Materials and Design 116 (2017) 352–358

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Selective laser melting of weak-textured commercially pure titanium

with high strength and ductility: A study from laser power perspective
X.P. Li a,⁎, J. Van Humbeeck b, J.P. Kruth a
a
KU Leuven (University of Leuven), Department of Mechanical Engineering, Leuven 3001, Belgium
b
KU Leuven (University of Leuven), Department of Materials Engineering, Leuven 3001, Belgium

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Different laser powers led to different

phase formation, microstructure, tex-
ture and mechanical properties of
SLMed CP Ti.
• A weak-textured CP Ti with isotropic
mechanical properties was achieved
using high laser power
• A strong-textured CP Ti with anisotrop-
ic mechanical properties was obtained
using low laser power
• The mechanism was attributed to the
formation of α′ phase as a result of
the higher cooling rates at high laser
power.
• The weak-texture CP Ti showed high ul-
timate compressive strength ~ 1.1 GPa
with a compressive strain ≥ 50%

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

Article history: In this study, fully dense commercially pure titanium (CP Ti) parts were successfully fabricated by selective laser
Received 1 November 2016
melting (SLM) using the same optimal laser energy density Ep but with two different laser powers: high laser
Received in revised form 19 November 2016
Accepted 6 December 2016 power EH ~250 W and low laser power EL ~50 W. It was found that at the same Ep different laser powers led
Available online 8 December 2016 to different phase formation, microstructure, texture and mechanical properties of the selective laser melting fab-
ricated (SLMed) CP Ti. A weak-textured CP Ti with isotropic mechanical properties was achieved using EH while a
Keywords: strong-textured CP Ti with anisotropic mechanical properties was obtained using EL. The underlying mechanism
Commercially pure titanium was attributed to the formation of α' phase in the CP Ti as a result of the higher cooling rates at EH. The formation
Selective laser melting of α' phase also contributed to the observed high ultimate compressive strength ~1.1 GPa and high compressive
Martensitic phase transformation strain ≥50% in the SLMed weak-textured CP Ti at EH. This study provides important insights into the role of laser
Crystallographic texture
energy in the SLM fabrication of CP Ti with tailorable crystallographic texture and thus mechanical properties.
Mechanical properties
© 2016 Elsevier Ltd. All rights reserved.

1. Introduction power generation, chemical, petrochemical, heat management, space-

Commercially pure titanium (CP Ti), as an attractive engineering
material, has applications in a wide spectrum of industries including
⁎ Corresponding author.
E-mail address: xiaopeng.li@kuleuven.be (X.P. Li).
craft and biomedical devices due to its excellent corrosion resistance,
good weldability and fabricability as well as excellent biocompatibility
[1]. However, its relatively low strength as compared to other high
strength Ti alloys impedes its further applications where mechanical
properties are also important. Unfortunately, due to the sluggish re-
sponse of CP Ti to heat treatment, the options for strengthening CP Ti

http://dx.doi.org/10.1016/j.matdes.2016.12.019
0264-1275/© 2016 Elsevier Ltd. All rights reserved.
 X.P. Li et al. / Materials and Design 116 (2017) 352–358
are relatively few and limited, mainly solid solution strengthening by
oxygen in particular [1]. However, oxygen is detriment to its corrosion
resistance and biocompatibility [1]. To address this problem, fabrication
of ultrafine grain CP Ti as an alternative is being sought recently to im-
prove its mechanical properties strength while retaining its excellent
corrosion resistance and biocompatibility [2].
Recently, selective laser melting (SLM), as a powder based metal ad-
ditive manufacturing (AM), has enjoyed a rapid development [3]. When
compared to traditional fabrication processes, the unique layer-wise
fabrication process of SLM renders SLM many advantages e.g. high free-
dom of customization, high materials usage efficiency and fabrication of
complex geometry parts and so on. Importantly, the high heating and
cooling rates during SLM enable the fabrication of metal parts with
very fine and tailorable microstructure, e.g. Al-Si and Ti alloys, metal ma-
trix composites as well as bulk metallic glasses [4–11]. Similarly, fine mi-
crostructures including lath α, acicular α' and refined zig-zag α' can also
be manipulated in SLM fabricated CP Ti parts through controlling the
process parameters [12,13]. As a result, the SLMed CP Ti shows a high
hardness ~3.89 GPa and compressive strength ~1136 MPa [13]. Also im-
portant is that no addition of other alloying element is needed and
hence no corrosion resistance or biocompatibility sacrifice. This suggests
that SLM is a promising alternative to fabrication of CP Ti with fine struc-
ture and hence enhanced mechanical properties. It is known that a
strong-textured microstructure tends to develop in the SLMed metal
parts, e.g. Ta and high-silicon steel due to the existence of directional
heat flux and large thermal gradient during SLM [14,15]. This strong tex-
tured microstructure will result in anisotropy in mechanical properties
of the fabricated metal parts, which is not desirable in many cases.
When this comes to CP Ti, this problem becomes severer due to the in-
trinsic anisotropy of its hexagonal close packed (hcp) crystal structure.
Previous studies have shown that CP Ti can suffer from cleavage fracture
at low temperature and high strain rates when the local normal stress
across the cleavage plane exceeds a critical value [1]. Based on this, the
crystallographic texture in CP Ti directly affects the propensity for cleav-
age since the relative orientations of the basal plane and the loading axis
affect the normal stress component across the cleavage plane. In addi-
tion, the crystallographic texture in CP Ti also plays an important role
in determining its biomedical properties [16,17]. This is due to the for-
mation of different oxide layer structures on different crystallographic
textures. For example, the surface consisting of more densely packed
basal planes promote the formation of Ti-OH which can in turn enhance
the cell-substrate interactions [17]. Therefore, understanding the forma-
tion of crystallographic texture in SLMed CP Ti and manipulation of the
texture is very important and necessary. However, to the knowledge of
the authors, no work has been reported on the influence of laser energy
on the texture formation in SLMed CP Ti.
In this work, fully dense (relative density ≥ 99%) and crack-free CP Ti
(Grade 1) parts were fabricated by SLM using the same optimal laser en-
ergy density Ep but with two different laser powers: high laser power EH
~250 W and low laser power EL ~50 W. The influence of laser power on
the phase formation, microstructure evolution, texture and mechanical
properties was investigated. A relation between laser power, micro-
structure and mechanical properties was established and the underly-
ing mechanism was discussed and provided. The findings of this work
provide important insights into the role of laser energy in the SLM fab-
rication of CP Ti with tailorable crystallographic texture and thus me-
chanical properties.
2. Experimental procedures
CP Ti powder (Grade 1) from LPW, UK was used in this study. The
powder size ranges from 15 to 45 μm, as shown in Fig. 1a. Selective
laser melting (SLM) was conducted on an in-house built SLM machine
equipped with a fibre laser which has a maximum power of 300 W at
the part bed. Two sets of optimal processing parameters were used to
353
fabricate fully dense (relative density ≥ 99%) and crack-free CP Ti
cubes with a dimension of 10 × 10 × 10 mm (see Fig. 1b). One was
using high laser power EH ~ 250 W (the SLMed samples were named
SHP in the following text) and the other was using low laser power EL
~ 50 W (the SLMed samples were named SLP in the following text).
The layer thickness was set at 30 μm and protective high purity argon
gas was used for all the builds to minimise oxidation.
The phase formation and microstructure of the CP Ti parts were char-
acterized using X-ray diffraction (XRD, Seifert 3003 T/T, Cu Kα radiation,
operated at 40 kV and 40 mA with a step size of 0.02° and scanning
speed 2°/min) and light optical microscope (LOM). The crystallographic
texture and grain size of the fabricated CP Ti parts were studied using
electron backscattered diffraction (EBSD) using a TSL orientation imag-
ing microscope system mounted on a Philips XL30 scanning electron mi-
croscopy (SEM) with a tungsten gun. The step size was 0.3 μm for all the
EBSD measurements.
Compression tests were carried out on cylindrical samples with a di-
ameter of 5 mm and a height of 10 mm on an Instron 5985 machine at a
constant strain rate of 1 mm/min. All the cylindrical samples were pre-
pared from the SLMed CP Ti cubes using electric discharge machining
(EDM) either along the building direction (BD) or perpendicular to
the building direction which is also the scanning direction (SD), as illus-
trated in Fig. 1c.
3. Results
3.1. Phase transformation and microstructure
The XRD patterns of the CP Ti raw powder and SLM fabricated CP Ti
samples SHP and SLP along two different cross-sections (BD and SD) are
shown in Fig. 2. It can be seen that both SHP and SLP exhibited similar
XRD patterns as the CP Ti raw powder for both cross-sections (BD and
SD), signifying that no formation of new phases was detected after
SLM. However, the relative peak intensity of (102) and (110) in SLP
along the SD cross-section decreases compared with that in the SHP
(along both BD and SD cross-sections) as well as SLP (along the BD
cross-section). Given that the same XRD experimental settings were
used for all the sample measurements, the relative intensity variation
implies that a different crystallographic texture was probably developed
in the sample SLP along the SD cross-section.
The microstructure of the SLM fabricated CP Ti samples SHP and SLP is
shown in the LOM images in Fig. 3. It can be seen that SHP consisted of a
large number of acicular-like grains while a small amount of coarse lath-
like grains can also be observed. According to previous studies [12],
these acicular-like grains were α' phases which were formed as a result
of rapid cooling of β phase from β-transus temperature (Tβ ~ 890 °C for
CP Ti Grade 1). The coarse lath-like grains were α phases which were
formed as a result of slow cooling of β phase from β-transus tempera-
ture. In contrast, SLP exhibited a very different microstructure, where
only elongated and equiaxed grains can be readily seen. These elongat-
ed and equiaxed grains were all α phases. In addition, the grains in SHP
also had a relatively smaller size than the grains in SLP. This will be de-
tailed in the following section.
3.2. Crystallographic texture
The microstructure of the SLM fabricated CP Ti samples SHP in both BD
and SD cross-sections is shown in the EBSD inverse pole figures (IPF) in
Figs. 4a and b, respectively. Elongated and equiaxed grains can be ob-
served throughout the whole samples along both the BD and SD cross-
sections (Figs. 4a and b). These grains were randomly oriented which
can be confirmed by the random colour in the IPF images. The corre-
sponding pole figures (PF) derived from the IPF in Figs. 4a and b are
shown as insets. It is clear that the CP Ti sample SHP showed no specific
crystallographic orientation preference along both BD and SD cross-
sections. The microstructure of the SLM fabricated CP Ti samples SLP
354 X.P. Li et al. / Materials and Design 116 (2017) 352–358
Fig. 1. (a) Morphology the CP Ti (Grade 1) starting powder; (b) SLM fabricated CP Ti cubes (10 × 10 × 10 mm) and (c) Cylindrical sample prepared from the SLMed CP Ti cubes using
electric discharge machining (EDM). Inset is the sketch showing the samples cut either along the building direction (BD) (red arrows) or perpendicular to the building direction which
is also the scanning direction (SD).
along both BD and SD cross-sections are shown in the EBSD inverse pole
figures (IPF) in Figs. 5a and b, respectively. In contrast to SHP, mainly elon-
gated grains can be observed throughout the entire sample in the BD
cross-section (Fig. 5a). These elongated grains showed a strong crystallo-
graphic texture, as evidenced by the overall blue colour in the IPF image.
In the meantime, both elongated and equiaxed grains can be readily seen
in the SD cross-section (Fig. 5b), which was similar to the sample SHP in
the SD direction. The corresponding PF derived from the IPF in Figs. 5a
and b are shown as insets. It was clear that a strong crystallographic tex-
ture was developed in SLP along the BD direction while no apparent tex-
ture can be observed along the SD direction. To further analyse the
texture in sample SLP in the BD cross-section, the orientation distribution
function (ODF) corresponding to the samples SLP in the BD cross-section
is shown in Figs. 6. The major volume fraction of the material was distrib-
uted around g1{φ1 = 60°, ϕ = 90°, φ2 = 60°}, i.e. close to (11-20)[1-105],
with a large spread around it. In addition, secondary peaks were also
present around g2{φ1 = 0°, ϕ = 60°, φ2 = 45°}, i.e. close to (134-4) [3-
2-10]. These texture components are different from the well-known
crystallographic texture in cooled-rolled and recrystallised CP Ti, e.g.
strong texture component {11−23}〈10−10〉 and weak component
{10−13}〈11−20〉 [18].
The grain size distribution of the CP Ti samples SHP and SLPmeasured
in both BD and SD cross-sections is shown in Fig. 7. It is clear that SHP had
Fig. 2. The XRD patterns of the CP Ti raw powder and SLM fabricated CP Ti samples SHP and
SLP along two different cross-sections (BD and SD). Red dotted rectangular is a guildance
for eyes, highlighting the relative intensity change of the peaks in the XRD patterns.
a smaller grain size (average size ~ 2.6 μm) than SLP (~3.0 μm) in the BD
cross-section while no big difference can be seen in the SD cross-section
(average size of both ~3.1 μm).
3.3. Mechanical properties
The compressive stress-strain curves for the SLM fabricated CP Ti
samples SHP and SLP cut along both BD and SD directions are shown in
Fig. 8. Interestingly, noticeable barrelling can be observed in all the test-
ed samples after the compressive strain exceeded a certain value, as
shown in the inset of Fig. 8. All the samples were flattened without com-
plete fracture. This was an indication of the excellent ductility of SLM
fabricated CP Ti samples. In this study, the ultimate compressive
strength (σUCS) was chosen at a certain compressive strain where ap-
parent barrelling can be observed. That was 50% and 45% for sample
SHP and SLP, respectively. It can be seen that SHP showed almost identical
compressive stress-strain curves along both BD and SD directions, with
a σUCS around 1.1 GPa. This indicated that there was no apparent
mechanical properties anisotropy in the sample SHP. In contrast, SLP
showed different compressive stress-strain curves along BD and
SD directions. That was the sample SLP showed a higher σUCS around
0.9 GPa along BD direction than the σUCS along SD direction which
was around 0.7 GPa, signifying the existence of mechanical proper-
ties anisotropy in the sample SLP. The mechanical properties of SLM
fabricated samples in this work were compared with previous
reported SLM fabricated CP Ti (Grade 2), coarse-grained (CG-Ti)
and ultrafine-grained (UFG-Ti) CP Ti, as shown in Table 1 [13,19].
Clearly, S HP exhibited excellent compressive strength and strain,
which were comparable to the previous reported SLMed CP Ti (Grade
2) samples and higher than other coarse-grained and ultrafine-grained
CP Ti.
4. Discussion
4.1. Phase formation and microstructure of SLMed CP Ti
It is known that the β → α phase transformation from β-transus in
CP Ti can occur martensitically or by a diffusion-controlled nucleation
and growth process [1]. Whether this phase transformation occurs mar-
tensitically or not mainly depends on the cooling rates and can also be
influenced by alloy composition, e.g. solute content in CP Ti [1]. Higher
cooling rates facilitate the martensitic phase transformation while suffi-
cient low cooling rates give rise to the diffusion-controlled phase
 X.P. Li et al. / Materials and Design 116 (2017) 352–358 355

Fig. 3. Light optical microscope (LOM) images of the microstructure of the SLM fabricated CP Ti samples (a) SHP and (b) SLP along the building direction (BD).

transformation process [1,20]. Given that the same CP Ti (Grade 1) pow- SLM. According to previous studies, RSLM can be estimated by the follow-
der was used for all the builds in this study, the phase transformation ing equation [21]:
was expected to be mainly dictated by the cooling rates RSLM during
RSLM ¼ G  RS ¼ G  v  cosθ ð1Þ

Fig. 4. EBSD orientation maps of the SLM fabricated CP Ti sample SHP measured in a section Fig. 5. EBSD orientation maps of the SLM fabricated CP Ti sample SLP measured in a section
plane along the (a) building direction (BD) and (b) scanning direction SD. The plane along the (a) building direction (BD) and (b) scanning direction SD. The
corresponding pole figures (PF) are shown in (c) and (d), respectively. The colour code corresponding pole figures (PF) are shown in (c) and (d), respectively. The colour code
representing the crystal orientation is included. representing the crystal orientation is included.
356 X.P. Li et al. / Materials and Design 116 (2017) 352–358

Fig. 6. Orientation distribution function (ODF) plots of the SLM fabricated CP Ti sample SLP corresponding to the EBSD scans shown in Fig. 5a.

where G is the thermal gradient and RS is the solidification rate. The RS
can be estimated by the product of the laser scanning speed v and the
angle between the laser scanning direction and the solidification direc-
tion of the solidifying material θ. The CP Ti samples SHP and SLP were fab-
ricated using the same Ep (in this study Ep ∝ vE where E is the laser power
and v is the laser scan speed). This means that SHP was fabricated using
a higher v while SLP was fabricated using a lower v. In the meantime,
due to the higher laser energy EH used when building SHP, the thermal
gradient G in SHP was also expected to be higher than that in SLP. All of
these resulted in a higher cooling rate RSLM in SHP when compared to
SLP. This explains why α' formed in SHP while no α' was observed in SLP
(see Fig. 3).
It is noteworthy that the large difference in RSLM in this study would
probably be a reflection of different melting behaviour occurring in the
SLM of CP Ti. According to previous studies [22,23], two melting modes
named keyhole mode and conduction mode exist during the interaction

Fig. 8. The compressive stress-strain curves for the SLM fabricated CP Ti samples (a) SHP
Fig. 7. The grain size distribution of the SLM fabricated CP Ti samples SHP and SLP measured and (b) SLP cut along the building direction (BD) (red line) and the scanning direction
in the cross-sections along the building direction (BD) and scanning direction (SD). (SD) (blue line). Insets show the CP Ti samples before and after compression.
 X.P. Li et al. / Materials and Design 116 (2017) 352–358
Table 1
Compressive mechanical properties of CP Ti produced by different techniques, σUCS repre-
sents the ultimate compressive strength, ε represents the maximum compressive strain.
CG-Ti and UFG-Ti mean coarse-grained and ultrafine-grained CP Ti, respectively.
Conditions σUCS(GPa) ε(%)
SLM (Grade 1 CP Ti) 1.1 No fracture being observed (≥50%)
SLM (Grade 2 CP Ti) 1.1 51
CG-Ti 0.8 60
UFG-Ti 0.9 35
between the laser and the materials during SLM, which play a critical
role in determining the final microstructure of the SLMed parts. The
melting mode is related to the materials properties and can be regulated
by varying the SLM processing parameters. Based on the work of King
[24], the criteria for keyhole threshold can be written as:
pffiffiffiffiffiffi
E kT b π3
pffiffiffiffiffiffiffiffi ≥ pffiffiffiffi
3 A D
vd
where d is the laser beam diameter, k is the thermal conductivity, D
is the thermal diffusivity, A is the laser absorptivity and Tb is the boiling
temperature of the material. This implies that when the same laser en-
ergy density Ep is applied, the higher the laser power E the higher the
tendency for the materials to undergo a keyhole mode will be. In this
study, two different laser powers E were used, which means that SHP
(fabricated at high laser power EH ~250 W) probably underwent a key-
hole melting mode where SLP (fabricated at low laser power EL ~50 W)
underwent a conduction melting mode. However, future studies are
needed to further confirm the melting mode in SLM of CP Ti with differ-
ent laser powers.
4.2. Texture and mechanical properties of SLMed CP Ti
In general, SLMed metal parts show a strong-textured microstruc-
ture due to the directional heat flux and large thermal gradient existing
during the SLM process [5,25–27]. For example, a heavy textured micro-
structure has been observed in SLM processed Ta with a 90° zig-zag
scanning pattern [15]. The 〈111〉 fibre texture in Ta was ascribed to
the epitaxial grain growth due to the partial remelting of the previous
layer, and to a competitive growth mechanism and specific global heat
transfer direction during SLM. Similar results were also observed in
high-silicon steel fabricated using SLM [14]. In both cases, the crystallo-
graphic texture can be altered or modified by varying the scanning pat-
terns. The underlying mechanism lies in the manipulation of the heat
transfer behaviour during SLM.
In this study, a strong directional heat transfer during SLM also
existed in both SHP and SLP. This means that a strong-textured micro-
structure should be expected in both SHP and SLP since only a 90° zig-
zag scanning pattern was used. However, this is not the case according
to Figs. 4 and 5, signifying that there might be another competitive
mechanism influencing the crystallographic texture formation during
SLM of CP Ti. Although it is known that the β → α transformation fol-
lows the Burger's orientation relationship where a random texture is
expected [1], previous studies have shown that in many cold rolled Ti
a strong texture develops during the β → α transformation [28–30].
This strong texture is caused by variant selection during the solidifica-
tion process which can be influenced by many factors including the so-
lidification condition and phase transformation [31]. Since the same
scanning pattern and no preheating were used for both SHP and SLP,
SHP should exhibit a more general and directional heat transfer when
compared to SLP due to the high laser power EH used. This means that
the weak-texture observed in SHP was probably mainly caused by the
martensitic phase transformation during SLM. A similar result has also
been reported in electron beam melting (EBM) of CP Ti [32].
357
It is worth pointing out that there are a few influential factors for the
variant selection or crystallographic texture formation during β → α (or
β → α′) phase transformation in Ti, e.g. stresses generated by volume
change as well as some characteristic grain boundaries which favours
Reference nucleation of certain orientation and etc. [33]. Since the martensitic
This work phase transformation in this study happened at a relatively high tem-
[13] perature (martensite start temperature Ms ~850 °C), any stresses devel-
[19]
oped would be relieved. Hence, the texture formation in this study
[19]
would probably be mainly influenced by the characteristic grain bound-
aries which favoured nucleation of statistical variant orientations during
β → α′ martensitic phase transformation. However, since there was no
or very limited β Ti phase left in the CP Ti [1], it is difficult to clarify the
grain boundary relation between them. Therefore, further detailed in-
vestigation will be needed to verify this hypothesis. Another close look
of the IPF and PF (Fig. 4) reveals that SHP is not completely textureless.
Some of the regions still showed a preferential crystal orientation. This
means that although the martensitic phase transformation can influ-
ence the texture development during SLM of CP Ti the heat flow behav-
ð2Þ
iour still plays an important role in texture formation. Therefore, the
formation of texture during SLM of CP Ti in this study is actually a com-
petitive mechanism between heat flow and the martensitic phase
transformation.
As a result of the formation of α' phase and the weak-textured mi-
crostructure in SHP, SHP showed isotropical mechanical properties
along the BD and SD directions and a higher compressive strength
than that of SLP. Althougth α' is less ductile than α phase in CP Ti,
there was still a large fraction of α phase formed in SHP (Fig. 3a). This
probably explains why SHP showed a large elongation and apparent
barrelling without complete fracture, similar to SLP (Fig. 8). Further-
more, since the formation of α' phase is related to the cooling rates dur-
ing SLM which depends on the SLM processing parameters, the
proportion of α' phase can also be controlled through varying the SLM
processing parameters. This provides another promising method to ob-
tain SLM fabricated weak-textured CP Ti with tailorable mechanical
properties.
5. Conclusion
In this work, fully dense CP Ti parts were fabricated using the same
laser energy density Ep but with different laser powers: high laser
power EH ~ 250 W and low laser power EL ~ 50 W. The influence of
laser power on the phase formation, microstructure evolution, crystallo-
graphic texture and mechanical properties of SLMed CP Ti was system-
atically studied. Following points can be drawn from this study:
(1) Although the same Ep was used, the CP Ti fabricated using EH ex-
hibited martensitic phase transformation with the formation of
acicular-shaped α' phase while only elongated and equiaxed α
phase formed in the CP Ti fabricated using EL. The underlying rea-
son was attributed to the higher cooling rates during SLM at EH.
(2) As a result of the formation of α' phase, a weak-textured micro-
structure was developed in the CP Ti fabricated using EH while a
strong-textured microstructure was obtained in the CP Ti fabri-
cated using EL.
(3) The weak-textured CP Ti fabricated using EH exhibited isotro-
pic mechanical properties along the building (BD) and scan-
ning (SD) directions with an ultimate compressive strength
(σUCS) ~ 1.1 GPa and a compressive strain ≥50%. This was compa-
rable to the previous reported SLMed CP Ti (Grade 2) samples
and higher than other coarse-grained and ultrafine-grained CP Ti.
Acknowledgements
This work was supported by the Belgian Agency for Innovation by
Science and Technology (IWT) Strategic Basic Research (SBO) project
“MultiMet”.
358 X.P. Li et al. / Materials and Design 116 (2017) 352–358
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