Journal of Materials Science & Technology 57 (2020) 51–64

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Research Article

Selective laser melting of near-␣ titanium alloy Ti-6Al-2Zr-1Mo-1V:

Parameter optimization, heat treatment and mechanical performance
Chao Cai a , Xu Wu a , Wan Liu b , Wei Zhu a , Hui Chen c , Jasper Chua Dong Qiu d ,
Chen-Nan Sun d , Jie Liu a,∗ , Qingsong Wei a,∗ , Yusheng Shi a
a
State Key Laboratory of Materials Processing and Die & Mould Technology, Huazhong University of Science and Technology, Wuhan, 430074, China
b
Hubei Rehabilitation Assistive Technology Centre, Wuhan, 430074, China
c
Department of Mechanical Engineering, National University of Singapore, Singapore, 117575, Singapore
d
Singapore Institute of Manufacturing Technology, A*STAR, 73 Nanyang Drive, Singapore, 637662, Singapore

a r t i c l e i n f o a b s t r a c t

Article history: This paper presents a comprehensive study conducted to optimize the selective laser melting (SLM)
Received 25 November 2019 parameters and subsequent heat-treatment temperatures for near-␣ high-temperature titanium alloy
Received in revised form 8 January 2020 Ti-6Al-2Zr-1Mo-1 V (TA15), which is widely used in the aerospace industry. Based on the surface mor-
Accepted 3 March 2020
phology and relative density analysis, the optimized process parameters were: laser power from 230 W
Available online 12 May 2020
to 380 W, scan speed from 675 mm/s to 800 mm/s, scan spacing of 0.12 mm, and layer thickness of
0.03 mm. The effects of the laser power and the layer thickness on the phase constitutions, microstruc-
Keywords:
ture features, as well as room-temperature and high-temperature (500 ◦ C) tensile properties, were then
Selective laser melting
Near-␣ titanium
studied to obtain an in-depth understanding of SLM-built TA15. Six typical temperatures (650, 750,
Heat treatment 850, 950, 1000 and 1100 ◦ C) covering three representative temperature ranges, i.e., martensite partial
High-temperature tensile properties decomposition temperature range, martensite complete decomposition temperature range and above ␤
transus temperature, were subsequently selected as heat-treatment temperatures. The heat treatment-
microstructure-mechanical property relationships of SLM-built TA15 were elucidated in detail. These
results provide valuable information on the development of SLM-built TA15 alloy for industrial appli-
cations, and these findings are also beneficial to additive manufacturing of other near-␣ Ti alloys with
desirable high-temperature properties.
© 2020 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science &
Technology.

1. Introduction porosity and composition segregation [3]. Machining of titanium

Titanium and its alloys are extensively applied in the aerospace,
marine, defense industries, and biomedical devices as they have
an excellent combination of outstanding mechanical strength,
low density, extraordinary corrosion resistance, and remark-
able bio-compatibility. As a result, many titanium alloy parts
with good mechanical properties and complex geometries have
been designed and manufactured to meet the specific service
environments, especially those involving aerospace and defense
applications [1,2]. Currently, the manufacture of these titanium
alloy products mainly relies on casting and machining. Unfortu-
nately, cast titanium alloy parts generally have relatively weak
mechanical properties resulting from metallurgical defects, e.g.,
∗ Corresponding authors.
E-mail addresses: hustliuj@hust.edu.cn (J. Liu), wqs xn@hust.edu.cn (Q. Wei).
alloys is challenging owing to their poor thermal conductivity,
the propensity to harden under strain, a large amount of material
waste, and high manufacturing costs [4].
Selective laser melting (SLM) can be used to custom-fabricate
nearly fully-dense components directly from computer-aided-
design (CAD) models using a highly focused laser beam to melt
metallic powders in a layer-by-layer manner selectively. SLM,
allowing for a high degree of flexibility to achieve complex designs,
shorter processing time, and high forming accuracy, can overcome
the limitations of conventional methods as above-mentioned [5].
Ever since the invention of the SLM process in the late 1990s, this
promising technique has continuously attracted the attention of
academic and industrial researchers regarding the fabrication of
titanium alloys. Qiu et al. applied a square-island scanning strat-
egy to realize better homogeneous thermal distribution within
(␣ + ␤) type Ti-6Al-4 V parts, and then adopted hot isostatic press-
ing as a post-treatment to relieve thermal stress and close pores

https://doi.org/10.1016/j.jmst.2020.05.004
1005-0302/© 2020 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science & Technology.
52 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
Fig. 1. (a, b) Morphology and size distribution of the as-received TA15 powder, (c) an HRPM-II type SLM machine and the SLM scanning strategy, and (d) printed metallographic
and tensile specimens.
in the printed parts [6]. The resultant parts showed tensile proper-
ties comparable to those of thermo-mechanically processed and
annealed counterparts. Xu et al. designed innovative SLM pro-
cessing routes to decompose unflavored ␣ martensite into a
lath-like (␣ + ␤) microstructure in-situ with tunable length scales
ranging from 0.15 ␮m to 0.18 ␮m by controlling the tempera-
ture field in the previously solidified layers within the 600−850 ◦ C
temperature range [7]. The SLM-built parts with such lath-like
(␣ + ␤) microstructures exhibited superior tensile strength, which
markedly exceeded ASTM standards as well as the majority of
Ti-6Al-4 V samples fabricated by other additive manufacturing pro-
cesses. Sabban et al. explored a novel heat treatment procedure,
involving repeated thermal cycling close to but below the ␤ transus
(␤tr ) temperature, to eliminate acicular martensite and gener-
ate globular ␣ grains to improve room-temperature strength and
toughness [8]. Apart from (␣ + ␤) type Ti-6Al-4 V alloy, the process-
microstructure-property relationships of many SLM-built ␣-type
titanium alloys (e.g. pure titanium [9] and Ti-5Al-2.5Sn [10]) and
␤-type titanium alloys (e.g. Ti-24Nb-4Zr-8Sn [11], Ti-13Nb-13Zr
[12], and Ti-5Al-5V-5Mo-3Cr [13]) have also been investigated.
The studies mentioned above mainly focus on how to improve
room-temperature mechanical performance by optimizing the
processing parameters and post-heat treatments. However, cer-
tain near-␣ Ti alloys are specially designed for harsh and
high-temperature environments encountered in the aerospace
applications. Evaluating their mechanical properties at the cor-
responding usage temperatures is more valuable than evaluating
their room-temperature properties for technical guidance and
industrial applications [14–17]. However, studies that report on
the high-temperature mechanical performance of SLM-fabricated
near-␣ Ti alloys are few.
Ti-6Al-2Zr-1Mo-1 V (TA15), is a type of near-␣ titanium alloy
that is widely used in the large-scale production of integral com-
ponents with irregular geometries for the aerospace industry. The
moderate strength of this alloy at both room and high tempera-
tures makes it optimal for the fabrication of bulkheads and nacelle
center beam frames [18]. The development of advanced SLM tech-
nique provides new opportunities to manufacture such key TA15
components with geometrical complexity. Therefore, in this work,
a systematic investigation on optimizing the SLM process parame-
ters and post-heat treatments for TA15 was carried out to evaluate
the feasibility of the SLM technique as an alternative method to
manufacture this near-␣ Ti alloy. The study focused on investigat-
ing and establishing an in-depth understanding of the correlations
between microstructural characteristics and tensile performance
(at room temperature and 500 ◦ C) for SLM-built TA15. This research
should be meaningful for the additive manufacturing of specific
near-␣ Ti alloys applied in high-temperature environments, and
should further promote the SLM process as a potential technique
for the fabrication of difficult-to-process components demanding
high mechanical properties in the aerospace field.
2. Experimental procedures
2.1. Powder material
Gas-atomized TA15 powder particles, showing near-spherical
shape with a mean size (D50 ) of 34.9 ␮m (Fig. 1(a) and (b)), were
purchased from AMC Powders Company, China.
2.2. SLM experiment and heat treatment
In this work, laser power (180 W to 380 W), scan speed
(300 mm/s to 800 mm/s), layer thickness (0.03 and 0.06 mm)
and constant scan spacing (0.12 mm) were adapted on our self-
developed machine for sample preparation using a baseplate
 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
Fig. 2. Chart of SLM processing parameters for TA15 alloy. Three typical optical metallographic (OM) images demonstrate over-melted, well-melted, and porous top surfaces
of printed samples, which are represented by red, green, and blue, respectively.
Fig. 3. Relative density histogram of the printed samples.
preheating temperature of 200 ◦ C and the 67◦ scanning direction
rotation between successive layers [19]. Cubes with a dimension of
5 mm × 5 mm × 5 mm were printed using these processing param-
eters for density testing. Then, metallographic specimens, and
room-temperature and high-temperature tensile samples, were
fabricated using the preliminary optimized processing parameters,
as shown in Fig. 1(d).
Heat treatments were applied to the samples manufactured
using the optimal SLM processing parameters. Six representative
temperatures of 650, 750, 850, 950, 1000, and 1100 ◦ C were selected
as heat-treatment temperatures under a heating rate of 10 ◦ C/min,
a holding time of 2 h and furnace cooling.
2.3. Microstructural and mechanical testing
The densities of the samples were determined using Archimedes
method. The SLM-built samples were tested by an x-ray diffrac-
tion (XRD) machine equipped with a Cu anticathode (␭ = 1.5406 Å)
operated at 35 kV and 40 mA under a continuous scan mode for
phase identification. The metallographic samples were ground, pol-
ished and etched with Kroll reagent for 20 s. The microstructural
observations were characterized by Quanta650 FEG, and the crys-
tallographic orientation of the samples was examined using Sirion
200 instrument with a TSL/EDAX system (Holland). Before elec-
53
Fig. 4. X-ray diffraction patterns of the as-received powder and the SLM-processed
samples with different laser power.
tron backscatter diffraction (EBSD) analysis, the samples were first
re-mechanically polished, and then electrolytically polished in 8
% perchoric acid and 92 % ethanol solution at 27 V under 25 ◦ C
for 25 s. A scan speed of 5◦ /min was conducted over a wide range
of 2 = 20◦ –80◦ on all samples. Transmission electron microscopy
(TEM) was conducted using an FEI Tecnai G20 machine.
Room-temperature and high-temperatures (500 ◦ C) tensile
tests were carried out on SLM-built samples with and without heat
treatment using a Zwick/Roell Z010 machine with a cross-head
speed of 1 mm/min.
3. Results
3.1. Effects of SLM processing parameter
3.1.1. Preliminary processing parameter study
The metallurgical quality, densification level, and associated
mechanical performance of SLM-printed metal parts are dependent
on two main parameters: laser power and scan speed [20,21]. Thus,
these two crucial parameters (laser power from 180 W to 380 W
and scan speed from 300 mm/s to 800 mm/s) were chosen to print
5 mm × 5 mm × 5 mm block samples for preliminary processing
parameter optimization. Based on the top-surface morphologies of
the printed samples, the processing window was divided into three
representative zones, i.e., high energy density zone (Zone A), suit-
54 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
Fig. 5. Low-magnification side-surface morphologies of the printed samples: (a) S17, (b) S18, (c) S19, and (d) S20.
able energy density zone (Zone B), and insufficient energy density
zone (Zone C), as shown in Fig. 2. High laser power coupled with
low scan speed, resulted in high energy densities, causing over-
melted top surfaces and microscopic balling effect, which were also
reported in SLM-built Ti-6Al-4 V and Ti-5Al-2.5Sn alloys [22,23]. An
adequate energy density input into the TA15 powder bed formed
stable melt pools with proper overlap ratios, successive tracks, and
a dense surface. An insufficient energy input resulted in melt pools
with a relatively narrow width, giving rise to inadequate over-
lap ratios and weak metallurgical bonding between adjacent melt
tracks.
The relative density of all printed samples (25 in total) was
measured by the Archimedes’ principle to further determine the
optimal processing parameter range, and the results are shown in
Fig. 3. Printed samples S14, S17-S20, and S23-S25 had high densities
of greater than 99.5 %. Therefore, according to the top surface mor-
phology and bulk density, a laser power from 230 W to 380 W and
a scan speed from 675 mm/s to 800 mm/s were deemed as the opti-
mized parameter ranges for SLM-built TA15 alloy. Because of the
narrow optical scan speed range, the broad laser power range has a
more significant impact on the microstructure and mechanical per-
formance of the SLM-built samples. Hence, the effect of laser power
on the microstructure and mechanical performance of samples S17
to S20 was studied further.
3.1.2. Effect of laser power on microstructure and mechanical
properties
Fig. 4 shows the XRD spectrum of the as-received powder and
the SLM-built samples (S17, S18, S19, and S20). XRD peaks corre-
sponding to the ␤ phase were not detected, and overall diffraction
peaks of HCP ␣ -Ti could be identified as a result of the rapid melt-
ing/solidification of TA15 alloy during the SLM process, leading to
the formation of this non-equilibrium phase [6].
Fig. 5 shows the low-magnification side-surface morpholo-
gies of samples S17, S18, S19, and S20. Martensite-dominated
microstructures, consisting of a substantial amount of needle-like
␣ martensite with a nano-sized width and a length below 200 ␮m
embedded within the columnar prior-␤ phase were observed in all
samples. Other than melting the current powder layer, the laser can
penetrate through several previously deposited layers during the
layer-wise melting process, which leads to the solidification and
epitaxial growth of the prior-␤ phase along the steep temperature
gradient in the building direction. It should be noted that there
was an overall increasing tendency in the width of the columnar
prior-␤ grain boundaries from approximately 80 ␮m–200 ␮m as
laser power increased. The width of the columnar prior-␤ grains
is mainly determined by the width of the melt pool and its heat-
affected zone. It is reasonable to state that the width of the melt
pool and its heat-affected zone are proportional to the laser power
if all other parameters are kept constant. Moreover, most of the aci-
cular martensitic ␣ phase within the same prior-␤ grain showed
an approximate orientation of ± 45◦ to the prior-␤ grain bound-
aries, because of the Burgers orientation relationship between the
␤ and ␣ phases during the fast solidification SLM process [6,24].
To observe the microstructure in more detail, sample S17
was observed under high-resolution TEM (HRTEM), as shown in
Fig. 6. Apart from the needle-like ␣ matrix, several parallel fine
twins with a nanoscale thickness could be distinctly observed and
were also verified by the HRTEM measurement (Fig. 6(d)). These
nanoscale twins could be classified into two different categories:
deformation twins and annealing twins. The former are induced
by the residual stress from the mismatched cooling rates between
 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64 55

Fig. 6. TEM results of SLM-built sample S17: (a) bright-field image, (b) magnified image of nano-size twins in Area A, (c) HRTEM image of nano-size twins in Area B, (d)
magnified image of needle-like structures, and (e), (f), and (g) correspond to the SAD patterns of points I, II, and III in (d), respectively.

the top layer and the previously solidified layers during the SLM Table 1
Room-temperature and high-temperature tensile properties for the printed TA15
process, while the latter result from the previously solidified lay-
alloy samples under varied SLM processing parameters and heat treatments.
ers being re-heated or partially re-melted again during melting
of the top layer, which has a similar effect as an annealing treat- Samples Room temperature 500 ◦ C
ment. Nanoscale twins are beneficial to enhance the strength and UTS (MPa) EI (%) UTS (MPa) EI (%)
ductility of the SLM-built TA15 simultaneously, which was demon-
S17 1422.1 ± 50.2 9.5 ± 1.5 990.2 ± 2.2 15.6 ± 1.9
strated and discussed in our previous study [19]. The ␣ and ␣ phases S18 1362.6 ± 46.2 9.3 ± 0.4 949.6 ± 19.6 13.6 ± 3.2
possess a similar HCP crystalline structure and characteristic XRD S19 1349.8 ± 26.7 5.6 ± 0.1 909.4 ± 40.1 12.5 ± 0.4
diffraction peaks. It is difficult to distinguish between the needle- S20 1063.6 ± 136.9 7.5 ± 0.5 939.5 ± 20.7 15.3 ± 1.7
like ␣ and ␣ phase structures using only the XRD examination; the S26 1234.2 ± 53.1 7.3 ± 0.7 907.5 ± 4.9 11.8 ± 0.4
S26 + HT1 1207.3 ± 3.8 8.9 ± 0.1 853.2 ± 10.7 12.5 ± 1.1
␣ phase has a crystal structure with a c/a ratio of approximately S26 + HT2 1123.6 ± 14.0 11.3 ± 0.7 757.1 ± 7.0 13.4 ± 1.1
1.58, which is slightly lower than that of the ␣ phase (1.59–1.60) S26 + HT3 1024.9 ± 19.5 9.0 ± 0.4 715.3 ± 4.3 13.0 ± 0.9
[25]. From the selected area diffraction (SAD) results shown in S26 + HT4 936.5 ± 4.9 8.0 ± 1.0 639.8 ± 6.7 14.3 ± 0.9
Fig. 6(e)-(g), the c/a values of the successive lath-like structures S26 + HT5 906.9 ± 5.5 5.8 ± 0.2 602.0 ± 5.6 15.9 ± 5.0
S26 + HT6 780.6 ± 7.2 3.8 ± 0.4 596.3 ± 5.6 15.6 ± 2.5
I, II, and III were 1.581, 1.578, and 1.575, respectively, confirming
Wrought TA15 [24] 965 18.8 680 24.8
that the needle-like structures are the ␣ phase.
Top-surface EBSD crystal orientation and inverse pole figure
(IPF) maps of the four samples are shown in Fig. 7. The overall
microstructures of these four samples showed similar fine grains, ature and 500 ◦ C. Sample S17 exhibited the highest UTS (1422 MPa
presenting basket-weave morphologies consisting of interlaced and 990 MPa) and EL (9.5 % and 15.6 %) at room temperature
needle-like martensitic phase. and 500 ◦ C, respectively. The room-temperature tensile strength of
Table 1 summarizes the ultimate tensile strength (UTS) and these samples continuously decreased with increasing laser power.
elongation (EL) of samples S17, S18, S19, and S20 at room temper- The high-temperature tensile strength did not exhibit an evi-
dent declining tendency, suggesting that room-temperature tensile
56 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64

Fig. 7. Top-surface EBSD grain orientation and IPF maps of TA15 samples: (a) S17, (b) S18, (c) S19, and (d) S20.

strength was more sensitive to laser power than high-temperature strate a significant difference among the four samples. All samples
tensile strength for SLM-built TA15 alloy. presented a ductile fracture behavior with coarse and deep dimples
The fracture surfaces of the tensile specimens at room temper- observed on the fracture surface.
ature are shown in Fig. 8. The fracture surface of sample S17 was
almost fully covered by near-equiaxed dimples, indicative of a duc-
3.1.3. Effect of layer thickness on microstructure and mechanical
tile fracture feature and good ductility. For sample S18, the fracture
properties
surface was also mainly decorated by dimples, along with some
The layer thickness increment is a more effective method to
near-spherical pores, suggesting a relatively weaker metallurgi-
shorten printing time and improve forming efficiency in contrast to
cal bonding. This is one of the reasons why the tensile strength
increasing the scan speed or the hatch spacing. Hence, in the follow-
of sample S18 was slightly lower than that of sample S17. With
ing study, the layer thickness was increased from 30 ␮m to 60 ␮m
the increase of laser power to 330 W (sample S19), the fracture
and the remaining parameters were kept the same as those used
morphology transformed into a brittle rupture; a high number of
for S17, as this sample possessed the best tensile properties among
typical river-like cleavage patterns could be seen. When the higher
the other printed parts manufactured using optimized parameters.
laser power of 380 W was applied, the fracture surface of sample
The sample printed with 60 ␮m layer thickness is denoted as S26
S20 consisted of cleavage steps, tear ridges, fine spherical pores,
hereafter.
and near-equiaxed dimples, implying a brittle-ductile mixed-mode
The side-surface OM images of the microstructures of samples
fracture behavior. All fracture morphologies were consistent with
S17 and S26 are shown in Fig. 10. The length of prior-␤ phase
the tensile results presented in Table 1.
boundaries spanned the entire surface along the build direction for
The high-temperature fracture surfaces of the four specimens
sample S17, while the length in sample S26 was less than 200 ␮m.
are shown in Fig. 9. Compared with the room-temperature fracture
This occurs because the layer-wise tracks break off the link of the ␤
surfaces, the high-temperature fracture features did not demon-
phase along the printing direction. This implies that for sample S26,
 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64 57

Fig. 8. Fracture surfaces of the four samples: (a) S17, (b) S18, (c) S19, and (d) S20 after tensile testing at room temperature.

Fig. 9. Fracture surfaces of the four samples: (a) S17, (b) S18, (c) S19, and (d) S20 after tensile testing at 500 ◦ C.
58 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
Fig. 10. Side-surface OM microstructures of samples under various layer thicknesses: (a) S17 with 30 ␮m layer thickness and (b) S26 with 60 ␮m layer thickness.
Fig. 11. X-ray patterns of untreated S26 sample and S26 samples with heat treat-
ments HT1 (650 ◦ C), HT2 (750 ◦ C), HT3 (850 ◦ C), HT4 (950 ◦ C), HT5 (1000 ◦ C), and
HT6 (1100 ◦ C).
the top layer absorbs most of the laser energy, resulting in insuf-
ficient laser energy available to penetrate through the previously
deposited layers. It is also difficult for this laser energy to gener-
ate a sufficient temperature gradient for ␤ phase growth along the
vertical direction.
The tensile strength of sample S26 at room temperature and
500 ◦ C was slightly lowered by 13.2 % and 8.4 %, respectively,
in comparison to those of sample S17 (Table 1). It is notewor-
thy that the tensile strength of sample S26 was still superior to
its wrought counterpart at both room temperature and 500 ◦ C,
whereas the ductility of both S17 and S26 was lower than that
of the wrought one [26]. High tensile strength coupled with poor
ductility is a common phenomenon for SLM-built metallic parts,
especially for titanium alloys. The ␣ martensitic phase is a hard and
brittle non-equilibrium phase that is weak in resisting crack initi-
ation and propagation, leading to SLM-built titanium alloys with
superb strength but low elongation. The undesired ␣ martensitic
phase can decompose into a more stable and ductile lath-like ␣/␤
structure above its decomposition temperature. Accordingly, six
different heat-treatment temperatures were chosen to realize ␣
martensitic phase transformation into an ␣/␤ mixed structure with
tunable length and to obtain an attractive combination of strength
and ductility for SLM-built TA15, as discussed in the following sec-
tion.
3.2. Effect of heat-treatment temperature
The room-temperature and high-temperature tensile strength
values of sample S26 were slightly lower than those of sample S17,
yet were 27.9 % and 33.4 % higher than those of the wrought sample
[26], respectively. More importantly, the manufacturing time can
be shortened by half when the layer thickness is increased from
30 ␮m to 60 ␮m. In this regard, the S26 parameters are more time-
saving and are more likely to be applied in industrial production.
Consequently, S26 samples were selected for the heat-treatment
temperature optimization study.
Martensite begins to transform into the ␣/␤ structure at 575 ◦ C
[7], and the complete decomposition of martensite is obtained at
temperatures above 800 ◦ C [27]. The ␤tr temperature of TA15 alloy
was calculated using the linear regression analysis proposed by Guo
et al., given as follows [28]:
␤tr = 882 + 21.1[Al]–6.9[Zr]–9.5[Mo]–11.8[V]
Here [M] is the weight fraction of the alloy element M. For the
chemical composition of Ti-6Al-2Zr-1Mo-1 V, the ␣tr temperature
of 973.5 ◦ C was determined by this equation. Based on the ini-
tial martensite decomposition temperature of 575 ◦ C, the complete
decomposition temperature of 800 ◦ C, and the ␤tr temperature
of 973.5 ◦ C, six different temperatures in the three representative
temperature ranges were chosen and applied in the following heat-
treatment experiments.
(i) Heat-treatment temperatures of 650 ◦ C and 750 ◦ C in the
martensite partial decomposition temperature range.
(ii) Heat-treatment temperatures of 850 ◦ C and 950 ◦ C in the
martensite complete decomposition temperature range.
(iii) Heat-treatment temperatures of 1000 ◦ C and 1100 ◦ C in the
range above the ␤tr temperature.
The heat-treated samples at 650, 750, 850, 950 1000, and
1100 ◦ C are denoted as HT1, HT2, HT3, HT4, HT5, and HT6, respec-
tively. X-ray diffraction patterns of untreated S26 and heat-treated
samples are shown in Fig. 11. All diffraction peaks of ␣ /␣ phases
could be detected in all samples, and a weak diffraction peak for
the (110) plane of the ␤ phase at 38.4 ◦ C was found in the post-
treated samples HT3, HT4, HT5, and HT6. This result indicated that
(i) the minor amount of ␤ phase in samples HT1, and HT2 was
insufficient to produce observable diffraction peaks in the XRD
examination, owing to the incomplete decomposition of the ␣
phase; (ii) the HCP-Ti phase was still the dominant phase, even
for samples treated above the ␤tr temperature.
 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64 59

Fig. 12. Microstructures of untreated S26 sample and heat-treated samples in the partial martensitic decomposition temperature range: (a, b) untreated S26, (c, d) HT1
(650 ◦ C), and (e, f) HT2 (750 ◦ C). White and yellow arrows indicate needle-like structure and lath-like structures, respectively.

The microstructures of untreated S26 sample and heat-treated
samples HT1 and HT2 are shown in Fig. 12. Partial needle-like struc-
tures were retained and the decomposed needle-like ␣ martensitic
phase transformed into fine lath-like ␣/␤ structures with hundred-
nanometer thickness in HT1 sample. When the heat treatment
temperature was increased to 750 ◦ C, most of the needle-like struc-
tures faded away and turned into a mixture of microstructures
comprised of the nano-sized ␤ phase embedded within the lath-
like ␣/␤ structure spacing in sample HT2. The transformation from
the ␤ phase into the ␣ phase during the SLM process is a diffu-
sionless transformation because of the super high cooling rate of
104 -106 ◦ C/s, causing the supersaturated ␤-phase stabilizing ele-
ments (Zr, Mo, and V) to become trapped in the ␣ phase. During
the heat treatment, the ␣ phase will nucleate along the needle-like
␣ boundaries, and ␤-phase stabilizing elements are expulsed from
the ␣ /␣ phases, resulting in the nano-sized ␤ phase forming within
the lath-like structures.
When the heat-treatment temperatures were further increased
to the martensite complete decomposition temperature range, the
needle-like ␣ structure disappeared, and lath-like ␣/␤ structures
were homogeneously distributed within samples HT3 and HT4, as
shown in Fig. 13. When the heat-treatment temperatures were
increased to above the ␤tr temperature, as shown in Fig. 14, the
microstructures of samples HT5 and HT6 showed a typical Wid-
manstatten structure composed of coarse lamellar and lath-like
structures with greater than 10-micrometer thickness, which was
much coarser than that of the heat-treated samples below the
␤tr temperature. This is because the atom diffusion coefficient in
HCP ␣-Ti is two orders of magnitude lower than that in BCC ␤-Ti,
and the grain will be much easier to grow once the heat temper-
60 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
Fig. 13. Microstructures of heat-treated samples in the complete martensitic decomposition temperature range: (a, b) HT3 (850 ◦ C) and (c, d) HT4 (950 ◦ C).
Table 2
Microstructure type and constituent phase of the S26 sample and heat-treatment
samples in this study.
Sample Microstructure type and constituent phase
S26 Full needle-like ␣ martensitic phase
HT1 Fine lath-like (␣ + ␤) with needle-like ␣ martensitic phase
HT2 Fine lath-like (␣ + ␤) with minority needle-like ␣ martensitic phase
HT3 Full lath-like (␣ + ␤)
HT4 Full lath-like (␣ + ␤)
HT5 Lath-like (␣ + ␤) with minority coarse lamellar (␣ + ␤)
HT6 Coarse lamellar (␣ + ␤) with minority lath-like (␣ + ␤)
ature exceeds the ␤tr temperature [15]. This can be verified by
EBSD results, as shown in Fig. 15. The average grain size of sam-
ple HT5 was approximately twice as large as that of sample HT4
even though the heat-treatment temperature was only increased
by 100 ◦ C. The variation of microstructure types and phase con-
stituents for heat-treated samples is summarized in Table 2.
A comparison diagram of tensile properties for the S26 sam-
ples with and without heat treatments at room temperature and
500 ◦ C is shown in Fig. 16. For the room-temperature tensile proper-
ties, the tensile strength of the heat-treated samples was inversely
proportional to the heat-treatment temperature. The elongation
of the heat-treated samples increased and reached its highest
value with the increase of heat-treatment temperature at the HT2
temperature, but then began to decrease for all the heat-treated
samples gradually. The high-temperature tensile strength of the
post heat-treated samples exhibited a linear improvement as the
heat-treatment temperature increased. In contrast, the ductility of
the heat-treated samples showed an opposite trend compared to
the high-temperature tensile strength.
4. Discussion
4.1. Laser power-microstructure-tensile property relationships
From the tensile results (Table 1), it can be concluded that
sample S17 exhibited the best tensile strength and elongation com-
bination compared to the three other optimized samples (S18,
S19 and S20). The room-temperature tensile strength gradually
decreased with increasing laser power, even though all the sam-
ples possessed an identical martensitic phase and a similar average
grain size (Fig. 7). This result can be attributed to three aspects as
follows.
(i) Relative density
A denser SLM-built part with less porosity is favorable to obtain
a better combination of strength and ductility. The relative den-
sities for samples S17, S18, S19 and S20 (Fig. 3) were 99.97 %,
99.81 %, 99.44 %, and 99.36 %, respectively, Additionally, the poros-
ity of samples S17, S18, S19, and S20 calculated from OM images
via Image-Pro Plus 6.0 software was 0.01, 0.024, 0.071, and 0.145,
respectively. The OM porosity results corresponded well with the
Archimedes’ results and with room-temperature tensile strength
results.
(ii) Metallurgical quality
From the room-temperature fracture surfaces (Fig. 8), many
dozens of micron-sized pores were observed in the S18 fracture
surface, which was a typical inter-particle facture feature stemming
from the weak metallurgical bonding among the melted powders.
 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
Fig. 14. Microstructures of heat-treated samples above the ␤tr temperature: (a, b) HT5 (1000 ◦ C) and (c, d) HT6 (1100 ◦ C). Yellow arrows indicate the lamellar structure.
In addition, a large number of pores with several micrometers in
size, similar to the as-received powder size were distributed on the
S19 and S20 facture surfaces. These findings imply that many met-
allurgical defects existed in samples S18, S19, and S20. Gu et al.
reported that high energy density would cause overheating and
instability in the melt pool as well as a reduction in the surface
energy of the melt pool, resulting in the splashing of small-sized
liquid droplets from the front of the liquid melt pool [22]. After
these small-sized droplets solidify, they will impede the uniform
spread of fresh powder on the previous layer and tend to induce
further defects such as porosity and cracks. This is also the reason
why the porosity of the printed samples continuously increases as
the laser power increases.
(iii) Hierarchical martensitic structures
From the high-magnification morphologies of printed samples
S17, S18, S19, and S20 (Fig. 17), hierarchical ␣ martensitic struc-
tures could be observed. Small colonies composed of numerous
aligned fine ␣ martensite (white arrows) were embedded into
the neighboring relatively coarser ␣ martensite spacing (yellow
arrows). These fine ␣ martensite colonies tended to form per-
pendicular to the coarser ␣ martensite. Yang et al. proposed that
the formation of hierarchical martensitic structures in SLM-built Ti
alloys were attributed to the previously deposited layers experienc-
ing multiple thermal cycles during the melting process of the top
layer(s) [29]. They argued that this interlaced hierarchical structure
could be a strong barrier to the movement of dislocations and thus
enhances the strength of printed samples. However, the density
of fine ␣ martensite gradually decreased with increasing the laser
power, as shown in Fig. 17, causing a decrease in the strengthening
61
effect of hierarchical martensitic structures and a decrease in the
tensile strength.
4.2. Heat treatment-microstructure-tensile property
relationships
(i) Reasons for the variation in the tensile strength of the heat-
treated samples
A decreasing trend in the tensile strength under both room-
temperature and high-temperature tensile testing conditions for
the heat-treated samples was shown in Fig. 16. This trend is mainly
associated with ␣ martensitic decomposition and grain growth.
The reduction in tensile strength for the heat-treated samples HT1
and HT2 originates from the hard and brittle martensite partial
decomposition into ␣ and ␤ phases. When heat-treatment tem-
peratures exceeded 800 ◦ C, the martensite completely decomposed
into ␣/␤ phases, and the average grain size became coarser with the
increase in the heat-treatment temperature, which resulted in the
decrease in tensile strength of samples HT3, HT4, HT5, and HT6.
(ii) Reasons for the variation in the ductility of the heat-treated
samples
Room-temperature and high-temperature ductility showed dif-
ferent trends in the six heat-treated samples (Fig. 16).
In the room-temperature tensile results, the ductility initially
improved in samples HT1 and HT2, as most of the brittle needle-like
␣ martensitic phase had been replaced by soft ␣/␤ lath structures
after heat treatments. Then, the ductility continuously decreased
for the samples treated below the martensite complete decom-
62 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64

Fig. 15. Top-surface EBSD grain orientation and grain size distribution maps: (a, b) untreated S26, (c, d) HT2, (e, f) HT4, and (g, h) HT5 samples.

position temperature range and for those treated above the ␤tr
temperature. It should be noted that although the ␣ martensitic
phase completely transformed into the desirable soft ␣/␤ lath
structure in sample HT3, its ductility was still lower than that of
sample HT2. HT2 was heat treated at a temperature of 750 ◦ C, which
is close to the martensite complete decomposition temperature of
800 ◦ C, which means that most of the ␣ martensite has decom-
posed into ␣/␤ lath and less ␣ martensite is retained in sample
HT2 (Fig. 12). With the increase of heat-treatment temperature,
the average grain size can increase, which is detrimental to elon-
gation. Thus, it can be speculated that grain coarsening offsets the
improvements in ductility brought about by the ␣ phase transfor-
mation into ␣ and ␤ phases sample HT3. In other words, sample
HT2 obtained an excellent combination of strength and ductility
because of the synergistic effect of fine lath-like (␣ + ␤) and minor-
ity needle-like ␣ martensitic structures. When the heat-treatment
temperature further increased, a reduction in ductility resulted
from the grain growth.
The high-temperature ductility showed a similar decreasing
trend for the room-temperature test results of samples HT1, HT2,
and HT3. However, when the heat-treatment temperature was
above 950 ◦ C, the high-temperature ductility presented an opposite
 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
Fig. 16. Comparison diagram of room-temperature and high-temperature tensile
properties for the S26 samples without and with heat treatments. The blue frames
show the corresponding tensile testing temperatures. The five-pointed stars and
squares represent tensile strength and elongation, respectively.
trend compared to the room-temperature ductility. This is perhaps
because HT4, HT5, and HT6 samples possess a higher amount of
␤ phase, as these three heat treatment temperatures are close to
or above the ␤tr temperature. The BCC-␤ phase with 12 slip sys-
tems has better plastic deformation capacity than the HCP-␣ phase
with 3 slip systems. Furthermore, the influence of grain growth on
weakening ductility will decrease at high-temperature conditions,
because the slip or climb of dislocations is intensified and enhanced
at these high temperatures.
Fig. 17. High-magnification morphologies of the printed samples: (a) S17, (b) S18, (c) S19, and (d) S20. The yellow and white arrows indicate coarse and fine ␣ martensite,
respectively.
63
5. Conclusions
Highly-dense SLM-built TA15 parts with a desirable combina-
tion of tensile strength and ductility were successfully fabricated
via the optimization of printing parameters and subsequent heat
treatments in this work. The following conclusions can be drawn.
(1) The SLM processing window for TA 15 alloy could be divided
into three representative zones, i.e., high energy density zone,
suitable energy density zone, and insufficient energy density
zone. The laser power (230 W to 380 W) and the scan speed
(675 mm/s to 800 mm/s) were the optimized processing param-
eter range for the SLM-built TA15 alloy because of suitable
melting-pool overlap ratios, dense surface morphologies, and
high relative densities.
(2) In the laser power study, the SLM-built sample with 230 W laser
power (S17) showed the best tensile strength and elongation
combination than compared to the three other optimized-
parameter samples (S18, S19, and S20), which resulted from
the joint effect of relative density, metallurgical quality, and
hierarchical martensitic structure.
(3) A slight decrease in the room-temperature and high-
temperature tensile strength values were observed for sample
S26 with 60 ␮m layer thickness compared to those of sample
S17 with 30 ␮m layer thickness when other processing param-
eters were kept constant. However, the tensile strength of the
S26 sample was still higher than that of the wrought counter-
parts.
(4) The microstructure types and phase constituents of heat-
treated samples under three representative temperature
64 C. Cai et al. / Journal of Materials Science & Technology 57 (2020) 51–64
ranges experienced a successive evolution: fine lath-like (␣ + ␤)
with needle-like ␣ martensitic phase → full lath-like (␣ + ␤) →
coarse lamellar (␣ + ␤) with lath-like (␣ + ␤). The heat-treated
sample at 750 ◦ C obtained an attractive combination of strength
and ductility due to the synergistic effect of the soft lath-like
␣/␤ structure and hard needle-like ␣ martensitic phase.
Acknowledgements
This work was financially supported by the National Key
Research and Development Program of China “the Clinical Appli-
cation of Personalized Implant Prosthesis Additive Manufacturing
Process Research” (No. 2016YFB1101303), the National Natural Sci-
ence Foundation of China (Nos. 51705170 and 51905192) and the
China Postdoctoral Science Foundation (Nos. 2017M620312 and
2018T110756).
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