metals
Article
Effect of HIP Defects on the Mechanical Properties of Additive
Manufactured Ti6Al4V Alloy
Ohad Dolev 1 , Tomer Ron 2, * , Eli Aghion 2
Citation: Dolev, O.; Ron, T.; Aghion,
E.; Shirizly, A. Effect of HIP Defects
on the Mechanical Properties of
Additive Manufactured Ti6Al4V
Alloy. Metals 2022, 12, 1210. https://
doi.org/10.3390/met12071210
Academic Editor: Matteo Benedetti
Received: 7 June 2022
Accepted: 13 July 2022
Published: 17 July 2022
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Copyright: © 2022 by the authors.
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Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Metals 2022, 12, 1210. https://doi.org/10.3390/met12071210
and Amnon Shirizly 1,2
1 Faculty of Mechanical Engineering, Technion, Haifa 3200003, Israel; dolev.ohad@gmail.com (O.D.);
a.shirizly@gmail.com (A.S.)
2 Department of Materials Engineering, Ben-Gurion University of the Negev, P.O. Box 652,
Beer-Sheva 8410501, Israel; egyon@bgu.ac.il
* Correspondence: toron@post.bgu.ac.il
Abstract: The expanding use of Additive Manufacturing (AM) technology enables engineers and
designers to plan and manufacture highly complex geometries that are impossible to manufacture
with any other conventional technology. When comparing this with building parts using powder
bed technology, the main differences found in the quality of the products concern fracture toughness,
fatigue, and inferiority in tensile tests. To overcome these issues, the Hot Isostatic Press (HIP)
procedure may be used to improve the material quality by reducing product porosity. Regarding
fatigue, the standard procedure consists of HIP and the machining of specimens to their final geometry.
However, in many AM parts, geometrical complexity does not enable complementary machining.
Recently, some AM vendors integrated in-process milling capabilities into their machines, in an
attempt to address this challenge. In this study, the authors examine the effect of the HIP procedure
on representative samples in order to demonstrate its effect on the final products of TI-6Al-4V parts.
The results indicate that the fatigue limit of HIPed parts can increase by 12%; however, a dramatic
decrease in the fatigue limit was observed if any failure in the HIP process occurred. The authors
suggest an optional procedure to improve performance in such cases.
Keywords: Selective Laser Melting (SLM); Ti-6Al-4V; fatigue; fracture toughness; Hot Isostatic
Press (HIP)
1. Introduction
The high strength and the high specific strength of Ti-6Al-4V alloy at moderate and
elevated temperatures, along with its excellent corrosion resistance, have led to its exten-
sive use in the automotive and aerospace industry sectors [1–3]. Mirgal et al. [4] describe
titanium as “the metal for the 21st Century” due to its superior strength and density in
comparison to other materials used in the automotive industry. This extensive use of
titanium has contributed to its implementation within AM technologies. The variety of AM
processes and technologies (for example: powder bed fusion (PBF), laser bed fusion [5,6],
electron beam AM (EBAM) [7–9], powder deposition (PB) [10], wire deposition [11–13],
etc.) are promising new methods for extremely complex geometries [14–16]. The use
of AM technology was first regarded as a rapid prototyping technology aiming to assist
engineers in design and to speed up product development on the path to production. Over
time, AM technologies have emerged and matured, demonstrating process advantages
along with superior physical and mechanical properties. Interest in AM technologies has
increased along with the demand for final parts. While the standards for conventionally
manufactured TI-6Al-4V part tensile properties [17], fracture toughness [18], fatigue per-
formance [19] and other properties are familiar and satisfy guidelines for testing, only a
few standards are available for AM parts, and they are still under development via ASTM
F42 committees [20,21]. Beretta and Romano [22] performed a comprehensive literature
review comparing AM products with those produced using traditional manufacturing
https://www.mdpi.com/journal/metals
Metals 2022, 12, 1210 2 of 11

processes; they emphasized the fatigue properties of AISi10Mg and Ti-6Al-4V and the ap-
parent sensitivity with regard to defects and inhomogeneity in AM parts. Wycisk et al. [23]
presented a simulation and analysis of crack propagation and fatigue results on defective
samples with porosity and surface defects. They showed that the endurance limits of the
as-built samples were significantly lower than for polished specimens. Ganor et al. [24]
and Tiferet et al. [25] used a powder bed electron beam melting technology for Ti-6Al-4V
and performed HIP according to ASTM F2924 [26]; they showed an increase in the bulk
density and a drastically improved elongation by almost 200%, with a slight decrease in
the yield and ultimate strengths. Previous investigation into fatigue data for SLM and
EBM Ti-6AL-4V was summarized by Quintus Technologies AB and Oak Ridge National
Laboratory [27] and relayed in Leuders et al.’s study [28]. The HIPed specimens’ fatigue
limit was significantly improved from below 300 MPa to 550 MPa at 107 cycles. Gün-
ther et al. [29] reported that the HIP process improved the fatigue performance of EBM
and Selective Laser Melting (SLM), and it was similar to that of a conventional Ti-6Al-4V
material. Sanaei and Fatemi [30] published a comprehensive review on defects in the AM
of metals and their effect on fatigue performance; they observed that the pore size and
location affect fatigue life and that for “machined surface specimens, defects dominated the
fatigue performance and by reducing defects after HIP microstructural inhomogeneities
mainly affected the fatigue performance”. Fracture toughness is another key factor in
understanding the qualities of the material and the parts. Horiya and Kishi [31] studied the
fracture toughness of conventionally manufactured titanium alloys and set guidelines for
improving the fracture toughness. They reported that, for the same titanium alloys, the KIC
value widely varies at the same tensile strength and generally improves with coarsening
microstructure. Dhansay et al. [32] studied the fatigue and fracture toughness and crack
propagation of Ti-6Al-4V in SLM samples at two orientations. They indicated that with
stress-relieving heat treatments, the fracture mechanics parameters of fatigue and fracture
toughness had a strong correlation between conventional Ti-6Al-4V and SLM samples
produced with EOSINT M280. The fracture toughness outcome of Dhansay et al. is higher
than for the data reported by Hooreweder et al. [33].
In this study, the influence of post-processing on parts made by Ti-6Al-4V manufac-
tured by an AM SLM technique was investigated. The paper focuses on the effect of the HIP
process and its role as a key factor for reducing defects and improving fracture toughness
and fatigue limits. The experimental procedure and the results of various post-processing
operations are explained in detail to emphasize the importance of the final manufacturing
procedures and their possible effect on the final products.

2. Materials and Methods

Specimens of Ti-6Al-4V alloy were built by direct metal AM (DMLS) using an EOS
M280 powder bed machine (EOS, Krailling, Germany) equipped with a 200 W Nd-YAG laser
with a beam diameter of 80 microns. The samples were fabricated using 30-micron layers of
TI-6Al-4V powder with a size distribution between 20 and 63 microns. All specimens were
produced by adopting standard parameters given by the machine manufacturer, and were
manufactured along the Z-direction according to the ISO/ASTM52921-13 standard [21] with
the aim of examining the critical direction of the parts. The chemical composition of LPW
powder shown in Table 1 was analyzed by X-ray fluorescence (XRF) (ARL PERFORM0 X,
Thermo Fisher Scientific, Waltham, MA, USA) for the metal’s compositions and inert gas
fusion (IGF) (LECO, St. Joseph, MI, USA) for hydrogen quantitative content of gases. The
composition is similar to ASTM F2924 [26].
Metals 2022, 12, 1210 3 of 11

Table 1. The chemical composition of the Ti-6Al-4V powder used for samples preparation.
Metals 2022, 12, x FOR PEER REVIEW 3 of 12
Composition [%] Al V Fe O C N H Y Ti
LPW powder 6.38 3.98 0.18 0.09 0.014 0.014 0.0011 <0.0003 Bal.
ASTM F2924 Up to Up to Up to Up to
5.50–6.75 3.50–4.50
5.50– Up to 0.30
Up to UpUp
to 0.20
to Up to Up to Bal.
requirement
ASTM F2924 [24]
requirement [24] 3.50–4.50 Up0.08
to 0.08 0.05 0.015 Up0.005
to 0.005 Bal.
6.75 0.30 0.20 0.05 0.015
The
The parts
parts were
were stress-relieved
stress-relieved by by heat
heat treatment
treatment at at aa temperature
temperature ofof 650
650 °C
◦ C for
for 33 hh
under a 5 10− 5 [Tor] vacuum atmosphere prior to their separation from
under a 5 × 10 [Tor] vacuum atmosphere prior to their separation from the Ti-6Al-4V base the Ti-6Al-4V
base
plate.plate. In order
In order to evaluate
to evaluate the influence
the influence of theof thetreatment
HIP HIP treatment on mechanical
on mechanical proper-
properties, the
ties, the specimens were divided into two groups—the first was left as
specimens were divided into two groups—the first was left as it was, and the second was it was, and the
second
HIPed. was HIPed.
Tensile, Tensile,
fracture fractureand
toughness, toughness, andspecimens
fatigue test fatigue test specimens
were machined were machined
to the desired
to the desired geometries out of the first group as follows: (Figure 1a—tensile
geometries out of the first group as follows: (Figure 1a—tensile samples in accordance with samples in
accordance with ASTM E8 [17], Figure 1b—Compact-Tension (CT25)
ASTM E8 [17], Figure 1b—Compact-Tension (CT25) specimen in accordance with ASTM specimen in accord-
ance with[18],
E399-17 ASTMandE399-17 [18], and Figure
Figure 1c—fatigue 1c—fatigue
samples following samples
ASTMfollowing ASTM E466 [19]).
E466 [19]).

Geometriesand
Figure 1.1.Geometries
Figure and dimensions
dimensions of of samples:
samples: (a) tensile
(a) tensile samples
samples (ASTM
(ASTM E8),Compact-Ten-
E8), (b) (b) Compact-
Tension (CT25) specimen (ASTM E399-17), (c) fatigue samples (ASTM
sion (CT25) specimen (ASTM E399-17), (c) fatigue samples (ASTM E466). E466).

The second
The second group
group of of specimens
specimenswere
wereHIP-treated
HIP-treatedininaa1000
1000bar
barunder
underargon
argonenviron-
environ-
ment for 2 h at 920 ± 10 ◦ C with a controlled up-and-down temperature slope, as shown
ment for 2 h at 920 ± 10 °C with a controlled up-and-down temperature slope, as shown
◦ C is in the middle of the recommended range of the
in Figure
in Figure 2.2. The
The temperature
temperature of of 920
920 °C is in the middle of the recommended range of the
given standard
given standard [24].
[24]. In
In addition,
addition,according
accordingtotoprevious studies
previous that
studies examined
that thethe
examined influence
influ-
of the HIP temperature on the mechanical properties, the recommended HIP temperature
ence of◦ the HIP temperature on the mechanical properties, the recommended HIP tem-
is 920 C with 2 h 1000 bar [24,25]. The tensile and CT25 samples were then machined,
perature is 920 °C with 2 h 1000 bar [24,25]. The tensile and CT25 samples were then ma-
while the fatigue samples were machined after the HIPing process in order to be correlated
chined, while the fatigue samples were machined after the HIPing process in order to be
with the final complicated AM parts. A schematic illustration of the sample preparation is
correlated with the final complicated AM parts. A schematic illustration of the sample
shown in Figure 3.
preparation is shown in Figure 3.
 Metals 2022,12,
Metals 12, xFOR
FORPEER
PEERREVIEW
REVIEW 4 4ofof 12
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2022, 12,x1210 4 of12
11

Figure The
Figure2.2.2.The HIPed
TheHIPed temperature
HIPedtemperature and
temperatureand pressure
andpressure over
pressureover time.
overtime.
time.
Figure

Figure3.3.3.Schematic
Figure
Figure Schematicillustration
Schematic illustrationofof
illustration ofthe
thepost-process
the post-processsample
post-process samplepreparations.
sample preparations.
preparations.

Thetensile
The
The tensiletests
tensile testswere
wereperformed
performed
performedfor for as-built
foras-built
as-built stress
stress
stress relief
relief
relief samples,
samples,
samples, and
andand after HIP,
after
after 33
HIP,
HIP,
3samples
samples
samples were
werewere tested.
tested.
tested. The
The The tensile test
tensiletest
tensile wascarried
testwas carriedout outaccording
out accordingto
according toASTM
to ASTME8/E8M-16a
ASTM E8/E8M-16a
E8/E8M-16a
StandardTest
Standard
Standard TestMethods
Test Methods
Methods forfor
for Tension
Tension
Tension Testing
Testing
Testing ofofMetallic
Metallic
of Metallic Materials
Materialsat 24at◦atC2424
Materials °Ctemperature,
temperature,
temperature,
°C using
using
an an
Instron Instron
8802 8802
testing testing
machine machine
(250 kN (250 kN
loadcell) loadcell)
and an and an
Instron
using an Instron 8802 testing machine (250 kN loadcell) and an Instron 2620-602 exten- Instron
2620-602 2620-602 exten-
extensometer.
The tensile
someter.
someter. The
The test crosshead
tensile
tensile test speed was
testcrosshead
crosshead speed1 mm
speed was
was per minute.
1 1mm
mmper The elongation
perminute.
minute. was measured
Theelongation
The elongation wasmeas-
was on
meas-
25 mm
ured on(about
25 mm 4 times
(about the
4 diameter
times the of the
diameter specimens).
ured on 25 mm (about 4 times the diameter of the specimens). of the specimens).
All
All fracture
Allfracture toughness
toughnesstests
fracturetoughness tests were
tests were
were carried
carried
carried out according
out
out according
according to to
the ASTM
tothe
theASTM
ASTM E399 Standard
E399
E399 Test
Standard
Standard
Method
TestMethod
Test for Linear-Elastic
Method forLinear-Elastic
for Plane-Strain
Linear-Elastic Fracture
Plane-Strain
Plane-Strain Toughness
Fracture
Fracture KICKIC
Toughness
Toughness of Metallic
KIC ofofMetallicMaterials.
Metallic The
Materials.
Materials.
test
The includes
test fatigue
includes crack
fatigue initiation
crack and
initiation propagation
and from
propagation a notch
from a
The test includes fatigue crack initiation and propagation from a notch and static loadingand
notch static
and loading
static up to
loading
Metals 2022, 12, 1210 5 of 11

fracture, including determination of the fracture load. The pre-cracking loading was carried
out using an Instron 8801 testing machine (Dynacell, Dynamic Load Cell +/− 100 kN)
under load control with a sinusoidal waveform in air at 22 ± 3 ◦ C and at 15 Hz frequency.
The cyclic loading of the fatigue pre-cracking was applied with the load ratio R = 0.1 and a
maximum load of 3 kN (200–500 K cycles). The maximum stress intensity in the terminal
(2.5 %) stage of fatigue crack growth did not exceed 80% of the estimated KIC of the material.
The crack propagation was monitored using a crack opening displacement gage (COD gage)
and by visually examining crack growth on the sides of the specimens. Two sets of compact
type CT25 samples were prepared and tested for mode I fracture toughness: the as-built
stress relief and HIPed specimens. In both cases, the final machined geometry was carried
out prior to the tests and complied with the ASTM E399 standard [18]. The specimen
notches were parallel to the built plate and perpendicular to the building direction, in order
to examine the weak direction of the parts.
The fatigue sample preparation (according to ASTM E399-17) included building cylin-
ders, heat treatment, and machining to the final geometry (as shown in Figure 1). The
loading cycles were chosen and the fatigue loading was activated. In this process, the
external surface was removed prior to testing. In this procedure, the built material was
examined without any other interference. In this study, the authors intended to evaluate
additional defects that might influence the fatigue limits of the built specimens due to
the HIP process. For this purpose, a set of samples was prepared and tested according to
the ASTM E399-17 [18] standard. The fatigue test was performed according to the ASTM
E466-15 [19] standard with a focus on the high cycle section. A force-controlled constant
amplitude uni-axial loading was carried out using an Instron 8801 testing machine (Dy-
nacell, Dynamic Load Cell +/− 100 kN) under load control with a sinusoidal waveform.
The specimens were fixed using Instron fatigue-rated hydraulic wedge grips and cyclic
loading was applied with the load ratio R = 0.1. The cyclic loading was carried out in an
atmospheric environment at 23 ± 2 ◦ C and 25 Hz frequency up to 107 loading cycles or
until failure occurred. The cyclic loading was performed at several loads to obtain the
fatigue curve and fatigue limit.
To explore the mechanical properties of the final product with or without the HIP,
several samples were produced and tested for fatigue life limits:
i. As built (stress relief and machined);
ii. HIPed and machined—a common procedure according to the fatigue standard;
iii. Machined and HIPed—to resemble complex geometries that cannot machined after
being built.

3. Results and Discussion

3.1. Tensile Tests: Tensile Properties Were Measured in the Build Direction
The tensile test results are shown in Table 2. The as-built stress relief and the HIPed
samples are satisfactory and coincide with the ASTM F2924 [26] standard for Ti-6Al-4V.
When comparing the as-built and HIPed samples, the HIPed elastic modulus and yield
strength were shown to decrease, but are within the standard deviation of the ASTM
requirement, while the elongation and reduction in area increased.

Table 2. Tensile test results of as-built stress relief and HIPed samples.

Elastic Modulus Yield Stress Ultimate Stress Elongation Reduction of

[MPa] [MPa] [MPa] [%] Area [%]
As-built stress relief 111,665 ± 3971 1092.9 ± 7.6 1174.1 ± 6.1 8.7 ± 0.3 29 ± 1.4
As-built stress relief and HIP 109,000 ± 4242 855.9 ± 5.7 949.3 ± 10 15.3 ± 0.6 42.8 ± 2.6
Requirement (ASTM) 113,800 860 920 8
Metals 2022, 12, x FOR PEER REVIEW 6 of 12

Metals 2022, 12, 1210 6 of 11

Requirement
113,800 860 920 8
(ASTM)
3.2. Fracture Toughness
3.2. Fracture toughness
The calculated fracture toughness is given in Table 3. It is noted that the average crack
size isThe calculated
calculated fromfracture toughness
five locations is given
in each in Table
sample. The3. It is noted
average that
crack thewas
size average crack
measured
by SEM,
size as shownfrom
is calculated in Figure 4.
five locations in each sample. The average crack size was measured
by SEM, as shown in Figure 4.
Table 3. Fracture toughness KIC of as-built stress relief and the HIPed samples.
Table 3. Fracture toughness KIC of as-built stress relief and the HIPed samples.
KIC
√
Specimen Average Crack Size [mm] Fracture Load [KN]
Average Crack Fracture Load [MPa K m]IC
Specimen
1 16.92 Size 𝒎𝒎 5.95 𝑲𝑵 𝑴𝑷𝒂√𝒎
53.42 a

2 1 15.97 16.92 8.13 5.95 53.42 a

45.65
2 14.22 15.97 8.13 45.65
3 7.16 41.60 b
As-built stress relief 3 14.22 7.16 41.60 b
As-built stress
4 relief 13.50 8.19 43.21
4 13.50 8.19 43.21
5 13.67 8.28 44.66
5 13.67 8.28 44.66
Average Average 44.544.5
1 1 12.21 12.21 18.36 18.36 83.60
83.60
2 2 13.05 13.05 16.35 16.35 82.51
82.51
As-built stress
3 relief 3 13.67 13.67 15.76 15.76 86.18
86.18 b b

As-built stress relief and HIP and4HIP 414.02 a 14.02 a 14.97 14.97 85.80
85.80
5 13.46 16.00 85.06
5 13.46 16.00 85.06
Average 84.6
Average 84.6
Requirement (ASTM) Annealed plate 75
Requirement (ASTM) Annealed plate 75
Requirement (ASTM) STA plate 42.9
Requirement (ASTM) a STA plate
—The overall crack length (starter notch 42.9 exceeds
and fatigue crack) during the pre-crack operation
athe
—Therecommended value (starter
overall crack length (0.55 Wnotch
max). b—The central flat fracture area was not parallel to the starter
and fatigue crack) during the pre-crack operation exceeds the recom-
value (0.55 W max). b —The central flat fracture area was not parallel to the starter notch plane.
notch plane.
mended

Figure4.4.Typical
Figure Typicalfracture
fractureofofCT25
CT25sample
sampleaccording
accordingtotoASTM
ASTME399
E399Standard.
Standard.

The as-built
The as-built stress relief
relief (vacuum-treated 600 ◦for
(vacuum-treatedatat600◦C 3 h)3 fracture
C for toughness
h) fracture is sim-
toughness is
ilar to that
similar of Ti-6Al-4V
to that of Ti-6Al-4Vgrade
grade5 material in STA
5 material condition
in STA as aasresult
condition of the
a result α’ phase
of the mi-
α’ phase
crostructure of of
microstructure thethe
built material,
built duedue
material, to the
to rapid solidification
the rapid in theinprocess.
solidification The HIPed
the process. The
HIPed samples (1000 bar argon environment for 2 h at 920 ◦ C) pass a recrystallization
Metals 2022, 12, 1210 7 of 11

process, annealing the material and increasing the fracture toughness to more than that of a
Metals 2022, 12,conventional annealed
x FOR PEER REVIEW plate. Similar results were presented in [34,35]. 7 of 12

3.3. Fatigue
HIPed samples
samples and
(1000defects—In general, HIP
bar argon environment for is
2 hused
at 920to°C)improve material quality
pass a recrystallization and
process,
annealing
to extend the fatigue lifetheofmaterial and increasing
cyclic loading partsthe andfracture toughness
structures. Oneto more
of thethan that of a con-
advantages of
ventional annealed plate. Similar results were presented in [34,35].
the AM process is its ability to relatively easily manufacture an extremely complex shape
that is difficult 3.3.
or impossible
Fatigue to manufacture with other conventional technologies [36,37].
Complex geometries HIPed samples andthe
do not enable entire part
defects—In to be
general, HIPmachined; therefore,
is used to improve some
material surfaces
quality and
remain with their as-built
to extend theroughness
fatigue life ofand might
cyclic loadingcontain a stress
parts and concentration
structures. One of the that reduces
advantages of
the fatigue limit theofAM the working
process part compared
is its ability to relatively to themanufacture
easily standard test samples.
an extremely This effect
complex shape
has been testedthat and is difficult
reported or impossible to manufacture
in the literature with other
[22,38,39]. The conventional
effect of thetechnologies
built surface [36,37].
on
tensile strengthComplex geometries
was reported by do not enable
Dzugan the[40]
et al. entire
andpart
the to effect
be machined;
on fatiguetherefore, some sur-
performance
faces remain with their as-built roughness and might contain a stress concentration that
was reported by Greitemeier et al. [41] and Sanaeia and Fatemi [42]; they showed that the
reduces the fatigue limit of the working part compared to the standard test samples. This
surface roughness effecthas
hasabeen
high effect
tested andand reduces
reported in thethe fatigue[22,38–39].
literature limit. The effect of the built sur-
The test results
face onof thesestrength
tensile samples wasare presented
reported by Dzuganin Figure 5 and
et al. [40] and compared
the effect onto thoseper-
fatigue in
the published dataformance of Wycisk et al. by
was reported [23]. For standard
Greitemeier Ti-6Al-4V
et al. [41] laser
and Sanaeia andpowder
Fatemi bed [42]; AM
they
machine samples, showedthe that the surface
achieved roughnesslimit
endurance has aofhightheeffect and reduces
current study thewas fatigue limit. while
570 MPa,
The test results of these samples are presented in Figure 5 and compared to those in
the value presented by Wycisk et al. was 500 MPa for polished specimens. Only 210 MPa
the published data of Wycisk et al. [23]. For standard Ti-6Al-4V laser powder bed AM
was achieved for “as-built”
machine samples,samples
the achieved(without
endurance surface removal).
limit of the current The
studyenhanced
was 570 MPa, limit
while is
significantly lower duepresented
the value to surface crack initiation.
by Wycisk et al. was 500Kasperovich
MPa for polished et specimens.
al. [39] compared
Only 210 MPa the
fatigue results wasbetween
achieved as-built HIPed
for “as-built” samples
samples to HIPed
(without and machined
surface removal). samples;
The enhanced limit isthey
sig-
indicate a large nificantly
reduction lowerindue theto fatigue
surface crack
loads initiation.
and cycleKasperovich et al.due
of failure [39] compared
to the surfacethe fa-
tigue results between as-built HIPed samples to HIPed
roughness. In some AM technologies, the part can be machined to the final geometry and machined samples; they indi-
cate a large reduction in the fatigue loads and cycle of failure due to the surface roughness.
during the built operation. An example for hybrid AM, including subtractive processes, is
In some AM technologies, the part can be machined to the final geometry during the built
given in [43,44].operation. An example for hybrid AM, including subtractive processes, is given in [43,44].

Figure 5. FatigueFigure 5. Fatigue behavior of DMLS TiAl6V4 alloy in a high cycle—as-built and machined samples.
behavior of DMLS TiAl6V4 alloy in a high cycle—as-built and machined samples.
The fatigue life and maximum stress of the three types of sample are shown in Figure
The fatigue6; life and maximum stress of the three types of sample are shown in Figure 6;
as expected, the HIPed and machined samples reach the highest fatigue limit of 707
as expected, theMpa,
HIPed and machined
the as-built stress reliefsamples reachsamples
and machined the highest fatigue
achieved limit
a fatigue ofof707
limit 570 Mpa,
Mpa,
the as-built stress
whilerelief and machined
the HIPed and machined samples
failed atachieved a fatigue
lower loads and low limit of 570 Mpa, while
cycle fatigue.
the HIPed and machined failed at lower loads and low cycle fatigue.
Metals
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Figure
Figure6. Fatigue
Fatiguebehavior
behaviorof
ofDMLS
DMLSTiAl6V4 alloy with various preparation methods.
Figure 6.6. Fatigue behavior of DMLS TiAl6V4alloy
TiAl6V4 alloywith
withvarious
variouspreparation
preparationmethods.
methods.

The
The failed
The failed HIPed
failed HIPed and
HIPed and machined
and machined samples
machined samples were
samples were examined
were examined via
examined via SEM
via SEM micrography
SEM micrography to
micrography to
to
evaluate their
evaluate their
evaluate failures.
their failures. The microstructure
failures. The microstructure
microstructure of of a typical
of aa typical HIPed
typical HIPed
HIPed and and machined
and machined sample
machined sample is
sample isis
shown
shownin
shown inFigure
in Figure7.
Figure 7.7.A
AAthin
thinoxidation
thin oxidationlayer
oxidation layerof
layer of5–10
of 5–10microns
5–10 micronsof
microns ofthe
of thealpha
the alphacase
alpha casewas
case wasobserved
was observed
observed
and
and measured
and measured in
measured in Figure
in Figure 7a,b.
7a,b. The
Figure 7a,b. The alpha
The alpha case
alpha case area
case area was
area was aaa lighter
was lighter shade
lighter shade in
shade in contrast,
contrast, and
in contrast, and
and
smoother
smoother than
smoother than the
than thealpha–beta
the alpha–beta region.
alpha–beta region. The
region. The alpha
alpha case
alpha case layer
case layer is
layer is harder
is harder than
harder thanthe
than the Ti-6Al-4V
the Ti-6Al-4V
Ti-6Al-4V
material
material
materialandand reduces
andreduces
reducesthe the material’s
thematerial’s
material’s fatigue
fatigue
fatigue limit
limit
limit [45].
[45]. The
The
[45]. The surface
surface
surface alpha
alpha case
alpha case
on on
case onthe
the sam-
samples
the sam-
ples
might might
occur occur
due to due
the to the
impurity impurity
of the of
argon the argon
during during
the HIP
ples might occur due to the impurity of the argon during the HIP process. In order the
process. HIP In process.
order to In order
remove to
thisto
remove
layer, the this layer,
samples the
were samples
etched were
for 15 etched
min for
using 15
HNO3 min using
(370 HNO3
gr/liter)
remove this layer, the samples were etched for 15 min using HNO3 (370 gr/liter) and HF (370
and HFgr/liter)
(30 and
gr/liter) HFto
(30
(30gr/liter)
ensure to
toensure
the removal
gr/liter) ensure ofthe removal
removalof
a 50-micron
the ofaa50-micron
layer layer
and all signs
50-micron layerofand
the all
and allsigns
alpha of
ofthe
case.
signs Thealpha
the HIPed
alpha case. The
fatigue
case. The
HIPed
samples fatigue samples
prior tosamples
HIPed fatigue prior
etchingprior to
and after etching
etching
to etching and
and after
areafter
shownetching are
in Figure
etching shown in
8. After
are shown Figure
in the 8.
removal
Figure After
of the
8. After the
removal
alpha
removal of
case, the
ofthe alpha
alphacase,
thesamples were
case, the samples
tested
the were
weretested
for fatigue
samples limits,for
tested andfatigue
for limits,
the results
fatigue areand
limits, shown
and the results
theto Figure
results are6.
are
shown
The to
fatigue Figure
limit 6.
of The
the fatigue
etched limit
samples of the etched
increased to samples
610 MPa, increased
shown to Figure 6. The fatigue limit of the etched samples increased to 610 MPa, but wasbut was to
lower 610 MPa,
than thebut was
HIPed
lower
and than
thanthe
machined
lower HIPed
HIPedand
thesamples. andmachined
machinedsamples.
samples.

Figure
Figure7.
Figure 7.7.Fracture
Fractureand
Fracture andmicrostructure
and microstructureof
microstructure ofHIPed
of HIPedand
HIPed andmachined
and machinedsample:
machined sample:(a,b)
sample: (a,b)typical
(a,b) typicalmicrostructures
typical microstructures
microstructures
of
of TiAl6V4
of TiAl6V4 after HIP treatment,
TiAl6V4 after HIP treatment, (c,d)
treatment, (c,d) fractography
(c,d)fractographyanalysis
fractographyanalysisof TiAl6V4
analysisofofTiAl6V4 alloy
TiAl6V4alloyafter
after
alloy fatigue
fatigue
after failure,
failure,
fatigue (e)
(e)
failure,
TiAl6V4
TiAl6V4 sample
sample after
afterfailure.
failure.
(e) TiAl6V4 sample after failure.
Metals2022,
Metals 2022,12,
12,1210
x FOR PEER REVIEW 99 of 11
12

Figure 8. Machined and HIPed specimens (with alpha case) (a) prior to etching, (b) after etching.
Figure 8. Machined and HIPed specimens (with alpha case) (a) prior to etching, (b) after etching.
The above results emphasize the difficulty in defining the fatigue limits of AM parts
with The abovegeometries
complex results emphasize the difficulty
that cannot in defining
be machined the fatigue limits
in post-processing of AM parts
operations, and
with complex geometries that cannot be machined in post-processing operations,
special care should be taken during the design of the parts regarding fatigue loading. and spe-
When
cial care should be taken during the design of the parts regarding fatigue loading.
the geometry includes a narrow pass or channels and HIP failure occurs, the etching process When
the geometry
might includes
not guarantee α’ aremoval
narrowand
passmight
or channels
exposeand
thisHIP
partfailure occurs, the
to preliminary etching
fatigue pro-
failure.
cess might not guarantee α’ removal and might expose this part to preliminary fatigue
failure.
4. Summary and Conclusions
In this paper, the mechanical properties of AM powder bed fusion Ti-6Al-4V following
4. Summary and Conclusions
various post-processing procedures were compared. Tensile, fracture toughness, and
fatigueIn tests
this paper, the mechanical
were performed, properties
and the results of AMcompared
were powder bedfor fusion
as-builtTi-6Al-4V follow-
stress relief and
ing various
after post-processing
HIP, according procedures
to the applicable were compared.
standards. Tensile,
In addition, fracturefatigue
additional toughness, and
samples
were machined
fatigue tests wereandperformed,
HIPed to the andgeometry of the
the results finalcompared
were samples. for
Thisas-built
post-process
stress simulates
relief and
the AM
after HIP,of according
complex partsto theand includesstandards.
applicable process machining
In addition,to additional
the final geometries, and
fatigue samples
subsequently, it cannot be machined. The significant results from the
were machined and HIPed to the geometry of the final samples. This post-process simu-above experimental
study are AM
lates the as follows:
of complex parts and includes process machining to the final geometries,
and subsequently,
(1) The HIPed anditmachined
cannot beoperation
machined.represents
The significant results
the quality of from the above
the Ti-6Al-4V experi-
material
mental study
built arepowder
in the as follows:
bed process.
(2)
(1) The
The comparison between the
HIPed and machined as-builtrepresents
operation stress reliefthe
and HIPedofspecimens
quality indicates
the Ti-6Al-4V an
material
improvement
built in the powderin thebed
material properties: elongation (75%), reduction in area (47%),
process.
(2) fracture toughness
The comparison (90%) the
between andas-built
fatiguestress
limitsrelief
(24%),
andasHIPed
well specimens
as a decrease in yield
indicates an
strength (21%) and tensile strength (19%).
improvement in the material properties: elongation (75%), reduction in area (47%),
fracture toughness (90%) and fatigue limits (24%), as well as a decrease in yield
5. Significant Results: Recommendations for High-Quality Parts
strength (21%) and tensile strength (19%).
(1) When designing parts for fatigue loading, special care should be taken with regard
to the unmachined
5. Significant surfaces due to the
Results: Recommendations fordramatic decreases
High-Quality Partsin the fatigue limits of
the parts.
(1) When designing parts for fatigue loading, special care should be taken with regard
(2) When the machining operation takes place during or after the building process and
to the unmachined surfaces due to the dramatic decreases in the fatigue limits of the
prior to the HIP process, special care should be taken with regard to the HIP procedure.
parts.
Any contamination in the gas environment may cause failure in the fatigue life
(2) When the machining operation takes place during or after the building process and
and limitations.
prior to the HIP process, special care should be taken with regard to the HIP proce-
(3) Failure in HIPed parts due to the alpha case layers can be removed by etching, which
dure. Any contamination in the gas environment may cause failure in the fatigue life
improves the fatigue limits in comparison to the as-built stress relief parts, but less
and limitations.
than HIPed and the machined samples.
(3) Failure in HIPed parts due to the alpha case layers can be removed by etching, which
improves the fatigue limits in comparison to the as-built stress relief parts, but less
than HIPed and the machined samples.
Metals 2022, 12, 1210 10 of 11

(4) The applicable qualification standards for the examined mechanical properties cor-
relate with conventional materials and represent the properties of AM materials;
however, in many cases, they do not represent the geometry sensitivity of AM parts.

Author Contributions: O.D.: Investigation, Formal Analysis, Writing—Original Draft; T.R.: Investi-
gation; E.A.: Investigation; A.S.: Conceptualization, Methodology, Supervision, Writing—Original
Draft. All authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Experimental data from this study are available from the corresponding
author upon reasonable request.
Acknowledgments: The authors thank Frage from the Department of Materials Engineering at
Ben-Gurion University of the Negev for performing the HIP process in this research.
Conflicts of Interest: The authors declare no conflict of interest.

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