Journal of Alloys and Compounds 735 (2018) 1562e1575

Contents lists available at ScienceDirect

Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Effect of subtransus heat treatment on the microstructure and

mechanical properties of additively manufactured Ti-6Al-4V alloy
Xiang-Yu Zhang a, b, Gang Fang a, b, *, Sander Leeflang c, Amarante J. Bo
€ ttger d,
Amir A. Zadpoor c, Jie Zhou c
a
Department of Mechanical Engineering, Tsinghua University, 100084, Beijing, China
b
State Key Laboratory of Tribology, 100084, Beijing, China
c
Department of Biomechanical Engineering, Delft University of Technology, Mekelweg 2, 2628 CD Delft, The Netherlands
d
Department of Materials Science and Engineering, Delft University of Technology, Mekelweg 2, 2628 CD Delft, The Netherlands

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

Article history: As a powder-bed-based additive manufacturing technology, selective laser melting (SLM) offers high-
Received 21 September 2017 level flexibility and enables efficient fabrication of complex parts. In connection with complex thermal
Received in revised form events occurring during dynamic sequential layer-by-layer deposition, the as-built material is usually
21 November 2017
hierarchical at different length scales and possesses anisotropy at each level. As a result of a moderate
Accepted 23 November 2017
heating temperature of the baseplate and high cooling rates involved in the process, the as-built Ti-6Al-
Available online 24 November 2017
4V alloy has an a0 martensite microstructure. Microstructure evolution occurring during post-SLM heat
treatment is strongly affected by the stability of the initial acicular martensite. The present study was
Keywords:
Additive manufacturing
aimed at developing an optimum post-SLM heat treatment scheme at a temperature below the b transus
Titanium alloy temperature, based on the understanding of microstructure evolution occurring during subtransus
Heat treatment treatment and the resultant mechanical properties of the alloy. It was observed that the growth of the a
Phase transformation and b phases during the heat treatment was inhibited by the initial a0 phase. A higher heating tem-
Mechanical properties perature could effectively improve microstructure homogeneity on a micrometer-scale to some extent.
Heating temperature affected the strength and fracture strain of the alloy far more than cooling rate. A
post-SLM heat treatment at a temperature of 850  C or higher could lead to an improvement of fracture
strain to the level of the forged counterpart, accompanied by the losses in yield strength and ultimate
compressive strength from the as-built values. Full annealing (i.e., subtransus treatment at a high
temperature) was thus recommended to be an appropriate post-SLM heat treatment for Ti-6Al-4V.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction technology for metallic materials, most noticeably SLM to produce,

Selective laser melting (SLM) is an additive manufacturing (AM)
technology to build parts up from powdered material layer by layer
[1]. The powder bed fusion process offers great flexibility in
manufacturing complex parts of small quantities and even custom
parts, for example, patient-specific implants used in the biomedical
field.
Ti-6Al-4V is the most common titanium alloy extensively used
in the biomedical and aerospace industries. In recent years, it has
gained increasing attention along with the development of the AM
* Corresponding author. Department of Mechanical Engineering, Tsinghua Uni-
versity, 100084, Beijing, China.
E-mail address: fangg@tsinghua.edu.cn (G. Fang).
for example, unit-cell-based load-bearing porous implants [2,3],
bio-functionalized scaffolds [4e6] and many other medical devices
[7]. Analytical modeling [8], computational modeling [9] and
experimental studies [10e12] have been performed to optimize the
open-architecture design of AM parts in relation to mechanical
performance. Other research in the field has focused on micro-
structure control and defect minimization to achieve optimum
mechanical properties of SLM Ti-6Al-4V by optimizing SLM process
parameters and post-SLM heat treatment parameters [13e15].
Indeed, mechanical strengths (i.e., yield strength and ultimate
tensile or compressive strength) of SLM Ti-6Al-4V comparable and
even superior to those of the as-forged or as-cast Ti-6Al-4V coun-
terpart, reaching or even exceeding 1 GPa, have been achieved [16].
However, the following two questions, being critically important
for the widespread applications of SLM Ti-6Al-4V, especially as

https://doi.org/10.1016/j.jallcom.2017.11.263
0925-8388/© 2017 Elsevier B.V. All rights reserved.
 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
certified products for biomedical and aerospace applications, are
still being tackled.
1) How to produce defect-free parts with a homogenous micro-
structure and full density? The following four SLM process pa-
rameters are considered to be of crucial importance for
minimizing defects, most notably cracks and pores [17]: the
power of the energy source, scan speed, hatch distance and layer
thickness for a given laser beam diameter [18].
2) What is the optimal post-SLM heat treatment for the Ti-6Al-4V
alloy? In connection with the complex thermal history, the as-
built Ti-6Al-4V alloy usually has an inhomogeneous micro-
structure, being distinctly different from that of the cast coun-
terpart, high residual stress, and low ductility. Clearly, post-SLM
heat treatment is needed to homogenize the as-built micro-
structure, release residual stress and improve ductility at a
minimum loss in strength.
Cracks and pores are the two major types of defects in the as-
built SLM Ti-6Al-4V alloy; the former is caused by partial melting
of powder particles and thus a lack of fusion and the latter is caused
by the turbulences of protective gas, typically argon. These defects
negatively affect the tensile and fatigue properties of the SLM Ti-
6Al-4V alloy, as evidenced by the presence of these defects on
fracture surface, observed by Vilaro et al. [19] and Kasperovich et al.
[14]. Vilaro et al. [19] further indicated that defects with sharp
angles, induced by a lack of fusion, caused the premature failure of
SLM Ti-6Al-4V and the negative effect of the defects on the me-
chanical properties depended on their geometry and orientation.
The number density and sizes of the defects could be effectively
reduced by optimizing the main SLM process parameters, as
mentioned earlier.
Residual stress and poor ductility are usually dealt with by
applying a post-SLM heat treatment. The heat treatment for the Ti-
6Al-4V alloy is typically classified into two groups, according to the
heating temperature. When the heating temperature is above the b
transus temperature of 995  C [16], the heat treatment is called
supertransus treatment, while the heat treatment performed at a
temperature below the b transus temperature is called subtransus
treatment [20].
The as-solidified microstructure of Ti-6Al-4V is typically
composed of two phases: a with a hexagonal close-packed (HCP)
crystal structure and b with a body-centered cubic (BCC) crystal
structure. The morphologies of the a and b phases strongly affect
the mechanical properties of the alloy [21]. With increasing cooling
rate applied during solidification and subsequent cooling, the
microstructure of Ti-6Al-4V tends to change from a globular
structure to a lamellar structure. At highly non-equilibrium con-
ditions, as encountered during SLM that involves rapid cooling at
rates as high as 104 K/s [19], however, a fine, acicular, fully
martensitic microstructure, composed of the a0 phase only, is
usually formed. In addition, due to the dynamic sequential layer-
by-layer deposition and varied thermal history of the material
from the baseplate, which is only moderately heated, all the way to
the top, the microstructural morphology of the as-built Ti-6Al-4V
alloy is inevitably hierarchical and entails a number of structural
features at different length scales. The structure feature at each of
the length scales exhibits anisotropy that is considered to influence
the overall mechanical properties of the as-built Ti-6Al-4V alloy
negatively.
(i) Green part scale (dozens to hundreds of millimeters),
determined by the part feature size.
(ii) Laser scanning path scale determined by e.g., laser beam
diameter (30e150 mm) and layer thickness (20e90 mm)
1563
[15,22]. Laser spot size and scan strategy are related to the
structure feature at this length scale as well.
(iii) Columnar prior b grain size (100e200 mm). Prior b grains are
oriented in parallel with the build direction [23].
(iv) a0 needle size. The width of a0 needles is usually smaller than
1 mm, whereas the length of a0 needles can be dozens of
micrometers long [22]. Acicular a0 itself contains hierarchical
structures as well (prior a0 , secondary a0 , tertiary a0 and
quartic a0 ) [22].
The microstructure of heat-treated SLM Ti-6Al-4V on the other
hand depends primarily on heating temperature, soaking time and
cooling rate, in addition to its initial microstructure. It is generally
agreed that a lamellar microstructure corresponds to improved
fracture toughness, fatigue crack propagation resistance and
oxidation resistance, while a globular microstructure corresponds
to improved strength, ductility and fatigue crack initiation resis-
tance. Lütjering found that a colony size within prior b grains was
the most crucial factor determining the mechanical properties of
aþb titanium alloys [24]. The effective slip length in the lamellar
microstructure had a positive correlation with a colony size and the
latter decreased with increasing cooling rate from the b phase field.
He further pointed out that increasing slip length promoted
microcrack propagation and as a result reduced the ductility of
dual-phase titanium alloys. Therefore, for improving mechanical
properties, it is necessary to limit a colony size. The studies of
Ruirun and Kim revealed that the strength and ductility of aþb
titanium alloys decreased with increasing a colony size [25,26].
Therefore, in the choice of heat treatment conditions, it is also
important to limit a colony size.
The as-built SLM Ti-6Al-4V alloy usually has a fine a0 micro-
structure, a high yield strength and a high ultimate tensile strength
(UTS) of over 1 GPa, but a low elongation value (<10%) [27], being
much lower than that of the as-forged or as-cast counterpart.
During a post-SLM heat treatment at a temperature above 400  C,
the initial a0 phase decomposes [15] and the aþb phases form. With
increasing temperature applied during the heat treatment, a and b
laths become thicker. When the temperature is high enough, a fully
lamellar structure may be formed. The effect of heat treatment on
the resultant mechanical properties strongly depends on the initial
a0 phase and its decomposition during the heat treatment. The
dependence of ductility on heat treatment temperature is not al-
ways unique; some researchers reported a trend of rising ductility
with increasing temperature [16,28e30], whereas others observed
a downward trend of fracture strain [14,20]. Obviously, the micro-
structure evolution of the as-built Ti-6Al-4V alloy during heat
treatment is far more complex than that of the as-forged or as-cast
counterpart.
Some researchers chose supertransus treatment for SLM Ti-6Al-
4V [16,19,20], during which the columnar prior b phase shattered
into small pieces and the equiaxed b phase was formed. However,
in this temperature range, severe microstructure coarsening
occurred and, as a result, the yield strength and ultimate tensile
strength significantly declined, while the ductility exhibited little
improvement. Subtransus treatment, on the contrary, could lead to
moderately improved ductility while maintaining the strengths of
the alloy at a high level. Vrancken et al. [16] applied both super-
transus and subtransus treatments to the SLM Ti-6Al-4V alloy and
performed tensile tests. Their results showed that the tensile yield
strength of the SLM Ti-6Al-4V alloy decreased and the fracture
strain increase nearly linearly with rising heating temperature up
to 1000  C, regardless of cooling rate. They pointed out that tradi-
tional treatments typically applied to the wrought counterpart,
such as mill annealing, b annealing and duplex annealing, would
not lead to the usual or expected results in the case of SLM Ti-6Al-
1564 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
4V. Khorasani et al. [31] performed tensile tests of SLM Ti-6Al-4V
after annealing treatments typically applied to the wrought coun-
terpart and compared its mechanical properties with those of
wrought Ti-6Al-4V. It was found that the additively manufactured
Ti-6Al-4V alloy possessed a much higher strength than the wrought
counterpart. Huang et al. [20] found that the stabilization of the a0
phase in the additively manufactured titanium alloy could have a
strong influence on the effect of the heat treatment and the
martensite stabilization could be made use of in subtransus treat-
ment. Charpy impact tests of SLM Ti-6Al-4V were conducted and it
was found that the toughness of SLM Ti-6Al-4V remained un-
changed or slightly decreased after full annealing or stress relieving
treatment [32]. It was however not clear that under what heat
treatment conditions, more specifically at which heating temper-
ature, the martensite stabilization could be utilized to retain the
refined microstructure achieved during SLM and to achieve an
optimum result of post-SLM heat treatment in terms of a balanced
combination of strength and ductility.
In attempt to provide answers to the second question raised at
the beginning of this section, the present study was conducted to
establish the relationships between subtransus heating tempera-
ture and the compressive mechanical properties of SLM Ti-6Al-4V.
The effect of cooling rate after subtransus treatment on the
microstructure and mechanical properties of the SLM Ti-6Al-4V
alloy was also investigated.
2. Material and experimental methods
2.1. Starting material and SLM
A Ti-6Al-4V powder (grade 23) supplied by Advanced Powders
& Coatings, Canada, with a median particle size of 31.6 mm, was
used in SLM to produce cylindrical samples. Its chemical compo-
sition is given in Table 1. Cylindrical samples with a diameter of
8 mm and a height of 13 mm were 3D printed in the axial direction
(AD) by using an SLM machine (Realizer, SLM-125, Germany) for
microstructural observation and mechanical tests. Layers were
scanned by pulse laser, following a zigzag pattern. The scanning
direction shifted 10 for the next layer, as schematically illustrated
in Fig. 1. The adoption of this scanning strategy was intended to
achieve a relative density as high as possible (>99.5%).
2.2. As-forged and annealed Ti-6Al-4V
Forge and annealed Ti-6Al-4V alloy bars with extra low in-
terstitials (ELI) and a diameter of 20 mm, used in the present study,
were supplied by ICNIS International, which were processed to
meet the specification of ASTM F136-98 applied for wrought
annealed Ti-6Al-4V ELI to be used in the manufacture of surgical
implants. The microstructure of the as-received material was
composed of equiaxed a grains with an average size of around 6 mm,
as shown in Fig. 2, confirming the as-annealed metallurgical state
of the alloy.
2.3. Heat treatment and microstructure observation
Prior to the heat treatment, the as-built samples were placed in
Table 1
Chemical composition of the powder used in this research (by weight percent).
Element C O N H Fe Al V Ti
Content (wt%) 0.02 0.10 0.02 0.0019 0.19 6.4 4.0
a tube furnace with argon flushing for 4 h. Heating rate was set at
10  C/min. Two cooling rates were applied; furnace cooling (FC)
was applied by turning off the furnace while air cooling (AC) was
applied by taking samples out of the furnace, allowing them to cool
in air. Soaking time of 2 h was chosen and it was kept unchanged for
all the experiments so as to exclude its effect on the resultant
microstructure and mechanical properties. Eleven groups of sam-
ples were subjected to heat treatments at different heating tem-
peratures and cooling modes, as listed in Table 2. Note that Group
F7 had a heating temperature of 1000  C, being slightly above the b
transus temperature of 995  C (according to the value given in the
literature [16]) to allow full b phase formation. To determine the
exact b transus temperature of the alloy under investigation, dif-
ferential scanning calorimetry (DSC) was performed by heating the
as-built sample to 1230  C at a heating rate of 8  C/min, followed by
cooling to room temperature at a rate of 8  C/min.
The as-built and as-heat-treated samples were ground using
2000 grid SiC paper, polished using 1 mm diamond paste and etched
by an etchant composed of 1 ml HF, 5 ml HNO3 and 10 ml H2O. A
digital microscope (Keyence, VHX-5000, Japan) and a scanning
electron microscope (SEM, JEOL, JSM-IT100, Japan) were used to
characterize the microstructures of the samples. Fracture surfaces
after compression tests were characterized using the same SEM. To
determine the evolution of the constituent phases in the alloy
during the heat treatment, X-ray diffraction (XRD) was performed.
A diffractometer (Bruker, D8 Advance, Germany) was used in the
Bragg-Brentano geometry with Cu Ka radiation. Samples were
scanned from 10 to 130 2q at a step size of 0.030 and a counting
time of 2 s per step.
2.4. Mechanical tests
Hardness tests were conducted using a microhardness tester
(DuraScan, G5, Austria) at an indentation load of 100 N and a dwell
time of 15 s. Ten indentations were made on each sample.
Considering the low ductility of the as-build material,
compression tests were considered to be more appropriate than
tension tests. Prior to compression tests, the as-built and as-heat-
treated samples were machined into specimens with a diameter
of 6 mm and a length of 9 mm so as to remove a rough, oxidized and
less dense outer layer. The laser scanning path on the sample sur-
face was removed during machining so that the measured
strengths and fracture strain would represent the real mechanical
properties of the bulk material. Due to the high strength of the ti-
tanium alloy, the maximum compression load could reach 40 kN. If
a universal mechanical testing machine had been used, specimen
holders and highly stressed machine parts would inevitably have
undergone considerable elastic deformation, thereby affecting the
load-displacement curve and the characteristic compressive prop-
erty values of the specimen, such as Young's modulus, yield
strength, ultimate compressive strength and fracture strain. To
minimize the uncertainties, in this research, compression tests
were performed at room temperature using a thermomechanical
testing machine (DSI, Gleeble 3500, US), according to the ASTM E9 -
89a standard. The speed of moving anvil was 0.045 mm/s. To
exclude the deformation of the anvils inevitably occurring during
the compression tests, five compression tests without a specimen
being mounted between the anvils were run to obtain load-
displacement curves. The average deformation of the anvils was
used for subtraction from the measured total deformation of the
specimen. Five specimens in each group (Table 2) were tested and a
mean value was obtained. For comparison purposes, forged Ti-6Al-
Balance
4Al alloy specimens were subjected to the same tests.
 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575 1565

Fig. 1. Schematic illustrations of (a) a cylindrical sample additively manufactured in the axial direction (AD) and (b) laser scanning paths on layer n and on next layer (nþ1).

3. Results and discussion

3.1. Hierarchical structure features and microstructure of the as-

built Ti-6Al-4V alloy

As expected, hierarchical structure features at different length

scales were indeed observed, including laser footprint, columnar
prior b grains, a0 phase clusters and acicular a. On the top surface of
cylindrical samples, the laser scanning path could be easily recog-
nized under optical microscope (Fig. 3a). This feature was consid-
ered to be negative for the as-built material, because increased
surface roughness and anisotropy would potentially lead to early
crack initiation and premature failure under loading, especially
under dynamic loading in an unfavorable direction [14].
Fig. 2. Equiaxed aþb microstructure of the as-received forged and annealed Ti-6Al-4V Columnar prior b grains with diameters of 100e200 mm were
alloy. oriented in parallel with the build direction (Fig. 3b). The width of
the prior b column phase had a positive correlation with the hatch
space applied, which was 80 mm in this case. During the SLM pro-
Table 2 cess, complex thermal conditions were imposed on the samples,
Parameters of heat treatment applied to the as-built samples.
including fast cooling at rates up to 104 K/s. The baseplate tem-
Sample group Temperature ( C) Cooling mode perature was low (200  C) and the powder bed temperature must
F1 600 FC have been much lower than the decomposition temperature of the
F2 730 FC a0 martensitic phase. As a result, the microstructure of the as-built
F3 800 FC samples was nearly full a0 martensite. Fig. 3c shows fine, acicular a0
F4 850 FC
needles with widths of <1 mm inclined at specific angles of 0, 30, 60
F5 900 FC
F6 950 FC and 90 relative to each other. This anisotropic structure feature
F7 1000 FC corresponds to the symmetry of the hexagonal lattice and follows
A1 800 AC the Burgers relationships between the a0 and b phases [33,34]. The
A2 850 AC interlaced martensite boundaries were expected to have an inher-
A3 900 AC
itance effect on the morphology of the new phases formed during
A4 950 AC
subsequent heat treatment. The aspect ratio of the acicular a0 phase
FC ¼ furnace cooling; AC ¼ air cooling.
varied over a wide range of 15e50 (Fig. 3d) and it was thus a highly
anisotropic brittle phase.
2.5. Statistical analysis In comparison with the XRD pattern of the as-forged and
annealed material, the XRD pattern of the as-built samples failed to
In this paper, the data obtained from the mechanical tests are show b phase peaks at 39.5 and 57.5 (Fig. 4), indicating the absence
presented as mean ± deviations. The SPSS statistics software was of this phase in the SLM material. The lattice parameters a and c of
used to calculate the p value and find statistically significant dif- the HCP phase were 0.2925 and 0.4666 nm, respectively, being in
ference. Comparison was made with the one-way analysis of vari- agreement with the values of a ¼ 0.2931 nm and c ¼ 0.4681 nm for
ance (ANOVA) or two-way ANOVA (using the cooling rate and the a0 phase [35].
heating temperature as the two independent variables), followed The anisotropic structure features at different length scales are
by performing Tukey's test. A p value of less than 0.05 was governed by some specific mechanisms operating during the SLM
considered significant. process. For example, laser footprint reflects the chosen process
1566 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
Fig. 3. Hierarchical structure features in the as-built Ti-6Al-4V alloy: (a) laser scanning path (the arrows indicate the laser scanning direction); (b) columnar prior b grains in
relation to the build direction; (c) angles between acicular a0 needles; (d) an SEM image of the acicular a0 phase.
parameters, such as laser scanning direction, hatch space and layer
thickness. Columnar prior b grains are always parallel to the build
direction, because of the epitaxial growth of the prior b phase
during the SLM process. These columnar grains adopt the growth
direction of the grains from the previous layer and thus grain
growth occurs in the direction of maximum temperature gradient
[36].
3.2. b transus temperature
To determine the exact b transus temperature and define
appropriate subtransus treatment conditions, DSC was performed
Fig. 4. XRD pattern of the as-built Ti-6Al-4V alloy in comparison with that of the
forged and annealed counterpart.
first. As shown in Fig. 5, the SLM Ti-6Al-4V samples used in this
study exhibited a b transus temperature of 985.81  C. This b transus
temperature was similar to the value found by Yolton et al. [37]. The
heat treatment F7 (Table 2) just above the determined b transus
temperature was performed to verify the decomposed a0 / b
transformation. Fig. 6a shows equiaxed b grains and secondary aþb
lamellae inside, confirming that the prior columnar b grains indeed
split and became equiaxed grains and the columnar feature dis-
appeared. The average diameter of equiaxed b grains was over
300 mm. Thus, the supertransus treatment F7 indeed eliminated the
anisotropy of prior b columns. The width of a grain boundary was
about 5 mm. The observed microstructural features were indeed
those typical of the alloy after a heat treatment at a temperature
above the b transus temperature. By contrast, the samples treated
at a lower temperature (e.g., F6 in Table 2) still had clear columnar
prior b boundary (Fig. 6b), confirming that the heating temperature
was indeed below the b transus temperature.
The equiaxed b phase formation during supertransus treatment
has been considered to be driven by the reduction of interfacial
energy. Such a heat treatment, e.g., F7 applied in this research, has
been proven to be effective in changing columnar prior b grains
[23]. However, the coarse a phase at the prior b boundaries would
negatively affect the mechanical continuity within the structure of
the SLM Ti-6Al-4V alloy, making it very difficult to achieve much
improved strength and ductility, as confirmed by Vrancken et al.
[16] and Huang et al. [20].
3.3. Microstructure evolution during subtransus treatment
3.3.1. Subtransus treatment followed by furnace cooling
The initial microstructure of the SLM Ti-6Al-4V is of critical
importance for the microstructure evolution during subsequent
heat treatment. The predominant fine acicular a0 phase in the as-
built Ti-6Al-4V alloy is the main cause for the unsatisfactory
 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
Fig. 5. DSC thermogram of the SLM Ti-6Al-4V alloy during heating.
outcome when a conventional heat treatment for the alloy is
applied. Compared to the equiaxed a phase in the as-forged and
annealed Ti-6Al-4V alloy, the a0 phase in the as-built material has a
much smaller feature size (<1 mm). It is actually a metastable phase
and contains high densities of dislocations and twins. The a0 phase
in the SLM Ti-6Al-4V alloy is expected to slow down the growth of
new grains formed during subsequent heat treatment, leading to a
fine aþb lamellar structure. The holding temperatures at the cho-
sen heat treatment conditions (F1eF6 in Table 2) were all below the
b transus temperature determined. It would be of great interest to
determine a heating temperature, at which a refined structure
could be largely retained after the heat treatment.
When SLM Ti-6Al-4V was heated up to ~400  C, martensite
started to decompose [15]. At first, the a phase nucleated at the
boundary of the acicular a0 phase, pushing vanadium in the alloy to
the boundary of the newly formed acicular a phase. The b phase
then formed in the vanadiumerich area between the a phase laths.
Fig. 7 shows a series of microstructures formed at different holding
temperatures, all below the b transus temperature. After heating to
600  C and holding for 2 h, residual stress in the as-built material
was partly released, the a0 phase was partially decomposed but the
prior a0 phase could still be clearly seen (Fig. 7b). The aspect ratio of
prior a0 needles remained in the range of 20e50 and the width was
around 1 mm.
It was reported that residual stress could be completely relieved
by holding at 730  C for 2 h [38]. During holding at this tempera-
ture, the initial martensite would decompose into aþb lamellae.
Fig. 6. Microstructures of (a) SLM Ti-6Al-4V heat-treated at F7 condition (1000  C/2 h/FC) and (b) SLM Ti-6Al-4V heat-treated at F6 condition (950  C/2 h/FC).
1567
This microstructural change was indeed observed (Fig. 7c and d);
the initial acicular martensite changed into a particle-like
morphology at 730  C and the feature size (width) changed only
slightly as compared with the as-built material. Although the a0
phase already started to decompose during holding at 730  C, the
temperature was still too low to bring about significant changes in a
phase size. The decrease of dislocation density in the a phase [23]
and the decomposition of the a0 phase were the two major
microstructural changes occurring during the stress-relief heat
treatment.
In the material exposed to a heating temperature exceeding
800  C, a b (110) peak appeared in the XRD pattern at 2q ¼ 39.5
(Fig. 8) and the initial acicular microstructure was gradually
transformed into the lamellar aþb phases (Fig. 7e and f). The width
of the lamellar structure kept increasing with increasing heating
temperature and, in the meantime, the element-partitioning effect
became more pronounced, as a result of a higher diffusion rate at a
higher temperature (Fig. 9). With increasing temperature up to
850  C, the average width of aþb lamellar structure increased
rather slowly, as shown in Fig. 10. The restricted growth could be
attributed to the hindering effect of the lamellar a and b bound-
aries. In addition, different growth orientations of neighboring a
laths prevented the grain boundaries from migrating in the axial
direction of a and b laths, leading to limited aspect ratio changes.
However, after samples were heat-treated at temperatures above
900  C, clear increases in lamella width (4.14 ± 2 mm) and decreases
in aspect ratio were observed, as compared to the microstructures
of the alloy heat-treated at lower temperatures. In addition, with
increasing heating temperature, the a phase fraction reduced, e.g.,
73% at 850  C and 23% at 950  C [39,40]. Furthermore, with
increasing heating temperature, the growth-inhibiting effect
became weaker and lamellar grains started to coarsen, driven by
the reduction of interfacial energy. As a result, the grains with large
a lath aspect ratios were scattered in the microstructure after a heat
treatment at a high temperature.
Usually, a colony is formed during slow cooling after an
annealing treatment from the b single-phase filed and the initial a
colony size is restricted by the prior b grain size. In the case of the
SLM Ti-6Al-4V alloy, however, the initial microstructure is a0 and,
during subsequent subtransus treatment, the initial acicular
martensite gradually decomposes into aþb in the shape of colony
containing parallel a lamellae. With increasing temperature, as
shown in Fig. 7, a lamellae started coarsening and a colony width
increased simultaneously. When heating temperature reached
850  C or higher, large grains and over-grown a colony became
apparent, as can be seen in Fig. 7e, f, g and h. The slip length, which
is an important factor determining the ductility of the Al-6Al-4V
alloy, is positively related to the a colony size [25] and thus a
1568 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575

Fig. 7. Optical microstructures of SLM Ti-6Al-4V heat-treated at (a) 600, (c) 730, (e) 850 and (g) 950  C and SEM micrographs of SLM Ti-6Al-4V heat-treated at (b) 600, (d) 730, (f)
850 and (h) 950  C for 2 h, followed by furnace cooling. Some of a colonies are outlined by dotted white lines in (e) and (g).

Fig. 9. Element-partitioning effect in the material heat-treated at 850  C/2 h/FC. The
red line shows the EDS line scan position. (For interpretation of the references to
colour in this figure legend, the reader is referred to the web version of this article.)

lower fracture strain would normally be expected after the heat

Fig. 8. XRD patterns of SLM Ti-6Al-4V heat-treated at (a) 730, (b) 850 and (c) 950  C
for 2 h, followed by furnace cooling.
treatment at 950  C.
When the heating temperature was raised to 950  C, a lath
aspect ratio in the lamellar structure declined further and the
microstructure even showed a tendency toward a globular struc-
ture (compare Fig. 7h with g). The globular structure formed at a
temperature above 900  C was indeed observed by other re-
searchers [16,17]. Some of a grains gradually became more globular
 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
Fig. 10. a/a0 lamella sizes of the SLM Ti-6Al-4V alloy heat-treated at different
conditions.
than others and the morphological anisotropy vanished. Thus, the
subtransus treatment at a high temperature, but still below the b
transus temperature, could be utilized to lessen the microstructural
anisotropy induced during SLM. However, this homogenizing effect
was only noticeable for structure features smaller than the a cluster
scale and any other geometrically anisotropic features equal to or
larger than the prior b column scale were largely retained after
subtransus treatment.
Fig. 10 shows a strong correlation of a or a0 lamella width with
heating temperature. Below 850  C, the growth was quite moder-
ate. At temperatures above 900  C, however, significant lamella
width growth occurred (>4 mm). Both the trend and lamella width
values were in good agreement with the findings of other re-
searchers. The comparison with the literature values further
confirmed the decisive role of heat treatment temperature chosen
for post-SLM processing in determining the microstructure feature
size.
3.3.2. Subtransus treatment followed by air cooling
Air-cooled (AC) samples showed similar microstructure evolu-
tion to furnace-cooled (FC) samples during subtransus treatment;
the width of a and b lamellae increased with rising heating tem-
perature. The a lath widths of AC samples were slightly smaller
than those of FC samples. As shown in Fig. 10, a lath widths and
grain sizes of AC samples were similar to reported values
([14,16,17,19,20,28,29,41]) at the same heating temperatures. The
values increased from 870 ± 49 nm (A1 sample group) to
3.6 ± 0.87 mm (A4 sample group) with rising heating temperature
from 800 to 950  C.
Fig. 11 shows the microstructure evolution of AC samples heat-
treated at relatively high temperatures (i.e., 850 and 950  C). It was
noticed that AC samples heat-treated at 850  C still possessed a
very fine microstructure, while a higher temperature (950  C) close
to the b transus temperature strongly promoted grain growth, as
clearly visible in Fig. 11b. Due to a relatively higher cooling rate, the
b phase in air-cooled samples transformed to a finer lamellar
structure (indicated by dotted white lines in Fig. 11c), being
different from the aþb lamellar microstructure of furnace-cooled
samples (Fig. 11d).
XRD of A1eA4 sample groups (Table 2), as shown in Fig. 12,
revealed the presence of the b (110) phase in the heat-treated alloy
after air cooling, being similar to FC samples. The effect of element
1569
partitioning in AC samples was however less pronounced as
compared to FC samples, due to relatively faster cooling. When the
heating temperature was increased to 950  C, a transformed b
structure started to appear in air-cooled samples, as shown in
Fig. 11b and c. It is a bi-lamella structure formed by secondary a
laths precipitated in the b matrix [42]. Overall, the observed
microstructure evolution clearly indicated that the feature size of
the lamellar structure was more sensitive to heating temperature
than cooling rate.
The microstructures of A1eA4 sample groups after the heat
treatments all inherited the growth direction of the acicular a0
phase and the boundaries of prior b grains. The subtransus treat-
ment did not eliminate the microstructural anisotropy, although it
resulted in a0 decomposition, lamella growth and element diffu-
sion. The interwoven microstructure of the initial martensite and
its stabilization severely hindered the grain growth.
3.4. Microhardness
It is widely recognized that microhardness change is closely
related to the microstructure evolution of the as-built Ti-6Al-4V
alloy during subsequent heat treatment. The hardness of the as-
built material was 365 HV, being lower than the values of both
the furnace-cooled and air-cooled samples heat-treated at 600  C
(z390 HV). The increase in hardness due to the heat treatment at
600  C was attributed to the refinement of the a0 phase that was
partially decomposed.
As can be seen from Fig. 13, with increasing heating temperature
applied in the heat treatment followed by furnace cooling, hardness
reduced significantly from 393 HV (600  C) to 328 HV (950  C)
(p < 0.05), as a result of the progressive decomposition of the a0
phase and increases in a lath width and grain sizes. For air-cooled
samples, however, with rising temperature, hardness declined
first to 329 HV and then increased to 356 HV. When samples were
air-cooled from 850  C to 950  C, a transformed b phase (i.e., the a-
Widmanst€ atten microstructure or basket weave structure) was
formed (indicated by dotted white lines in Fig. 11c) and the grain
sizes were slightly smaller than those of furnace-cooled samples.
The fine aþb laminar structure formed during air cooling contrib-
uted to the raised hardness value after the treatment at 950  C.
Moreover, a faster cooling rate might have promoted the regener-
ation of residual stress. It is likely that both factors contributed to
the second rise of hardness after the heat treatment at a temper-
ature of 950  C (Fig. 13).
3.5. Compressive properties
The a0 phase in the as-built Ti-6Al-4V alloy is a supersaturated
substitutional solid solution, instead of an interstitial solid solution.
As such, the strengthening effect of the alloying elements in the
titanium alloy is much weaker than that in many other alloys. The
fine, interlaced lamellar a0 microstructure contributes to high
fracture strength at the cost of ductility.
Fig. 14 shows a compressive stress-strain curve of the as-built Ti-
6Al-4V alloy in comparison with that of the as-forged and annealed
counterpart. It was found that the as-built Ti-6Al-4V alloy
possessed a much higher yield strength ss (1292.5 ± 45.3 MPa) and
ultimate compressive strength su (1602.8 ± 59.6 MPa) than the as-
forged counterpart, whose ss and su were 783.9 ± 13.9 and
1349.7 ± 11.6 MPa, respectively. However, the fracture strain εmax of
the as-built Ti-6Al-4V was only 13%, being far lower than that of the
as-forged and annealed Ti-6Al-4V alloy (21%). In addition, the as-
built SLM specimens failed quickly after yielding without
showing a distinct work-hardening effect (Fig. 14), indicating poor
deformability.
1570 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575

Fig. 11. Optical micrographs of samples heat-treated at (a) 850 and (b) 950  C for 2 h, followed by air cooling. SEM micrographs of samples heat-treated at (c) 950  C/2 h/AC and (d)
950  C/2 h/FC.

Fig. 13. Microhardness values of the alloy heat-treated at different temperatures. Test
groups marked with the same letter (I or II) are not significantly different (p > 0.05)
(one-way ANOVA, Tukey's test).

Fig. 12. XRD patterns of the SLM Ti-6Al-4V alloy heat-treated at (a) 800, (b) 850, (c)
900 and (d) 950  C for 2 h, followed by air cooling.

In general, there are four major factors that limit the ductility
and improve the fracture strength of the SLM Ti-6Al-4V alloy:

(i) Constituent phase. The as-built material is composed of

martensite only and has a high strength and hardness value.
The needle-shaped martensite is a brittle phase and thus the
initial material has a poor ability to deform.
(ii) The morphology of microstructure. Compared with equiaxed
grains in the as-forged and annealed material, needle-
shaped a0 is highly anisotropic and unable to accommodate Fig. 14. Compressive stress-strain curve of the as-built SLM Ti-6Al-4V alloy in com-
strains evenly. parison with that of the forged and annealed counterpart.

(iii) Residual stress and defects. Residual stress in the as-built

material is induced by high cooling rates involved in SLM.
 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
During deformation, stress concentrations near defects, e.g.,
cracks, pores and dislocations, cause early failure of the as-
built material.
(iv) Crystallographic texture. The microstructure of SLM Ti-6Al-
4V is highly anisotropic due to rapid cooling and large tem-
perature gradients involved in the SLM process. Crystallo-
graphic texture must be considered in accounting for the
mechanical anisotropy and poor ductility of the as-built
material.
During compression tests, all specimens (including heat-treated
ones) were crushed and fractured along an angle of 45 to the
compression axis. For the specimens heat-treated at 800  C/2 h/FC,
for example, their fracture surfaces (Fig. 15a) had three morpho-
logical features, i.e., the dominant ‘river-like’ surface, quasi-
cleavage fracture (Fig. 15b) and shallow dimples (Fig. 15c). These
characteristics of the fracture surfaces indicated that the fracture
was typical of brittle fracture. The brittle fracture must have been
related to the lamellar structure formed in subtransus-treated
specimens, which was favorable for a high fracture strength, but
not for a high fracture strain. The quasi-cleavage fracture was found
mostly near the edges of the fracture surfaces and its area fraction
increased with rising heating temperature.
Fig. 16 shows the compressive stressestrain curves of specimens
heat-treated at different temperatures. Both ss and su of furnace-
cooled specimens showed a clear downward trend with rising
heating temperature. su showed a slower descending trend than
the yield strength ss at high heating temperatures. As to furnace-
cooled specimens, when the heating temperature increased from
600 to 950  C, the yield strength ss decreased from 1301.7 ± 11.4 to
965.1 ± 9.1 MPa (p < 0.05), and the ultimate compressive strength
su decreased from 1532.0 ± 27.3 to 1388.4 ± 10.2 MPa (p < 0.05), as
shown in Fig. 17 and Table 3. The reductions in strength were
accompanied by improvements in ductility; the fracture strain
increased from 16.2 ± 0.2% to 24 ± 0.2% (p < 0.05). In addition, with
increasing heating temperature, an enhancement in the work-
hardening effect was clearly observable.
For the specimens heat-treated at different subtransus
Fig. 15. Fracture surface of the SLM Ti-6Al-4V alloy heat-treated at 800  C/2 h/FC (a) and enlarged images of area A (b) and area B (c).
1571
treatment conditions, their mechanical property changes were
analyzed in connection with microstructure evolution. The speci-
mens heat-treated at the condition of F1 (600  C/2 h/FC) had slight
increases in yield strength and fracture strain, as compared to the
as-built material. The increases could be explained by the partial
decomposition of martensite and the relief of residual stress,
because residual stress is generally considered to be a cause for
early failure. In other words, the relief of residual stress is helpful in
improving the deformability.
When the specimens were heated to 730  C, followed by furnace
cooling, the yield strength and ultimate compressive strength were
about 100 MPa lower than those of the specimens heat-treated at
600  C, as can be seen in Table 3. As mentioned above, significant
changes in microstructure took place at 730  C; a particle-shaped
morphology tended to form; the volume fraction of the a0 phase
decreased; residual stress was fully released after two-hour
soaking.
During the heat treatment at a temperature exceeding 800  C,
martensite was fully decomposed and a lamellar aþb microstruc-
ture was formed, as confirmed by microstructural observations.
Microstructure coarsening must have been the main factor causing
the reduction in strength with rising heating temperature (Table 3).
The phase transformation is a quasi-steady process and element
diffusion proceeded further during slow cooling after the heat
treatment. The difference in maximum vanadium solubility be-
tween the a phase and the b phase was much greater than that of
aluminum, while the volume fractions of a and b varied insignifi-
cantly between the specimens heated to different temperatures,
followed by furnace cooling at a very low cooling rate (about 3 K/
min). Therefore, the element-partitioning effect was stronger for
the material heat-treated at a higher temperature, which nega-
tively affected the mechanical continuity of the material and led to
reduced fracture strain. However, because of the effect of initial
microstructure stabilization, the growth of a colony size was
limited and the strengths of the Ti-6Al-4V alloy heat-treated at a
high temperature remained at a high level, e.g., the yield strengths
of the alloy heat-treated at different heating temperatures being
200e300 MPa higher than the yield strength of the as-forged and
1572 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575

Fig. 16. Compressive stress-strain curves of (a) furnace-cooled and (b) air-cooled SLM Ti-6Al-4V specimens.

Fig. 17. Mechanical properties of the as-built Ti-6Al-4V alloy (denoted as a heating temperature of zero in the figure) and those of the as-heat-treated SLM Ti-6Al-4V alloy as a
function of heating temperature: (a) yield strength, (b) ultimate compressive strength, (c) fracture strain and (d) yield strength to ultimate compressive strength ratio. Test groups
marked with the same letter (I or II) are not significantly different (p > 0.05) (one-way ANOVA, Tukey's test).

annealed counterpart (Table 3). residual stress and reduction in microstructural anisotropy. It is
The deformability of the alloy was enhanced with increasing worth noting that the maximum compressive strain showed a
heating temperature, which could be attributed to the relief of positive correlation with a colony size at high temperature
 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575 1573

Table 3 intended to improve the ductility of the as-built material with

Mechanical properties of the SLM Ti-6Al-4V alloy heat-treated at different minimum sacrifice in strength. Fig. 17 illustrates the relationships of
conditions.
strengths and fracture strain with heating temperature and cooling
Treatment ss (MPa) su (MPa) εmax (%) r (%) rate. During the heat treatment at a temperature above 800  C, the
As-forged 783.9 ± 16.4 1346.9 ± 12.1 21.5 ± 1.0 0.58 initial a0 phase was believed to be fully decomposed and the
As-built 1292.5 ± 45.3 1602.8 ± 59.6 13.2 ± 0.3 0.79 limiting effect of the initial microstructure on the growth of grain
600  C/2 h/FC 1301.7 ± 11.4 1532.0 ± 27.3 16.2 ± 0.2 0.85 size played an important role in maintaining the yield strength at a
730  C/2 h/FC 1169.2 ± 10.4 1432.6 ± 14.7 19.8 ± 0.2 0.82
relatively high level. The heat-treated SLM Ti-6Al-4V alloy had a
800  C/2 h/FC 1122.0 ± 4.2 1431.9 ± 2.0 20.0 ± 1.3 0.78
850  C/2 h/FC 1070.9 ± 8.2 1417.0 ± 4.3 21.9 ± 0.3 0.76 lamellar structure and the mechanical properties would vary with
900  C/2 h/FC 1012.2 ± 6.6 1392.5 ± 9.5 21.8 ± 1.2 0.73 the lamella width. Fig. 17a shows that the yield strength declined
950  C/2 h/FC 965.1 ± 9.1 1388.4 ± 10.2 24.1 ± 0.2 0.69 almost linearly from 800 to 950  C. However, the descending trend
800  C/2 h/AC 1084.5 ± 15.3 ± ±
1420.0 5.2 21.3 1.0 0.76
of su was much less steep, especially when the heating temperature
850  C/2 h/AC 1027.5 ± 35.8 1442.3 ± 9.9 22.1 ± 0.9 0.71
900  C/2 h/AC 1023.9 ± 4.4 1389.2 ± 2.4 20.5 ± 0.6 0.74
exceeded 850  C (Fig. 17b), and the FC and AC specimens showed no
950  C/2 h/AC 996.3 ± 7.9 1389.9 ± 15.0 23.6 ± 1.3 0.72 significant difference (p ¼ 0.8, Two-way ANOVA). This phenome-
non was probably caused by the over-grown a colony and the
increased slip length that hindered macro-crack propagation and
(>800  C). This is inconsistent with the normally expected trend postponed fracture during compressive testing [24]. The ductility of
that a larger colony size corresponds to a longer effective slip the material showed a nearly linear rising trend (Fig. 17c) with
length, leading to a reduction in ductility, as found by Lütjering increasing heating temperature. In addition, in comparison with
[24]. The inconsistency of the present results with the finding of the effect of cooling rate and the effect of soaking time (5 h, 2 h and
Lütjering could be caused by the highly complex and diversified 3 h) [16] on the mechanical properties, it is obvious that heating
crystallographic orientations of aþb laths in SLM Ti-6Al-4V. In temperature is the most important influential factor.
addition, micro-crack propagation resistance was largely retained To quantify the deformability, another material property index -
by the strong local anisotropy of the lamellar microstructure, yield strength to ultimate compressive strength ratio r was intro-
thereby preventing the material from early failure during duced. As illustrated in Fig. 17d, for both furnace- and air-cooled
compressive testing. specimens, over a heating temperature range of 600e950  C, the
As described earlier, the aspect ratio of the aþb lamellar struc- r parameter showed a linear declining trend, indicating increasing
ture decreased with rising heating temperature; some longer deformability. Although the AC specimens heat-treated at 850  C
lamellae were shattered into smaller pieces, because of the cross showed no significant difference from those treated at 900  C and
growth of other grains. The microstructure of the samples heat- 950  C (p > 0.05), the lowest r value (r < 0.7) was found in this
treated at 950  C even showed a tendency of becoming globular. temperature range. This decline corresponded to the decrease in
The ability to accommodate strains was improved for the samples microhardness. Clearly, a heat treating temperature around 850  C
heat-treated at a high temperature in the aþb temperature range, should be avoided, if air cooling is to be applied. These results
leading to an enhanced fracture strain value. proved that the subtransus treatment in general improved the
The air-cooled specimens showed a similar trend of decreasing work-hardening ability of the alloy. A positive correlation between
strength with rising heating temperature. When the heating tem- the heating temperature and the plasticity-promoting effect was
perature was increased from 800 to 950  C, the ss and su values thus established; the deformability of the alloy was much
decreased from 1084.5 ± 15.3 to 996.3 ± 7.9 MPa (p < 0.05) and improved, after a full annealing treatment at 900 or 950  C.
1420.0 ± 5.2 to 1389.9 ± 15.0 MPa (p < 0.05), respectively (Fig. 17 To develop a correlation between the characteristic size of
and Table 3). The values of ss, su and εmax had no significant dif- microstructure and the mechanical strength of the heat-treated
ferences from those of furnace-cooled specimens. The similar me- SLM material, the variations of yield strength and compressive
chanical properties of the material cooled at different rates would strength were plotted against the reciprocal of the square root of
be associated with similar microstructure feature sizes. For the lamella width (d1/2), as shown in Fig. 18. The yield strength of FC
samples heat-treated at a temperature well below the b transus samples showed an approximate positive linear correlation with
temperature (e.g., 900  C), the volume fractions of the aþb phases d1/2, this hardening effect is consistent with Hall-Petch law
would not be different between furnace-cooled and air-cooled (sy ¼ s0 þ k$d1/2). However, the samples with the finest micro-
samples. Although a multi-phase aþbþa0 microstructure was structure (d1/2 > 1.07 mm1/2) possessed a significantly higher
formed after air cooling from 950  C, a0 laths formed inside prior b strength than other samples, this result further indicated that the
grains would not be sufficient to bring about a significant microstructure morphology and phase content of SLM Ti-6Al-4V
improvement in the strength of the alloy. Nevertheless, the yield would greatly improve the hardening effect of as-built materials.
strength of the specimens heat-treated at 950  C/2 h/AC was about Both furnace-cooled and air-cooled specimens possessed high ss
30 MPa higher than that of the specimens heat-treated at the same (>1 GPa) and su (>1.4 GPa) values, when the lamella width was
temperature but cooled in furnace. smaller than 1 mm (d1/2 > 1 mm1/2). Typically, a finer acicular
It is worth noting that air-cooled specimens exhibited a lower microstructure corresponds to a higher yield strength (slip length
yield strength at 800  C and a higher yield strength at 950  C, as and a colony size being equal to the width of individual a plates). It
compared to the strength values of the furnace-cooled specimens, also contributes to micro-crack resistance of the material. The
indicating a small range of variations, as can be seen from the strengths markedly declined when the lamella width was increased
stress-strain curves in Fig. 16b. The increased yield strength of the to 3.5 mm (d1/2 < 0.53 mm1/2), both ss and su falling below 1 GPa,
specimens heat-treated at 950  C, followed by air cooling, could be which would not be favorable for industry application. With such a
explained by the formation of the a0 phase during relatively rapid plot, it would be possible to estimate the mechanical strength of the
cooling. The compressive strength of air-cooled specimens showed SLM Ti-6Al-4V alloy by characterizing its microstructure.
no distinct difference in the relatively high annealing temperature
range, compared with that of furnace-cooled specimens. 4. Conclusions
In the present study, the subtransus treatments applied were
Ti-6Al-4V samples produced by means of selective laser melting
1574 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
1/2
Fig. 18. Variations of ss and su with d of heat-treated Ti-6Al-4V (d is the lamella
width).
(SLM) possessed high strengths but poor ductility. In selecting the
type of post-SLM heat treatment, it was intended to utilize the
initial refined a0 phase and obtain a fine aþb lamellar structure by
applying subtransus treatment. The research on the effect of
heating temperature and cooling rate on the microstructure evo-
lution and mechanical properties of SLM Ti-6Al-4V led to the
following conclusions.
(1) The as-built Ti-6Al-4V alloy had hierarchical structure fea-
tures at different length scales, namely the green part scale
(>1 mm), laser scanning scale (dozens to hundreds of mi-
crometers, determined by the SLM process parameters),
prior b columnar size (z200 mm), a0 clusters (limited by the
width of columnar prior b) and a0 needle width (<1 mm). For
the purpose of microstructure homogenization, subtransus
treatment was effective for the structure features smaller
than the a0 cluster scale (dozens of micrometers).
(2) The stabilization of the a0 phase had a strong influence on its
decomposition and grain growth during subsequent heat
treatment. Slow increase in grain size was observed when
the subtransus treatments at different temperatures were
applied. The a/a lath size remained nearly unchanged
(<2 mm) after a stress relief treatment at 600  C/2 h or 730  C/
2 h. The a/a0 lath size showed a strong correlation with
heating temperature, illustrating the importance of the
initial microstructure and heating temperature applied in
post-SLM heat treatment. Only when the heating tempera-
ture exceeded 900  C, a lamella width growth became
apparent (>4 mm).
(3) Morphological features of the microstructure of the alloy
significantly influenced its mechanical properties. The
growth orientation and the fine initial a0 structure had a
significant restricting effect on microstructure evolution
during post-SLM heat treatment. Both the yield strength ss
and ultimate compressive strength su of the subtransus-
treated SLM Ti-6Al-4V alloy showed a declining trend with
rising heating temperature. Enhancements in deformability
and work-hardening effect were observed with increasing
heating temperature. The final mechanical properties of the
alloy showed clear correspondence to the microstructure
changes; the strengths of the heat-treated alloy corre-
sponded to its lamella width.
(4) All specimens heat-treated below the b transus temperature
had higher yield strengths and compressive strengths than
those of the as-forged counterpart. A full annealing treat-
ment at 850  C or a higher temperature led to fracture strain
values comparable to the value of the as-forged Ti-6Al-4V
alloy.
(5) Cooling rate did not significantly affect the mechanical
properties of the heat-treated SLM Ti-6Al-4V alloy. For
furnace-cooled and air-cooled specimens, the best
compressive properties were obtained after a heat treat-
ments at 850  C/2 h/FC or 900  C/2 h/FC; the specimens had a
high yield strength (over 1 GPa), a high ultimate compressive
strength (about 1.4 GPa) and good ductility (εmax > 20%).
Acknowledgements
Authors (Xiang-Yu Zhang and Gang Fang) gratefully acknowl-
edge the partial financial support from State Key Lab of Tribology,
China (project No. SKTL2016B11). Xiang-Yu Zhang acknowledges
the partial financial support from the Tsinghua Scholarship for
Overseas Graduate Studies. The support of Ing. R.W.A. Hendrix from
the Delft University of Technology in carrying out the XRD mea-
surements is gratefully acknowledged.
References
[1] I. Gibson, D. Rosen, B. Stucker, Additive Manufacturing Technologies, Springer,
New York, 2010, https://doi.org/10.1007/978-1-4939-2113-3.
[2] R. Wauthle, S.M. Ahmadi, S.A. Yavari, M. Mulier, A.A. Zadpoor, H. Weinans,
J. Van Humbeeck, J.-P. Kruth, J. Schrooten, Revival of pure titanium for
dynamically loaded porous implants using additive manufacturing, Mater. Sci.
Eng. C 54 (2015) 94e100, https://doi.org/10.1016/j.msec.2015.05.001.
[3] S.A. Yavari, R. Wauthle , J. van der Stok, A. Riemslag, M. Janssen, M. Mulier, J.-
P. Kruth, J. Schrooten, H. Weinans, A.A. Zadpoor, Fatigue behavior of porous
biomaterials manufactured using selective laser melting, Mater. Sci. Eng. C 33
(2013) 4849e4858, https://doi.org/10.1016/j.msec.2013.08.006.
[4] J. Van Der Stok, D. Lozano, Y.C. Chai, S. Amin Yavari, A.P. Bastidas Coral,
J.A. Verhaar, E. Go mez-Barrena, J. Schrooten, H. Jahr, A.A. Zadpoor, Osteosta-
tin-coated porous titanium can improve early bone regeneration of cortical
bone defects in rats, Tissue Eng. Pt. A 21 (2015) 1495e1506, https://doi.org/
10.1089/ten.tea.2014.0476.
[5] J. van der Stok, H. Wang, S. Amin Yavari, M. Siebelt, M. Sandker, J.H. Waarsing,
J.A. Verhaar, H. Jahr, A.A. Zadpoor, S.C. Leeuwenburgh, Enhanced bone
regeneration of cortical segmental bone defects using porous titanium scaf-
folds incorporated with colloidal gelatin gels for time-and dose-controlled
delivery of dual growth factors, Tissue Eng. Pt. A 19 (2013) 2605e2614,
https://doi.org/10.1089/ten.tea.2013.0181.
[6] J. Van der Stok, O.P. Van der Jagt, S. Amin Yavari, M.F. De Haas, J.H. Waarsing,
H. Jahr, E.M. Van Lieshout, P. Patka, J.A. Verhaar, A.A. Zadpoor, Selective laser
melting-produced porous titanium scaffolds regenerate bone in critical size
cortical bone defects, J. Orthop. Res. 31 (2013) 792e799, https://doi.org/
10.1002/jor.22293.
[7] A.A. Zadpoor, J. Malda, Additive manufacturing of biomaterials, tissues, and
organs, Ann. Biomed. Eng. 45 (2017) 1e11, https://doi.org/10.1007/s10439-
016-1719-y.
[8] A.A. Zadpoor, R. Hedayati, Analytical relationships for prediction of the me-
chanical properties of additively manufactured porous biomaterials, J. Biomed.
Mater. Res. A 104 (2016) 3164e3174, https://doi.org/10.1002/jbm.a.35855.
[9] R. Hedayati, H. Hosseini-Toudeshky, M. Sadighi, M. Mohammadi-Aghdam,
A. Zadpoor, Computational prediction of the fatigue behavior of additively
manufactured porous metallic biomaterials, Int. J. Fatig. 84 (2016) 67e79,
https://doi.org/10.1016/j.ijfatigue.2015.11.017.
[10] R. Hedayati, M. Sadighi, M. Mohammadi-Aghdam, A. Zadpoor, Analytical re-
lationships for the mechanical properties of additively manufactured porous
biomaterials based on octahedral unit cells, Appl. Math. Model. 46 (2017)
408e422, https://doi.org/10.1016/j.apm.2017.01.076.
[11] S.A. Yavari, S. Ahmadi, R. Wauthle, B. Pouran, J. Schrooten, H. Weinans,
A. Zadpoor, Relationship between unit cell type and porosity and the fatigue
behavior of selective laser melted meta-biomaterials, J. Mech. Behav. Biomed.
43 (2015) 91e100, https://doi.org/10.1016/j.jmbbm.2014.12.015.
[12] J. de Krijger, C. Rans, B. Van Hooreweder, K. Lietaert, B. Pouran, A.A. Zadpoor,
Effects of applied stress ratio on the fatigue behavior of additively manufac-
tured porous biomaterials under compressive loading, J. Mech. Behav. Bio-
med. 70 (2017) 7e16, https://doi.org/10.1016/j.jmbbm.2016.11.022.
[13] E. Sallica-Leva, R. Caram, A. Jardini, J. Fogagnolo, Ductility improvement due to
martensite a0 decomposition in porous Tie6Ale4V parts produced by selec-
tive laser melting for orthopedic implants, J. Mech. Behav. Biomed. 54 (2016)
 X.-Y. Zhang et al. / Journal of Alloys and Compounds 735 (2018) 1562e1575
149e158, https://doi.org/10.1016/j.jmbbm.2015.09.020.
[14] G. Kasperovich, J. Hausmann, Improvement of fatigue resistance and ductility
of TiAl6V4 processed by selective laser melting, J. Mater. Process. Technol. 220
(2015) 202e214, https://doi.org/10.1016/j.jmatprotec.2015.01.025.
[15] W. Xu, M. Brandt, S. Sun, J. Elambasseril, Q. Liu, K. Latham, K. Xia, M. Qian,
Additive manufacturing of strong and ductile Tie6Ale4V by selective laser
melting via in situ martensite decomposition, Acta Mater. 85 (2015) 74e84,
https://doi.org/10.1016/j.actamat.2014.11.028.
[16] B. Vrancken, L. Thijs, J.-P. Kruth, J. Van Humbeeck, Heat treatment of Ti6Al4V
produced by selective laser melting: microstructure and mechanical proper-
ties, J. Alloys Compd. 541 (2012) 177e185, https://doi.org/10.1016/
j.jallcom.2012.07.022.
[17] L. Facchini, E. Magalini, P. Robotti, A. Molinari, S. Ho €ges, K. Wissenbach,
Ductility of a Ti-6Al-4V alloy produced by selective laser melting of prealloyed
powders, Rapid Prototyp. J. 16 (2010) 450e459, https://doi.org/10.1108/
13552541011083371.
[18] A. Simchi, H. Pohl, Effects of laser sintering processing parameters on the
microstructure and densification of iron powder, Mater. Sci. Eng. A 359 (2003)
119e128, https://doi.org/10.1016/S0921-5093(03) 00341e1.
[19] T. Vilaro, C. Colin, J.-D. Bartout, As-fabricated and heat-treated microstructures
of the Ti-6Al-4V alloy processed by selective laser melting, Metall. Mater.
Trans. A 42 (2011) 3190e3199, https://doi.org/10.1007/s11661-011-0731-y.
[20] Q. Huang, X. Liu, X. Yang, R. Zhang, Z. Shen, Q. Feng, Specific heat treatment of
selective laser melted Tie6Ale4V for biomedical applications, Front. Mater.
Sci. 9 (2015) 373e381, https://doi.org/10.1007/s11706-015-0315-7.
[21] C. Leyens, M. Peters, Titanium and Titanium Alloys: Fundamentals and Ap-
plications, Wiley-VCH, Weinheim, 2003, https://doi.org/10.1002/3527602119.
[22] J. Yang, H. Yu, J. Yin, M. Gao, Z. Wang, X. Zeng, Formation and control of
martensite in Ti-6Al-4V alloy produced by selective laser melting, Mater. Des.
108 (2016) 308e318, https://doi.org/10.1016/j.matdes.2016.06.117.
[23] S. Wu, Y. Lu, Y. Gan, T. Huang, C. Zhao, J. Lin, S. Guo, J. Lin, Microstructural
evolution and microhardness of a selective-laser-melted Tie6Ale4V alloy
after post heat treatments, J. Alloys Compd. 672 (2016) 643e652, https://
doi.org/10.1016/j.jallcom.2016.02.183.
[24] G. Lütjering, Influence of processing on microstructure and mechanical
properties of (aþb) titanium alloys, Mater. Sci. Eng. A 243 (1998) 32e45,
https://doi.org/10.1016/S0921-5093(97) 00778e8.
[25] C. Ruirun, Z. Deshuang, G. Jingjie, M. Tengfei, D. Hongsheng, S. Yanqing,
F. Hengzhi, A novel method for grain refinement and microstructure modi-
fication in TiAl alloy by ultrasonic vibration, Mater. Sci. Eng. A 653 (2016)
23e26, https://doi.org/10.1016/j.msea.2015.12.001.
[26] Y.-W. Kim, Effects of microstructure on the deformation and fracture of g-TiAl
alloys, Mater. Sci. Eng. A 192 (1995) 519e533, https://doi.org/10.1016/0921-
5093(94)03271-8.
[27] H.K. Rafi, N.V. Karthik, H. Gong, T.L. Starr, B.E. Stucker, Microstructures and
mechanical properties of Ti6Al4V parts fabricated by selective laser melting
and electron beam melting, J. Mater. Eng. Perform. 22 (2013) 3872e3883,
https://doi.org/10.1007/s11665-013-0658-0.
[28] M. Tho €ne, S. Leuders, A. Riemer, T. Tro €ster, H. Richard, Influence of heat-
1575
treatment on selective laser melting productsee.g. Ti6Al4V, in: Proc. of the
23rd International Solid Freeform Fabrication Symposium, University of
Texas, Austin, 2012, pp. 492e498.
[29] S. Leuders, M. Tho €ne, A. Riemer, T. Niendorf, T. Tro € ster, H. Richard, H. Maier,
On the mechanical behaviour of titanium alloy TiAl6V4 manufactured by
selective laser melting: fatigue resistance and crack growth performance, Int.
J. Fatig. 48 (2013) 300e307, https://doi.org/10.1016/j.ijfatigue.2012.11.011.
[30] A. Popovich, V. Sufiiarov, E. Borisov, I. Polozov, Microstructure and mechanical
properties of Ti-6Al-4V manufactured by SLM, Key Eng. Mater. 651e653
(2015) 677e682, https://doi.org/10.4028/www.scientific.net/KEM.651-
653.677.
[31] A.M. Khorasani, I. Gibson, M. Goldberg, G. Littlefair, On the role of different
annealing heat treatments on mechanical properties and microstructure of
selective laser melted and conventional wrought Ti-6Al-4V, Rapid Prototyp. J.
23 (2017) 295e304, https://doi.org/10.1108/RPJ-02-2016-0022.
[32] E. Yasa, J. Deckers, J.P. Kruth, M. Rombouts, J. Luyten, Charpy impact testing of
metallic selective laser melting parts, Virtual Phys. Prototyp. 5 (2010) 89e98,
https://doi.org/10.1080/17452751003703894.
[33] J. Qazi, O. Senkov, J. Rahim, F.S. Froes, Kinetics of martensite decomposition in
Tie6Ale4VexH alloys, Mater. Sci. Eng. A 359 (2003) 137e149, https://doi.org/
10.1016/S0921-5093(03) 00350e00352.
[34] E. Aeby-Gautier, A. Settefrati, F. Bruneseaux, B. Appolaire, B. Denand,
M. Dehmas, G. Geandier, P. Boulet, Isothermal a00 formation in b metastable
titanium alloys, J. Alloys Compd. 577 (2013) S439eS443, https://doi.org/
10.1016/j.jallcom.2012.02.046.
[35] G. Welsch, R. Boyer, E. Collings, Materials Properties Handbook: Titanium
Alloys, ASM Int., Materials Park, Ohio, 1993.
[36] T. Bormann, B. Müller, M. Schinhammer, A. Kessler, P. Thalmann, M. de Wild,
Microstructure of selective laser melted nickeletitanium, Mater. Charact. 94
(2014) 189e202, https://doi.org/10.1016/j.matchar.2014.05.017.
[37] C.F. Yolton, F.H. Froes, R.F. Malone, Alloying element effects in metastable beta
titanium alloys, Metall. Trans. A 10 (1979) 132e134, https://doi.org/10.1007/
BF02686421.
[38] Y. Combres, B. Champin, Traitements thermiques des alliges de titane, Tech-
niques de I'ingenieur, 1991.
[39] I. Katzarov, S. Malinov, W. Sha, Finite element modeling of the morphology of
b to a phase transformation in Ti-6Al-4V alloy, Metall. Mater. Trans. A 33
(2002) 1027e1040, https://doi.org/10.1007/s11661-002-0204-4.
[40] R. Pederson, O. Babushkin, F. Skystedt, R. Warren, Use of high temperature X-
ray diffractometry to study phase transitions and thermal expansion prop-
erties in Ti-6Al-4V, Mater. Sci. Technol. 19 (2003) 1533e1538, https://doi.org/
10.1179/026708303225008013.
[41] V. Cain, L. Thijs, J. Van Humbeeck, B. Van Hooreweder, R. Knutsen, Crack
propagation and fracture toughness of Ti6Al4V alloy produced by selective
laser melting, Addit. Manuf. 5 (2015) 68e76, https://doi.org/10.1016/
j.addma.2014.12.006.
[42] G. Wegmann, J. Albrecht, G. Lütjering, K.-D. Folkers, C. Liesner, Microstructure
and mechanical properties of titanium castings, Z. Metallkd. 88 (1997)
764e773.