Materials Characterization 164 (2020) 110358

Contents lists available at ScienceDirect

Materials Characterization
journal homepage: www.elsevier.com/locate/matchar

Comparison study on microstructure and mechanical properties of Ti-6Al-4V T

alloys fabricated by powder-based selective-laser-melting and sintering
methods
⁎ ⁎
Q. Yana, B. Chena, , N. Kanga, X. Lina, , S. Lva, K. Kondohb, S. Lic, J.S. Lia
a
State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi'an 710072, Shaanxi, China
b
Joining and Welding Research Institution, Osaka University, 11-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan
c
School of Materials Science and Engineering, Xi'an University of Technology, Xi'an 710048, China

A R T I C LE I N FO A B S T R A C T

Keywords: To better understand the structure-mechanical properties relation of additively manufactured Ti-6Al-4V (Ti64)
Titanium alloys alloys, a comparison study was performed on Ti64 alloys fabricated by powder-based selective laser melting
Selective laser melting (SLM) and sintering methods. It is found that the SLM Ti64 alloy has prior β grains filled with (lath α + needle
Spark plasma sintering α′) structure. While Ti64 alloys sintered over and below β → α transformation temperature have widmanstatten
Microstructures
α + β and lamellar α + β structure, respectively. The SLM Ti64 alloy has higher strength and hardness than
Mechanical properties
sintered alloys, but possesses similar Young's modulus to the spark plasma sintered alloy. The mechanisms
leading to the different mechanical properties are discussed based on phase compositions and contents. The
results suggest that SLM Ti64 alloys potentially have better mechanical performance compared with those
fabricated by conventional sintering methods.

1. Introduction Utilizing the computer controlled laser directional deposition, it is

possible to design as-built products with a complication model above
Ti-6Al-4V, abbreviated as Ti64, is a double-phase (α + β) titanium all, such as orthopedic joints in human being [7] and three-dimensional
(Ti) alloy widely used in automobile, aerospace, navigation, petroleum porous parts [8]. Secondly, AM consolidation has very low material
and medical industries because of its excellent properties of low den- waste and high material efficiency. As a special kind of powder me-
sity, high specific modulus and superior corrosion resistance [1,2]. As tallurgy (PM), the AM process utilizes accurately fed spherical powder
one of the popular alloys with high “buy to fly” ratios, Ti64 has been particles with micron diameters and melt/sinter specific areas designed
occupying about half of the market share of Ti alloy products all over by CAD. In addition, the surface of AM-fabricated can be comparatively
the world since 1950s [3]. In despite of the popular applications of flat with small roughness, which only needs slight surface polish prior
Ti64, the comparatively high price has hindered its wider application to practical uses [9]. Finally, thanks to the CAD controlling and laser
areas. For cost reduction, there is a great demand to use fabrication directional deposition, AM can realize the exact rebuilt of selected areas
processes with net-shaped consolidation, low material waste and high within a sample, which is almost impossible for conventional methods.
efficiency. However, such characteristics are difficult to achieve in In despite of the advantages of AM process, the uses of AM Ti and its
conventional methods, such as casting [4], hot pressing [5] and sin- alloy parts are still at infancy, mainly due to their structural problems,
tering [6]. It is urging to explore in-expensive and efficient methods to such as large tensile residual stresses, anisotropy and defects [3,10,11].
fabricate Ti64 with excellent mechanical properties. In order to solve those problems, many researchers have investigated
Recently emerged additive manufacturing (AM) methods, mainly the impact of the parameters of laser energy density and scanning
including selective laser melting (SLM), electron beam melting and strategy on the microstructure and mechanical performance. For ex-
directed energy deposition, have drawn great attention for their out- ample, Song et al. [9] examined the influence of the laser power and
standing advantages over conventional processing methods. Firstly, AM scanning speed on the formability of Ti64 bulks via SLM. They found
is a net shaped process. Equipped with computer-aided design (CAD), that a high laser power and low scanning speed produced cracks be-
AM has high geometrical freedoms compared with traditional methods. cause of the excessive laser energy input. Meanwhile, with increasing

⁎
Corresponding authors.
E-mail addresses: [email protected] (B. Chen), [email protected] (X. Lin).

https://doi.org/10.1016/j.matchar.2020.110358
Received 16 February 2020; Received in revised form 21 April 2020; Accepted 27 April 2020
Available online 30 April 2020
1044-5803/ © 2020 Elsevier Inc. All rights reserved.
Q. Yan, et al. Materials Characterization 164 (2020) 110358

the scanning speed, the powder bed changed from continuous melting
into partial melting due to insufficient laser energy input. Qiu et al. [12]
surveyed the anisotropy behaviors of SLM-fabricated Ti64 in the ver-
tical laser deposition direction and the horizontal orientation. The
tensile test results indicated that the horizontal direction possessed a
higher UTS (~1200 MPa) as well as a limited elongation, while the
vertical direction exhibited a lower UTS (~1100 MPa) and generally
good elongation. In addition, even after post hot isostatic pressing, the
anisotropy phenomenon still existed. Kumar et al. [13] compared AM
Ti64 parts under different laser scan rotation angles (67°–90°). The
results suggested that 67° angle suppressed the formation of prior β
grains, resulting in the houndstooth-shape of melt zone boundaries
which would be the crack initiation during deformation. Those results
illustrated that individual factors had effect on the materials processing,
and eventually on textures and mechanical properties. However, it is
difficult to distinguish the specific contribution of the processing factors
to the performances. More efforts should be done to understand the
relationships among process parameters, microstructure and mechan-
ical properties of AM Ti64 parts. Fig. 1. Morphology of raw Ti64 powders.
Another way to better understand AM Ti64 alloys is a comparison of
the microstructure and mechanical properties of Ti64 processed by AM wavelength of 1070 nm, a maximum power of 200 W in continuous
and conventional methods. From recent review papers [3,14] on AM Ti laser mode as well as a spot size of 70 μm. At first, the raw Ti64
alloys, it seems that as-built SLM Ti64 alloys can have improved tensile powders of 5 kg were loaded into a container. And then, the chamber
strength up to over 1200 MPa compared with those fabricated by temperature was heated up to 373 K with a vacuum of ~1 Pa in the
conventional casting and sintering methods. However, it is unable to building room. Finally, the sample was produced with a laser power of
reach the conclusion that SLM Ti64 alloys have better mechanical 200 W, a scanning speed v of 1000 mm·s−1, a thickness of 30 μm layer,
properties because there are great scatterings in the tensile strength a hatch spacing (h) of 105 μm (Fig. 2c). Each layer scanning trace that
(960–1269 MPa) and elongation (1.4–10.2%) of SLM Ti64 [3]. More- followed a zigzag pattern was rotate 67° one by one with an alternate
over, since distinct raw Ti64 powders were used in SLM and conven- continuous laser mode.
tional processing methods, the difference in alloy compositions and
powder morphology would produce discrepancy in properties. There-
fore, a direct comparison between AM and conventional methods is 2.2. Microstructural characterization
greatly demanded.
In this study, we utilized the same powders to fabricate Ti64 alloys The as-fabricated Ti64 alloy samples were machined by electric
by SLM and some typical sintering methods. The density, micro- spark cutting to designed bulks for a series of tests including density
structure and mechanical performance were characterized to figure out measurements, microstructural characterization and mechanical
the mechanism of discrepancy in mechanical properties. The results testing. The density was measured by the Archimedes method for more
suggested that α′/α, widmanstatten and α + β structures formed under than three times and an average value was achieved. Bulk samples were
different processes. The relationship of processing parameters, micro- polished and then etched by a solution of 5 ml of HF, 10 ml HNO3 and
structures and mechanical properties will be discussed. 85 ml HF [15]. After that, the microstructure characterization of Ti64
bulks was performed via scanning electron microscopy (SEM, TESCAN
2. Experiment VEGA 3 LMU, 3 nm/30 kV, 127 eV). Energy dispersive spectrometer
(EDS) and electron backscattered diffraction (EBSD) characterizations
2.1. Materials and fabrication methods were performed in a double focused ion beam system (Helios NanoLab
G3 UC). The scanning step sizes for EBSD were 0.1 μm for the SLM-built
In this work, the commercially available gas atomized Ti64 powders Ti64 alloy, 0.2 μm for the HP-manufactured Ti64 sample and 1 μm for
(53–103 μm supplied by Sino-Euro Materials Technologies of Xi'an Co., the SPS-manufactured Ti64 alloy, respectively. The nanoscale micro-
LTD.) were used as the raw material (Fig. 1) for hot pressing (HP), spark structure of the SLM sample fabricated by ion thinning (Leica RES102)
plasma sintering (SPS) and selective laser melting (SLM). In the HP was observed by a high-resolution transmission electron microscopy
process, 45 g powders were poured into a graphite die with external (TEM, FEI Talos F200X TEM, 200 kV). The crystallographic structure
diameter of 100 mm and internal diameter of 30 mm (Fig. 2a). Then the and phases were analyzed by X-ray diffraction (XRD, Shimadzu poly-
Ti64 powders was sintered in HP (a maximum load of 3 × 104 kg) at crystalline), using Cu Ka (λ = 1.54 Å) radiation with a power of 3 kW.
sintering temperature of 1195 K for 1 h at a pressure of 30 MPa and a The scan speed was 2.8°·min−1. The elements contents of oxygen, hy-
vacuum of 4.3 × 10−2 Pa. drogen and nitrogen were measured by LECO ONH836.
In the SPS process, the raw powder, 127 g Ti64 powders was first
loaded into a graphite die with external diameter of 76 mm and internal 2.3. Mechanical properties
diameter of 30 mm (Fig. 2b). After that, the raw powder was prepressed
and put into the SPS (LABOX-330, Japan) sintering room with a va- Room temperature tensile tests were conducted on a microcomputer
cuum of ~0.5 Pa. The sintering temperature was 1273 K and keeping control electronic universal testing machine (INSTRON 3382, US) at a
time was 30 min (50 K·s−1 heated to 773 K, 30 K·s−1 heated to 1073 K, strain rate of 10−4 s−1. The tested samples were machined to dog-bone-
and then 20 K·s−1 heated to 1213 K, finally 10 K·s−1 heated into shaped specimens with 40 mm in length, 2 mm in thickness, 20 mm in
1273 K). During sintering, the vacuum was lowered to be < 0.1 Pa. The gauge length and 4 mm in gauge width. In hardness testes, the polished
sample was cooled down in the furnace for about 4 h. The applied samples were tested on a micro/macro automatic hardness testing
pressure during SPS was constantly held on 30 MPa. system (LECO, US) with a load of 300 N keeping for 13 s. The hardness
In the SLM process, the SLM machine AM250 supplied by RENIS- test was repeated ~50 times randomly on the surface with a diagonal
HAW Co. UK was used. It was equipped with a SPI laser system with a length ~40 μm of a diamond indentation shape and the average value

2
Q. Yan, et al. Materials Characterization 164 (2020) 110358

Fig. 2. Illustration of Ti64 processing methods: (a) HP, (b) SPS, (c) SLM.

was calculated. In nano-indentation tests, the polished samples were

displayed on a nano-mechanical testing system (Bruker, US) with a
maximum load of 8000 mN keeping for 2 s. Three random points were
tested on the surface, and the average value was adopted.

3. Results and discussion

3.1. Microstructure

The XRD patterns of as-built Ti64 alloys fabricated by different

processes are shown in Fig. 3. Because of the very small difference in
lattice parameters of hexagonal close-packed (hcp, P63/mmc) α and α′,
it is quite difficult to distinguish these two phases according to the XRD
results [16,17]. Notwithstanding, the α′ phase forms rarely in con-
ventional consolidation processes with low cooling rates, including HP
and SPS processes in this study where furnace cooling was applied with
a cooling rate of ~5 K·min−1. Meanwhile, α′ phase was usually found in
Ti64 alloys fabricated by rapid cooling processes such as the SLM
[12,18] which has an extremely high cooling rate of ~105 K·s−1 [19]
and creates large residual stress in the whole bulk [20]. Therefore, α
and α′ phases are dominant in the HP/SPS and SLM Ti64 alloys, re- Fig. 3. XRD patterns of Ti64 samples fabricated by different processes.
spectively. Moreover, there are two β peaks with inferior intense, viz.
39.8° in the SPS-manufactured Ti64 alloy and 71.7° in both the SPS-
Fig. 4a is a reconstructed three-dimensional image of the SLM Ti64
manufactured and HP-fabricated Ti64 alloy samples, close to the strong
alloy observed in three directions (X, Y and Z, where Z is the deposition
α peaks, namely 40.7° and 71.2° respectively. It suggests that the vo-
direction). It is clear to observe that the martensite (α′) needles have
lume fraction of β is much lower than that of α in the three Ti64 alloys,
same orientations in each plane at microscale, as shown in Fig. 4b–g.
and there is little β in the as-fabricated Ti64 by SLM, which agrees with
The martensite orientation changes at different layers (Fig. 4b–c),
previous studies [21–23].
which should be due to the rotation laser scan strategy of 67° with an
Fig. 4 shows the polishing microstructures of the as-built Ti64 alloy
alternate continuous laser mode [13]. Fig. 4e shows a prior β columnar
sample by SLM observed at different directions and magnifications.

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Q. Yan, et al. Materials Characterization 164 (2020) 110358

Fig. 4. SEM of SLM-fabricated Ti64 alloy: (a) 3D microstructure as-manufactured Ti64 via SLM and Z presenting the laser decomposition direction. (b–c) the X-Z
plane, (d–e) Y-Z plane and (f–i) X-Y plane. Short orange arrows indicate voids. (For interpretation of the references to color in this figure legend, the reader is referred
to the web version of this article.)

Table 1
Density and phase size of as-built Ti64 alloys fabricated by different processes.
Process Density (g·cm−3) Relative density (%) Size

SLM 4.38 97.3 Needle α′ width: ~1 μm, length: ~30 μm

SPS 4.41 98.1 α colony size: ~150 μm
HP 4.41 98.0 α laths width: ~3 μm, length: ~30 μm.
β laths length: ~8 μm

Fig. 5. SEM of SPS-fabricated Ti64 alloy at two magnifications.

crystal filled with full α′ growing along the Z axis, which is due to the voids with submicron size in the as-fabricated SLM Ti64 alloy (marked
epitaxial grain growth dominating on the bottom of the melt pool and by orange arrows in Fig. 4c–e and g–h), which should be owing to the
the elongated β grains oriented towards the center of the melt pool immersion gas and its shrinking during rapid consolidation. In addition,
[19,24]. Moreover, the martensite orientation rotates 30–60° at each unfused powder particles are occasionally observed and they lead to
adjacent scan area (Fig. 4f and g). Meanwhile, there are many closed broad gaps (as shown in Fig. 4h and i), which may be attributed to the

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Q. Yan, et al. Materials Characterization 164 (2020) 110358

Fig. 6. SEM of HP-manufactured Ti64 alloy at different magnifications. (b) and (c) are the box area in (a) and (b), respectively.

Fig. 7. EBSD of SLM-built Ti64 alloy: (a) 3D model of as-built Ti64 via SLM with bond contrast. (b–d) IPF of as-made Ti64 by SLM at different orientation.

occasional coarse powder particles and the comparatively low laser SPS temperature of ~1273 K over the β → α transformation tempera-
density [9]. The defects of voids and unfused powders may lead to the ture (~1263 K [18,22,25]). While, the HP alloy (Fig. 6a–c) is a typical
decrease of density. Thus, the densities of as-built Ti64 alloys are α + β lamellar double-phase structure. The width and length of the α
measured and the results are listed in Table 1. It is seen that the density laths are ~3 μm and ~30 μm, respectively. β laths with width in sub-
and relative density of SLM-built Ti64 alloy are slightly smaller than micron scale exist at the boundaries of α laths. Such morphology is a
those of the two alloys by SPS and HP. It is thus deduced that the small result of sintering temperature in α + β zone and the comparatively
pores (Fig. 4c–i) and small amount of cracks (Fig. 4h and i) in SLM Ti64 slow cooling down rate.
do not have obvious effect on density. The EBSD results of SLM-built Ti64 samples are displayed in Fig. 7.
The SPS-manufactured Ti64 alloy (Fig. 5) has widmanstatten Due to the high cooling rate of the SLM process, a sufficient driving
structure that consists of long α laths inside prior β. The prior β size, or force is yielded to form full α/α′ laths structure [26]. It can be observed
the grain size is as large as ~150 μm because of the comparatively high that there is a similar orientation of α′ inside the prior β boundary,

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Q. Yan, et al. Materials Characterization 164 (2020) 110358

Fig. 8. EBSD of as-built Ti64 via SPS and HP respectively: (a) and (b) IPF of α phase in SPS and HP. (c) IPF of β phase in HP.

Fig. 9. TEM of SLM-fabricated Ti64 alloy: (a) Dark field image. (b) Bright field and (c) SAED of α in (a). (d–f) Elements distribution in (a). (d) Ti element. (e) Al
element. (f) V element.

Table 2 image of the HP-fabricated Ti64 alloy shows that α laths generally
The O, N, H element content of as-built Ti64 by different methods. elongate along the α growth direction (Fig. 8b). However, there seems
Process O content (wt%) N content (wt%) H content (wt%)
to be a 〈111〉 orientation of elongated β (Fig. 8c), which is probably
caused by the axial load pressure during consideration.
SPS 0.14 0.012 0.0016 The TEM microstructure of the SLM-fabricated Ti64 alloy is shown
HP 0.15 0.030 0.0020 in Fig. 9. The bright field transmission electron micrographs (Fig. 9a
SLM 0.22 0.039 0.0066
and b) illustrate that there are many laths with different lengths in
different direction. The selected area electron diffraction (SAED) of the
while the orientation changes in adjacent layers, due to the afore- marked circle area in Fig. 9b reveals the HCP crystal structure with an
mentioned 67° rotation of scan path in each layer. Moreover, no pre- interplanar spacing of 0.2648 nm along {1010} (Fig. 9c). This value is
ferred orientation of α′ laths is observed in the inverse polar figure (IPF) slightly larger than that of α-Ti, namely 0.2555 nm, possibly due to the
images of as-built Ti64 via SLM (Fig. 7b–d). In addition, the prior β lattice distortion caused by the stress and defects during consolidation
grains along the non-laser deposition direction appear to be in a co- [27]. However, it is difficult to distinguish the α′ from α via SAED result
lumnar crystal state (Fig. 7b–d), which is due to the epitaxial grain because of the similar HCP crystal lattice constant, while there are a
growth along the central of the melt pool during SLM consolidation subtle change in c/a values of α′ (1.58) and α (1.59–1.6) respectively
[19]. The IPF image of SPS-manufactured Ti64 emerges a state of coarse [13,28]. An EDS mapping analysis was performed at the area corre-
columnar α without a preferred orientation (Fig. 8a). While the IPF sponded to the image (Fig. 9a) and the elements (Ti, Al and V)

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Q. Yan, et al. Materials Characterization 164 (2020) 110358

respectively. It is probably caused by the limited vacuum state (~1 Pa)

during SLM [30], especially in discontinuous SLM process [8], which is
a little higher than those of the used SPS and HP (< 0.1 Pa). However,
the differences of these contents are small, all < 0.1 wt%, which may
have small effect on the microstructures and properties of Ti64 alloys.

3.2. Mechanical performance

Fig. 10 shows the nominal tensile stress-strain curves of Ti64 alloys

fabricated by different methods and the obtained properties are sum-
marized in Table 3. Comparing with Ti64 alloys fabricated by SPS and
forging, Ti64 fabricated by SLM possesses a high yield strength
(946 MPa, 12% improvement), a high ultimate tensile strength (UTS,
1151 MPa, 24% improvement) and high hardness (408 Hv, ~20%
improvement). Notwithstanding, the plasticity of SLM-built Ti64 alloy
is limited at 4.4%, which is similar to that of the SPS alloy (4.6%) but
much smaller than that of the forged alloy (15%). Compared with lit-
eratures on SLM Ti64 alloys [31–34], it is found that the tensile prop-
erties of the SLM Ti64 alloy in the present study fall into the range
Fig. 10. Tensile performance of Ti64 alloys manufactured by different methods.
reported by previous studies (Table 3).
The comparatively low tensile strength and good plasticity of the
forged Ti64 alloy are due to the α + β structure with high volume
distributions are shown in Fig. 9d–f. It can be clearly observed that the fraction of soft and ductile β phase [35]. The comparative low tensile
elements of Al and V distribute uniformly without any obvious element strength and poor plasticity of the SPS Ti64 alloy should be due to the
segregation. There is no noticeable difference in elements distribution exceedingly large prior β size of the widmanstatten structure
among different phases, which can confirm that α/α′ phase may not (~150 μm, Fig. 5). The high tensile strength of SLM Ti64 alloys is
cause serious elements segregation [29]. predominant because of the observed fine α/α′ structure (Figs. 4 and 7)
The light elements of oxygen, hydrogen, nitrogen are difficult to be which has been proved to be high strength and tough [36,37]. How-
identified in EDS. Therefore, their contents were measured in bulk ever, the poor plasticity is related to the structural defects, mainly
samples by a combustion method and the results are listed in Table 2. It consisting of pores and unfused areas (Fig. 4). Since the pores or voids
illustrates that those atmospheric elements in SLM-built Ti64 alloy are a are closed, very fine (~2 μm) and few (< 1 vol%) (Fig. 4), they may
little higher than that of Ti64 alloy samples fabricated by SPS and HP have little influence on the mechanical properties [32]. Therefore, the

Fig. 11. SEM of tensile fracture in as-built Ti64 by SLM: (a) the whole fracture image and (b) the magnification box area in (a). (c) Cracks in as-built Ti64. (d) A brittle
fracture area. (e) A selected magnification area in (d). (f) The specific magnification area in (c). (For interpretation of the references to color in this figure, the reader
is referred to the web version of this article.)

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Q. Yan, et al. Materials Characterization 164 (2020) 110358

Fig. 12. SEM of tensile broken area in SPS-fabricated Ti64 alloys: (a) The mixed brittle and ductile broken area. (b) The magnification box area in (a). (c) The
interface between ductile and transgranular broken area. (d) The ductile broken area.

Table 3
Mechanical properties of as-built Ti64 via different methods.
Process Tensile properties Hardness Reference

δ0.2 (MPa) UTS (MPa) El. (%) HV

SPS 847 ± 12 931 ± 12 4.6 ± 0.8 336 ± 20 This work

Forged 846 ± 17 932 ± 14 15.0 ± 0.6 – This work
HP – – – 342 ± 15 This work
SLM 946 ± 10 1151 ± 9 4.4 ± 0.7 408 ± 40 This work
962 ± 47 1166 ± 25 1.7 ± 0.3 – [31]
1137 ± 20 1206 ± 8 7.6 ± 1.7 – [31]
1066 ± 91 1148 ± 80 5.4 ± 3.8 – [32]
978 ± 5 1143 ± 6 11.8 ± 0.5 – [33]

poor ductility should be related to the large-sized unfused areas in SLM

Ti64 alloys (Fig. 4h and i).
Fig. 11 depicts the fracture of morphology of as-built Ti64 via SLM
after tensile testing. It is observed that there are some unfused powder
particles (marked in yellow arrow at Fig. 11a–d) and cracks (marked in
blue arrow at Fig. 11c). Fig. 11c illustrates a large vertical crack
Fig. 13. Nanoindentation load-depth curves of as-built Ti64 alloys.
(~20 μm in width and ~100 μm in length) on the fracture surface,
which is probably enlarged during tensile test by the unfused particle
(Fig. 4i). In despite of many defects, there are still a large number of transgranular fracture is clearly observed (Fig. 12a and b), owing to the
dimples on the fracture surface (Fig. 11f, the magnified box in Fig. 11c), limited deformability of the coarse grains. However, there are still a
which suggests that the SLM-fabricated Ti64 failed in ductile mode large number of dimples in the fracture, agreeing with the moderate
during tensile testing. However, there are some areas with brittle ductility (4.6% in elongation) of the SPS Ti64 alloy (Table 3).
fracture characteristics closed to the unfused area (Fig. 11d). From the Fig. 13 shows the nano-indentation test results of as-fabricated Ti64
local view (Fig. 11e), it illustrates that the unfused area trend to form alloys. It is observed that the nano-indentation curves of the SLM-built
stress concentration, where the induced cracks is growing instability Ti64 at different planes are fitting very well, which suggests the iso-
lead to transgranular fracture. Therefore, the unfused areas lead to poor tropy of Young's modulus. In addition, the measured Young's modulus
ductility of SLM Ti64 alloys. With the SPS-fabricated Ti64 alloys, of SLM-built Ti64 is 95.4 ± 2.1 GPa which is similar to that of SPS-

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Q. Yan, et al. Materials Characterization 164 (2020) 110358

Talents Promotion Plan of Xi'an Association for Science and

Technology.

Data availability

The raw data required to reproduce these findings are available to

download from 10.17632/5pkzvmrr45.1.

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