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Journal of Manufacturing Processes 64 (2021) 1517–1528

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Journal of Manufacturing Processes


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Rotary friction welding of additively manufactured 17-4PH stainless steel


H.R. Lashgari a, *, S. Li a, C. Kong b, M. Asnavandi c, Sh. Zangeneh d
a
School of Materials Science and Engineering, University of New South Wales, Sydney, NSW, 2052, Australia
b
Mark Wainwright Analytical Centre (MWAC), University of New South Wales, Sydney, NSW, 2052, Australia
c
School of Chemistry, University of New South Wales, Sydney, NSW, 2052, Australia
d
Department of Materials and Textile Engineering, Faculty of Engineering, Razi University, Kermanshah, Iran

A R T I C L E I N F O A B S T R A C T

Keywords: The aim of the present study is to investigate the effect of rotary friction welding (RFW) on the microstructure,
Rotary friction stir welding tensile properties, hardness, wear resistance and corrosion properties of the weld joint of an additively manu­
Selective laser melting factured solid cylinder made of 17-4PH stainless steel. Significant grain refinement was observed in the welding
17-4PH stainless steel
zone (WZ) due to the plastic deformation and dynamic recrystallization. The morphology of the grains changed
Microstructure
Corrosion and wear
from columnar in the as-printed condition to equiaxed in the welding zone. The microhardness of the WZ is ≈10
% higher than the heat affected zone (HAZ) due to the grain refinement but still lower (≈27 %) than the as-
printed microstructure which contains nano-sized carbides and less retained austenite (γfcc) due to the rapid
solidification. The precipitation of Cr-rich carbides was observed in the WZ and HAZ leading to sensitization and
decrease of corrosion resistance (up to ≈90 %). Cu-rich clusters were formed at the interface of Cr-rich carbides/
matrix in the WZ and HAZ due to the cube-cube orientation relationship. The depletion of matrix from Cr and Cu
in the welding zone decreased the stability of martensite after friction welding leading to the formation of 7–10
% retained austenite. At low load (2 N), the wear resistance of as-printed microstructure (base metal, BM) was
found to be superior to WZ and HAZ. However, at intermediate and high loads (5 N and 10 N), the wear
resistance of WZ was either better or comparable to the as-printed microstructure. Adhesion and Oxidative wear
were the main wear mechanisms at all loads during the reciprocating action. Oxide films grow until they reach a
critical thickness prior to becoming unstable and spalling off to form wear debris.

1. Introduction industries.
Despite the advantages of SLM process to produce near-net-shaped
Selective Laser Melting (SLM) is an advanced manufacturing (AM) components with excellent dimensional accuracy, it suffers from poor
technique which has been successively utilised to produce components surface quality and surface roughness owing to layer-wise nature of SLM
with complex shape and geometries via layering and fusing successive process. As a result, friction welding (FW) can be effectively employed to
layers of powder material on the basis of a computer-aided design (CAD) post-process for microstructural modification and enhancement of sur­
model [1–3]. face properties. Friction Stir Welding (FSW) and Friction Stir Processing
SLM process can be treated as a micro laser welding process since one (FSP) are two well-known solid-state process that can be utilised to join
powder layer is spread over the build-plate at a time and fused to the (i.e. FSW) or modify (i.e. FSP) the microstructure of the functional
previous later. Therefore, it is essential to avoid and/or minimise defects materials in microscopic scale in order to improve the mechanical
such as microporosities, microshrinkages, balling defects, oxidations, properties of the weld joint (i.e. FSW) or improve the surface properties
lack of welding, inclusions and so on via optimization of the (i.e. FSP) via manipulation of the generated heat during process and
manufacturing parameters such as laser power, scanning speed, layer strain input, simultaneously [6,7]. In addition, the maximum dimension
thickness, scanning strategy, and hatch spacing [4,5]. As a result, the of the components manufactured by SLM is limited to the size of the
structural and mechanical integrity of the additively manufactured build-plate, therefore, joining additively manufactured components
components and their reliability during service are quite crucial in order using solid-state welding process such as Rotary Friction Welding (RFW)
to comply with rigorous obligations of navy, aerospace, and automotive and Linear Friction Welding (LFW) seem to be essential and in particular

* Corresponding author.
E-mail address: h.lashgari@unsw.edu.au (H.R. Lashgari).

https://doi.org/10.1016/j.jmapro.2021.03.008
Received 12 November 2020; Received in revised form 2 March 2021; Accepted 4 March 2021
Available online 16 March 2021
1526-6125/© 2021 The Society of Manufacturing Engineers. Published by Elsevier Ltd. All rights reserved.
H.R. Lashgari et al. Journal of Manufacturing Processes 64 (2021) 1517–1528

Fig. 1. Rotary friction welding process of additively manufactured 17-4PH stainless steel cylinder.

for additively manufactured components made of alloys difficult to weld interconnected network of silicon eutectic and reduced the number of
such as titanium and aluminium alloys etc. microvoids leading to better surface finish, higher ductility, and
Singh et al. [8] investigated the microstructure and mechanical consequently enhanced fatigue life. Microstructural homogenization,
properties of FSWed Ti-6Al-4 V alloy produced by electron beam breakdown of columnar grains and formation of equiaxed grains in
melting (EBM) process. Grain refinement was observed near the (WC-10 FSPed SLMed AlSiMg alloy were some considerable microstructural
%Co) tool-workpiece interface which was attributed to the fast cooling features observed by Maamoun et al. [14].
rate and shear deformation [8]. Moeini et al. [9] explored the effect of Due to the complexity and cost of the additively manufactured
the FSP process on the surface properties of the additively manufactured components, repair and restoration are important to return the damaged
Al-12Si alloy. It was shown that the combination of the severe plastic components into life cycle using FSW and/or FSP process. Rotary fric­
deformation and dynamic recrystallization resulted in significant grain tion welding process may also be needed to join additively manufac­
refinement. However, the measured hardness of the FSPed surface was tured components in the shape of cylindrical tubes and rods. Hence, it is
lower than the SLMed Al-12Si alloy which was attributed to the disso­ essential to understand how these techniques affect the microstructure
lution of the fine silicon eutectic and microstructural coarsening [9]. and mechanical properties of additively manufactured components.
Later it was concluded that the FSP process could effectively improve the The aim of the present study is to understand the feasibility of rotary
corrosion resistance of the FSPed zone in Al-12Si alloy mostly owing to friction welding in SLM manufactured 17-4PH stainless steel alloy cyl­
the microstructural modification and high cooling rate. inder. To authors best knowledge, the solid-state welding of additively
The low cycle fatigue (LCF) performance of FSPed Al-12Si alloy manufactured parts is not investigated yet and far from understood. For
produced by SLM process was considered by Moeini et al. [10]. It was this reason, this paper is aimed at investigating the microstructure, wear
shown that the LCF performance of the FSW samples was inferior to SLM resistance, corrosion properties, tensile properties, and microhardness
samples. The lower LCF lives of the FSW specimens stemmed from of the solid-state weld joint in an additively manufactured 17-4PH
microstructural heterogeneity, near surface microporosities, and lack of stainless steel cylinder. Advanced material characterization techniques
fusion [10]. such as X-ray diffraction (XRD), scanning electron microscopy (SEM),
In an interesting study conducted by Sadhu et al. [11], the surface of electron back scatter diffraction (EBSD), and high-resolution trans­
the H13 tools steel was deposited with Stellite 6 (CoCr) using Direct mission electron microscopy (HRTEM) were utilised to study the
Laser Metal Deposition (DLMD) process and the performance of the FSW microstructural evolution.
tools was examined against the CuCrZr sheet. It was shown that despite
exposure to high temperature during FSW (≈1000 ◦ C), the hard surfaced 2. Materials and experimental methods
tool was able to sustain its shape and geometry and showed almost no
sign of grooving marks indicative of good wear resistance. The trivial Cylindrical shape samples (Ø25 mm × 30 mm) made of 17-4 PH
wear rate of the Stellite 6 coated steel was attributed to the stainless steel were manufactured using a 3D Systems Prox300 SLM
grain-boundary carbides and solid solution strengthening mechanism machine. The morphology, particle size distribution, nominal compo­
inhibiting abrasion and deformation [11]. sition, the condition of gas atomised as-received powder, and
Rubino et al. [12] used the viability and potential of FSP to enhance manufacturing condition can be found elsewhere [15]. The laser power,
the surface quality of the additively manufactured Ti-6Al-4V alloy. It laser scanning rate, layer thickness and hatch-spacing were 127.5 W,
was concluded that the FSP decreased the surface roughness by 80 % 1200 mm/sec, 40 μm, and 50 μm, respectively. Conventional lathe
and eliminated the internal porosities. The recrystallized grain was machine was utilized for rotary friction welding of the cylindrical shape
achieved in the stir zone (SZ) whereas grain coarsening was observed in samples, as shown in Fig. 1.
the heat affected zone (HAZ) and transition zone (TZ) [12]. The as-printed and friction welded samples were sectioned, ground
The FSP process was shown to have improved the fatigue perfor­ and then mechanically polished to a mirror finish using a colloidal silica
mance of SLMed AlSiMg alloy [13]. In fact, FSP broke down the solution (0.04 μm). Fry’s reagent (40 mL HCl, 5 g CuCl2, 30 mL water,

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electropolished in 95 % acetic acid + 5 % perchloric acid at room


temperature at 30 V for 30 s. The electropolished sample surface tilted
at 5◦ was further treated with a Hitachi IM4000 low energy Ar ion miller
operating at 5 kV in flat mode for 20 min.
The hardness of the FSWed samples was measured using Vickers
micro-hardness on the polished and ultrasonically cleaned surfaces. The
load and holding time were 1 kgf and 15 s, respectively, and 30 indents
were conducted on each sample starting from the welding zone and
moving towards the base metal.
For corrosion testing, the specimens were abraded up to P2000
emery paper, degreased ultrasonically in ethanol followed by rinsing in
milli-Q water before immersing into 500 mL 3.5 % NaCl solution. The
samples were chosen from the welding zone, heat affected zone and base
metal and the size of each sample was 20 mm × 5 mm. Electrochemical
measurements were conducted using CH Instrument 660 with a three
electrode setup. A platinum spring and Ag/AgCl (3 M KCl) were used as
the auxiliary and reference electrodes, respectively. The distance be­
Fig. 2. The cross-section of the friction welded samples. The arrow shows the tween sample and the Pt spring was set to be 20 mm. The samples were
direction of reciprocating wear test. held in the NaCl solution for 24 h to reach steady state and then open
circuit potential (OCP) was measured. The potentiodynamic polariza­
25 mL ethanol) was employed to etch and reveal the microstructure of tion was conducted by sweeping the potential at a scan rate of 1 mV.s− 1
the friction welded specimens (etching time 30 s-1 min). For phase from – 400 mV to +300 mV. To ensure the repeatability and repro­
identification, X-ray diffraction technique (Empyrean 2 PANalytical X- ducibility of the results, each experiment was repeated three times.
ray Diffraction System) with Co Kα (λ = 1.788965 Ǻ) from 2θ = 40–130◦ Dry sliding wear tests were performed on a linearly reciprocating
with step size of 0.026 and step time of 210 (s) was utilized. High score ball-on-flat tribometer (CSEM Tribometer) at room temperature. Three
plus software was used for phase calculation and peak analysis. Scan­ different loads were applied for wear testing, i.e. 2, 5, and 10 N. The
ning electron microscopy (field-emission scanning electron microscope, sliding speed, frequency, wear distance and stroke length were 30 mm/
NanoSEM 450) equipped with energy dispersive X-ray spectroscopy s, 2.38 Hz, 30 m (3750 cycles), and 4 mm, respectively. Details of the
(EDS) was used for microstructural study. wear testing experiment can be found elsewhere [15,16]. The regions
The TEM samples were prepared using focused ion beam milling subjected to corrosion and reciprocating wear testing are shown in
(FIB) method. The high-resolution TEM was conducted using a Philips Fig. 2.
CM-200 field emission gun operated at 200 kV, equipped with a Bruker Finite element analysis (FEA) was employed to examine the degree of
Esprit energy dispersive X-ray spectroscopy (EDS) system. The electron temperature rise during friction welding. The analysis was carried out
back scatter diffraction (EBSD) analysis was carried out using an Oxford using Abaqus software in nonlinear mode, quasi-static with thermo­
Aztec 4.0HKL EBSD system with a Symmetry CMOS detector. This EBSD mechanical coupling. A fully coupled temperature-displacement pro­
system is attached to a Thermo Fisher Helios G4 UXe Plasma Focused Ion cedure was utilized in the simulation. The rods were modelled as
Beam and Elstar electron column with UC + technology. The axisymmetric. The element formulation used was the fully coupled
100 × 75μm2 mapping with a step size of 0.4 μm was done on the temperature-displacement axisymmetric elements with twist degrees of
electropolished surface at 20 kV with a 70◦ pre-tilt sample holder. The freedom (element type CGAX4HT), where the twist degree of freedom
hit rate for all samples was 98.5 ± 0.5 %. The polished samples were enables modelling of rotation and shear deformation in the out-of-plane

Fig. 3. (a) Weld configuration (b) mesh distribution in the axisymmetric model.

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Fig. 4. SEM micrographs of welding zone (WZ), thermo-mechanically affected zone (TMAZ), heat affected zone (HAZ), and base metal (BM) after friction welding.

direction. The hybrid formulation is required to handle the incom­


pressible nature of the material during the plastic flow. In this welding
simulation, the kinetic energy during rotation is converted to the ther­
mal energy at the frictional interface. The co-effect of frictional sliding
and plastic deformation generates heat and contributes to the temper­
ature rise in the rods. Full Newton iteration is used for the nonlinear
solution. Automatic time stepping is based on the maximum tempera­
ture change in each increment. Results from the previous increment are
used as the initial estimate in the current increment, with the parabolic
extrapolation technique adopted to transfer the previous state to the
current state. A pressure of 150 MPa is applied to the top surface of the
upper rod which was rotated at a velocity of 62.8 rad/s. The main
challenge in modelling of the friction welding is the analysis and
determination of the coefficient of friction (μ). It should be noted that
the coefficient of friction changes continuously during the welding
cycle, i.e., μ > 1 at the beginning and μ ≈ 0 when the temperature
reaches the melting point at the interface. For simplicity, the coefficient
of friction was set to be constant throughout the modelling, and the
value of the friction coefficient was chosen μ = 0.5 since the duration of Fig. 5. The distribution of temperature across the weld interface.
the welding process was short. The mesh used in this simulation is
divided into two regions for each rod. Near the weld interface, smaller this technique. During the welding operation, the material exchanges
elements were generated to increase the accuracy of simulation (see heat with the surrounding environment by convection and radiation.
Fig. 3). The two rods used in the simulation are the same material with a Heat losses by convection is represented by Eq. 1, while heat losses by
length of 17 mm, and radius of 12.5 mm. The rods are in contact initially radiation is expressed by Eq. 2.
at the intended weld interface and the initial temperature is set at room
temperature. ΦC = hc (T − T∞ ) (1)
The Arbitrary Lagrangian Eulerian (ALE) technique was used for the
Φr = σε(T 4 − T∞
4
) (2)
simulation of friction welding process. The ALE formulation is an in­
termediate method between the Lagrangian, and Eulerian methods
where hc is the coefficient of convection, T the surface temperature of
which allows the arbitrary and independent movement of mesh inside
the object, T∞ the temperature of the surrounding fluid, σ is Stefan-
the domains with respect to the material. ALE formulation is a standard
Boltzmann constant and ε is the emissivity of the object.
numerical approach for solving large strain deformation problems
encountered in metal-forming and high-speed impact applications. In
other words, greater distortion of the continuum can be handled using

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3. Results and discussion

Fig. 4 shows the SEM micrographs of the WZ, TMAZ, HAZ, and BM
(unaffected area) after friction welding. The friction welding has
changed the morphology of the grains from elongated columnar to
equiaxed grains. In the as-printed microstructure (Fig. 4d), columnar
grains grow along the easy growth direction (i.e. < 100> in bcc and fcc
metals) and they are stretched from one grain to another as long as the
easy axis growth is parallel to the heat flow direction. However, the co-
effect of severe plastic deformation and temperature rise during friction
welding caused dynamic recrystallization in the WZ, TMAZ, and HAZ
changing the morphology of the grains from columnar to equiaxed
grains.
Finite element analysis (FEA) was employed to examine the degree of
temperature rise during friction welding, as shown in Fig. 5. The tem­
perature distribution at the weld joint reveals that the temperature can
reach as high as ≈1100 ◦ C after two seconds in friction welding. This
temperature is slightly higher than the conventional solution tempera­
Fig. 6. The XRD patterns of the WZ, HAZ, and BM. ture (i.e. 1040 ◦ C) used to homogenise the commercial 17-4PH stainless

Fig. 7. Pattern quality maps, phase maps, and pole figures in welding zone (WZ) and base metal (BM).

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Fig. 8. High-resolution TEM image, showing the precipitation of Cr-rich carbides in the WZ and Cu-clustering at the interface of carbide/matrix.

steel. the formation of reversed austenite by Ni-partitioning in Cr-depleted


The Creq and Nieq of the current alloy was calculated according to zone [15,18]. The distribution of austenite (reversed and/or retained)
WRC-1992 diagram and were found to be 17.034 and 8.28, respectively. is more uniform as compared to as-printed microstructure where
Based on the Creq/Nieq ratio (≈ 2.05 for the current alloy), it can be retained austenite is formed at the grain boundaries owing to the large
assumed that significant amount of ferrite is present if Creq/Nieq >1.8 strain at the grain boundaries and microsegregation of
[17]. It seems that during friction welding, the temperature rises to δ + γ austenite-stabilizing elements (such as Ni and N) [15]. The TMAZ con­
region. Under equilibrium condition, δ-ferrite transform to austenite and tains equiaxed grains indicative of dynamic recrystallization in this re­
austenite transform to α-ferrite + M23C6 (M = Cr, Fe, Mo) carbides. The gion. According to FEA analysis, the estimated temperature rise in TMAZ
transformation of δ-ferrite → γ-austenite requires time and under high is ≈900− 1000 ◦ C. The microstructure of TMAZ is similar to HAZ but
cooling rate, the occurrence of this transformation is highly unlikely. contains less lathy-ferrite. This zone is severely deformed and subjected
Perhaps, this explains the presence of lathy-type ferrite (δ-ferrite→ lathy to frictional heat near the WZ.
α-ferrite) in the WZ and HAZ, as shown in Fig. 4a-b. The Kurdju­ The grain size was decreased from a few hundred micron in the BM to
mov–Sachs (K-S) orientation relationships between δ-ferrite and less than 10 μm in the WZ, as can be seen in the inset of Fig. 7. The grain
austenite encourages the formation of lathy ferrite. refinement in the WZ is due to the continuing rotation of subgrains by
The XRD patterns taken from the WZ, HAZ, and BM are illustrated in absorption of dislocations at the grain boundaries and increase of
Fig. 6. The volume fraction of austenite was calculated using integrated misorientation angle and their gradual transformation into grain
intensities of the diffraction peaks. It was deduced that the volume boundaries [7]. The strong texture formed along the build direction was
fraction of retained austenite increased from 2% in the BM to 7.1 % in diminished after friction welding mostly due to the formation of new
the WZ. The intensity of γ111 peak increased considerably in the WZ and recrystallized grain, as shown by the pole figures in Fig. 7.
new austenite peaks appeared at 2θ values of 89.58◦ , 111.32◦ , and Precipitation of Cr-rich carbides (Cr23C6 and/or Cr7C3) and NbC-type
119.14◦ corresponding to γ220, γ311, and γ222, respectively. carbides were observed in the WZ and HAZ of the friction welded
The microstructure of the WZ and BM was further analysed using specimens, as shown by high-resolution TEM images, X-ray map and line
EBSD. The EBSD images of the WZ and BM, phase map and inverse pole scan in Figs. 8 and 9. In other words, the matrix has become sensitized
figures are shown in Fig. 7. The dynamic recrystallization caused by the due to the diffsuin of carbon and chromium and formation of chromium
co-effect of temperature rise and plastic deformation in friction welding carbides at the grain boundaries or between martensite laths. This also
led to the formation of equiaxed grains. The volume fraction of austenite explains the slight shift in the position of ά110 towards higher 2θ values,
(blue colour in phase map) was also increased in the WZ and HAZ. This is as shown by dotted line in Fig. 6. This indicates the decrease of lattice
attributed to the lower cooling rate in friction welding as compared to parameter in the WZ zone which is attributed to the precipitation of Cr-
cooling rate in SLM process and depletion of Cr in matrix (as a strong rich carbides and Cu-clustering at the interface of carbides/matrix. The
α-stabilizer element) due to the precipitation of Cr23C6. This promotes size of Cr-rich carbides is within 1− 3 μm. This indicates that the cooling

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Fig. 9. High-resolution TEM image, showing the precipitation of Cr-rich carbides and NbC carbides in the HAZ.

was reported in Tavares’s study [19] where presence of NbC carbides


was not able to stop the sensitization of 17-4PH stainless steel during
aging at T≥495 ◦ C. According to the FEA simulation, the temperature
can rise up to 1100 ◦ C during friction welding and this has led to the
precipitation of Cr-rich carbides during cooling due to the slower cool­
ing rate and longer retention time in RFW process. Although, the
duration of friction welding process was about a minute, but it seems
that the presence of high density of dislocations introduced during re­
petitive heating/cooling cycles in SLM printing parts accelerated the
diffusion rate of Cr and C atoms significantly. Clustering of Cu atoms was
also observed at the interface of Cr-rich carbides/matrix, as shown in
X-ray map in Fig. 8. This could be due to the similarity of the crystal
structure of Cu and Cr23C6 and/or M7C3 carbides (both are cubic),
providing preferential sites for Cu atoms to diffuse and form clusters
during cooling. In addition to lower cooling rate in friction welding
when compared to cooling rate in SLM printing, the depletion of matrix
from α-stabilizing elements such as Cr and Mo would also promote the
formation of austenite in the matrix.
Fig. 10 shows the variation of Vickers-micro hardness from the weld
Fig. 10. Vickers micro-hardness from the weld centreline (WZ) towards the
centreline towards the base metal. As one can see, the hardness of the
base metal (BM).
WZ is ≈10 % greater than the thermomechanically affected zone
(TMAZ) and HAZ area. This is attributed to the grain refinement caused
rate was not high enough after friction welding to prevent the precipi­
by dynamic recrystallization during friction welding. However, when
tation of chromium carbides. The chromium carbides (M23C6) usually
compared to the BM, the hardness of the WZ is considerably lower than
precipitate within the temperature range of 600− 850 ◦ C in austenitic
the initial microstructure formed after printing. This is due to the rapid
stainless steel. However, in our previous study on the heat treatment
solidification in SLM process, fine distribution of secondary phases such
response of additively manufactured 17-4PH stainless steel [15], we
as carbides, extremely high-density of dislocation, and lower volume
showed that the precipitation of M23C6 and/or M7C3 carbides took place
fraction of retained austenite in the matrix. But the variation of hardness
at higher temperature during solution treatment (1040 ◦ C) leading to
is greater in the BM as compared to WZ, TMAZ, and HAZ. This large
sensitization. The presence of Nb as a strong carbide former (NbC-type
deviation could be due to the difference in grain size in BM (whereas in
carbides) did not help to prevent the sensitization. Similar observation
WZ the grain size seems to be more uniform) and presence of porosities

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Fig. 11. (a) Tensile curve of the friction welded specimen, (b), fracture surface showing microvoids and dimples, and (c) oxide film on the fracture and, (d) its
associated EDS point analysis.

Fig. 12. (a) Time dependence of corrosion potential, and (b) Polarization curves measured in 3.5 % NaCl solution.

in the matrix. The hardness of TMAZ is slightly higher than HAZ which revealed the presence of oxide films on the fractured surface, decreasing
can be attributed to the plastic deformation caused development of the strength of bonding at the weld centreline. The optimization of the
dislocation based substructures in this zone. friction welding parameters is currently under investigation in order to
The true stress-strain curve of the tensile sample machined from the eliminate these defects and reach the mechanical strength required for
friction welded joint and SEM micrographs of the fractured surfaces are typical 17-4PH stainless steels. Apart from that, the presence of fine and
shown in Fig. 11. The ultimate tensile strength (UTS) of the friction small conical equiaxed dimples indicates that numerous nucleation sites
welded joint is ≈ 650 MPa which is lower than the typical mechanical are activated before coalescence to form larger dimples. Large and small
properties of 17-4PH stainless steel in H1150 M condition, i.e. UTS≈ oxide inclusions and carbides in the matrix provide nucleation sites for
850 MPa after aging at 620 ± 5 ◦ C for 4 h. The fractography images microvoids.

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Table 1 post-thermal treatment of additively manufactured 17-4PH stainless


Corrosion potential (Ep) and corrosion current density (ic) in BM, HAZ, and WZ. steel [15], we showed that precipitation range of M23C6/M7C3 carbides
Sample Ep (V) ic (mA/cm2) varied from aging temperature (≈480 ◦ C) to solution temperature
5 (≈1040 ◦ C).
BM − 0.1531 6.858 × 10−
HAZ − 0.1617 1.198 × 10− 4 The polarization curves of the specimens measured in the 3.5 % NaCl
WZ − 0.3091 1.286 × 10− 4 solution are displayed in Fig. 12b and the fitted corrosion parameters
including corrosion potential (Ep, V) and corrosion current density (ic,
mA/cm2) are presented in Table 1. The anodic and cathodic polarization
curves correspond to the dissolution of sample and evolution of
hydrogen gas in anode and cathode, respectively.
The anodic branch of the polarization curve of BM shifted to the left
when compared to WZ which is associated with reduced anodic kinetics.
The corrosion potential of BM is more positive than HAZ and WZ which
indicates that BM sample is more passive than WZ and HAZ samples. The
corrosion current density of WZ and HAZ samples are ≈75 % and ≈87 %
greater than BM, showing higher corrosion rate of WZ and HAZ as
compared to the initial microstructure (i.e. BM). The surface of the WZ
and HAZ samples is more active than BM and the distribution of alloying
elements in the matrix and in particular Cr and Cu plays a major role in
determining the corrosion resistance. The presence of Cr and Cu in the
solid solution helps to form a passive layer, protecting the alloy from
additional corrosion, leading to enhanced corrosion performance.
However, the formation of Cr-rich carbides during cooling period and
clustering of Cu atoms at carbide/matrix interface (see Figs. 8 and 9)
decreased the amount of Cr and Cu in the solid solution, serving as local
cathodes and promoting localised corrosion.
Fig. 13. Wear coefficient of WZ, HAZ, and BM at 2 N, 5 N, and 10 N loads.
The wear coefficient (probability of formation of wear debris) and
the coefficient of friction in WZ, HAZ, and BM under three different
loads, i.e. 2 N, 5 N, and 10 N, are shown in Figs. 13 and 14. As once can
Open circuit potential (Ecorr) of the WZ, HAZ, and BM was measured
see, the unaffected microstructure (BM) shows the highest wear resis­
in 3.5 % NaCl solution for a period of 24 h, as shown in Fig. 12a. The
tance at 2 N. As load increases from 2 N to 5 N, the wear rate of BM
sample taken from HAZ showed the most positive potential followed by
increases and then decreases at 10 N. The HAZ microstructure shows
BM and WZ. In general, with the improvement of passivity, the Ecorr
better wear behaviour at intermediate load as compared to BM and WZ,
often increases (i.e. shifts to more positive values) and when localised
and at 10 N force, the wear resistance of WZ and BM are almost similar.
corrosion takes place (for example pitting), the Ecorr decreases (i.e. shifts
The low wear rate of the BM at 2 N load can be explained in terms of
to more negative values). In other words, corrosion potential exhibits
higher hardness of as-printed microstructure and uniform distribution of
the tendency to passivation at open circuit and the higher the corrosion
alloying elements in the matrix due to the rapid solidification. In addi­
potential the more passive is the material [20]. The Ecorr of WZ vs. time
tion, since the direction of reciprocating action is perpendicular to the
is more negative and continues to decrease overtime and this shows less
build direction (directional columnar growth), more resistance is pro­
passivity. This behaviour could be due to the fine grain size (more grain
vided against the slipping. As the load is increased from 2 N to 5 N, the
boundaries) and in particular the precipitation of Cr-rich carbides and
wear rate is increased by a factor of ≈17, leading to the formation of
depletion of matrix from Cr and Cu elements. In our previous work on

Fig. 14. The coefficient of friction of WZ, HAZ, BM at: (a) 2 N load, (b), 5 N load, and (c) 10 N load.

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H.R. Lashgari et al. Journal of Manufacturing Processes 64 (2021) 1517–1528

other regions. Therefore, it can be concluded that the adhesion and


oxidative wear were the main wear mechanism at intermediate and high
loads. Once the oxide layer reaches a critical thickness, it starts to
become unstable and delaminate from the surface forming oxide debris.
A crack running along the sliding direction is shown in the inset of
Fig. 16 (BM, 10 N), forming due to the repetitive heat and stress cycles
similar to the fatigue crack. The composition of the oxide films in all
regions (i.e. BM, HAZ, and WZ) seems to be similar. The difference in
wear resistance between BM, HAZ, and WZ at different loads is
explained in terms of difference in microstructure, grain size, volume
fraction of retained austenite and presence of Cr-rich carbides in the
matrix.
Carbides are brittle and they provide nucleation sites for the initia­
tion of cracks during reciprocating action. Microstructure plays a sig­
nificant role in the wear resistance of martensitic stainless steel.
Retained austenite can transform into martensite due to the stress
induced transformation. The work-hardening caused by this trans­
formation decreases the wear rate at high load. The sample taken from
WZ has more retained austenite than HAZ and BM. When subjected to
10 N load under reciprocating action, γ→M phase transformation can
cause significant work-hardening leading to better wear resistance. At
intermediate load (5 N), carbides provide resistance against the propa­
gation of dislocations resulting in better wear resistance in HAZ sample.
However, upon increasing load to 10 N, carbides are pulled out from the
matrix excessively leading to higher wear coefficient. In addition, the
grain refinement induced by dynamic recrystallization in the WZ and the
change of morphology from columnar to fine equiaxed improved the
wear resistance of WZ at 10 N load and make it quite comparable to the
wear property of BM.

4. Conclusions
Fig. 15. The microstructure of the (a) WZ, and (b) BM.

Rotary friction welding of additively manufactured 17-4PH stainless


considerable wear particles. The increase of load from 5 N to 10 N
cylinder was investigated using advanced materials characterisation
almost halved the wear rate.
techniques and corrosion, wear and mechanical properties of the weld
The coefficient of friction varies with load, microstructure, and dis­
joint were examined. Following conclusions can be drawn from the
tribution of alloying elements in the matrix. The increase of load from
results:
2 N to 10 N slightly decreased the coefficient of friction in all samples.
As seen in Fig. 14, the coefficient of friction (CoF) is smoother at higher
1 The microstructure of the WZ and HAZ changed from the elongated
loads and more erratic at lower loads. At light load, the oxide films
columnar to fine equiaxed morphology owing to the co-effect of
generated on the surface are thin and break off faster before they grow
temperature rise and plastic deformation resulting in dynamic crys­
further and become stable. For the higher applied loads, the temperature
tallization. Finite element analysis revealed that the temperature can
at the contact point is higher and the oxide film grows and becomes
go up to 1100 ◦ C during friction welding.
thicker overtime under reciprocating action. Oxide films on the surface
2 The precipitation of Cr-rich carbides and Cu-clustering at carbide/
can act as a solid lubricant leading to decrease in CoF, as shown in
matrix interface were observed in the WZ and HAZ causing sensiti­
Fig. 14.
zation and lower corrosion resistance as compared to unaffected area
At intermediate load (5 N), the wear resistance of WZ and HAZ is
(i.e. base metal).
greater than the BM. This could be due to the isotropic microstructure of
3 The microstructure of the WZ and HAZ is a combination of lathy
the WZ and HAZ and considerable grain refinement after friction
ferrite, retained/reversed austenite, and lath martensite. The distri­
welding when compared with columnar structure of the BM. In addition,
bution of austenite in WZ is more uniform when compared to as-
the volume fraction of porosities in the WZ and HAZ is lower than the
printed microstructure where retained austenite was concentrated
initial microstructure due to the welding and elimination of porosities
at the grain boundaries.
during friction action, as shown in Fig. 15. These porosities provide
4 The presence of dimples on the fracture surface indicates that the
nucleation sites for the initiation and propagation of cracks during wear
mode of fracture is ductile. However, oxide films had negative in­
test leading to lower wear resistance at intermediate load. The highest
fluence on the tensile strength and further optimization is required to
wear resistance at 5 N load was observed in HAZ sample despite the
eliminate these defects.
lower hardness of HAZ as compared to WZ and BM. However, as load
5 Adhesion and oxidative wear were the main wear mechanism. At low
increases from 5 N to 10 N, the wear rate increases abruptly. The tem­
load (2 N), the wear resistance of the as-printed microstructure was
perature increases at contact points with increasing load leading to
higher whilst by the increase of load to 5 N and 10 N, welding zone
significant surface oxidation. The SEM micrographs of the worn surfaces
showed better wear behaviour. This was attributed to the elimination
at 5 N and 10 N loads are shown in Fig. 16 and the results of the point
of porosities in WZ, presence of hard carbides, and austenite (γ) →
analysis in Fig. 16 are listed in Table 2.
Martensite (M) phase transformation during wear test.
As one can see, the worn surfaces are covered with oxide layer in
some regions whereas this layer seems to have been delaminated in

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Fig. 16. The SEM micrographs of the worn surfaces in BM, HAZ, and WZ at two different loads (5 N and 10 N).

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