maps of smaller (~0.02 mm2) and larger nanoindentation areas (~2.3 mm2). EBSD creates 2D
maps of crystal orientation from cross-sections to find the relationship between the
* This section is reproduced from M.J. Uddin, E. Ramirez-Cedillo, R.A. Mirshams, H.R. Siller, Nanoindentation
and electron backscatter diffraction mapping in laser powder bed fusion of stainless steel 316L, Mater. Charact. 174
(2021) 111047. https://doi.org/10.1016/j.matchar.2021.111047, with permission from Elsevier.
41
crystallographic planes with proper indexing of nanoindents for the characterization of anisotropic
behavior and micro-mechanical properties at the sub-micron scale. The mirror-polished samples
were pre-tilted by 70º to escalate the diffraction efficiency during the acquisition. OIM Analysis™
(v8) software with Neighbor Pattern Averaging and Reindexing (NPAR™) was used to achieve
the best possible microstructural characterization and data analysis, and TEAMTM EBSD analysis
system was used for EBSD data acquisition. Harmonic textures were generated and harmonic
series expansion was used as the calculation method with a Gaussian smoothing angle of 5֯.
The area of interest was identified and focused on SEM. Custom auto-focus and auto-
brightness/contrast routines were initiated to boost the similarity of the image contrast from layer
to layer. These custom algorithms were implemented versus the vendor-provided algorithms
because they influence the information from previous layers to improve the reliability of the
results. For each focused full-frame region, secondary electron (SE) and backscattered electron
(BSE) images were collected from the same area. Both images were pixelated, covering an area of
µm2/mm2, acquired with an accelerating voltage of 20 kV, a working distance of 12 mm to 14
mm depending on the sample dimension, a pixel dwell time of 0.1 s, and a beam current of 6.1 nA.
Approximately, a quarter of the full region of interest on the BSE images shows that although there
is a contrast between the polycrystalline grains, it is preposterous to characterize the grain
boundary interfaces because of the high plastic strains evolved during the AM solidification
process. Moreover, the pores and defects locations are observed in the BSE image as dark regions.
The scan areas were varied from 165 µm × 135 µm (for smaller maps) to 1.72 mm × 1.35 mm (for
larger maps), the step size was in the range of 0.3 µm to 5 µm depending on the scan area and
condition of the sample’s surface, and the average Confidence Index (CI) of EBSD acquisition
was around 0.90 to 0.96 which confirms valid scans for further studies. The L-PBF AISI 316L
42
parts have a face-centered cubic (FCC) crystal structure or γ-phase (austenite). The selected
austenite phase on the OIM software contained the information necessary to model the EBSD
images produced by the expected phase in the sample. The hardness and indentation modulus of
each indent was identified from the nanoindentation data on the EBSD maps and the correlation
between different crystallographic planes, VED, and those micro-mechanical properties were
thoroughly studied to better explain the anisotropy and heterogeneity in microstructure and micro
mechanical behavior.
Optical microscopes were used after submerging the polished surface in an etchant to
observe the microstructures after proper calibration, and ESEM and NanoSEM were utilized for
the study of grain morphologies. Planar and cellular grain morphologies are very common in L-
PBF AM 316L due to thermal gradients that occurred during the fabrication process as the
combined results of rapid solidification, remelting of powder particles, and repeated heating-
cooling cycles.
2.10 Porosity Analysis*
A non-destructive microscopic technique Zeiss XRADIA Versa 520 X-ray microscope
(XRM) has been utilized to determine the volume percentage (%) pores (micro-cracks if there are
any) in L-PBF 17-4 PH as-built and irradiated stainless steel parts. A volume of 2.9 × 2.9 × 2.9
mm3 has been scanned with a voxel size of 1 μm and an objective lens of 4X. Pores vol.% is the
ratio of volume hold by pores and cracks on the scanned volume to the total scanned volume of
the sample. Primary scan parameters that are used to generate X-ray tomograms have been
Elsevier.
43
summarized in Table 7. Data and images are analyzed in Dragonfly and ImageJ software.
Table 7: XRM Scan parameters

Parameter Value/info
Imaging mode Tomography
Binning 2
Voltage 140 KV
Current 64.34 μA
Source filter HE4
Objective 4X
Sample theta -180֯ to 180֯
Exposure time 2 sec
Pixel size 3 μm
No. of projections 2401
Width 2.9 mm
Height 2.9 mm
Depth 2.9 mm
Volume 25.75 mm3
Voxel size 1 μm
2.11 Fabrication of Micropillars by Focused Ion Beam (FIB)
Micropillars were fabricated on AM 17-4 PH stainless steel parts in as-built and irradiated
conditions using FEI Nova FIB/SEM 230 by utilizing coarse and fine milling using a 30.0 kV
operating voltage and a milling current in the range of 20 nA to 0.3 nA depending on the materials
etching responses. Modifications to the operating condition of FIB were made if it was necessary.
Micropillars of various diameters (2 μm to 5 μm) were milled with a diameter to height ratio of 1:
2-2.5. A very fine milling procedure was performed while fabricating 2 μm micropillars.
44
CHAPTER 3
RESULTS AND DISCUSSIONS
3.1 Nanoindentation and Electron Backscatter Diffraction Mapping in Laser Powder Bed
Fusion of Stainless Steel 316L*
This research work presents the anisotropic behavior in microstructure and micro-
mechanical properties of L-PBF AISI 316L as well as conventional 316L stainless steels based on
the observation of electron backscatter diffraction (EBSD) and nanoindentation maps in relation
to various volumetric energy densities (VED) and grains at different crystallographic orientations.
It was noticed that the variations of VED, calculated from different process parameters
combinations, have an influence on crystallographically oriented grain growth evolution affecting
the nanoindentation performance. This progression was responsible for the variation in grain size
and average misorientation angles and was found to have an important role in determining the
micro-mechanical behavior. The highest nanoindentation response was obtained at a VED=56.67
J/mm3, with an average indentation modulus of 196.77 GPa and hardness of 3.68 GPa. From
Texture Pole Figures (PFs) and Inverse Pole Figures (IPFs) of EBSD maps, it was revealed that
the highest texture strength of <101> oriented grains along with the evolution and domain of
<111> oriented grains enhanced the micro-mechanical properties at that VED value. The other
causes of this behavior are the relatively lower grain size (11.62 μm) and a higher average
misorientation angle (11.74°) when comparing it with the rest of the L-PBF AISI 316L parts. The
additional but undesirable strong <001> texture somehow contributed to the slight mitigation of
the micro-mechanical properties in conventional AISI 316L stainless steels and these parts were
found to be comparatively less anisotropic than the parts obtained from the L-PBF process.
* This section is reproduced from M.J. Uddin, E. Ramirez-Cedillo, R.A. Mirshams, H.R. Siller, Nanoindentation
and electron backscatter diffraction mapping in laser powder bed fusion of stainless steel 316L, Mater. Charact. 174
(2021) 111047. https://doi.org/10.1016/j.matchar.2021.111047, with permission from Elsevier.
45
3.1.1 Energy Dispersive X-ray Spectroscopy (EDS)
The weight percentage of each possible element in Table 8 was analyzed by quantitative
analysis by FEI ESEM. Most of the elements were in the range of LPW’s range, nevertheless, the
EDS measurement was not able to quantify the percentage of Carbon (C), Nitrogen (N), and
Phosphorus (P), and collectively, these three elements were only accounted for 0.155 wt% and
mapping showed no segregation. Thus, EDS quantitative analysis was in good agreement with the
balance of the alloys and similar findings were reported in the literature [118]. Cu, Mn, Mo, and
Si weight percentages showed lower values than expected and in the case of O and S, the weight
percentage was found to be slightly higher than the supplier’s composition data.
Table 8: Elemental quantitative analysis of AISI 316L powder by energy dispersive spectroscopy
(EDS)
Element
wt%
Symbol Name
C Carbon NA
Cr Chromium 17.4
Cu Copper 0.24
Fe Iron 66.25
Mn Manganese 1.43
Mo Molybdenum 0.89
N Nitrogen NA
Ni Nickel 12.27
O Oxygen 0.69
P Phosphorous NA
S Sulphur 0.3
Si Silicon 0.58
3.1.2 Nanoindentation Results
One-way analysis of variance (ANOVA) of nanoindentation hardness and modulus results
by Minitab is shown in Figure 12, Table 9, and Table 10 with a confidence level of 95%. This
analysis is very useful when a categorial factor and a continuous response are assuming each data
46
has equal variance (Tukey comparison procedure). It helps to determine whether the means of two
groups of properties are different. The interval plots as shown in Figure 12 display the confidence
intervals for the differences between the means of indentation modulus and hardness for the
selected comparison method. It can be stated from Figure 12 that the hardness found by the
nanoindentation experiment is not statistically significant (since the α-value is more than 0.05
which is the significance level) compared to the indentation modulus which was found to be
statistically very significant. In Figure 12(b) interval plot of hardness, the means are seemed to be
displaced with different values of volumetric energy densities. However, by running a mean
comparison, a trend can be identified that the mean at VED of 56.67 J/mm3 is the highest in the
set of experiments.
Figure 12: Regression analysis (ANOVA) of nanoindentation hardness and modulus data with
various VED; (a) Interval plot of indentation modulus and (b) interval plot of hardness with a
confidence level of 95%.
Table 9: Analysis of variance (ANOVA) of the influence of volumetric energy density (VED) on the
indentation modulus (significance level, α =0.05)
Degrees of Adj Sum of Adj Mean
Source F-value P-value
Freedom Squares Squares
VED 4 8761 2190.2 4.01 0.004
Error 135 73683 545.8
Total 139 82444
47
Table 10: Analysis of variance (ANOVA) of the influence of volumetric energy density (VED) on
hardness values by nanoindentation (significance level, α =0.05)
Degrees of Adj Sum of Adj Mean
Source F-value P-value
Freedom Squares Squares
VED 4 1.747 0.4368 1.33 0.261
Error 130 42.6 0.3277
Total 134 44.347
The mean indentation modulus and hardness values were observed to be in the range of
175 GPa to 196.77 GPa and 3.40 GPa to 3.68 GPa respectively for L-PBF AISI 316L stainless
steels parts. The mean indentation modulus and hardness were found for the conventional AISI
316L sample to be 189.15 GPa and 3.60 GPa respectively. As per the ASM handbook [119], the
indentation modulus of conventional AISI Type AISI 316L stainless steel is 193 GPa, slightly
higher than the value found in this study. The L-PBF AISI 316L part that was fabricated with 56.67
J/mm3 VED exhibited the best micro-mechanical response with respect to indentation modulus
(196.77 GPa) and hardness (3.68 GPa). Further increase in VED after 56.67 J/mm3, a decrease in
indentation modulus as well as hardness was noticed. The lowest mean indentation modulus and
hardness were found in the parts with the highest VED of 83.33 J/mm3 valued as 175 GPa and
3.40 GPa respectively which were very close to the values found on VED 45.24 J/mm3 as 177.27
GPa (indentation modulus) and 3.43 GPa (hardness).
Nanoindentation load-displacement curves generally provide a mechanical fingerprint of
the response of a material to contact deformation. The unloading curves obtained in the
nanoindentation tests were found to be well behaved (exhibiting almost linear behavior) and those
curves did not display considerable elastic recovery. Thus, the nanoindentation test was confirmed
to obtain valid mechanical property data for L-PBF and conventional AISI 316L parts.
48
3.1.3 Grain Morphology and Microstructures
Detailed grain morphologies are shown in Figure 13 and Figure 14. Microstructural
characteristics located in layer-layer weld pool boundary and track-track weld pool boundary are
shown in Fig. 5. Different regions of microstructural characteristics were found in the
metallographic study and different crystallographic grain growth modes were observed in SEM,
which confirmed some distinctive morphologies, as reported in many recent studies of L-PBF of
AISI 316L [120–131].
Figure 13: SEM images showing build direction (BD) and grain morphology of L-PBF AISI 316L
parts with different volumetric energy density (VED); (a) and (b) VED = 45.24 J/mm3, (c) and (d)
VED = 50 J/mm3, (e) and (f) VED = 56.67 J/mm3.
49
SEM scans of L-PBF AISI 316L parts (VED of 45.24 J/mm3 to 56.67 J/mm3) and their
corresponding magnified scans are shown in Figure 13(a) to Figure 13(f). Features of each part are
outlined in the figures for a better understanding. Cellular morphologies along with dendritic
crystallographic (region 1) and planar grain region (region 2) were found to appear in every sample
either clearly visible on the figures or on higher magnification scans. Additionally, a variation in
the growth orientation of dendritic structures was observed. The finest cellular structures were
found in the parts with a volumetric energy density of 56.67 J/mm3 (Figure 13(c), and Figure 13(d))
and 50 J/mm3 (Figure 13(e), and Figure 13(f)). Planar interface growth was noticed as the principal
crystal growth pattern in the black dashed area (region 2). The growth of new crystalline layers of
planar grains formed epitaxially at the solidified cellular grains along the fusion line in the normal
direction shown in Figure 13(d) and Figure 13(f), which is consistent with the findings in our
previous study. Planar and finer cellular microstructures are very common microstructures found
in L-PBF techniques for a similar types of stainless-steel grades. A distinct type of solidification
process associated with inhomogeneous nucleation of grains in a new weld pool of L-PBF AISI
316L parts is responsible to create the parts having anisotropic and heterogenous microstructures.
Additionally, directional heat extraction, repeated melting, and rapid solidification on the same
layer of powder metal particles play an important role as reported in one study [67]. Variations in
grain size are found in different fabrication planes to build direction and hence, anisotropy in
mechanical properties is proven to be evident in another study [132]. In the present study, planar
interface growth was noticed as the principal crystal growth pattern in the black dashed area
(region 2). The growth of new crystalline layers of planar grains formed epitaxially at the solidified
cellular grains along the fusion line in the normal direction shown in Figure 13(d) and Figure 13(f),
which is true according to theory and literature [133,134].
50
The angle between the growth orientation of dendrites and the tangential of fusion may be
affected not only by heat flux direction but also by preferred growth orientation related to the
crystal structure. Researchers studied and determined the reason for the variation of the planar
grains in the weld pool [128]. They found out that there is a relationship between the preferred
growth direction and the preferred crystal orientation of the planar grains.
In another study, it was predicted that Marangoni flow could change the heat flux direction,
which could cause convective heat transfer and flow of fluid within a melt pool. Eventually, this
phenomenon could lead to altering growth orientation along the fusion line as shown in Figure
13(d) and Figure 13(f) with finer black dash lines. Similar findings were reported in a study [135].
The crystallographic growth mode was noticed to change from planar to cellular and finally to
dendritic solidification mode as illustrated in Figure 13(d) where planar grain growth was observed
along with line AP and dendritic grain growth was observed along with line AD in agreement with
[123]. These distinct solidification modes can be attributed to changes in temperature distribution
across AP and AD within the weld pool during the manufacturing process. Planar growth along
AP is favorable due to the higher thermal gradient; on the other hand, the thermal gradient is lower
along AB, which results in the formation of a constitutional undercooling zone and instigates a
dendritic growth mode. For higher volumetric energy density parts, coarser grains were found later
in the quantitative analysis of EBSD data. Theoretically, grains choose to develop in the
crystallographic orientation of the parent grains in stainless steels manufactured by L-PBF, and
simultaneously, grains prefer to grow along the heat transfer direction, arising the competitive
process among grains. Furthermore, part of the previously solidified layer is exposed to the melting
and cooling cycle during the L-PBF fabrication process. In the same fashion, the phenomenon of
remelting of the same solidified layers unquestionably refrains from nucleation for solidification
51
which sanctioned the commencing of epitaxial growth at the partially remelted grains and that
facilitates the growth of grains perpendicular to the curvature of the weld lines, as illustrated in
Figure 14(a) to Figure 14(c). It is worth to mention that crystallographic orientation of cellular
sub-grains was observed to develop at around 45o away from the building direction and met at
pool boundaries as visible from Figure 14(b).
Figure 14: SEM images showing planar and cellular dendritic grains with build direction (BD) of L-
PBF AISI 316L parts with volumetric energy density (VED)=50 J/mm3; (a) area of SEM scan, (b)
cellular dendritic structures with preferential 45o angle growth with pool boundary, and (c) planar
grains.
Microstructural characteristics were studied using an optical microscope. These
characteristics are shown in Figure 15(a) to Figure 15(b) with details. Polished samples were dried
52
by following standard procedure, where defects and pores were visible even with naked eyes, and
etched with Marble’s (4g CuSO4 and 20 ml HCl added to 20 ml distilled water) reagent as long as
the sample surface seemed to be lightly reacted with it. Successive weld pool layers are visible as
two lines (one dashed and one solid black lines) in Figure 15(a) and weld pools overlap partially
at a particular angle because of the scan rotation [120]. The weld pools are wider and less uniform
than the layer thickness (50 µm) which confirms the remelting of the previously solidified layer.
The overlapping nature of the weld pool is a confirmation of the successful fusion of powder
particles and strong bonding within successive layers. Coarsening of grains was observed with
parts with increasing volumetric energy density.
Figure 15: Microstructures of L-PBF AISI 316L parts with different process parameters; (a) VED =
50 J/mm3, (b) VED = 56.67 J/mm3.
One grain seems to extend over two consecutive layers as marked with the white arrow in
Figure 15(a) and this can be addressed as epitaxial grain growth. The grain orientations take place
according to solid nucleus surface orientation (surface of the previously applied layer which
determines the surface of the crystallization) during the solidification process in laser powder bed
fusion [127,129]. Grains were found to grow toward the weld pool center line and upon reaching
a certain size their surface met and formed grain boundaries. Moreover, the presence of heavy
53
elements such as Mo and the accumulation of these elements could also contribute to a high
solidification rate and corresponding constitutional undercooling [118].
3.1.4 Electron Backscattered Diffraction (EBSD) Maps
The electron backscattered diffraction (EBSD) maps along with harmonic texture i.e. pole
figure (PF) and inverse pole figure (IPF) are illustrated in Figure 16, Figure 17, and Figure 18 for
all L-PBF AISI 316L parts. In all these figures, volumetric energy density is shown to increase
downward. In Figure 16, EBSD maps of L-PBF AISI 316L parts with the lowest volumetric energy
density are displayed (VED= 45.24 J/mm3 (Figure 16(a)) and 50 J/mm3 (Figure 16(d)). These maps
were generated on the region of indents. The black triangular areas are shown in Figure 19 and
labeled with micro-mechanical response i.e. hardness and indentation modulus for better
visualization of indents together with the grain orientation. Scans were generated from a very small
area (0.02 mm2) to larger areas (2.13 mm2) to illustrate the surface texture of oriented grains, and
changes in grain orientation and to study the extent of anisotropy with the variation of volumetric
energy density. In order to quantify the effect of VED on the texture intensities of L-PBF AISI
316L parts, the texture index (PFs) and texture (IPFs) are also introduced. The pole figures quantify
the texture intensity for three crystallographic direction families <001>, <101>, and <111> with
respect to the front view of the sample (top surface). On the other hand, inverse pole figures are
2D representations of orientations. IPFs can be plotted as points and each point represents a sample
direction. Crystallographic directions in the sample coordinate system are plotted in a pole figure
whereas sample directions in the crystallographic coordinate system are plotted in an inverse pole
figure.
The colors on the EBSD maps are related to the orientation of crystal structures in the
samples fabricated perpendicular to the building direction. It is noticeable from the maps that the
54
grains are randomly oriented and consist of finer, coarse, and elongated grains. Elongated grains
were found to build up almost perpendicularly to the weld pool lines as shown in Figure 16(a) and
Figure 16(d). Some of the grains, marked in Figure 16 and Figure 18, were very large over 100
µm in size. It is noticeable that the very large grains were found to be mostly <101> oriented (green
color in IPF color map). The values of indentation modulus found in <101> oriented grains were
around 170 GPa to 180 GPa. A number of elongated grains in the scanned EBSD maps were
noticed to decrease with the increase in VED in all L-PBF parts. Parallelly, the increase in the
number of grains oriented in the <101> direction was observed with increasing VED.
Figure 16: EBSD maps of L-PBF AISI 316L parts showing one of three nanoindentation regions with
the variation of volumetric energy density; (a) EBSD and IPF color map, (b) texture PF and (c)
texture IPF of parts (VED = 45.24 J/mm3), and (d) EBSD map, (e) texture, and (f) texture IPF of
parts (VED = 50 J/mm3).
55
Figure 17: EBSD maps of L-PBF AISI 316L parts showing one of three nanoindentation regions with
the variation of volumetric energy density; (a) EBSD map, (b) texture PF and (c) texture IPF of parts
(VED = 56.67 J/mm3), and followed by (d) EBSD map and IPF color map, (e) texture PF and (f)
texture IPF of parts (VED = 66.67 J/mm3).
The maximal texture indexes (PFs) for parts with VED of 45.24 J/mm3 and 50 J/mm3 were
calculated as 3.886 and 2.917 respectively and a strong <110> texture was found in both parts. For
isotropic materials, the texture index is equal to unity. The tendency to evolve towards <001> and
<111> poles from strong <110> texture was observed with increasing VED. The IPFs indicated
that the <101> highly texture strength was found in all the parts regardless of the extent of VED
for the front view of the samples [001]. The parts with a VED of 56.67 J/mm3 were highly <101>
and <001> textured (Figure 17(c)) compared to other parts and possibly could be the reason for
exhibiting higher micro-mechanical responses. The EBSD map generated for the part with a VED
of 83.33 J/mm3 (Figure 18) was identical to the lowest VED parts except the strongest <110>
textured with a maximal texture index of 4.177 and the highest texture strength of 3.269 among all
56
the parts. This part displayed the most anisotropic behavior with relatively lower indentation
modulus and hardness when considering smaller area scans. Texture strength did not show any
particular type of trend to relate with VED in small area scans illustrated in Figure 16 to Figure
18. It is noticeable from these figures that there is a change in color of crystallized grains with the
variations in VED.
The increase in VED was responsible for evolving to more <101> and <001> oriented
grains in the microstructures. Considering larger area scans, that are added as supplementary
material in Appendix, clearly revealed a strong relationship between harmonic textures and
volumetric energy density along with a better understanding of the certain crystallographic
orientation of grains.
Figure 18: EBSD map of L-PBF AISI 316L parts showing one of three nanoindentation regions with
the variation of volumetric energy density; (a) EBSD map, (b) texture PF and (c) texture IPF of parts
(VED = 83.33 J/mm3), and (d) original image quality map of part with VED = 50 J/mm3, and (e) IPF
color map.
57
Figure 19: EBSD maps of all L-PBF AISI 316L parts marked as rectangles in Fig. 16, Fig. 17 and Fig.
18. All indents are labeled with indentation modulus (IM) and hardness (H) generated by the
nanoindentation experiment; (a) VED = 45.24 J/mm3, (b) VED = 50 J/mm3, (c) VED = 56.67 J/mm3,
(d) VED = 66.67 J/mm3, (e) VED = 83.33 J/mm3, and (f) original Image Quality (IQ) of part with VED
= 66.67 J/mm3 and IPF color map.
There was a similarity in textures and microstructures observed in parts with VED of 45.24
J/mm3, 50 J/mm3, and 56.67 J/mm3. The planar grains were more present and visible in these parts
than in the parts with higher VED (66.67 J/mm3 and 83.33 J/mm3). It is known that the preferential
growth direction for FCC structured materials such as AISI 316L is <001>. The grains started to
grow from the weld line area in the closer region of <001> direction indicated on the IPF color
58
map, and each layer melted at least two times and contributed to the reduction in grain width as
well as to a change in the final texture of the EBSD cross-section. Identical results were discovered
in recent literature [120]. As reported in another study, a strong epitaxy is noticed with planar grain
in <001> and <011> directions [136]. In this study, it was observed that the dendritic cells
nucleating epitaxially tend to grow most rapidly and thus eliminating other orientations gradually
since those cells require less nucleation energy. The elongated grains became wider and larger in
size on the surface of L-PBF AISI 316L fabricated parts with increasing VED and it was due to
the directional solidification and thus related to the epitaxial growth. Newly nucleated grains of
small planar shapes in zigzag orientations were spotted around the intersections of the weld pool
boundaries. In contrast, dominant orientations of the grains were not so evident on the parts with
higher volumetric energy density. The elastic modulus and hardness of each indent in one region
of the nanoindentation array of each L-PBF part, were labeled and identified on the EBSD maps
and these are shown together in Figure 19.
Notable anisotropic behavior in hardness and indentation modulus (IM) depending on the
crystallographic orientation of grains was observed in all the parts regardless of the amount of the
volumetric energy density. Gradual decrease in preferential orientation <101> (green color) and
gradual increase in preferential orientation <111> and <100> (increase in blueish and reddish
color) were noticed. Grains oriented in mixed yellow-green colored in IPF (the mid-region of
<011> and <001> line on the IPF) showed higher values in hardness and indentation modulus as
in Figure 19(a) as compared to <133> (around mid-region of <101> to <111>). The indent with
the highest indentation modulus (198.2 GPa) was found to be intersected with a few grains (left
bottom indent in Figure 19(a)). As the VED increases, the fraction of blueish and greenish color-
oriented grains started to evolve and dominate in EBSD maps as it has been already discussed.
59
Figure 20: (a) EBSD maps of conventionally manufactured AISI 316L stainless steel, (b) texture PF,
(c) texture IPF, (d) rectangular area with indent’s hardness (H) and indentation modulus (IM), (e)
original IQ, and, (f) IPF color map.
The purple color-oriented grains appeared more in 56.67 J/mm3 parts when compared to 50 J/mm3
and 66.67 J/mm3 parts and could be one of the possible reasons for exhibiting enhanced micro-
mechanical responses compared to all the parts regardless of the extent of VED. The indent in the
middle of the last row in Figure 19(c) displayed the highest IM = 226.6 GPa. The blue and purple
color-oriented grains were transformed to reddish and green color-oriented grains with increasing
VED (as shown in Figure 18(a) and Figure 19(e)) and those particular grain orientations eventually
contributed to a decrease in the values of IM and hardness in parts with VED = 66.67 J/mm3.
Completely <001> (red color in IPF) oriented grains displayed IM of around 145 GPa to 150 GPa
and yellow-colored grains exhibited slightly higher IM values in 150s GPa as it is clearly
noticeable from Figure 19(d) and Figure 19(e). Retained purple and blueish color-oriented grains
60
continued to show higher IM and hardness. As a whole, it can be said that an overall decrease in
micro-mechanical behavior was noticed. With the increase in VED, EBSD maps displayed almost
all red and green colored grains on the top surface of the L-PBF AISI 316 L part and those grains
collectively contributed and lowered the average values of IM and hardness.
3.1.5 Validation of the Indentation Results
The indentation micro-mechanical properties within a particular crystallographic
orientation of a single larger grain were studied and illustrated in Figure 21.
Figure 21: Indentation modulus (IM) and hardness (H) within same crystallographic orientation
grains from EBSD maps of AISI 316L parts with (a) VED = 56.67 J/mm3 and (b) VED = 66.67 J/mm3.
For this purpose, two L-PBF 316L parts with VED of 56.67 J/mm3 and 66.67 J/mm3 were selected.
Grains 1, 2, and 3 were chosen from the EBSD scan as shown in Figure 17(a) and grains 4, 5, 6,
7, 8, and 9 were chosen from the EBSD scan as shown in Figure 17(d). The average hardness
values, indentation modulus, and standard deviations (SD) were shown along with crystallographic
orientation in Figure 21. For the grain with <112> direction (grain 1), four indents were made and
61
average hardness and indentation modulus were found to be 2.89 GPa and 171.95 GPa
respectively. As discussed in earlier sections, and validating previous results, the evolution of
blue/dark blue/sky blue grains in parts with 56.67 J/mm3 exhibited higher hardness and indentation
modulus when compared with other crystallographic orientated grains. <122> oriented grains
showed the highest average hardness at 3.66 GPa and indentation modulus at 210.70 GPa. Pink
and red colored grains with orientations <114> and <001> respectively showed lower values in
indentation micro-mechanical properties. It was observed that <001> oriented grain (9) displayed
the lowest average values indentation modulus determined by nanoindentation as 161.67 GPa with
a standard deviation of 9.83. Whereas, the green-colored grain (<101>) exhibited the lowest
average hardness values of 2.8 GPa with a standard deviation (SD) of 0.61.
3.1.6 Misorientation Angle and Grain Size Estimation
The misorientation angles distribution can also influence the micro-mechanical properties
as high angle grain boundaries (HAGBs) pose larger resistance to start a dislocation motion than
low angle grain boundaries (LAGBs) and therefore, materials with a higher number fraction of
HAGBs can lead to relatively higher average indentation modulus and hardness values generated
by nanoindentation experiment. Simplifying the misorientation angle distribution to the average
misorientation angle could be a simple way to explain if there is any relationship between the
misorientation angle and micro-mechanical properties. In Figure 22, micro-mechanical behaviors
of all L-PBF AISI 316L parts are summarized with average grain size and average misorientation
angles. These quantitative analysis values were derived from larger EBSD maps for better
reliability, and those maps are provided in the Appendix as supplementary data.
Generally, low angle grain boundaries (LAGBs) or sub-grain boundaries are those with a
misorientation angle of less than 5°. Larger misorientation angle such as more than 10° yields high
62
angle grain boundaries. Misorientation angles were found to increase with an increase of the VED
as shown in Figure 22 for samples with VED between 45.24 J/mm3 and 56.67 J/mm3. Nevertheless,
misorientation angles were found to decrease after that range for the parts with VED of 66.67
J/mm3 and 83.33 J/mm3, a behavior that requires further studies. The average misorientation angle
of conventional AISI 316L stainless steel was computed as 13.23° and it was higher than all the
AISI 316L parts fabricated by L-PBF. In summary, the sample with a VED of 56.67 J/mm3
exhibited the highest misorientation angle of 11.74° and displayed enhanced micro-mechanical
properties among all of the L-PBF parts.
The average cell size of cellular grains was determined approximately from higher
magnification images of all the L-PBF 316L parts, considering the cellular grains are circular. The
grain morphology was found to be not uniform throughout all the parts with different VEDs. The
average cellular cell size of parts with VED of 45.24 J/mm3, 50 J/mm3, 56.67 J/mm3, 66.67 J/mm3,
and 83.33 J/mm3 was found to be 1.08 μm, 0.34 μm, 0.75 μm, 1.23 μm, and 1.02 μm respectively.
Figure 22: Effect of grain size and misorientation angle on indentation modulus and hardness based
on volumetric energy density (VED).
In case of grain size analysis from OIM quantitative analysis of EBSD scans, the parts
(except parts with VED of 45.24 J/mm3) having higher average indentation and hardness exhibited
the finer grains with proper distribution of all types of grains discussed in the previous section.
63
Similar to the misorientation angle case, the grain size in diameter was noticed to increase with
the increase of VED starting from parts having a VED of 45.24 J/mm3 to 56.67 J/mm3. The size
of grains usually increases at higher temperatures (less grain boundary and HAGBs areas) and
mostly the finer grain structure is preferable to achieve slightly enhanced mechanical properties.
The finest grains were found on parts fabricated with the lowest VED of 45.24 J/mm3 which size
was 9.22 µm in average, and parts fabricated with a VED of 66.67 J/mm3 displayed the coarsest
grains (13.77 µm). The upward trend was found consistent when increasing the VED and the
average grain sizes were 17.21 µm, 18.24 µm, and 20.75 µm for the parts with VED 45.24 J/mm3,
56.67 J/mm3, and 83.33 J/mm3 respectively. Compared to L-PBF AISI 316L parts, conventionally
manufactured 316L exhibited finer and similar-sized grains with 5.97 µm (average in diameter)
due to the absence of a complex solidification process followed by directional grain growth. In
this study, it would be worth stating that the L-PBF parts with higher average misorientation angles
along with relatively smaller average grains displayed enhanced micro-mechanical properties i.e.
higher indentation modulus and hardness value.
3.1.7 Conclusions on Nanoindentation, Anisotropy, and Mechanical Properties
The use of nanoindentation in combination with electron backscatter diffraction mapping
is useful to characterize the anisotropy in micro-mechanical properties and microstructure in
additively manufactured parts made of AISI 316L alloy. After performing this characterization
methodology, the key findings can be summarized as follows:
The mode of crystallization and preferential grain growth exert an influence on the micro-
mechanical properties in L-PBF processed parts. L-PBF parts with VED 56.67 J/mm3 displayed a
similar fraction of <101> oriented grains when compared with other L-PBF parts with a variation
of VED but, the evolution of grains oriented along the line <001> to <111> (blue/blueish to light
64
purple in IPF color map) was highly visible and unique among all the other L-PBF parts. The
indents on <111> grain orientations displayed relatively higher values of indentation modulus and
hardness in the nanoindentation experiment and generated a higher value of misorientation angles
as well. The evolution of certain grain orientations was observed and a change in micro-mechanical
properties was reported with the variation of volumetric energy density. The evolution of particular
crystallographic orientations of grains in parts with VED of 56.67 J/mm3 (not observed in other L-
PBF parts) was most probably responsible for exhibiting better micro-mechanical properties. The
higher angle grain boundary region acts as a strong barrier against dislocation movement.
Dislocations pile-up when that region has gone under stress and prevent crack propagation at a
certain limit. The relatively lower grain size accompanied by a higher average misorientation
angle of L-PBF AISI 316L parts with VED of 56.67 J/mm3 enhanced the micro-mechanical
properties when compared to other fabricated parts with different VED.
The conventional AISI 316L stainless steel showed the lowest texture strength, but the
indentation modulus and hardness were lower than that of L-PBF AISI 316L parts with a VED of
56.67 J/mm3. Strong <101> and <001> oriented textures were visible from the texture IPFs. There
is a possibility that this additional but undesirable strong <001> texture somehow contributed to
the mitigation on the micro-mechanical properties. In general, parts with microstructures of the
finer grains are supposed to exhibit superior mechanical properties. The average grain size of L-
PBF AISI parts with VED of 45.24 J/mm3 was calculated to be the lowest among all L-PBF parts
at 9.22 μm and unexpectedly, those parts did not display the best micro-mechanical responses. It
also requires further investigations in future studies.
In summary, micro-mechanical anisotropy was found in all the L-PBF AISI 316L parts
regardless of the amount of volumetric energy density and the extent of anisotropy was addressed
65
by the grain morphology and the quantitative means of the analysis of data, generated by the
electron backscattered diffraction maps such as texture PFs, texture IPFs, misorientation angles,
and grain size. In-depth cell size analysis on different grain, morphologies should be evaluated
further, to fully correlate and compare their micro-mechanical characteristics with the help of
nanoindentation.
The combined study of nanoindentation with EBSD mapping is an alternative methodology
for enriching qualification protocols, of additively manufactured metallic components, in addition
to existing macro-mechanical evaluation via tensile testing. Future works should include additional
experimental procedures to correlate indentation response with macro-mechanical behavior and
porosity characterization.
3.2 Effects of Proton Irradiation on Nanoindentation Strain-Rate Sensitivity and

Microstructural Properties in L-PBF 17-4 PH Stainless Steels*
Laser powder bed fusion has been proven to be an effective manufacturing process to
fabricate 17-4 PH stainless steel parts with acceptable quality outputs. In this study, the effects of
1 MeV proton irradiation (with a fluence of 1×1019 ions/cm2) damage of depth 5 μm on the surface
of L-PBF 17-4 PH steels are investigated in terms of micro-mechanical properties, microstructure,
and strain-rate sensitivity. Strain-rate sensitivity of as-built (unirradiated) and irradiated 17-4 PH
stainless steel were studied in different strain rates of 0.01, 0.05, 0.1, 0.25, 0.5, 0.75, and 1 s-1, and
for each strain rate 100 indentations were made. Micro-mechanical properties, yield, and
maximum shear strength of proton-irradiated L-PBF 17-4 stainless steel parts were substantially
affected by means of a significant change in strain rates, concretely at strain rates higher than 0.25
Elsevier.
66
s-1 when compared to as-built parts at two different volumetric energy densities. These final
findings are relevant due to the applications of these alloys in the fabrication of components
subjected to irradiation and extreme working conditions and are factors to consider when
evaluating the use of additive manufacturing to fabricate intricate nuclear parts.
3.2.1 X-ray Diffraction (XRD) Analysis
XRD analysis confirms the presence of mostly martensitic phase both in as-built and
irradiated 17-4 PH stainless steel parts. XRD X-ray could not detect the austenitic phase on the
materials and it could not be able to distinguish between the body-centered cubic (BCC) ferrite
phase and body-centered tetragonal (BCT) martensite phase since low carbon (≤ 0.02 wt.%)
stainless steels exhibit a very small magnitude of lattice distortion in BCT martensitic phase [137].
Three prominent peaks have been found at 2θ angles of 44.341, 64.508, and 81.630 degrees as
shown in Figure 23, and XRD data agree with the literature found regarding additively
manufactured 17-4 PH stainless steels [138–143].
Figure 23: X-ray diffraction measurements of L-PBF 17-4 PH as-built (AB) and irradiated (IR)
stainless steel parts.
67
3.2.2 Micro-Mechanical Properties by Nanoindentation
Nanoindentation hardness and modulus data are analyzed for as-built and irradiated L-PBF
17-4 PH stainless steel parts fabricated in two different volumetric energy densities (i.e. 54.76
J/mm3 and 61.11 J/mm3). In this study, the focus has been given mainly on the analysis of
indentation hardness data since strain-rate sensitivity (SRS) is directly related to hardness data
from nanoindentation. Variations in hardness data due to proton irradiation against different strain
rates are shown in Figure 24 and effects of irradiation on indentation modulus data are shown in
Figure 25. Statistical one-way ANOVA analysis has been performed by Origin® and primary
important statistical data are enlisted in Table 11 and Table 12. To find the strain-rate sensitivity,
two additional strain rates have been selected for both irradiated parts within the designated
irradiated area. The easiest features on hardness vs. strain rates plots in the case of both L-PBF 17-
4 PH stainless steel parts are increment of hardness with higher strain rates and irradiation shift of
hardness level within the irradiation zones. Furthermore, irradiated parts display higher reading of
the indentation hardness with increasing strain rates. Different mechanisms of dislocations play
important role in the plastic deformation of irradiated stainless steels under nanoindentation
experiment. The gliding of dislocations in plastically deformed regions could be affected by
defects created by irradiation: DLs (dislocation loops), SSDs (statistically stored dislocations),
GNDs (geometrically necessary dislocations), solute atoms, lattice friction, and clusters of defects
made of alloy atoms [144]. In irradiated stainless steels, there are three hardening mechanisms
namely DL hardening, dislocation hardening, and intrinsic hardening. Hardness can also vary
under various irradiation doses. Lower doses result in a lower reading of hardness for the same
material, which is supposed to be higher in extent when compared to the same as-built material
[145,146]. The unique solidification process involved with laser powder bed fusion of 17-4 PH
68
stainless steels results in anisotropy in microstructure and micro-mechanical properties
[71,97,112,140–149], which agrees with the results found in this study. Mean hardness and
indentation modulus is observed to vary for each strain rate for both L-PBF as-built and irradiated
17-4 PH stainless steel parts.
Figure 24: Nanoindentation hardness plot against different strain rates (histogram) for as-built and
irradiated L-PBF (54.76 J/mm3 and 61.11 J/mm3) 17-4 PH steel parts.
It is observed from the hardness plot in different strain rates of 17-4 PH steel parts that at
higher strain rates the parts are more sensitive and hardness values rise rapidly for both irradiated
parts, especially after 0.5 s-1 strain rate. For example, in L-PBF 17-4 PH steel parts with VED of
54.76 J/mm3, the mean hardness jumps 137.2% to 175.6% (4.27±1.09 GPa to 10.74±1.98 GPa)
and 72.4% to 102.2% (5.21±0.75 GPa to 10±2.19 GPa) for VED 61.11 J/mm3 parts in strain rate
of 1 s-1 due to irradiation hardening effects. Whereas, at a low strain rate of 0.01 s-1, mean hardness
increases 90% to 120% (3.14±0.84 GPa to 6.31±1.26 GPa) for VED 54.76 J/mm3parts and 70.6%
to 132.5% (3.42±0.91 GPa to 6.62±0.78 GPa) for VED 61.11 J/mm3 parts.
69
Table 11: Statistical One-way ANOVA of hardness data
Strain Standard SE of R- Coeff. of

Mean F-vale Prob>F
rate (s-1) Deviation Mean square variance
0.01 3.140 0.840 0.091
VED = 54.76 0.05 3.481 0.828 0.092
J/mm3 (as- 0.1 3.622 0.476 0.062 0.185 0.232 21.260 8.19E-16
built) 0.5 4.013 0.873 0.096
1 4.270 1.092 0.131
0.01 6.310 1.259 0.127
0.05 6.541 0.923 0.095
VED = 54.76 0.1 6.606 0.852 0.086
J/mm3 0.25 6.585 0.678 0.083 0.647 0.151 197.140 2.83E-142
(irradiated) 0.5 6.984 0.622 0.064
0.75 8.548 0.903 0.090
1 10.740 1.981 0.199
0.01 3.423 0.912 0.092
VED = 61.11 0.05 4.014 0.670 0.071
J/mm3 (as- 0.1 4.095 0.614 0.064 0.457 0.170 86.048 5.56E-53
built) 0.5 4.975 0.593 0.071
1 5.281 0.747 0.092
0.01 6.616 0.779 0.080
0.05 6.625 0.531 0.054
VED = 61.11 0.1 6.824 0.641 0.065
J/mm3 0.25 6.766 0.536 0.056 0.536 0.147 124.487 2.51E-104
(irradiated) 0.5 7.392 0.998 0.110
0.75 8.165 0.955 0.100
1 10.002 2.185 0.220
The one-way ANOVA model fits moderately well for all the hardness data of as-built and
irradiated parts except as-built 54.76 J/mm3 due to a lower value of the coefficient of determination
(R2) at a significance level of α = 0.05. Additionally, a sufficiently large F-value or P-value smaller
than the significance value of α = 0.05 means the model is significant for all as-built and irradiated
L-PBF 17-4 PH stainless steel parts.
Indentation modulus plot as in Figure 25 that is plotted against strain rates exhibit the
reverse behavior of hardness plot as in Figure 24. Higher strain rates influence heavily modulus
values in all as-built and irradiated L-PBF 17-4 PH stainless steel parts. At a small loading rate
70
that impact is not very noteworthy. Interestingly, irradiation enhances and increases indentation
modulus in all cases. As an example, the mean indentation modulus for the as-built VED 54.76
J/mm3 part measured with 0.01 s-1 strain rate is calculated to be 180.04±31.36 GPa, and the same
experimental setup yields a mean of 217.36±31.74 GPa in the irradiated part. In the case of L-PBF
VED 61.11 J/mm3 17-4 PH stainless steel, indentation modulus is determined as 190.60±33.59
GPa in the as-built part and 231±19.03 GPa in the irradiated part. At a strain rate of 1 s-1, ANOVA
analysis (Table 12) generates a modulus mean of 100.08±20.26 GPa for as-built and 128.02±26.76
GPa for irradiated 54.76 J/mm3 part. Very high values of F-values indicate the models are
significant in all samples, and consequently, P-values are smaller than the significance level of
=0.05 which is an indicator that the influence of strain rates on indentation modulus is
statistically significant at different VED values.
Figure 25: Nanoindentation modulus plot against different strain rates (mean plot and standard
deviation as error) for (a) as-built and (b) irradiated L-PBF 54.76 J/mm3 and 61.11 J/mm3 17-4 PH
steel parts.
71
Table 12: Statistical One-way ANOVA of indentation modulus data
Strain Standard SE of R- Coeff. of

Mean F-vale Prob>F
rate (s-1) Deviation Mean square variance
0.01 180.044 31.362 3.382
VED = 54.76 0.05 177.786 22.690 2.521
J/mm3 (as- 0.1 198.025 16.462 2.143 0.654 0.143 176.88 7.12E-85
built) 0.5 163.907 21.615 2.373
1 100.077 20.261 2.422
0.01 217.363 31.740 3.206
0.05 219.637 21.722 2.229
VED = 54.76 0.1 221.708 21.236 2.145
J/mm3 0.25 212.887 15.846 1.936 0.694 0.124 244.35 2.15E-162
(irradiated) 0.5 189.077 19.768 2.028
0.75 152.066 22.276 2.228
1 128.016 26.765 2.690
0.01 190.594 33.585 3.393
VED = 61.11 0.05 210.503 25.298 2.667
J/mm3 (as- 0.1 210.101 20.339 2.132 0.581 0.157 141.90 5.97E-76
built) 0.5 165.690 35.144 4.231
1 114.539 28.141 3.464
0.01 231.001 19.026 1.942
0.05 233.129 13.979 1.419
VED = 61.11 0.1 230.441 13.616 1.390
J/mm3 0.25 230.224 15.862 1.663 0.798 0.102 424.49 2.38E-220
(irradiated) 0.5 195.948 23.005 2.541
0.75 158.889 26.906 2.805
1 125.796 26.703 2.684
The influence of higher strain rates on the modulus values of L-PBF 17-4 stainless steel
parts are most probably due to a few factors. Firstly, anisotropy in mechanical property behavior
of ductile BCC crystal structures of stainless steels such as 17-4 PH (0.07% Carbon), and 316L
(0.03% Carbon). Secondly, higher strain rates facilitate to arise an effect which is known as ‘Pile-
up effect’ [150]. Nanoindenter channel which computes the indenter contact area on the sample
surface under predicts the true contact area when pile-up begins and therefore, it is plausible that
the channel over predicts the indentation modulus values. In instrumented indentation techniques,
the contact area is calculated indirectly as a function of modulus and stiffness:
72
𝜋𝜋𝑆𝑆 2
𝐴𝐴𝐸𝐸 =
4𝐸𝐸𝑅𝑅2
where AE = contact area, S = stiffness, and Er = reduced modulus of elasticity
Thirdly, the viscoelasticity phenomenon drives a material to behave like a liquid as the
velocity of displacement raises. At lower strain rates, L-PBF 17-4 PH stainless steel parts have
enough time to stretch with a lower indentation load (around 200 mN) before reaching maximum
indentation depth (in this case 1500 nm), whereas, at higher stain rates, it requires higher
indentation load (more than 300 mN) because of insufficient time to make the indent on the surface
of the parts.
3.2.3 EBSD Microstructural Characterization
The microstructural study of L-PBF 17-4 PH stainless steel parts has been performed and
reported in many recent open literature. However, no study reported the microstructural
characterization on irradiated 17-4 PH parts so far. Directional and rapid cooling characteristics
make the L-PBF a unique and non-equilibrium solidification process with the presence of a very
high-temperature gradient. Rapid cooling rate such as 105-106 K/s makes the equilibrium phase
diagram invalid and pre-solidified metals undergo cyclic heating and cooling during the L-PBF
printing process resulting in non-equilibrium microstructural characteristics in 17-4 PH stainless
steel parts [151]. According to the equilibrium phase diagram of 17-4 PH stainless steel, during
cooling from melted steel at a high temperature above the liquidus line, the ferrite (BCC) phase
forms first and with further cooling, the austenite (FCC) phase starts to form through pretectic
reaction of high-temperature ferrite and present liquid phase. Additional solidification at a rapid
cooling rate initiates the formation of martensitic (BCC) transformation and the martensite phase
continues to form [152]. The microstructure and texture of the as-built L-PBF 17-4 PH stainless
73
steel parts rely on the powder particle’s initial chemical composition [140]. In the second stage,
austenite transforms to martensite as a melted layer of 17-4 PH powder particles cool down, but,
not all of the austenite phase can transform into martensite as the solidification process continues.
Thus, L-PBF 17-4 PH stainless steel part contains retained austenite (FCC and metastable phase
at room temperature) grains are found to be extremely small and this phenomenon inhibits the
kinetics of the phase transformation [112,153,154]. This presence of retained austenite is also
suspected to possibly inhibit the precipitation of copper-rich particles during the aging process that
hardens and strengthens the alloy [155]. Processing atmosphere conditions are also noted to affect
the produced alloy phase composition. Both nitrogen and argon are commonly used as
atmospheres for producing powders via gas atomization and shielding gases in LPBF processing
of 17-4 powders. In this present study, Argon gas has been used as a built atmosphere and produces
a mostly martensitic microstructure, which is consistent with the literature [139,156]. The
martensitic body-centered tetragonal (BCT) phase is problematic to distinguish in EBSD scanning
due to the c/a ratio close to unity but, it is quite easier to identify the face-centered cubic (FCC)
austenite phase. That is the reason, martensite is referred to as BCC/BCT in inverse pole figure
(IPF) in Figure 26 to Figure 29 [156,157]. It is obligatory to be noted that the BCC phase can be
referred to as either the martensite or ferrite, since these two phases are not possible to distinguish
by the XRD as well as the EBSD technique. The martensite in stainless steels with carbon content
less than 0.2%, which is the case of 17-4 PH steel (~0.07 % C), has a BCC structure similar to
ferrite.
Similar to literature, equiaxed austenite (FCC) grains are found to be very fine compared
to coarse martensite grains and located mostly near grain and melt pool boundaries where the
atomic arrangement is more irregular and martensite can no longer grow [158]. Elongated grains
74
are found in all samples and these grains tend to grow from melt pool boundaries with a favored
growth along <100> orientation as shown in Figure 26 to Figure 29. It is also clear that the area
where indents are made on the surface austenite phase reveals because indents penetrate around
1500 nm and expose more grain boundaries as shown in phase maps (Figure 26(b), Figure 27(b),
Figure 28(b), and Figure 29(b)). Texture pole figures do not show a notable difference in intensity
on any particular crystal orientation in as-built and irradiated 17-4 PH parts and show an extent of
anisotropy in microstructure as well as in micro-mechanical behavior similar to L-PBF 316L
stainless steel parts which have been reported previously [12].
stainless steel part with VED = 54.76 J/mm3; (a) IPF map in the (X–Y) plane perpendicular to the
build direction, (b) phase map, (c) texture pole figure, (d) inverse texture pole figure, and (e) IPF
color maps of phases.
75
76
Figure 26(c) to Figure 29(c) also represent texture pole figures corresponding to the (X–Y)
plane of as-built and irradiated L-PBF 17-4 PH stainless. A strong fiber texture is detected with a
<100> direction favorably aligned with the build direction Z for as-built parts and in irradiated
parts, strong texture along <100> and <111> directions is observed. This fiber texture is the
common solidification texture for the cubic crystals such as FCC and BCC metals. Even though
stainless steels (less than 0.2% C) generally undergo the phase transformation BCC (ferrite) to
FCC (austenite) to BCC (martensite), ensuing in a more random texture [159]. Hence, the strong
fiber texture observed contradicts the occurrence of this transformation sequence. On the contrary,
77
the microstructure revealed is the one obtained directly after solidification, with no further solid-
state phase transformation which validates that the ferrite (BCC) phase has bypassed the austenite
(FCC) phase during L-PBF thermal cycles [151].
3.2.4 Correlation of Martensite Fractions to Process Parameters of L-PBF 17-4 PH As-Built and
Irradiated Stainless Steel Parts
Several open literatures have reported that the major martensitic phase, as well as other
phases (austenite and ferrite), present on laser powder bed fusion, processed 17-4 PH stainless
steels parts; although reported percentages of martensite are not consistent. Andelle et.al. [160]
reported a dual-phase austenite-ferrite phase. The effect of hot isostatic pressing (HIP) on the
densification, mechanical properties, and microstructures using gas atomized powders has been
investigated and it is found that density increases from 90% to 97% [149]. At lower VED (64 and
80 J/mm3) like in this study, long-columnar and fine equiaxed grains are observed; around 95%
martensite is reported which contributes to high hardness. Another study published recently
reported, confirms to find a mixed microstructure of austenite and martensite and austenite phase
was detected mostly at the grain boundaries of the melt pool and martensite inside the melt pools
[161]. It was not possible to distinguish between ferrite (BCC) and martensite (BCT). Lashgari et.
al. [162] investigated the effects of scanning pattern, build orientation, and single vs. double scan
on the microstructure of L-PBF 17-4 PH stainless steel parts and found the volume fraction of
retained austenite varied from 0.7% to 4.4% and austenite phase appeared in the grain boundaries
due to the large strains on those regions, high dislocations density, and finer grain size. L-PBF 17-
4 PH parts with gas atomized powders are found to decrease in grain size with increasing VED
from 64 to 84 J/mm3 [163]. Parts that are built vertically oriented have been found to contain
around 97% martensite in another study [112].
Quantitative analysis data of EBSD microstructural characterization of L-PBF 17-4 PH
78
parts are presented in Table 13 below with corresponding to hatch distance and scanning speed
used during the printing process. It is seen from the table that irradiation could not change the
phases present on the microstructures significantly, but a slight decrease in average grain size. This
could be due to irradiation-induced twins and plasticity during proton irradiation [164]. These
phenomena helped to form strain-induced martensite and mechanical twins to accommodate
additional strains caused by irradiation. These mechanisms are dependent on the stacking fault
energy and this energy usually increases with decreasing in grain sizes until the phase of martensite
is stabilized. A small fraction of the microstructure is found to be an austenitic phase. In Figure
26(b) to Figure 29(b), green and red colors represent martensite and retained austenite phase
respectively on the phase map generated from EBSDs. The lower VED (54.76 J/mm3) as-built part
is observed to have only around 1.8% austenitic phase and mostly a little over 98% martensitic
phase as shown in Figure 26(b). Whereas, 0.9 to 1.9% austenite and 98.5 to 99.1% martensite have
been determined in as-built 17-4 PH steel parts with VED = 61.11 J/mm3 as illustrated in Figure
28(b).
Table 13: Quantitative analysis of EBSD scans of as-built and irradiated L-PBF 17-4 PH stainless
steel parts
Hatch Scanning Phase %

VED Grain Misorientation
Distance Speed
(J/mm3) Size (μm) Angle (o)
(μm) (mm/s) % %
martensite austenite
54.76 700 4.9-8.35 98.1-98.2 1.8-1.9 19.54-21.17
As-built 120
61.11 600 5.35-6.87 98.5-99.1 0.9-1.5 17.54-20.3
54.76 700 4.1-5.2 97.5-98.5 1.5-2.5 17.3-23.12
Irradiated 120
61.11 600 4.97-5.0 98.5-98.6 1.4-1.5 20.05-21.44
According to the literature data, Hsu et. al. [165], percentages of martensite present in AM
as-built 17-4 PH parts increase with a decrease in scanning speed and an increase in volumetric
energy density with the same hatch distance and this is also true for this study. In that study, around
79
91% and 92.5% of martensite are found in 17-4 PH parts with 55 J/mm3 and 60 J/mm3 volumetric
energy density respectively (hatch distance = 100 μm). In this study, 91.1-98.2% and 98.5-99.9%
of martensite have been found with a volumetric energy density of 54.76 J.mm3 and 61.11 J/mm3
(hatch distance = 120 μm). Therefore, energy density, scanning speed, and hatch distance are vital
to process parameters as far as the fabrication of alloys in the L-PBF process is concerned. To
validate the percentages of martensite that have been derived from EBSD quantitative analysis in
this study, an empirical relationship (Eq. 10) can be considered from the literature [112]. Fractions
of martensite of L-PBF 17-4 PH stainless steels determined by experiment and as per Eq.10 are
shown in Table 14 below.
h
Mf = 0.142 �E + 56 �50 − 1�� + 76 (Eq. 10)
J
�Mf = martensite fraction, E = energy density � � , and h = hatch distance (μm)�
mm3
Table 14: Percentage of martensite phase according to experiment and Eq. 8 for L-PBF 17-4 PH
stainless steels from open literatures
Vol. Energy Hatch

Experimental % % of Martensite
AM Alloy Density Distance References
of Martensite according to Eq. 7
(J/mm3) (μm)
50 100 91 91.05
60 100 92.5 92.47 [165]
160 50 98 98.72
54 100 71 91.62
L-PBF 17-4 [166]
61 100 74 92.61
PH SS
68 50 66.27 85.66 [167]
65 100 75 93.18 [140]
106.67 50 93 91.15 [112]
85.7 70 93.8 91.35 [142]
As-built L- 54.76 120 98.15 94.91
PBF 17-4 PH
SS 61.11 120 98.8 95.81
This study
Irradiated L- 54.76 120 98 94.91
PBF 17-4 PH
SS 61.11 120 98.55 95.81
80
3.2.5 Porosity Analysis
Reconstructed X-ray microscope (XRM) 3D scans for L-PBF 17-4 PH stainless steel parts
including the irradiated zone are shown in Figure 30 and Figure 31 for two different volumetric
energy densities. It is very clear from the scans that both of the parts do not have any
cracks/microcracks (microcracks having a dimension of fewer than 1 μm are not considered since
the voxel size was set at 1 μm) but possesses a small volume fraction as pores i.e. very high density
that is randomly distributed within the parts. This ensures the credibility and exceptionally good
printing ability of the additively manufacturing technique that has been used to fabricate alloys
such as 17-4 PH stainless steels. Micro-mechanical property and microstructural characterizations
data exhibit very good strength and uniform finer grains microstructures. Unfortunately, any effect
of proton irradiation could not be detected by XRM since the irradiation depth was very small (~5
μm), and setting pixel size less than 1 μm did not generate good scans.
volume.
Pore % volume of 54.76 J/mm3 parts has been determined to be around 0.2755 %. A slice
of this part is shown in Figure 30(b) and random pore distribution has been observed as in Figure
30(c). For a slightly higher volumetric energy density of 61.11 J/mm3 17-4 PH parts, the pore %
81
volume has been calculated to be 0.1904 % (Figure 31). Therefore, it can be said that high density
L-PBF 17-4 PH stainless steel parts having no larger cracks are now easily manufacturable via
laser powder bed fusion.
volume.
Table 15: Percentage of porosity determined by using different methods for L-PBF 17-4 PH stainless
steels extracted from open literature.
Volumetric
Measuring
AM alloy energy density % of Porosity Reference
technique
(J/mm3)
106.67 0.55-0.73 X-ray CT [112]

41 1.3
54 0.4 Archimedes [166]
61 0
L-PBF 17-4 68 < 0.0183 X-ray CT [167]
PH SS 72.8 0 X-ray Micro CT [168]
43.4 - 60.76 ≤1 X-ray Micro CT [169]
54.17 0.01 X-ray Micro CT [170]
54.76 0.2755 X-ray Microscope
This study
61.11 0.1904 (XRM)
A list of some recent open literature regarding the porosity studies of L-PBF 17-4 PH parts
is presented in Table 15. Gu et. al. [171] studied the porosity of L-PBF 17-4 PH stainless steels in
82
the Archimedes method and found that % porosity decreases as volumetric energy density
increases. Similar to this study, they calculated 0.4 % and 0 % porosity in 54 J/mm3 and 61 J/mm3
volumetric energy density 17-4 PH parts fabricated by the same laser powder bed fusion
technology.
3.2.6 Strain-Rate Sensitivity (SRS) and Effect of Proton Irradiation on the Hardness
Measuring local micro-mechanical properties at different strain rates is pivotal to
investigate deformation mechanisms in materials regardless of the manufacturing or fabrication
methods. Nanoindentation has been used for local micro-mechanical property measurements,
especially in strain rates not more than 0.1 s-1. The usage of high indentation strain rates proved to
be very helpful to investigate rate-dependent properties recently [172–175]. In the current study,
strain-rate dependency on as-built and proton irradiated L-PBF 17-4 PH stainless steel parts have
been investigated and at the same time, an effort has been made to correlate the effects of
irradiation on microstructure, porosity, and micro-mechanical properties.
Load-displacement curves are represented in Figure 32 for as-built and in Figure 33 for
irradiated 17-4 PH stainless steels under various strain rates and these curves are generated in
continuous stiffness measurement technique at room temperature. It is notable that before holding
the stage, the load on samples increases with increasing strain rates at the same displacement into
the surface (1500 nm), and this phenomenon confirms that there is an effect of strain rate on the
hardness of L-PBF as-built and irradiated17-4 PH stainless steels [176]. As observed from the
curves, applying high strain rates move the load-displacement curves upward for both samples.
Due to the irradiation, nanoindentation hardness increases with an increase in strain rates thus
requiring more load to make the indenter impression or to reach the depth limit of 1500 nm into
the surface. A load of around 200 mN is observed for the deformation required to reach that depth
83
for as-built parts, whereas, more than 300 mN load is required to do so for proton irradiated parts.
No scientific reference has been found on nanoindentation deformation behavior via load-
displacement curves for additively manufactured 17-4 PH steels.
Figure 32: Load-displacement curves (P-h) for as-built L-PBF 17-4 PH stainless steel in different
strain rates, (a) VED = 54.76 J/mm3 and (b) VED = 61.11 J/mm3.
Figure 33: Load-displacement curves (P-h) for irradiated L-PBF 17-4 PH stainless steel in different
strain rates, (a) VED = 54.76 J/mm3 and (b) VED = 61.11 J/mm3.
To measure the strain-rate sensitivity (SRS, m), hardness data of 100 indents (10 by 10
arrays as shown in EBSD maps) was considered in each strain rate. To determine m, the plot as
shown in Figure 34 is plotted in a log-log scale according to the power-law relationship (Eq. 4).
84
Figure 34: Strain-rate sensitivity (SRS) determined by plotting the log-log scale of average hardness
and strain rate values and plots are drawn considering the density of the parts (normalized); (a) SRS
in as-built and (b) SRS in irradiated L-PBF 17-4 PH steels parts.
Table 16: Strain-rate of L-PBF 17-4 PH stainless steel using different approaches
Strain rates range
Strain-rate sensitivity (m) Approach
(s-1)
0.01 - 10 0.0199 - 0.0578 Tension test [175]
0.001 - 1000 0.0084 - 0.0183 Tension test [177]
0.072 - 0.094 (as-built) Nanoindentation
0.01 - 1
0.0086 - 0.597 (irradiated) [this study]
The hardness values on Y-axis are normalized by considering the actual density of L-PBF 17-4
PH stainless steel parts determined by XRM. To derive a second pattern for irradiated parts (linear
trend line is not observed similar to as-built part), additional two strain rates have been selected
(0.25 s-1 and 0.75 s-1). The strain-rate sensitivity, m, values for as-built 54.76 J/mm3 and 61.11
J/mm3 AM 17-4 PH stainless steel parts are calculated to be 0.072 and 0.094 respectively.
Irradiated 17-4 PH steel parts become harder (as per hardness values by nanoindentation) and m
values are calculated to be 0.014 for 54.76 J/mm3 parts and 0.0086 for 61.11 J/mm3 parts in lower
strain rates (0.01 s-1 to 0.25 s-1). In higher strain rates (0.5 s-1 to 1 s-1), m is calculated to be 0.597
for 54.76 J/mm3 and 0.424 for 61.11 J/mm3 L-PBF 17-4 PH parts. A couple of scientific studies
have been found on strain-rate sensitivity of L-PBF 17-4 PH stainless steel and the authors
85
investigated it in terms of tensile studies (not via instrumented indentation approach) [152,175]
and Table 16 represents comparative m values from those studies for same alloys fabricated by the
same technique.
3.2.7 Maximum Shear and Yield Strength Approximation
The maximum shear strength of as-built and irradiated L-PBF 17-4 parts have been
determined from the nanoindentation approach using the first displacement bursts methodology.
The first pop in the phenomenon is where the elastic to elastic-plastic deformation transition starts.
The P-h curves that are displayed in Figure 32 and Figure 33 are supposed to be fully elastic before
the pop-ins. The shift of pop-in event results with an increase in loading rate (i.e. increment in load
with time) and release of local stress in load-displacement curves [178]. These pop-ins are
observed when loading is intimately associated with the nucleation of dislocation sources [179].
Primary displacement bursts are more significant compared to later bursts, independent of strain
rates, and loads associated with these are used to analyze maximum shear strength in instrumented
indentation; hence, are more appropriate to investigate and explore dislocation activity with only
selecting a low strain rate nanoindentation experiments [108,180]. In Figure 32(a), displacement
bursts for as-built and irradiated 17-4 PH parts are shown extracted from the very initial portion
of load-displacement curves from Figure 32 and Figure 33 at 0.01 s-1 strain rate and impact of
irradiation on maximum shear and yield strength of 17-4 PH parts are shown in Figure 35(b). Table
17 is representing the calculated maximum shear strength of as-built and irradiated parts at the
lowest strain rate nanoindentation experiments according to Eq. 7 and Eq. 8 and Table 18 shows
the yield strength values of those parts and calculated according to Eq. 9 and Eq.10.
It is noteworthy to state that if the primary initial portion of the load-displacement curves
is plotted like Figure 35(a), some discrepancies are observed due to the course of elastoplastic
86
deformation in different random penetration depths into the surface of 17-4 PH parts by revealing
multiple displacement bursts in each curve as shown in highlighted ellipses [179]. This
phenomenon is intimately related to the plastic deformation mechanism (i.e. dislocation nucleation
and propagation) and each displacement burst takes place at a different load (i.e. stress)
contributing to increasing the maximum indentation load. Besides, as-built parts exhibit mini
displacement (in black and red ellipse regions) bursts, and irradiated parts display comparatively
bigger displacement bursts (blue and green ellipse regions). Minor bursts affirm that nucleated
dislocations suppress dislocation activity happening due to barriers to the movement of
dislocations [180]. Therefore, minor displacement pop-ins in irradiated parts refer to more
resistance to plastic deformation and resulted in comparatively higher maximum shear strength.
Figure 35: (a) First displacement pop-ins in load-displacement curves for as-built and irradiated L-
PBF 17-4 PH stainless steel parts and (b) effect of irradiation on maximum shear strength at 0.1 s-1
strain rate nanoindentation tests.
Table 17: Maximum shear strength of as-built and irradiated L-PBF 17-4 PH steel parts at 0.01s-1
strain rate with loads associated with first displacement bursts.
Modulus of Reduced Max. shear Shear
First displacement
Samples elasticity modulus strength modulus
pop-in load (mN)
(GPa) (GPa) (GPa) (GPa)
54.76 J/mm3 (As-built) 0.01685 ± 0.002 10.43
54.76 J/mm3 (Irradiated) 0.01825 ± 0.001 10.71
187.3 [112] 170 7.2
61.11 J/mm3 (As-built) 0.02023 ± 0.004 11.09
61.11 J/mm3 (Irradiated) 0.02440 ± 0.003 11.8
87
Table 18: Yield strength of as-built and irradiated L-PBF 17-4 PH steel parts at 0.01s-1 strain rate.
Volumetric energy Average Vickers hardness Yield strength

density (VED) nanohardness (GPa) (kg/mm2) (MPa)
54.76 (As-built) 3.14 296.71 907.95

54.76 (Irradiated) 6.31 596.29 1824.65
61.11 (As-built) 3.42 323.41 989.65
61.11 (Irradiated) 6.62 625.20 1913.12
Figure 36: Hardness-displacement curves of as-built and irradiated 54.76 J/mm3 17-4 PH stainless
steel parts in different strain rates.
The calculated maximum shear strength from P-h curves from nanoindentation
experiments can be referred to as the theoretical shear strength of any alloy. As-built parts display
maximum shear strength as 10.43 GPa (54.76 J/mm3) and 11.09 GPa (61.11 J/mm3). As
mentioned before, irradiation effects slightly increase the shear strength of 17-4 parts. Modulus of
elasticity of L-PBF 17-4 PH stainless steel has been taken from recent literature using the same
additive manufacturing techniques as this study [112]. Irradiation affects heavily on the yield
strength of the stainless steel and Dolph et. al. [181] reported that this increase is attributed mostly
to the nucleation and growth of dislocation loops and pored under irradiation for iron-chromium
alloys.
88
The resulting hardness is plotted against the indentation depth into the L-PBF 17-4 PH SS
parts (VED = 54.76 J/mm3), which is defined and determined continuously during each separate
indentation experiment in Figure 36. Values of hardness are observed as shown in the plots to vary
very little after 400 nm displacement into the surface of the parts. This last statement is so true for
lower strain rates experiments; whereas, for increasing higher strain rates the hardness values are
stabilized later at 600 nm or 800 nm depth. These phenomena are true for 17-4 PH parts before
and after the proton irradiation. Hardness values are found to increase almost by a factor of 2 due
to the irradiation for each strain rate nanoindentation experiment. As for the highest strain rate (1
s-1), the hardness increases continuously up to 400-500 nm depth into the parts and stabilizes
within a range of hardness values. The resulting average hardness values for the parts with VED
54.76 J/mm3 are 4.27 GPa before the irradiation and 10.62 GPa after the irradiation for a strain
rate of 1 s-1. One of the reasons for this sudden jump in hardness values is irradiation damages by
proton irradiations which in turn work as obstacles for dislocations movement or sliding as
discussed in an earlier section [182].
Figure 37: Summary of micro-mechanical properties, quantitative analysis of EBSD maps, and
maximum shear strength of as-built (AB) and irradiated (IR) L-PBF 17-4 PH stainless steel parts
(based on EBSD scans performed on 1 s-1 strain rate nanoindentation areas).
89
To summarize, Figure 37 shows the change in hardness, indentation modulus, grain size,
and maximum shear stress due to proton irradiation from as-built additively manufactured 17-4
PH stainless steel parts in one plot. Based on EBSD microstructural characterization, average grain
size (μm) decreases because of proton irradiation in both 54.76 J/mm3 (8.35 μm to 4.1 μm) and
61.11 J/mm3 (5.35 μm to 5 μm) VED parts. Nanohardness, indentation modulus, and maximum
shear stress are found to increase with the increase in VED for as-built parts and irradiation shifts
those micro-mechanical properties further upward as the material becomes harder and more
sensitive to strain rate.
3.2.8 Conclusions of Irradiation Effects on Mechanical Properties and Microstructure
Firstly, this study validates that the additive manufacturing (laser powder bed fusion, L-
PBF) process is capable of printing 17-4 PH stainless steels very effectively and with 100%
integrity with less than 0.7% porosity (based on the map of X-ray tomography) and very fine grain
sizes of martensite.
Secondly, L-PBF 17-4 PH stainless steel parts are very sensitive to high strain rates and
irradiation further escalates the sensitivity notably after a strain rate of 0.25 s-1. Irradiated parts
made with 54.76 J/mm3 VED display a drastic rise in strain-rate sensitivity (m) from 0.014 to 0.597
and 0.0086 to 0.424 in the case of 61.11 J/mm3 parts inputting a maximum strain rate of 1 s-1.
Thirdly, experimentally higher martensite percentage (97.5 - 99.1%) has been found than
theoretically calculated (94.91 - 95.81%) and with constant hatch distance, higher VED contributes
to an increase in martensite percentage.
Fourthly, irradiation affects the average grain size of L-PBF 17-4 PH stainless steels and it
makes slightly finer grains when compared to as-built 17-4 PH stainless steels. It also makes the
90
alloy harder in term of nanohardness and contribute to an increment of the maximum shear strength
and affects the yield strength.
3.3 Small-Scale Mechanical Testing of Proton Irradiated L-PBF 17-4 PH Stainless Steels
Assessing the stress-stress characteristics of micro-scale volumes has been a challenge in
the field of engineering. The ability of nanoindenter with submicron level displacement and
accurate microscope-indenter calibration makes it easier for quite so many years. Small-scale
mechanical testing procedures have the capabilities to assess proficiently the effect of radiation in
micron-level structures (such as micropillars fabricated by focused ion beam (FIB)) on irradiated
L-PBF nuclear stainless steels such as 316L, 17-4 PH. This study provides uniaxial mechanical
responses of low volumes of as-built (AM) and irradiated 17-4 PH stainless steels and direct
correlation of the load-displacement i.e. stress-strain data to individual plastic deformation events
in terms of tension properties with the relation of micro-mechanical property responses generated
by the same nanoindenter with a different set-up.
3.3.1 Micro-Compression Testing, Observation of Micropillar Fractures, and Nanoindentation

Response
Micro-compression testing has gained momentum right after the introduction of the
focused ion beam (FIB) in the research industry as FIB sample manufacturing opened a new
window with its capability of fabricating well-defined geometries and low volume samples in sub-
micron level to any type of metallic alloys where hardness of that material is not a concerning
factor. Those low-volume micro-structures can lead to more sophisticated nano/micro-mechanical
behaviors if a proper experimental procedure is chosen and investigated systematically. FIB
processing techniques have minimized sample preparation effects of previously available sample
preparation techniques with the application of a controlled low-energy ion beam.
91
In this study, pillars are made with an aspect ratio of 2-2.50 (slight tapper at the bottom
which is considered while doing the calculation and making plots) and different diameters of 2
μm, 3 μm, and 5 μm. 2 μm micropillars are made only in an irradiated area so that the height falls
within the radiation damage depth of 5 μm. The micro-compression tests are done at a strain rate
of 0.1 s-1 and compressed micropillars are confirmed by observing them on the FIB followed by
load-displacement data extraction from the nanoindenter which would be converted to stress-strain
values, and thus, analysis of converted stress-strain curves would provide tension properties (such
as compressive yield strength,
Micropillars with different sizes on as-built AM 17-4 PH stainless steel parts (sample 1
with the volumetric energy density of 54.76 J/mm3 and sample 2 with 61.1 J/mm3 in Table 6) are
shown in Figure 38 and Figure 39. Micropillars with different sizes on irradiated AM 17-4 PH
stainless steel parts (sample 1 with the volumetric energy density of 54.76 J/mm3 and sample 2
with 61.1 J/mm3 in Table 6) are shown in Figure 40 and Figure 41.
Figure 38: Initial (top row) and after micro-compression (bottom row) micropillars of as-built AM
17-4 PH stainless steels with the volumetric energy density of 54.76 J/mm3 (sample 1); (a1) and (a2)
3 μm pillar, and (b1) and (b2) 5 μm pillar.
92
Figure 39: Initial (top row) and after micro-compression (bottom row) micropillars of as-built AM
3 μm pillar, and (b1) and (b2) 5 μm pillar.
Figure 40: Initial (top row) and after micro-compression (bottom row) micropillars of irradiated AM
2 μm pillar, (b1) and (b2) 3 μm pillar , and (c1) and (c2) 5 μm pillar.
93
Figure 41: Initial (top row) and after micro-compression (bottom row) micropillars of irradiated AM
2 μm pillar, (b1) and (b2) 3 μm pillar, and (c1) and (c2) 5 μm pillar.
When compared with the micro/nanoindentation test, micro-compression has the
noticeable lead of a relatively uniform stress/strain field. However, since the micro-compression
test is almost a couple of decades older technology to measure the strain-strain relation, there is no
standard yet. Some experimental variables may affect accurate measurements of strain and stress
[183]. These variables are the aspect ratio (the ratio of height h and diameter d of any micropillar),
dimensions of the substrate below the pillar, taper angle θ (>0) (the angle between the tangent of
wall and axis of the pillar), fillet angle, misalignment between axis of the pillar and the direction
of uniaxial compression load, and lastly, the strength of the substrate. The aspect of some of these
variables can be instinctively understood. For example, with a little amount of substrate volume,
the pillar would sink upon compression and the major portion of the deformation will be acting
upon the substrate instead of the pillar, which would lead to erroneous measurement of the load-
displacement data collection. In this study, this phenomenon has been observed. This sink-in effect
94
may be magnified for pillars with a large aspect ratio and suppressed for pillars with a large taper
angle. Pillars with larger aspect ratios could undergo early buckling upon applying compression
load. This intuitive argument indicates that these variables may be coupled together to influence
the accuracy of the micro-compression experimental measurement.
Deformation in single-crystal micron-scale pillars under compression has been
characterized in depth in many past studies [184,185]. Whereas consistently varying flow curves
are anticipated for bulk deformation in polycrystalline metallic alloys, intermittency and stochastic
flow are the trademark behaviors exhibited in single-crystal micro compression. Specimens
undergo elastic or near-elastic loading zone which creates step-ups in micro-compression loading
curves. Both as-built and irradiated AM 17-4 PH stainless steel micropillars in this study exhibited
this behavior with many small slip steps intermittently forming throughout the pillar volume during
plastic deformation, especially in the early period of the micro-compression testing procedure.
With the introduction of proton irradiation damage, however, obstacles to dislocation motion in
the form of a dense population of nanometer-scale Frank loops induce hardening by impeding
dislocation motion [186]. Higher stresses are necessary to initiate plastic deformation, as
dislocations must overcome irradiation-induced obstacles for the slip to occur. In studies
examining polycrystalline ion-irradiated austenitic stainless steels, this has been observed to result
in the sudden formation of defect-free channels, in which dislocations clear out irradiation defects
in a narrow channel, creating an easy path for additional dislocations to glide along. The result is
heterogeneous plastic deformation, in which strain is localized in a series of channels spaced 0.001
mm apart in each grain [187]. The proton-irradiated micro-compression specimens of this study
showed similar localization of strain, with often only two to three major slip steps forming in each
pillar of different sizes in diameter (Figure 40 and Figure 41). During the compression of an
95
irradiated pillar, each slip step forms unexpectedly and conveys a large amount of strain. As the
pillar is deformed more, strain likes to stay within these pre-existing slip steps, rather than
introducing new ones. This ultimately leads to significantly larger step heights on the irradiated
pillar surfaces than observed on the unirradiated pillars.
Figure 42: Load-displacement curves of as-built and irradiated AM 17-4 PH stainless steel parts with
two different volumetric energy densities (sample 1 = VED of 54.76 J/mm3 and sample 2 = VED of
61.11 J/mm3).
Load-displacement curves of as-built and irradiated AM 17-4 PH stainless steel parts with
two different volumetric energy densities are illustrated in Figure 42. As it seems from the plot,
the bigger the micropillar gets, it requires more load to be fractured [188]. The observed
differences in slip behavior can be quantified by first tallying the number of load drops observed
96
in the load-displacement curve for each pillar. Tests in this study were performed in displacement-
controlled mode using a fixed displacement rate and data acquisition rate. Following the initiation
of a slip event, strain rates are typically so high that only one or two data points are collected during
this time, resulting in a flat plateau in the load curve connecting the sparse data. However, the
indenter itself is load-controlled, such that when a sudden deformation event occurs, a feedback
loop detects the change in displacement and adjusts the applied indenter force accordingly. For an
event that occurs more quickly than the feedback loop can respond, such as the formation of a new
slip step, this then manifests as a steep load drop in the curve. Thus, the number of load drops in a
given load-displacement curve can be taken as an estimate of the number of slip steps in the pillar.
Figure 43: Engineering stress-strain curves of sample 1 (VED = 54.76 J/mm3) with different sizes of
micropillars of L-PBF 17-4 PH stainless steels in (a) as-built condition, (b) irradiation condition, and
(c) comparison between as-built and irradiation conditions.
97
Figure 44: Engineering stress-strain curves of sample 2 (VED of 61.11 J/mm3) with different sizes of
micropillars of L-PBF 17-4 PH stainless steels in (a) as-built condition, (b) irradiation condition., and
(c) comparison between as-built and irradiation conditions.
It is important to note that since load-displacement curves would be converted into stress-
stress curves to analyze as well as more insight will be presented on this research work in the
future, however, additional adjustments are required to do so as the strain was not measured
directly in micro-compression testing [189]. Engineering stress-strain curves of 2 μm to 5 μm
micropillars micro-compression tests are shown in Figure 43 and Figure 44 for sample 1(VED =
54.76 J/mm3) and sample 2 (VED of 61.11 J/mm3) respectively. To convert the load-displacement
curves equations are taken from some literatures [190–192]. All the pillars are connected to the
substrate (AM 17-4 PH SS) hence total displacement would be the summation of displacement of
98
the micropillar, indenter, and the substrate, and since, the displacement of the pillar can only be
applicable while converting to stress-strain curve, elastic deformation due to indenter and the
substrate must be eliminated.
The effect of irradiation on the compressive yield and ultimate tensile strength is very
clearly visible in AM 17-4 PH stainless steel parts fabricated by 54.76 J/mm3 (Figure 42 and Figure
43) and both of these properties have been observed to increase due to the irradiation effect. 2 μm
micropillar in the irradiated condition of sample 1 exhibited the highest compressive strength with
~ 244.57 MPa yield (approximate) and 375.08 MPa tensile strength. The percentage increases in
compressive yield strength were 97.31% (107.27 MPa to 211.65 MPa), and 36.8% (150.70 MPa
to 206.16 MPa) for 3 μm, and 5 μm, micropillars respectively in sample 1 because of radiation
damage; whereas 47.01% (213.58 MPa to 317.00 MPa) and 10.86% (286.40 MPa to 317.50 MPa)
increments were observed in compressive tensile strength for 3 μm and 5 μm micropillars from as-
built to irradiated areas.
Data derived from the stress-strain curves of samples 1 and 2 are listed in Table 19. In both
the samples, compressive yield and tensile strength are affected by the irradiation damage as the
hardness of the material is impacted due to radiation-induced strain hardening as reported in our
previous study [14]. Micro-compression on pillars regardless of diameters on sample 1 exhibited
superior compressive yield and tensile strength compared to sample 2. Diameter of 5 μm pillars
on sample 2, yield strengths were found to be unchanged from as-built (133.62 MPa) to irradiated
condition (133.43 MPa), though tensile strength increased from 233.54 MPa to 250 MPa. All 2
μm pillars were fabricated as their height falls within the radiation damage depth of 5 μm. It was
expected to generate the highest yield strength and tensile strength due to the radiation hardening
effect as discussed earlier. Yield and tensile strength were found to be the highest as expected as
99
244.57 MPa and 375.08 MPa in irradiated 17-4 PH sample 1. The results listed in Table 19 are
showing the tendency of variations relating to indentation hardness values reported in our previous
publication [14]. In as-built conditions, AM 17-4 PH stainless steel sample 1 generated lower
values in nanohardness compared to sample 2, and yield strengths of micropillars built on sample
1 exhibited higher values. In irradiated conditions, indentation hardness values were highly
affected (maximum average hardness of 10.71 GPa) by strain hardening effect due to irradiation
in sample 1 compared to sample 2 (10.06 GPa). That characteristic was probably responsible for
the resulting higher values in compressive yield strengths in 17-4 parts made with a VED of 54.76
J/mm3. Additionally, finer grains on irradiated sample 1 (4.1-5.2 μm) because of irradiation
damage could play a part in increasing the values of that mechanical property than that of sample
2 (4.97-5 μm).
Table 19: Ultimate tensile strength and yield strength determined from engineering stress-strain
curves of all the pillars in as-built and irradiated conditions.
Yield
Micropillar
3 strength Ultimate tensile
Sample # VED (J/mm ) Conditions diameter
(MPa) strength (MPa)
(μm)
(Approx.)
3 107.27 213.58
As-built
5 150.70 286.40
3
1 54.76 J/mm 2 244.57 375.08
Irradiated 3 211.65 314.00
5 206.16 317.50
3 146.67 237.09
As-built
5 133.62 233.54
3
2 61.11 J/mm 2 171.20 271.64
Irradiated 3 150.88 212.75
5 133.43 250.00
In a couple of the relevant open literature for direct metal laser sintering (DMLS) processed
17-4 PH stainless steel as-built parts average compressive yield strength was calculated to be in
the range of 688.52 ± 36.31 MPa - using the same nanoindenter equipment used in this study at
100
room temperature but with a lower strain rate of 0.0001 s-1 (in this study 0.01 s-1 strain rate was
used) [91]. Micropillars were fabricated with a 1:3 aspect ratio and all the micropillars were 4 μm
in diameter. Their processed 17-4 PH stainless steels have consisted of 82% retained austenite,
whereas, our study suggested that our processed 17-4 PH steel parts were made of 94.91% to
98.8% martensite. In their continuous study with the same alloy but shot-peening, average yield
strength was calculated to be 914 ± 12.73 MPa, and average UTS was found as of 1130.1 ± 17.68
MPa in the as-built condition which is way higher than what is found in this study [99]. It has been
declared in these studies that exceptional work-hardening was observed due to the presence of
retained austenite. A comparison of those findings with our study has been shown in Table 20:
Table 20: Comparison with other AM 17-4 PH stainless steel micropillar compression testing
literature (LP = laser power (Watts), HD = hatch distance (μm), LT = layer thickness (μm), SS =
scanning speed (mm/s), UTS = Ultimate tensile strength)
LP, HD, Micropillar Aspect Strain Yield strength,
AM 17-4 PH UTS, MPa
LT, SS size, μm ratio rate, s-1 MPa
As-built [91] 688.52±36.31 ---
200, 110,
4 1:3 0.0001
As-built shot 40, 750
914±12.73 1130 ± 17.68
peened [99]
As-built [This 213.58 -
220-230, 107.27-150.70
study] 286.40
120, 50, 2 to 5 1: 2-2.5 0.01
Irradiated [This
600-700 133.43-244.57 212.75-375.08
study]
No literature has been found on irradiated AM 17-4 PH stainless steel parts till the last was
reported. Orientation-based micropillar study on AM 316L materials reported a range of yield
strength from 198 MPa to 451 MPa in as-manufactured and from 476 MPa to 578 MPa in irradiated
conditions (32 dpa) [100]. Another study for proton irradiation of conventional 304 stainless steel
informed average yield strength of 272 ± 34 MPa in as-built condition, 834 ± 39 MPa in 10 dpa
damage, and 1070 ± 14 MPa in 100 dpa damage regions [193].
The lower values in compressive yield and ultimate tensile strength of AM 17-4 PH
stainless steel in this study could correspond to quite a few issues regarding micro-compression
101
testing of micropillars by the MTS nanoindenter. First of all, the strain rate chosen in this study as
0.01 s-1 is quite higher than the literature references mentioned above, since micro-mechanical
responses were not found satisfactory when choosing a much lower strain rate where the
nanoindenter was displacement controlled rather than load controlled. As in our previous study of
AM 17-4 PH stainless steel, it has been shown that the parts fabricated are very strain-rate
sensitive. That could be the second reason for lower values of compressive yield and tensile
strength. Additionally, slip steps, and load-displacement curves are machine-dependent material
responses while interpreting load drops, hardening, and elastoplastic fracture properties [194]. In
micro-compression micropillar testing, usually, the load-displacement curve is converted to an
engineering stress-strain curve by normalizing the load by the average cross-sectional area of the
micropillars and the displacement of those pillars’ height. Three unanticipated observations were
made in the literature due to sample size effects; a significant increase in yield strength at smaller
volume pillars, a stochastic variation in yield stress between the same diameter pillars, and load
drops in displacement controlled test [115,116,195,196]. Moreover, misalignment of flat punch
with respect to the sample top surface area obviously could corrupt load-displacement i.e. stress-
strain data as well as the deformation mode, and could lead to lower values in calculated
compressive yield and ultimate tensile strength [197,198]. Few factors such as non-uniaxial
loading during micro-compression, change in pillar cross-section throughout the pillar height, only
pillar volume can contain plastic deformation of the pillars could also be responsible for
inconsistent or unexpected micro-mechanical responses as the presence of these factors cannot be
discarded in this study [194].
3.3.2 Conclusions of Irradiation Effects on Small-Scale Mechanical Testing of AM 17-4 PH

Stainless Steel
One of the aims of this study was to understand and compare the synergy between
102
indentation properties i.e. approximate yield strength and small-scale micro-compression yield
strength which are relatable to radiation hardening effects. A strong agreement has been observed
between the heterogeneous plastic deformation behavior i.e. localization of strain of as-built and
irradiated micropillars in terms of major slip bands occurrence for the dislocation movement.
Higher stresses were required for micropillars fabricated in irradiated areas than in as-built areas.
For an example, 2 μm micropillars fabricated in irradiation conditions absorbed the highest amount
of uniaxial compressive load to start yielding with a compressive yield strength of 244.57 MPa
and a compressive UTS of 375.08 as expected since the whole height of the pillars was well within
the depth of radiation damage hence accompanied with higher hardness values when measured
with nanoindentation due to strain hardening effects of radiation. Overall proton irradiation
influenced (increment) the measured micropillar compressive yield and UTS values in both AM
17-4 PH stainless steel parts. Sample size effects were clearly visible in Figure 42 and Figure 43
for all the micropillars fabricated in irradiation conditions in both the 17-4 PH parts. As the
micropillars get smaller, the strength was observed to increase with one exception.
103
CHAPTER 4
CONCLUSIONS AND FUTURE WORKS*
Additively manufactured nuclear alloys that are used as materials in this study are getting
more attention and finding newer applications as this manufacturing process develops
permanently. The comprehensive package of mechanical properties and evaluation methods
presented in this dissertation is a mandatory source of data for AM 17-4 PH and 316L stainless
steel’s qualification processes, product reliability, and overall process integrity. In sequence, the
additive metallic powder materials are analyzed, then appropriate methodologies have been
developed, and mechanical and microstructural properties are reported in this study.
The use of nanoindentation in combination with electron backscatter diffraction mapping
has proven to be very useful to characterize the anisotropy in micro-mechanical properties and
microstructure in additively manufactured parts made of AISI 316L alloy. After performing this
characterization methodology, the key findings can be summarized as follows:
L-PBF parts with VED 56.67 J/mm3 exhibited a similar fraction of <101> oriented grains
similar to other parts with different VEDs but, a clear appearance of grains oriented along the line
<001> to <111> (blue/blueish to light purple in IPF color map) was observed and that was one
distinctive feature among all the other L-PBF parts. These grains were responsible for generating
higher indentation property values. The indentation properties on <111> grain orientations were
enhanced in the nanoindentation experiment and generated a higher value of misorientation angles
as well. The evolution of certain grain orientations was noticeable and variations in micro-
* The first half of this chapter is reproduced from a combination of 2 sources, both used with permission from
Elseiver: (1) M.J. Uddin, E. Ramirez-Cedillo, R.A. Mirshams, H.R. Siller, Nanoindentation and electron backscatter
diffraction mapping in laser powder bed fusion of stainless steel 316L, Mater. Charact. 174 (2021) 111047,
104
mechanical responses were reported. The higher angle grain boundary regions most probably
behaved as a strong barrier against dislocation movements and thus, increments over the
indentation hardness and modulus were taken place. Dislocations pile-up occurred when those
regions have gone under plastic deformation and prevented crack propagation at a certain limit.
Collectively the relatively lower grain size accompanied by a higher average misorientation angle
of L-PBF AISI 316L parts with VED of 56.67 J/mm3 also influenced the calculation of hardness
and modulus values.
The conventional AISI 316L stainless steel was noticed to have the lowest texture strength,
but the indentation modulus and hardness were lower than most L-PBF AISI 316L parts with a
VED of 56.67 J/mm3. Strong <101> and <001> oriented textures were visible from the texture
IPFs. A strong possibility is there that this additional but unwanted strong <001> texture someway
subsidized the mitigation of the values of indentation properties. Generally, parts with
microstructures of the finer grains are supposed to reveal superior mechanical properties. The
average grain size of L-PBF AISI parts with VED of 45.24 J/mm3 was calculated to be the lowest
among all L-PBF parts as 9.22 μm and unexpectedly, those parts did not display the best micro-
mechanical responses. It also requires further investigations in future studies.
In summary, micro-mechanical anisotropy was found in all the L-PBF AISI 316L parts
regardless of the amount of volumetric energy density and the extent of anisotropy was addressed
by the grain morphology and the quantitative means of the analysis of data, generated by the
electron backscattered diffraction maps such as texture PFs, texture IPFs, misorientation angles,
and grain size. In-depth cell size analysis on different grain morphologies should be evaluated
further, to fully correlate and compare their micro-mechanical characteristics with the help of
nanoindentation.
105
The combined study of nanoindentation with EBSD mapping is an alternative methodology
for enriching qualification protocols, of additively manufactured metallic components, in addition
to existing macro-mechanical evaluation via tensile testing. Future works should include additional
experimental procedures to correlate indentation response with macro-mechanical behavior and
porosity characterization.
This study authenticates that AM process is fully capable of fabricating nuclear alloys such
as 17-4 PH stainless steels very efficiently and with almost 100% integrity that only contains less
than 0.7% porosity (based on the map of X-ray tomography) with very fine martensitic grains
confirmed by the XRD. L-PBF 17-4 PH stainless steel parts are found to be very sensitive to high
strain rates i.e. high load rates and the fact that irradiation damage additionally intensifies the
sensitivity limit notably after a strain rate of 0.25 s-1. A severe rise in strain-rate sensitivity (m)
from 0.014 to 0.597 was noticed in parts with irradiated conditions made with 54.76 J/mm3 VED
and an increment from 0.0086 to 0.424 was in the case of 61.11 J/mm3 parts where a maximum
strain rate of 1 s-1 was applied during nanoindentation experiment. Additionally, the experimental
percentage of martensite (97.5 - 99.1%) was found to be higher than theoretically calculated (94.91
- 95.81%) values. With the same process parameters of AM such as hatch distance, an increase in
VED influenced the martensite percentage in all the parts. Lastly, a slight effect of irradiation was
observed over average grain size calculation. It made the 17-4 PH stainless steel harder in terms
of nanohardness as shown in the analysis. The behavior at the micro-scale seen in nanoindentation,
shows significant departures from the classical elastic–plastic models, mainly due to the size effect.
The study of this phenomenon on additively manufactured radiation-resistant alloys has been
limited, and layer-by-layer nanoindentation size effects and strain-rate sensitivity, with an increase
in load, have scarcely been explored on small-scale tests geometries. We developed new models
106
of strain rate sensitivity in AM proton irradiated alloys (1 MeV proton irradiation with a fluence
of 1×1019 ions/cm2), where we found that stainless steel parts are very sensitive to high strain
rates and irradiation further escalates the sensitivity notably after strain rate of 0.25 s-1 in parts
made at different processing volumetric energy densities. The irradiation makes the alloy harder
in terms of nano-hardness and contributes to an increment of the maximum shear strength affecting
the yield and shear strength, as shown in our recent publication.
Table 21: Summary of major mechanical properties calculated from indentation and small-scale
mechanical testing (for 3 μm) methods on as-built and irradiated 17-4 PH stainless steels
As-built Irradiated As-built Irradiated
54.76 J/mm3 54.76 J/mm3 61.11 J/mm3 61.11 J/mm3
Indentation Hardness
3.14 6.31 3.4225 6.61
(GPa)
Indentation Modulus
180.044 217.363 190.59 231
(GPa)
Indentation Yield
907.95 1824.65 989.65 1913.12
Strength (MPa)
Indentation Maximum
10.43 10.71 11.09 11.8
Shear Strength (GPa)
Micropillar
Compressive Yield 107.27 211.65 146.67 237.09
Strength (MPa)
Micropillar
Compressive Ultimate
213.58 314 150.88 212.75
Tensile Strength
(MPa)
In micro-compression testing of AM 17-4 PH stainless steel alloys, it was found that
micropillars fabricated in as-built conditions moving dislocations (slip system) were the major
deformation carrier with the presence of a little amount of very fine fabrication-induced pores.
Strain-hardening due to proton irradiation obviously impacted the micropillar compressive
properties as the irradiated AM 17-4 PH stainless steels have high indentation hardness compared
to as-built conditions. Fewer slip bands were observed in irradiated micropillar under uniaxial
compressive load. A strong agreement was observed between micro-mechanical properties
107
determined in the indentation method than micro-compression micropillar method considering
both as-built and irradiated conditions.
The development of qualification protocols for the evaluation of additively manufactured
parts with irradiation effects is an alternative to other testing protocols requiring extensive
experimentation, from which the extraction of important mechanical properties can be achieved.
Table 21 summarizes the most significant mechanical properties estimated from this study, taking
into account the consistency of the data and the reliability of the testing instruments and devices.
For this table, the values extracted from compression testing of 3 μm micropillars and
nanoindentation samples with a strain rate of 0.01 s-1 were considered.
It can be noted that the collection of procedures will be determinant to establish a clear
correlation between volumetric energy densities and irradiation effects. For the case of indentation
hardness, the highest VED produced hardening effects, and the combination of irradiation gives a
significant change in this mechanical property. In the case of Indentation Modulus, Indentation
Yield, and Maximum Shear Strength the trend is similar. For Micropillar Compressive Yield the
result shows that the highest energy density produced better results as well and irradiation is
increasing those values interestingly. However the consistency among nanoindentation data and
micropillar compression is seen in some instances and not through the whole set of experiments,
but the irradiation effects are very clear in the whole experimentation, which is a strong argument
that the qualification procedure presented here is valid. For the Micropillar Compressive Tensile
Strength, the behavior is the opposite, the lower energy density produced better results. More
investigation is needed to evaluate this mechanical property with micro-tensile samples fabricated
by focused ion beam to integrate a more comprehensive protocol for future designing and
manufacturing of irradiation resistant additively manufactured alloys.
108
Indentation and small-scale mechanical test yield properties of AM 316L stainless steels
can be studied in the future as this study could facilitate the qualification processes for various
intricate applications as well as a direct comparison could be made with AM 17-4 PH stainless
steels. Strain-rate sensitivity studies of AM 316L parts could also be crucial for load-sensitive
applications in various industries. Increasing the number of experimentations of micropillar micro-
compression tests of AM 17-4 PH stainless steel is required for a more accurate assessment of the
micro-mechanical properties. Micro-compression could be performed at a very lower strain rate
(0.0005 or lower) in the future with a different testing approach using the same nanoindenter
equipment so that it would be well compared with the literature available. Fabricating micropillars
in grains with specific crystallographic orientations could help elaborate the plastic deformation
mechanism on a broad scale for both process optimization and performance evaluation of
additively manufactured stainless steel alloys for nuclear applications. Introducing TEM studies
along with mechanical and microstructural characterizations could help in determining Schmid
factors for any fabricated micropillars with reduced data variations in different grain orientations
which is critical to calculate critical resolved shear stress and yield stress more accurately. The
strength of various microstructural phases such as retained austenite and martensite could also be
computed quantitatively in future works. In-situ micro-compression tests on small volumes can be
carried out in the future to convey more capability and control on the testing procedure.
109
REFERENCES
[1] T.D. Ngo, A. Kashani, G. Imbalzano, K.T.Q. Nguyen, D. Hui, Additive manufacturing
(3D printing): A review of materials, methods, applications and challenges, Compos. Part
B Eng. 143 (2018) 172–196. https://doi.org/10.1016/j.compositesb.2018.02.012.
[2] L. Cheng, X. Liang, J. Bai, Q. Chen, J. Lemon, A. To, On utilizing topology optimization
to design support structure to prevent residual stress induced build failure in laser powder
bed metal additive manufacturing, Addit. Manuf. 27 (2019) 290–304.
https://doi.org/10.1016/j.addma.2019.03.001.
[3] O. Ivanova, C. Williams, T. Campbell, Additive manufacturing (AM) and

nanotechnology: promises and challenges, Rapid Prototyp. J. 19 (2013) 353–364.
https://doi.org/10.1108/RPJ-12-2011-0127.
[4] S. Ganesh Sarvankar, S.N. Yewale, Additive Manufacturing in Automobile Industry, Int.
J. Res. Aeronaut. Echanical Eng. 7 (2019) 1–10.
[5] D. Delgado Camacho, P. Clayton, W.J. O’Brien, C. Seepersad, M. Juenger, R. Ferron, S.

Salamone, Applications of additive manufacturing in the construction industry – A
forward-looking review, Autom. Constr. 89 (2018) 110–119.
https://doi.org/10.1016/j.autcon.2017.12.031.
[6] D. Chantzis, X. Liu, D.J. Politis, O. El Fakir, T.Y. Chua, Z. Shi, L. Wang, Review on
additive manufacturing of tooling for hot stamping, Int. J. Adv. Manuf. Technol. 109
(2020) 87–107. https://doi.org/10.1007/s00170-020-05622-1.
[7] Z. Liu, B. He, T. Lyu, Y. Zou, A Review on Additive Manufacturing of Titanium Alloys
for Aerospace Applications: Directed Energy Deposition and Beyond Ti-6Al-4V, Jom. 73
(2021) 1804–1818. https://doi.org/10.1007/s11837-021-04670-6.
[8] E.M. Parsons, Lightweight cellular metal composites with zero and tunable thermal
expansion enabled by ultrasonic additive manufacturing: Modeling, manufacturing, and
testing, Compos. Struct. 223 (2019) 110656.
https://doi.org/10.1016/j.compstruct.2019.02.031.
[9] M. Salmi, Additive manufacturing processes in medical applications, Materials (Basel).

14 (2021) 1–16. https://doi.org/10.3390/ma14010191.
[10] P. Szymczyk-Ziółkowska, M.B. Łabowska, J. Detyna, I. Michalak, P. Gruber, A review

of fabrication polymer scaffolds for biomedical applications using additive
manufacturing techniques, Biocybern. Biomed. Eng. 40 (2020) 624–638.
https://doi.org/10.1016/j.bbe.2020.01.015.
[11] M. Javaid, A. Haleem, Current status and applications of additive manufacturing in

dentistry: A literature-based review, J. Oral Biol. Craniofacial Res. 9 (2019) 179–185.
https://doi.org/10.1016/j.jobcr.2019.04.004.
110
[12] E. Ramirez-Cedillo, M.J. Uddin, J.A. Sandoval-Robles, R.A. Mirshams, L. Ruiz-Huerta,
C.A. Rodriguez, H.R. Siller, Process planning of L-PBF of AISI 316L for improving
surface quality and relating part integrity with microstructural characteristics, Surf.
Coatings Technol. 396 (2020) 125956. https://doi.org/10.1016/j.surfcoat.2020.125956.
[13] M.J. Uddin, E. Ramirez-Cedillo, R.A. Mirshams, H.R. Siller, Nanoindentation and
electron backscatter diffraction mapping in laser powder bed fusion of stainless steel
316L, Mater. Charact. 174 (2021) 111047.
https://doi.org/10.1016/j.matchar.2021.111047.
[14] M.J. Uddin, H.R. Siller, R.A. Mirshams, T.A. Byers, B. Rout, Effects of proton
irradiation on nanoindentation strain-rate sensitivity and microstructural properties in L-
PBF 17–4 PH stainless steels, Mater. Sci. Eng. A. 837 (2022) 142719.
https://doi.org/10.1016/j.msea.2022.142719.
[15] O. T. Wohlers, I. Campbell, O. Diegel, Wohlers Report 2018, Fort Collins: Wohlers
Associates. (2018), Addit. Manuf. 22 (2018) 844–851.
[16] K.G. Prashanth, S. Scudino, H.J. Klauss, K.B. Surreddi, L. Löber, Z. Wang, A.K.
Chaubey, U. Kühn, J. Eckert, Microstructure and mechanical properties of Al–12Si
produced by selective laser melting: Effect of heat treatment, Mater. Sci. Eng. A. 590
(2014) 153–160. https://doi.org/https://doi.org/10.1016/j.msea.2013.10.023.
[17] C. Sun, Y. Wang, M.D. McMurtrey, N.D. Jerred, F. Liou, J. Li, Additive manufacturing
for energy: A review, Appl. Energy. 282 (2021).
https://doi.org/10.1016/j.apenergy.2020.116041.
[18] H. Attar, S. Ehtemam-Haghighi, N. Soro, D. Kent, M.S. Dargusch, Additive

manufacturing of low-cost porous titanium-based composites for biomedical applications:
Advantages, challenges and opinion for future development, J. Alloys Compd. 827
(2020) 154263. https://doi.org/10.1016/j.jallcom.2020.154263.
[19] J. den Boer, W. Lambrechts, H. Krikke, Additive manufacturing in military and

humanitarian missions: Advantages and challenges in the spare parts supply chain, J.
Clean. Prod. 257 (2020) 120301. https://doi.org/10.1016/j.jclepro.2020.120301.
[20] B.R. Betzler, B.J. Ade, A.J. Wysocki, P.K. Jain, P.C. Chesser, M.S. Greenwood, K.A.
Terrani, Transformational Challenge Reactor preconceptual core design studies, Nucl.
Eng. Des. 367 (2020) 110781. https://doi.org/10.1016/j.nucengdes.2020.110781.
[21] M. Hiser, A. Schneider, M. Audrain, A. Hull, Regulatory Research Perspective on

Additive Manufacturing for Nuclear Component Applications, J. Nucl. Mater. 546 (2021)
152726. https://doi.org/10.1016/j.jnucmat.2020.152726.
[22] M.W. Graham, J.C. King, T.R. Pavlov, C.A. Adkins, S.C. Middlemas, D.P. Guillen,
Impact of neutron irradiation on the thermophysical properties of additively
111
manufactured stainless steel and inconel, J. Nucl. Mater. 549 (2021) 152861.
https://doi.org/10.1016/j.jnucmat.2021.152861.
[23] W. Zhong, N. Sridharan, D. Isheim, K.G. Field, Y. Yang, K. Terrani, L. Tan,

Microstructures and mechanical properties of a modified 9Cr ferritic-martensitic steel in
the as-built condition after additive manufacturing, J. Nucl. Mater. 545 (2021) 152742.
[24] M. McMurtrey, C. Sun, R.E. Rupp, C.H. Shiau, R. Hanbury, N. Jerred, R. O’Brien,
Investigation of the irradiation effects in additively manufactured 316L steel resulting in
decreased irradiation assisted stress corrosion cracking susceptibility, J. Nucl. Mater. 545
(2021). https://doi.org/10.1016/j.jnucmat.2020.152739.
[25] M. Saleh, Z. Zaidi, M. Ionescu, C. Hurt, K. Short, J. Daniels, P. Munroe, L. Edwards, D.

Bhattacharyya, Relationship between damage and hardness profiles in ion irradiated
SS316 using nanoindentation - Experiments and modelling, Int. J. Plast. 86 (2016) 151–
169. https://doi.org/10.1016/j.ijplas.2016.08.006.
[26] B.P. Eftink, J.S. Weaver, J.A. Valdez, V. Livescu, D. Chen, Y. Wang, C. Knapp, N.A.
Mara, S.A. Maloy, G.T. Gray, Proton irradiation and characterization of additively
manufactured 304L stainless steels, J. Nucl. Mater. 531 (2020) 152007.
[27] S. Qin, Z. Wang, A.M. Beese, Orientation and stress state dependent plasticity and
damage initiation behavior of stainless steel 304L manufactured by laser powder bed
fusion additive manufacturing, Extrem. Mech. Lett. 45 (2021) 101271.
https://doi.org/10.1016/j.eml.2021.101271.
[28] W. Macek, R. Branco, J. Trembacz, J.D. Costa, J.A.M. Ferreira, C. Capela, Effect of
multiaxial bending-torsion loading on fracture surface parameters in high-strength steels
processed by conventional and additive manufacturing, Eng. Fail. Anal. 118 (2020)
104784. https://doi.org/10.1016/j.engfailanal.2020.104784.
[29] S. Spigarelli, C. Paoletti, M. Cabibbo, E. Cerri, E. Santecchia, On the creep performance

of the Ti‐6Al‐4V alloy processed by additive manufacturing, Addit. Manuf. 49 (2022)
102520. https://doi.org/10.1016/j.addma.2021.102520.
[30] T. Kurzynowski, E. Chlebus, B. Kuźnicka, J. Reiner, Parameters in Selective Laser

Melting for processing metallic powders, Proc. SPIE. 8239 (2012) 823914.
https://doi.org/10.1117/12.907292.
[31] J. Kim, S. Ji, Y.-S. Yun, J.-S. Yeo, A Review : Melt Pool Analysis for Selective Laser
Melting with Continuous Wave and Pulse Width Modulated Lasers, Appl. Sci. Converg.
Technol. 27 (2018) 113–119. https://doi.org/10.5757/ASCT.2018.27.6.113.
[32] J.H. Robinson, I.R.T. Ashton, E. Jones, P. Fox, C. Sutcliffe, The effect of hatch angle
rotation on parts manufactured using selective laser melting, Rapid Prototyp. J. 25 (2019)
289–298. https://doi.org/10.1108/RPJ-06-2017-0111.
112
[33] E. Liverani, A. Fortunato, A. Leardini, C. Belvedere, S. Siegler, L. Ceschini, A. Ascari,
Fabrication of Co–Cr–Mo endoprosthetic ankle devices by means of Selective Laser
Melting (SLM), Mater. Des. 106 (2016) 60–68.
https://doi.org/10.1016/j.matdes.2016.05.083.
[34] B. Vandenbroucke, J.-P. Kruth, Selective Laser Melting of Biocompatible Metals for
Rapid, Rapid Prototyp. J. 13 (2007) 148–159.
[35] N. Read, W. Wang, K. Essa, M.M. Attallah, Selective laser melting of AlSi10Mg alloy:
Process optimisation and mechanical properties development, Mater. Des. 65 (2015)
417–424. https://doi.org/10.1016/j.matdes.2014.09.044.
[36] X. Lou, D. Gandy, Advanced Manufacturing for Nuclear Energy, Jom. 71 (2019) 2834–
2836. https://doi.org/10.1007/s11837-019-03607-4.
[37] A. Hinojos, J. Mireles, A. Reichardt, P. Frigola, P. Hosemann, L.E. Murr, R.B. Wicker,
Joining of Inconel 718 and 316 Stainless Steel using electron beam melting additive
manufacturing technology, Mater. Des. 94 (2016) 17–27.
[38] W. Liu, J.N. DuPont, Fabrication of functionally graded TiC/Ti composites by laser
engineered net shaping, Scr. Mater. 48 (2003) 1337–1342. https://doi.org/10.1016/S1359-
6462(03)00020-4.
[39] B.E. Carroll, R.A. Otis, J.P. Borgonia, J.O. Suh, R.P. Dillon, A.A. Shapiro, D.C.
Hofmann, Z.K. Liu, A.M. Beese, Functionally graded material of 304L stainless steel and
inconel 625 fabricated by directed energy deposition: Characterization and
thermodynamic modeling, Acta Mater. 108 (2016) 46–54.
https://doi.org/10.1016/j.actamat.2016.02.019.
[40] L.D. Bobbio, B. Bocklund, R. Otis, J.P. Borgonia, R.P. Dillon, A.A. Shapiro, B.
McEnerney, Z.K. Liu, A.M. Beese, Characterization of a functionally graded material of
Ti-6Al-4V to 304L stainless steel with an intermediate V section, J. Alloys Compd. 742
(2018) 1031–1036. https://doi.org/10.1016/j.jallcom.2018.01.156.
[41] F.F. Noecker, J.N. DuPont, Functionally graded copper – steel using laser engineered net
shapingTM process, Int. Congr. Appl. Lasers Electro-Optics. 2002 (2002) 185430.
https://doi.org/10.2351/1.5066217.
[42] Y.M. Wang, T. Voisin, J.T. McKeown, J. Ye, N.P. Calta, Z. Li, Z. Zeng, Y. Zhang, W.
Chen, T.T. Roehling, R.T. Ott, M.K. Santala, P.J. Depond, M.J. Matthews, A. V. Hamza,
T. Zhu, Additively manufactured hierarchical stainless steels with high strength and
ductility, Nat. Mater. 17 (2018) 63–70. https://doi.org/10.1038/NMAT5021.
[43] A.J. Markworth, K.S. Ramesh, W.P. Parks, Modelling studies applied to functionally
graded materials, J. Mater. Sci. 30 (1995) 2183–2193.
https://doi.org/10.1007/BF01184560.
113
[44] K. Terrani, J. Kiggans, D. Chandler, C. Bryan, D. Pinkston, N. Sridharan, M. Gussev, M.
Norfolk, J. Burns, S. Suresh Babu, Additive Manufacturing of Research Reactor Control
Elements and Subsequent Neutron Irradiation, Trans. Am. Nucl. Soc. 114 (2016) 1229–
1230. http://inis.iaea.org/search/search.aspx?orig_q=RN:52032391.
[45] J.R. Burns, D. Chandler, B. Petrovic, K.A. Terrani, Depletion and lifetime performance
analysis of advanced manufactured control elements in the high flux isotope reactor
(HFIR), Proc. 2018 Int. Congr. Adv. Nucl. Power Plants, ICAPP 2018. (2018) 738–745.
[46] J. Rosales, I.J. van Rooyen, C.J. Parga, Characterizing surrogates to develop an additive
manufacturing process for U 3 Si 2 nuclear fuel, J. Nucl. Mater. 518 (2019) 117–128.
https://doi.org/10.1016/j.jnucmat.2019.02.026.
[47] A. V. Gelis, P. Kozak, A.T. Breshears, M.A. Brown, C. Launiere, E.L. Campbell, G.B.
Hall, T.G. Levitskaia, V.E. Holfeltz, G.J. Lumetta, Author Correction: Closing the
Nuclear Fuel Cycle with a Simplified Minor Actinide Lanthanide Separation Process
(ALSEP) and Additive Manufacturing (Scientific Reports, (2019), 9, 1, (12842),
10.1038/s41598-019-48619-x), Sci. Rep. 10 (2020) 1–11. https://doi.org/10.1038/s41598-
020-57574-x.
[48] G. Kalinin, V. Barabash, A. Cardella, J. Dietz, K. Ioki, R. Matera, R.T. Santoro, R.

Tivey, Assessment and selection of materials for ITER in-vessel components, J. Nucl.
Mater. 283–287 (2000) 10–19. https://doi.org/10.1016/S0022-3115(00)00305-6.
[49] B.S. Rodchenkov, Y.S. Strebkov, G.M. Kalinin, O.A. Golosov, Effect of ITER blanket
manufacturing process on the properties of the 316L(N)-IG steel, Fusion Eng. Des. 49–50
(2000) 657–660. https://doi.org/10.1016/S0920-3796(00)00359-8.
[50] R.K. Buddu, N. Chauhan, P.M. Raole, Mechanical properties and microstructural
investigations of TIG welded 40 mm and 60 mm thick SS 316L samples for fusion
reactor vacuum vessel applications, Fusion Eng. Des. 89 (2014) 3149–3158.
https://doi.org/10.1016/j.fusengdes.2014.10.006.
[51] C. Tan, G. Wang, L. Ji, Y. Tong, X.M. Duan, Investigation on 316L/W functionally
graded materials fabricated by mechanical alloying and spark plasma sintering, J. Nucl.
Mater. 469 (2016) 32–38. https://doi.org/10.1016/j.jnucmat.2015.11.024.
[52] D. Kong, X. Ni, C. Dong, X. Lei, L. Zhang, C. Man, J. Yao, X. Cheng, X. Li, Bio-
functional and anti-corrosive 3D printing 316L stainless steel fabricated by selective laser
melting, Mater. Des. 152 (2018) 88–101. https://doi.org/10.1016/j.matdes.2018.04.058.
[53] D. Dzhendov, T. Dikova, Application of selective laser melting in manufacturing of fixed

dental prostheses, J. IMAB - Annu. Proceeding (Scientific Pap. 22 (2016) 1414–1417.
https://doi.org/10.5272/jimab.2016224.1414.
[54] H. Zhou, Q. Fan, 3D reconstruction and SLM survey for dental implants, J. Mech. Med.
Biol. 17 (2017) 1–11. https://doi.org/10.1142/S0219519417500841.
114
[55] S.L. Sing, Concepts of Selective Laser Melting for Orthopaedic Implants BT - Selective
Laser Melting of Novel Titanium-Tantalum Alloy as Orthopaedic Biomaterial, in: S.L.
Sing (Ed.), Springer Singapore, Singapore, 2019: pp. 9–36. https://doi.org/10.1007/978-
981-13-2724-7_2.
[56] J. Čapek, M. Machová, M. Fousová, J. Kubásek, D. Vojtěch, J. Fojt, E. Jablonská, J.

Lipov, T. Ruml, Highly porous, low elastic modulus 316L stainless steel scaffold
prepared by selective laser melting, Mater. Sci. Eng. C. 69 (2016) 631–639.
https://doi.org/10.1016/j.msec.2016.07.027.
[57] K. Jha, J. Verma, C. Prakash, Fabrication and In Vitro Corrosion Characterization of

316L Stainless Steel for Medical Application BT - Biomaterials in Orthopaedics and
Bone Regeneration : Design and Synthesis, in: P.S. Bains, S.S. Sidhu, M. Bahraminasab,
C. Prakash (Eds.), Springer Singapore, Singapore, 2019: pp. 215–226.
https://doi.org/10.1007/978-981-13-9977-0_14.
[58] M.J.K. Lodhi, K.M. Deen, W. Haider, Corrosion behavior of additively manufactured
316L stainless steel in acidic media, Materialia. 2 (2018) 111–121.
https://doi.org/10.1016/j.mtla.2018.06.015.
[59] A.B. Kale, B.K. Kim, D.I. Kim, E.G. Castle, M. Reece, S.H. Choi, An investigation of
the corrosion behavior of 316L stainless steel fabricated by SLM and SPS techniques,
Mater. Charact. 163 (2020) 110204. https://doi.org/10.1016/j.matchar.2020.110204.
[60] K. Saeidi, X. Gao, Y. Zhong, Z.J. Shen, Hardened austenite steel with columnar sub-
grain structure formed by laser melting, Mater. Sci. Eng. A. 625 (2015) 221–229.
https://doi.org/10.1016/j.msea.2014.12.018.
[61] H.W. Huang, Z.B. Wang, J. Lu, K. Lu, Fatigue behaviors of AISI 316L stainless steel
with a gradient nanostructured surface layer, Acta Mater. 87 (2015) 150–160.
[62] D. Kong, X. Ni, C. Dong, L. Zhang, C. Man, X. Cheng, X. Li, Anisotropy in the
microstructure and mechanical property for the bulk and porous 316L stainless steel
fabricated via selective laser melting, Mater. Lett. 235 (2019) 1–5.
https://doi.org/10.1016/j.matlet.2018.09.152.
[63] X. Ni, D. Kong, Y. Wen, L. Zhang, W. Wu, B. He, L. Lu, D. Zhu, Anisotropy in
mechanical properties and corrosion resistance of 316L stainless steel fabricated by
selective laser melting, Int. J. Miner. Metall. Mater. 26 (2019) 319–328.
https://doi.org/10.1007/s12613-019-1740-x.
[64] J. Andrew, LA-UR-19-32212 Title : Author ( s ): Intended for : Nuclear Reactor

Materials and Anisotropy Issued :, (2019).
[65] Y.D. Im, K.H. Kim, K.H. Jung, Y.K. Lee, K.H. Song, Anisotropic Mechanical Behavior
of Additive Manufactured AISI 316L Steel, Metall. Mater. Trans. A Phys. Metall. Mater.
Sci. 50 (2019) 2014–2021. https://doi.org/10.1007/s11661-019-05139-7.
115
[66] S. Huang, S.L. Sing, G. de Looze, R. Wilson, W.Y. Yeong, Laser powder bed fusion of
titanium-tantalum alloys: Compositions and designs for biomedical applications, J. Mech.
Behav. Biomed. Mater. 108 (2020) 103775.
https://doi.org/10.1016/j.jmbbm.2020.103775.
[67] T. Pinomaa, M. Lindroos, M. Walbrühl, N. Provatas, A. Laukkanen, The significance of

spatial length scales and solute segregation in strengthening rapid solidification
microstructures of 316L stainless steel, Acta Mater. 184 (2020) 1–16.
[68] Y. Kok, X.P. Tan, P. Wang, M.L.S. Nai, N.H. Loh, E. Liu, S.B. Tor, Anisotropy and
heterogeneity of microstructure and mechanical properties in metal additive
manufacturing: A critical review, Mater. Des. 139 (2018) 565–586.
[69] Z. Sun, X. Tan, S.B. Tor, C.K. Chua, Simultaneously enhanced strength and ductility for
3D-printed stainless steel 316L by selective laser melting, NPG Asia Mater. 10 (2018)
127–136. https://doi.org/10.1038/s41427-018-0018-5.
[70] M.L. Montero-Sistiaga, M. Godino-Martinez, K. Boschmans, J.P. Kruth, J. Van

Humbeeck, K. Vanmeensel, Microstructure evolution of 316L produced by HP-SLM
(high power selective laser melting), Addit. Manuf. 23 (2018) 402–410.
[71] H.R. Lashgari, C. Kong, E. Adabifiroozjaei, S. Li, Microstructure, post thermal treatment
response, and tribological properties of 3D printed 17-4 PH stainless steel, Wear. 456–
457 (2020). https://doi.org/10.1016/j.wear.2020.203367.
[72] F. Ahmed, U. Ali, D. Sarker, E. Marzbanrad, K. Choi, Y. Mahmoodkhani, E. Toyserkani,

Study of powder recycling and its effect on printed parts during laser powder-bed fusion
of 17-4 PH stainless steel, J. Mater. Process. Technol. 278 (2020) 116522.
https://doi.org/10.1016/j.jmatprotec.2019.116522.
[73] A. Soltani-Tehrani, J. Pegues, N. Shamsaei, Fatigue behavior of additively manufactured

17-4 PH stainless steel: The effects of part location and powder re-use, Addit. Manuf. 36
(2020). https://doi.org/10.1016/j.addma.2020.101398.
[74] M. Alnajjar, F. Christien, V. Barnier, C. Bosch, K. Wolski, A.D. Fortes, M. Telling,

Influence of microstructure and manganese sulfides on corrosion resistance of selective
laser melted 17-4 PH stainless steel in acidic chloride medium, Corros. Sci. 168 (2020)
108585. https://doi.org/10.1016/j.corsci.2020.108585.
[75] S.J. Zinkle, K.A. Terrani, L.L. Snead, Motivation for utilizing new high-performance
advanced materials in nuclear energy systems, Curr. Opin. Solid State Mater. Sci. 20
(2016) 401–410. https://doi.org/10.1016/j.cossms.2016.10.004.
116
[76] N. Bibhanshu, M.N. Gussev, T.M. Rosseel, Complexity of deformation mechanism in
neutron-irradiated 304L austenitic stainless steel at microstructural scale, Mater. Charact.
178 (2021) 111218. https://doi.org/10.1016/j.matchar.2021.111218.
[77] Z. Wang, W.M. Mook, C. Niederberger, R. Ghisleni, L. Philippe, J. Michler,

Compression of nanowires using a flat indenter: Diametrical elasticity measurement,
Nano Lett. 12 (2012) 2289–2293. https://doi.org/10.1021/nl300103z.
[78] J.Y. Kim, J.R. Greer, Tensile and compressive behavior of gold and molybdenum single
crystals at the nano-scale, Acta Mater. 57 (2009) 5245–5253.
[79] C.S. Kaira, T.J. Stannard, V. De Andrade, F. De Carlo, N. Chawla, Exploring novel
deformation mechanisms in aluminum–copper alloys using in situ 4D nanomechanical
testing, Acta Mater. 176 (2019) 242–249. https://doi.org/10.1016/j.actamat.2019.07.016.
[80] M. Zamanzade, J.R. Velayarce, O.T. Abad, C. Motz, A. Barnoush, Mechanical behavior
of iron aluminides: A comparison of nanoindentation, compression and bending of
micropillars, Mater. Sci. Eng. A. 652 (2016) 370–376.
[81] E. Camposilvan, M. Anglada, Size and plasticity effects in zirconia micropillars

compression, Acta Mater. 103 (2016) 882–892.
[82] K. Chu, K. Yan, F. Ren, Q. Sun, A dual-pillar method for measurement of stress-strain
response of material at microscale, Scr. Mater. 172 (2019) 138–143.
https://doi.org/10.1016/j.scriptamat.2019.07.021.
[83] J.S. Weaver, M. Kreitman, J.C. Heigel, M.A. Donmez, Mechanical Property
Characterization of Single Scan Laser Tracks of Nickel Superalloy 625 by
Nanoindentation BT - TMS 2019 148th Annual Meeting & Exhibition Supplemental
Proceedings, in: Springer International Publishing, Cham, 2019: pp. 269–278.
[84] P. Hosemann, Small-scale mechanical testing on nuclear materials: Bridging the

experimental length-scale gap, Scr. Mater. 143 (2017).
[85] J.S. Weaver, V. Livescu, N.A. Mara, A comparison of adiabatic shear bands in wrought
and additively manufactured 316L stainless steel using nanoindentation and electron
backscatter diffraction, J. Mater. Sci. 55 (2020) 1738–1752.
https://doi.org/10.1007/s10853-019-03994-8.
[86] X. Wang, X. Gong, K. Chou, Scanning Speed Effect on Mechanical Properties of Ti-6Al-
4V Alloy Processed by Electron Beam Additive Manufacturing, Procedia Manuf. 1
(2015) 287–295. https://doi.org/10.1016/j.promfg.2015.09.026.
117
[87] X. Sun, F. Chen, H. Huang, J. Lin, X. Tang, Effects of interfaces on the helium bubble
formation and radiation hardening of an austenitic stainless steel achieved by additive
manufacturing, Appl. Surf. Sci. 467–468 (2019) 1134–1139.
https://doi.org/10.1016/j.apsusc.2018.10.268.
[88] A. Reichardt, R.P. Dillon, J.P. Borgonia, A.A. Shapiro, B.W. McEnerney, T. Momose, P.
Hosemann, Development and characterization of Ti-6Al-4V to 304L stainless steel
gradient components fabricated with laser deposition additive manufacturing, Mater. Des.
104 (2016) 404–413. https://doi.org/10.1016/j.matdes.2016.05.016.
[89] N.T. Aboulkhair, I. Maskery, C. Tuck, I. Ashcroft, N.M. Everitt, The microstructure and
mechanical properties of selectively laser melted AlSi10Mg: The effect of a conventional
T6-like heat treatment, Mater. Sci. Eng. A. 667 (2016) 139–146.
[90] H. Wang, A. Dhiman, H.E. Ostergaard, Y. Zhang, T. Siegmund, J.J. Kruzic, V. Tomar,
Nanoindentation based properties of Inconel 718 at elevated temperatures: A comparison
of conventional versus additively manufactured samples, Int. J. Plast. 120 (2019) 380–
394. https://doi.org/10.1016/j.ijplas.2019.04.018.
[91] B. AlMangour, J.M. Yang, Understanding the deformation behavior of 17-4 precipitate
hardenable stainless steel produced by direct metal laser sintering using micropillar
compression and TEM, Int. J. Adv. Manuf. Technol. 90 (2017) 119–126.
https://doi.org/10.1007/s00170-016-9367-9.
[92] A. Behroozfar, S. Daryadel, S.R. Morsali, S. Moreno, M. Baniasadi, R.A. Bernal, M.

Minary-Jolandan, Microscale 3D Printing of Nanotwinned Copper, Adv. Mater. 30
(2018) 1–6. https://doi.org/10.1002/adma.201705107.
[93] D. Gu, Y.C. Hagedorn, W. Meiners, G. Meng, R.J.S. Batista, K. Wissenbach, R.

Poprawe, Densification behavior, microstructure evolution, and wear performance of
selective laser melting processed commercially pure titanium, Acta Mater. 60 (2012)
3849–3860. https://doi.org/10.1016/j.actamat.2012.04.006.
[94] J.M. C. zasopismo W Żórawski, J Sienicki, S Kowalski, Additive manufacturing of

titanium with application of cold spray process, Tech. Trans. 10 (2018) 201–208.
https://doi.org/10.4467/2353737xct.18.158.9308.
[95] N.M. Everitt, N.T. Aboulkhair, I. Maskery, C.J. Tuck, I. Ashcroft, Nanoindentation
shows uniform local mechanical properties across melt pools and layers produced by
selective laser melting of AlSi 10Mg alloy, Adv. Mater. Lett. 7 (2016) 13–16.
https://doi.org/10.5185/amlett.2016.6171.
[96] M. Munther, T. Palma, F. Tavangarian, A. Beheshti, K. Davami, Nanomechanical

properties of additively and traditionally manufactured nickel-chromium-based
superalloys through instrumented nanoindentation, Manuf. Lett. 23 (2020) 39–43.
https://doi.org/10.1016/j.mfglet.2019.09.003.
118
[97] M.J. Uddin, E. Ramirez-Cedillo, R.A. Mirshams, H.R. Siller, Nanoindentation and
electron backscatter diffraction mapping in laser powder bed fusion of stainless steel
316L, Mater. Charact. 174 (2021) 111047.
[98] P. Hosemann, C. Shin, D. Kiener, Small scale mechanical testing of irradiated materials,
J. Mater. Res. 30 (2015) 1231–1245. https://doi.org/10.1557/jmr.2015.26.
[99] B. AlMangour, J.M. Yang, Improving the surface quality and mechanical properties by
shot-peening of 17-4 stainless steel fabricated by additive manufacturing, Mater. Des.
110 (2016) 914–924. https://doi.org/10.1016/j.matdes.2016.08.037.
[100] C.-H. Shiau, C. Sun, M. McMurtrey, R. O’Brien, F.A. Garner, L. Shao, Orientation-
selected micro-pillar compression of additively manufactured 316L stainless steels:
comparison of as-manufactured, annealed, and proton-irradiated variants, J. Nucl. Mater.
(2022) 153739. https://doi.org/10.1016/j.jnucmat.2022.153739.
[101] X. Wang, B. Zheng, K. Yu, S. Jiang, E.J. Lavernia, J.M. Schoenung, The role of cell
boundary orientation on mechanical behavior: A site-specific micro-pillar
characterization study, Addit. Manuf. 46 (2021) 102154.
https://doi.org/10.1016/j.addma.2021.102154.
[102] J. Menčík, Uncertainties and Errors in Nanoindentation, in: 2012.
[103] J.F. Ziegler, M.D. Ziegler, J.P. Biersack, SRIM - The stopping and range of ions in
matter (2010), Nucl. Instruments Methods Phys. Res. Sect. B Beam Interact. with Mater.
Atoms. 268 (2010) 1818–1823. https://doi.org/10.1016/j.nimb.2010.02.091.
[104] J.M. Young, S. Singh, T.A. Byers, D.C. Jones, B. Rout, Synthesis of crystalline phases in
space silicate analogues with helium ion irradiation, Nucl. Instruments Methods Phys.
Res. Sect. B Beam Interact. with Mater. Atoms. 443 (2019) 79–83.
https://doi.org/10.1016/j.nimb.2019.01.052.
[105] T.H. Pham, J.J. Kim, S.E. Kim, Estimating constitutive equation of structural steel using
indentation, Int. J. Mech. Sci. 90 (2015) 151–161.
https://doi.org/10.1016/j.ijmecsci.2014.11.007.
[106] D. Caillard, J.-L. Martin, Introduction BT - Thermally Activated Mechanisms in Crystal

Plasticity, Therm. Act. Mech. Cryst. Plast. 8 (2003) 3–9.
[107] V. Maier-Kiener, K. Durst, Advanced Nanoindentation Testing for Studying Strain-Rate

Sensitivity and Activation Volume, Jom. 69 (2017) 2246–2255.
https://doi.org/10.1007/s11837-017-2536-y.
[108] S. Vadalakonda, R. Banerjee, A. Puthcode, R. Mirshams, Comparison of incipient

plasticity in bcc and fcc metals studied using nanoindentation, Mater. Sci. Eng. A. 426
(2006) 208–213. https://doi.org/10.1016/j.msea.2006.04.001.
119
[109] A. Gouldstone, H.J. Koh, K.Y. Zeng, A.E. Giannakopoulos, S. Suresh, Discrete and
continuous deformation during nanoindentation of thin films, Acta Mater. 48 (2000)
2277–2295. https://doi.org/10.1016/S1359-6454(00)00009-4.
[110] S.Y. Park, Y.C. Kim, R.S. Ruoff, J.Y. Kim, Incipient plasticity and fully plastic contact
behavior of copper coated with a graphene layer, APL Mater. 7 (2019) 0–5.
https://doi.org/10.1063/1.5086333.
[111] L. Zhao, M. Alam, J. Zhang, R. Janisch, A. Hartmaier, Amorphization-governed elasto-

plastic deformation under nanoindentation in cubic (3C) silicon carbide, Ceram. Int. 46
(2020) 12470–12479. https://doi.org/10.1016/j.ceramint.2020.02.009.
[112] A. Yadollahi, N. Shamsaei, S.M. Thompson, A. Elwany, L. Bian, Effects of building

orientation and heat treatment on fatigue behavior of selective laser melted 17-4 PH
stainless steel, Int. J. Fatigue. 94 (2017) 218–235.
https://doi.org/10.1016/j.ijfatigue.2016.03.014.
[113] Fischer-Cripps AC , Author, Nicholson DW , Reviewer, Nanoindentation. Mechanical

Engineering Series, Appl. Mech. Rev. 57 (2004) B12–B12.
https://doi.org/10.1115/1.1704625.
[114] G.S. Was, Fundamentals of Radiation Materials Science, 2020.

https://doi.org/10.1016/B978-0-12-803581-8.00668-8.
[115] W.D. Nix, H. Gao, Indentation size effects in crystalline materials: A law for strain
gradient plasticity, J. Mech. Phys. Solids. 46 (1998) 411–425.
https://doi.org/10.1016/S0022-5096(97)00086-0.
[116] M.D. Uchic, D.M. Dimiduk, J.N. Florando, W.D. Nix, Sample dimensions influence
strength and crystal plasticity, Science (80-. ). 305 (2004) 986–989.
https://doi.org/10.1126/science.1098993.
[117] K.E. Knipling, D.J. Rowenhorst, R.W. Fonda, G. Spanos, Effects of focused ion beam
milling on austenite stability in ferrous alloys, Mater. Charact. 61 (2010) 1–6.
https://doi.org/DOI:101016/jmatchar200909013.
[118] J.R. Trelewicz, G.P. Halada, O.K. Donaldson, G. Manogharan, Microstructure and
Corrosion Resistance of Laser Additively Manufactured 316L Stainless Steel, Jom. 68
(2016) 850–859. https://doi.org/10.1007/s11837-016-1822-4.
[119] P.K. Samal, I.I.I. Warzel Roland, S.O. Shah, Powder Metallurgy Stainless Steels
Applications, in: Powder Metall., ASM International, 2015.
https://doi.org/10.31399/asm.hb.v07.a0006098.
[120] A. Leicht, C.H. Yu, V. Luzin, U. Klement, E. Hryha, Effect of scan rotation on the
microstructure development and mechanical properties of 316L parts produced by laser
powder bed fusion, Mater. Charact. 163 (2020) 2–10.
120
[121] A. Leicht, M. Rashidi, U. Klement, E. Hryha, Effect of process parameters on the
microstructure, tensile strength and productivity of 316L parts produced by laser powder
bed fusion, Mater. Charact. 159 (2020) 110016.
[122] Y. Song, Q. Sun, K. Guo, X. Wang, J. Liu, J. Sun, Effect of scanning strategies on the
microstructure and mechanical behavior of 316L stainless steel fabricated by selective
laser melting, Mater. Sci. Eng. A. 793 (2020) 139879.
https://doi.org/10.1016/j.msea.2020.139879.
[123] J.J. Marattukalam, D. Karlsson, V. Pacheco, P. Beran, U. Wiklund, U. Jansson, B.

Hjörvarsson, M. Sahlberg, The effect of laser scanning strategies on texture, mechanical
properties, and site-specific grain orientation in selective laser melted 316L SS, Mater.
Des. 193 (2020). https://doi.org/10.1016/j.matdes.2020.108852.
[124] U. Scipioni Bertoli, B.E. MacDonald, J.M. Schoenung, Stability of cellular

microstructure in laser powder bed fusion of 316L stainless steel, Mater. Sci. Eng. A. 739
[125] P. Krakhmalev, G. Fredriksson, K. Svensson, I. Yadroitsev, I. Yadroitsava, M.

Thuvander, R. Peng, Microstructure, solidification texture, and thermal stability of 316 L
stainless steel manufactured by laser powder bed fusion, Metals (Basel). 8 (2018).
https://doi.org/10.3390/met8080643.
[126] J. Suryawanshi, K.G. Prashanth, U. Ramamurty, Mechanical behavior of selective laser

melted 316L stainless steel, Mater. Sci. Eng. A. 696 (2017) 113–121.
[127] D. Wang, C. Song, Y. Yang, Y. Bai, Investigation of crystal growth mechanism during
selective laser melting and mechanical property characterization of 316L stainless steel
parts, Mater. Des. 100 (2016) 291–299. https://doi.org/10.1016/j.matdes.2016.03.111.
[128] Y. Zhong, L. Liu, S. Wikman, D. Cui, Z. Shen, Intragranular cellular segregation network
structure strengthening 316L stainless steel prepared by selective laser melting, J. Nucl.
Mater. 470 (2016) 170–178. https://doi.org/10.1016/j.jnucmat.2015.12.034.
[129] A. Röttger, J. Boes, W. Theisen, M. Thiele, C. Esen, A. Edelmann, R. Hellmann,

Microstructure and mechanical properties of 316L austenitic stainless steel processed by
different SLM devices, Int. J. Adv. Manuf. Technol. 108 (2020) 769–783.
https://doi.org/10.1007/s00170-020-05371-1.
[130] A. Aggarwal, S. Patel, A. Kumar, Selective Laser Melting of 316L Stainless Steel:
Physics of Melting Mode Transition and Its Influence on Microstructural and Mechanical
Behavior, Jom. 71 (2019) 1105–1116. https://doi.org/10.1007/s11837-018-3271-8.
[131] P. Lu, Z. Cheng-Lin, W. Liang, L. Tong, L. Xiao-Cheng, Research on mechanical

properties and microstructure by selective laser melting of 316L stainless steel, Mater.
Res. Express. 6 (2019). https://doi.org/10.1088/2053-1591/ab6b67.
121
[132] X. qing Ni, D. cheng Kong, Y. Wen, L. Zhang, W. heng Wu, B. bei He, L. Lu, D. xiang
Zhu, Anisotropy in mechanical properties and corrosion resistance of 316L stainless steel
fabricated by selective laser melting, Int. J. Miner. Metall. Mater. 26 (2019) 319–328.
https://doi.org/10.1007/s12613-019-1740-x.
[133] A. Leicht, U. Klement, E. Hryha, Effect of build geometry on the microstructural

development of 316L parts produced by additive manufacturing, Mater. Charact. 143
(2018) 137–143. https://doi.org/10.1016/j.matchar.2018.04.040.
[134] M.S. Pham, B. Dovgyy, P.A. Hooper, Twinning induced plasticity in austenitic stainless
steel 316L made by additive manufacturing, Mater. Sci. Eng. A. 704 (2017) 102–111.
[135] W.M. Tucho, V.H. Lysne, H. Austbø, A. Sjolyst-Kverneland, V. Hansen, Investigation of

effects of process parameters on microstructure and hardness of SLM manufactured
SS316L, J. Alloys Compd. 740 (2018) 910–925.
https://doi.org/10.1016/j.jallcom.2018.01.098.
[136] O. Andreau, I. Koutiri, P. Peyre, J.D. Penot, N. Saintier, E. Pessard, T. De Terris, C.

Dupuy, T. Baudin, Texture control of 316L parts by modulation of the melt pool
morphology in selective laser melting, J. Mater. Process. Technol. 264 (2019) 21–31.
https://doi.org/10.1016/j.jmatprotec.2018.08.049.
[137] M. Alnajjar, F. Christien, K. Wolski, C. Bosch, Evidence of austenite by-passing in a

stainless steel obtained from laser melting additive manufacturing, Addit. Manuf. 25
(2019) 187–195. https://doi.org/10.1016/j.addma.2018.11.004.
[138] A. Sathyanath, A. Meena, Microstructural evolution and strain hardening behavior of

heat-treated 17-4 PH stainless steel, Mater. Today Commun. 25 (2020) 101416.
https://doi.org/10.1016/j.mtcomm.2020.101416.
[139] S.D. Meredith, J.S. Zuback, J.S. Keist, T.A. Palmer, Impact of composition on the heat
treatment response of additively manufactured 17–4 PH grade stainless steel, Mater. Sci.
Eng. A. 738 (2018) 44–56. https://doi.org/10.1016/j.msea.2018.09.066.
[140] S. Vunnam, A. Saboo, C. Sudbrack, T.L. Starr, Effect of powder chemical composition
on the as-built microstructure of 17-4 PH stainless steel processed by selective laser
melting, Addit. Manuf. 30 (2019) 100876. https://doi.org/10.1016/j.addma.2019.100876.
[141] U. Ali, R. Esmaeilizadeh, F. Ahmed, D. Sarker, W. Muhammad, A. Keshavarzkermani,

Y. Mahmoodkhani, E. Marzbanrad, E. Toyserkani, Identification and characterization of
spatter particles and their effect on surface roughness, density and mechanical response
of 17-4 PH stainless steel laser powder-bed fusion parts, Mater. Sci. Eng. A. 756 (2019)
98–107. https://doi.org/10.1016/j.msea.2019.04.026.
[142] T.H. Hsu, Y.J. Chang, C.Y. Huang, H.W. Yen, C.P. Chen, K.K. Jen, A.C. Yeh,
Microstructure and property of a selective laser melting process induced oxide dispersion
122
strengthened 17-4 PH stainless steel, J. Alloys Compd. 803 (2019) 30–41.
[143] Y. Sun, R.J. Hebert, M. Aindow, Effect of heat treatments on microstructural evolution of
additively manufactured and wrought 17-4PH stainless steel, Mater. Des. 156 (2018)
429–440. https://doi.org/10.1016/j.matdes.2018.07.015.
[144] X. Xiao, L. Yu, Cross-sectional nano-indentation of ion-irradiated steels: Finite element

simulations based on the strain-gradient crystal plasticity theory, Int. J. Eng. Sci. 143
(2019) 56–72. https://doi.org/10.1016/j.ijengsci.2019.06.015.
[145] F. Röder, C. Heintze, S. Pecko, S. Akhmadaliev, F. Bergner, A. Ulbricht, E. Altstadt,

Nanoindentation of ion-irradiated reactor pressure vessel steels–model-based
interpretation and comparison with neutron irradiation, Philos. Mag. 98 (2018) 911–933.
https://doi.org/10.1080/14786435.2018.1425007.
[146] X.F. Liu, C.K. Tse, Impact of degree mixing pattern on consensus formation in social
networks, Phys. A Stat. Mech. Its Appl. 407 (2014) 1–6.
https://doi.org/10.1016/j.physa.2014.03.086.
[147] E. Ramirez-Cedillo, M.J. Uddin, J.A. Sandoval-Robles, R.A. Mirshams, L. Ruiz-Huerta,

C.A. Rodriguez, H.R. Siller, Process planning of L-PBF of AISI 316L for improving
surface quality and relating part integrity with microstructural characteristics, Surf.
Coatings Technol. 396 (2020) 125956. https://doi.org/10.1016/j.surfcoat.2020.125956.
[148] H. Irrinki, M. Dexter, B. Barmore, R. Enneti, S. Pasebani, S. Badwe, J. Stitzel, R.

Malhotra, S. V. Atre, Effects of Powder Attributes and Laser Powder Bed Fusion (L-
PBF) Process Conditions on the Densification and Mechanical Properties of 17-4 PH
Stainless Steel, Jom. 68 (2016) 860–868. https://doi.org/10.1007/s11837-015-1770-4.
[149] H. Irrinki, S.D. Nath, M. Alhofors, J. Stitzel, O. Gulsoy, S. V. Atre, Microstructures,

properties, and applications of laser sintered 17-4PH stainless steel, J. Am. Ceram. Soc.
102 (2019) 5679–5690. https://doi.org/10.1111/jace.16372.
[150] J. Hay, Strain-Rate Sensitivity of Thin Metal Films by Instrumented Indentation

Application Note, (n.d.) 1–8.
[151] M. Alnajjar, F. Christien, K. Wolski, C. Bosch, Evidence of austenite by-passing in a

stainless steel obtained from laser melting additive manufacturing, Addit. Manuf. 25
(2019) 187–195. https://doi.org/10.1016/j.addma.2018.11.004.
[152] X. Lin, Y. Cao, X. Wu, H. Yang, J. Chen, W. Huang, Microstructure and mechanical
properties of laser forming repaired 17-4PH stainless steel, Mater. Sci. Eng. A. 553
[153] T.H. Hsu, Y.J. Chang, C.Y. Huang, H.W. Yen, C.P. Chen, K.K. Jen, A.C. Yeh,
Microstructure and property of a selective laser melting process induced oxide dispersion
123
strengthened 17-4 PH stainless steel, J. Alloys Compd. 803 (2019) 30–41.
[154] S. Takaki, K. Fukunaga, J. Syarif, T. Tsuchiyama, Effect of grain refinement on thermal

stability of metastable austenitic steel, Mater. Trans. 45 (2004) 2245–2251.
https://doi.org/10.2320/matertrans.45.2245.
[155] H.K. Rafi, D. Pal, N. Patil, T.L. Starr, B.E. Stucker, Microstructure and Mechanical
Behavior of 17-4 Precipitation Hardenable Steel Processed by Selective Laser Melting, J.
Mater. Eng. Perform. 23 (2014) 4421–4428. https://doi.org/10.1007/s11665-014-1226-y.
[156] J.S. Weaver, J. Whiting, V. Tondare, C. Beauchamp, M. Peltz, J. Tarr, T.Q. Phan, M.A.
Donmez, The effects of particle size distribution on the rheological properties of the
powder and the mechanical properties of additively manufactured 17-4 PH stainless steel,
Addit. Manuf. 39 (2021) 101851. https://doi.org/10.1016/j.addma.2021.101851.
[157] S. Vunnam, S. Dobson, A. Saboo, D. Frankel, C. Sudbrack, T.L. Starr, Effect of Powder
Chemical Composition on Microstructures and, (2019) 463–477.
[158] L. Zai, C. Zhang, Y. Wang, W. Guo, D. Wellmann, X. Tong, Y. Tian, Laser powder bed
fusion of precipitation-hardened martensitic stainless steels: A review, Metals (Basel). 10
(2020). https://doi.org/10.3390/met10020255.
[159] S. Suwas, R.K. Ray, Crystallographic Texture of Materials, Springer London, 2016.
https://books.google.com/books?id=nstbvgAACAAJ.
[160] A. Kudzal, B. McWilliams, C. Hofmeister, F. Kellogg, J. Yu, J. Taggart-Scarff, J. Liang,

Effect of scan pattern on the microstructure and mechanical properties of Powder Bed
Fusion additive manufactured 17-4 stainless steel, Mater. Des. 133 (2017) 205–215.
[161] P. Leo, M. Cabibbo, A. Del Prete, S. Giganto, S. Martínez-Pellitero, J. Barreiro, Laser

defocusing effect on the microstructure and defects of 17-4ph parts additively
manufactured by slm at a low energy input, Metals (Basel). 11 (2021).
https://doi.org/10.3390/met11040588.
[162] H.R. Lashgari, Y. Xue, C. Onggowarsito, C. Kong, S. Li, Microstructure, Tribological

Properties and Corrosion Behaviour of Additively Manufactured 17-4PH Stainless Steel:
Effects of Scanning Pattern, Build Orientation, and Single vs. Double scan, Mater. Today
Commun. 25 (2020). https://doi.org/10.1016/j.mtcomm.2020.101535.
[163] H. Irrinki, J.S.D. Jangam, S. Pasebani, S. Badwe, J. Stitzel, K. Kate, O. Gulsoy, S. V.

Atre, Effects of particle characteristics on the microstructure and mechanical properties
of 17-4 PH stainless steel fabricated by laser-powder bed fusion, Powder Technol. 331
(2018) 192–203. https://doi.org/10.1016/j.powtec.2018.03.025.
124
[164] J. Lin, F. Chen, X. Tang, J. Liu, S. Shen, G. Ge, Radiation-induced swelling and
hardening of 316L stainless steel fabricated by selected laser melting, Vacuum. 174
(2020) 109183. https://doi.org/10.1016/j.vacuum.2020.109183.
[165] T.H. Hsu, P.C. Huang, M.Y. Lee, K.C. Chang, C.C. Lee, M.Y. Li, C.P. Chen, K.K. Jen,
A.C. Yeh, Effect of processing parameters on the fractions of martensite in 17-4 PH
stainless steel fabricated by selective laser melting, J. Alloys Compd. 859 (2021) 157758.
https://doi.org/10.1016/j.jallcom.2020.157758.
[166] B.S. Hengfeng Gu*, Haijun Gong*, Deepankar Pal*, Khalid Rafi*, Thomas Starr†,
Influences of Energy Density on Porosity and Microstructure of Selective Laser Melted
17- 4PH Stainless Steel, Mater. Sci. (2013) 117-99 ‫ ;ص‬8 ‫ﺷﻤﺎره‬.
[167] R. Rashid, S.H. Masood, D. Ruan, S. Palanisamy, R.A. Rahman Rashid, M. Brandt,
Effect of scan strategy on density and metallurgical properties of 17-4PH parts printed by
Selective Laser Melting (SLM), J. Mater. Process. Technol. 249 (2017) 502–511.
https://doi.org/10.1016/j.jmatprotec.2017.06.023.
[168] S. Romano, P.D. Nezhadfar, N. Shamsaei, M. Seifi, S. Beretta, High cycle fatigue
behavior and life prediction for additively manufactured 17-4 PH stainless steel: Effect of
sub-surface porosity and surface roughness, Theor. Appl. Fract. Mech. 106 (2020).
https://doi.org/10.1016/j.tafmec.2020.102477.
[169] D. Basu, Z. Wu, J.L.L. Meyer, E. Larson, R. Kuo, A. Rollett, Entrapped Gas and Process
Parameter-Induced Porosity Formation in Additively Manufactured 17-4 PH Stainless
Steel, J. Mater. Eng. Perform. (2021). https://doi.org/10.1007/s11665-021-05695-3.
[170] Z. Wu, D. Basu, J.L.L. Meyer, E. Larson, R. Kuo, J. Beuth, A. Rollett, Study of Powder
Gas Entrapment and Its Effects on Porosity in 17-4 PH Stainless Steel Parts Fabricated in
Laser Powder Bed Fusion, Jom. 73 (2021) 177–188. https://doi.org/10.1007/s11837-020-
04491-z.
[171] H. Gu, H. Gong, D. Pal, K. Rafi, T. Starr, B. Stucker, Influences of Energy Density on
Porosity and Microstructure of Selective Laser Melted 17-4PH Stainless Steel, in: 2013.
[172] Z. Li, T. Voisin, J.T. McKeown, J. Ye, T. Braun, C. Kamath, W.E. King, Y.M. Wang,
Tensile properties, strain rate sensitivity, and activation volume of additively
manufactured 316L stainless steels, Int. J. Plast. 120 (2019) 395–410.
https://doi.org/10.1016/j.ijplas.2019.05.009.
[173] B. Merle, W.H. Higgins, G.M. Pharr, Critical issues in conducting constant strain rate
nanoindentation tests at higher strain rates, J. Mater. Res. (2019).
https://doi.org/10.1557/jmr.2019.292.
[174] M. Zhang, J. Li, B. Tang, H. Kou, J. Fan, Mechanical characterization and strain-rate
sensitivity measurement of Ti-7333 alloy based on nanoindentation and crystal plasticity
modeling, Prog. Nat. Sci. Mater. Int. 28 (2018) 718–723.
https://doi.org/10.1016/j.pnsc.2018.10.003.
125
[175] X. Wang, Y. Liu, T. Shi, Y. Wang, Strain rate dependence of mechanical property in a
selective laser melted 17–4 PH stainless steel with different states, Mater. Sci. Eng. A.
792 (2020) 139776. https://doi.org/10.1016/j.msea.2020.139776.
[176] L. Tian, Z.M. Jiao, G.Z. Yuan, S.G. Ma, Z.H. Wang, H.J. Yang, Y. Zhang, J.W. Qiao,
Effect of Strain Rate on Deformation Behavior of AlCoCrFeNi High-Entropy Alloy by
Nanoindentation, J. Mater. Eng. Perform. 25 (2016) 2255–2260.
https://doi.org/10.1007/s11665-016-2082-8.
[177] T. LEBRUN, K. TANIGAKI, K. HORIKAWA, H. KOBAYASHI, Strain rate sensitivity

and mechanical anisotropy of selective laser melted 17-4 PH stainless steel, Mech. Eng.
J. 1 (2014) SMM0049–SMM0049. https://doi.org/10.1299/mej.2014smm0049.
[178] A. Nawaz, W.G. Mao, C. Lu, Y.G. Shen, Mechanical properties, stress distributions and
nanoscale deformation mechanisms in single crystal 6H-SiC by nanoindentation, J.
Alloys Compd. 708 (2017) 1046–1053. https://doi.org/10.1016/j.jallcom.2017.03.100.
[179] S.R. Jian, J.Y. Juang, Y.S. Lai, Cross-sectional transmission electron microscopy
observations of structural damage in Al0.16Ga0.84N thin film under contact loading, J.
Appl. Phys. 103 (2008). https://doi.org/10.1063/1.2836939.
[180] S. Sinha, R.A. Mirshams, T. Wang, S.S. Nene, M. Frank, K. Liu, R.S. Mishra,
Nanoindentation behavior of high entropy alloys with transformation-induced plasticity,
Sci. Rep. 9 (2019) 1–11. https://doi.org/10.1038/s41598-019-43174-x.
[181] C.K. Dolph, D.J. da Silva, M.J. Swenson, J.P. Wharry, Plastic zone size for
nanoindentation of irradiated Fe—9%Cr ODS, J. Nucl. Mater. 481 (2016) 33–45.
[182] W.B. Lee, Y.P. Chen, Simulation of micro-indentation hardness of FCC single crystals
by mechanism-based strain gradient crystal plasticity, Int. J. Plast. 26 (2010) 1527–1540.
https://doi.org/10.1016/j.ijplas.2010.01.011.
[183] H. Fei, A. Abraham, N. Chawla, H. Jiang, Evaluation of micro-pillar compression tests

for accurate determination of elastic-plastic constitutive relations, J. Appl. Mech. Trans.
ASME. 79 (2012) 1–9. https://doi.org/10.1115/1.4006767.
[184] H. Li, T. Zhu, N. Takata, M. Kobashi, M. Yoshino, Thermal activation process of plastic
deformation in Fe–18Cr single-crystal micropillars with high-density dislocations, Mater.
Sci. Eng. A. 819 (2021) 141459. https://doi.org/10.1016/j.msea.2021.141459.
[185] R. Niu, X. An, L. Li, Z. Zhang, Y.W. Mai, X. Liao, Mechanical properties and
deformation behaviours of submicron-sized Cu–Al single crystals, Acta Mater. 223
(2022). https://doi.org/10.1016/j.actamat.2021.117460.
[186] C.D. Hardie, S.G. Roberts, Nanoindentation of model Fe-Cr alloys with self-ion
irradiation, J. Nucl. Mater. 433 (2013) 174–179.
126
[187] Z. Jiao, G.S. Was, Impact of localized deformation on IASCC in austenitic stainless
steels, J. Nucl. Mater. 408 (2011) 246–256.
[188] A. Reichardt, A. Lupinacci, D. Frazer, N. Bailey, H. Vo, C. Howard, Z. Jiao, A.M.

Minor, P. Chou, P. Hosemann, Nanoindentation and in situ microcompression in different
dose regimes of proton beam irradiated 304 SS, J. Nucl. Mater. 486 (2017) 323–331.
[189] C.M. Sánchez Camargo, Mechanical multi-scale characterization of metallic materials by

nanoindentation test, 2019. http://www.theses.fr/2019ESAE0010/document.
[190] D. Tumbajoy-Spinel, S. Descartes, J.M. Bergheau, V. Lacaille, G. Guillonneau, J.

Michler, G. Kermouche, Assessment of mechanical property gradients after impact-based
surface treatment: Application to pure α-iron, Mater. Sci. Eng. A. 667 (2016) 189–198.
[191] L.J. Yu, H.W. Yen, J.Y. Wu, J.J. Yu, C.R. Kao, Micromechanical behavior of single
crystalline Ni3Sn4 in micro joints for chip-stacking applications, Mater. Sci. Eng. A. 685
[192] I.N. Sneddon, The relation between load and penetration in the axisymmetric boussinesq
problem for a punch of arbitrary profile, Int. J. Eng. Sci. 3 (1965) 47–57.
https://doi.org/https://doi.org/10.1016/0020-7225(65)90019-4.
[193] J.S. Weaver, S. Pathak, A. Reichardt, H.T. Vo, S.A. Maloy, P. Hosemann, N.A. Mara,
Spherical nanoindentation of proton irradiated 304 stainless steel: A comparison of small
scale mechanical test techniques for measuring irradiation hardening, J. Nucl. Mater. 493
(2017) 368–379. https://doi.org/10.1016/j.jnucmat.2017.06.031.
[194] G. Dehm, B.N. Jaya, R. Raghavan, C. Kirchlechner, Overview on micro- and

nanomechanical testing: New insights in interface plasticity and fracture at small length
scales, Acta Mater. 142 (2018) 248–282. https://doi.org/10.1016/j.actamat.2017.06.019.
[195] Q. Ma, D.R. Clarke, Size dependent hardness of silver single crystals, J. Mater. Res. 10
(1995) 853–863. https://doi.org/DOI: 10.1557/JMR.1995.0853.
[196] J.G. Swadener, E.P. George, G.M. Pharr, The correlation of the indentation size effect
measured with indenters of various shapes, J. Mech. Phys. Solids. 50 (2002) 681–694.
https://doi.org/10.1016/S0022-5096(01)00103-X.
[197] H. Zhang, B.E. Schuster, Q. Wei, K.T. Ramesh, The design of accurate micro-
compression experiments, Scr. Mater. 54 (2006) 181–186.
[198] C. Kirchlechner, J. Keckes, C. Motz, W. Grosinger, M.W. Kapp, J.S. Micha, O. Ulrich,
G. Dehm, Impact of instrumental constraints and imperfections on the dislocation
127
structure in micron-sized Cu compression pillars, Acta Mater. 59 (2011) 5618–5626.
128

Uddin Dissertation 2022

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Uddin Dissertation 2022

Uploaded by

Copyright:

Available Formats

INVESTIGATION OF STRUCTURE-PROPERTY EFFECTS ON NANOINDENTATION

AND SMALL-SCALE MECHANICAL TESTING OF IRRADIATED ADDITIVELY

MANUFACTURED STAINLESS STEELS

Mohammad Jashim Uddin, B.S., M.S.

Dissertation Prepared for the Degree of

UNIVERSITY OF NORTH TEXAS

Hector R. Siller, Major Professor

Nanoindentation and Small-Scale Mechanical Testing of Irradiated Additively Manufactured

pp., 21 tables, 44 figures, 198 numbered references.

mechanical testing of those materials, to investigate how irradiation affects microstructural

(electron backscatter diffraction) mapping is shown to be an alternative methodology for enriching

grains were found to be weaker in terms of indentation properties.

structure-property relationship. Both as-built and irradiated AM 17-4 PH micropillars exhibited

higher loads to initiate plastic deformation as dislocation must overcome irradiation-induced

Mohammad Jashim Uddin

guidance and mentorship throughout my research and dissertation. Additionally, I am so grateful

continuous support and advice in every step of my study.

collaboration, support, and helpful discussions.

ACKNOWLEDGEMENTS ........................................................................................................... iii

LIST OF TABLES ......................................................................................................................... vi

LIST OF FIGURES ..................................................................................................................... viii

CHAPTER 1. INTRODUCTION ................................................................................................... 1

CHAPTER 2. MATERIALS AND EXPERIMENTAL PROCEDURES .................................... 25

CHAPTER 3. RESULTS AND DISCUSSIONS.......................................................................... 45

CHAPTER 4. CONCLUSIONS AND FUTURE WORKS........................................................ 104

REFERENCES ........................................................................................................................... 110

Table 1: A literature review on nanoindentation study of similar AM metallic alloys (MC =

Table 7: XRM Scan parameters .................................................................................................... 44

Table 11: Statistical One-way ANOVA of hardness data ............................................................ 70

Table 12: Statistical One-way ANOVA of indentation modulus data.......................................... 72

Figure 2: Summary of dissertation investigations from AM to small-scale mechanical testing.

Figure 3: Research map with the outline of this study.................................................................. 15

Figure 5: Methodology of the proposal ........................................................................................ 26

Figure 6: Layer-by-layer micro-mechanical properties by small-scale mechanical testing ......... 29

1.1 Additive Manufacturing*

additive manufacturing techniques over traditional techniques is attributed to several advantages

to be fabricated using AM processes as traditional processes are more time-consuming, difficult,

Different additive manufacturing processes are described in the standard ISO-ASTM

contributions. Another growing market in AM is the production of the powder. Commercially

right guidelines, workflow, documentation, and characterization, optimized parameters can be

size of the component, variations in thickness, or the number of components. As microstructure

to be realized [18]. A distinguished advantage of AM techniques is mass customization i.e., the

AM processes remain to be major hurdles that inhibit mass production [19].

Nuclear Regulatory Commission is inspiring scientific communities to perform

investigations to the better understanding of the behavior of irradiated additively manufactured

to degradation, such as the evaluation of stress-corrosion cracking susceptibility, porosity,

crystallography, thermal diffusivity, anisotropy, and chemical heterogeneity, considering that AM

irradiation, is mandatory toward effective materials qualification.

materials at elevated temperatures. Long-term and time-dependent failure mechanisms such as

of the corrosion behavior of AM materials.

the process is fundamental to generate workflow or process guidelines. Firstly, processing

of stresses in all directions [32].

presented most influential parameters P (watts), vs (mm/s), LT (μm), and HD (μm).

in addition to characterization techniques such as porosity analysis, density measurements, and

tensile and hardness tests.

In summary, this dissertation is a package of a new strain-rate sensitivity model,

correlations between process-driven microstructures and micro-mechanical properties, and small-

1.2 Radiation-Resistant Alloys Manufacturing by Laser Powder Bed Fusion (L-PBF)

monitoring of each layer of material as it is manufactured, allowing for improved manufacturing

welding, or soldering) or to create functionally graded compositions, or even fully 3D patterned

phase, grain size, and composition-distributions aimed at optimizing the microstructure-properties

centrifugal contactors for small-scale demonstrations of separation techniques aiming to remove

equipment, pharmaceutical manufacturing, and medical implants. Particularly, the applications of

obtain optimum dynamic properties like fatigue resistance in comparison to conventionally