Acta Materialia 169 (2019) 45e59

Contents lists available at ScienceDirect

Acta Materialia
journal homepage: www.elsevier.com/locate/actamat

Full length article

Microstructural optimization through heat treatment for enhancing

the fracture toughness and fatigue crack growth resistance of selective
laser melted Tie6Ale4V alloy
Punit Kumar, Upadrasta Ramamurty*
School of Mechanical & Aerospace Engineering, Nanyang Technological University, Singapore, 639798, Republic of Singapore

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

Article history: The yield strength (sy) of Tie6Ale4V alloy, additively manufactured via selective laser melting (SLM) of
Received 1 January 2019
pffiffiffiffiffiffi
powder beds, can exceed 1000 MPa while possessing a mode I fracture toughness (KIc) of ~50 MPa m .
Received in revised form The possibility of enhancing KIc as well as fatigue crack growth resistance, without a significant penalty
18 February 2019
on sy, via a judicious heat treatment process that transforms martensitic a’, which is present in the as-
Accepted 4 March 2019
Available online 6 March 2019
SLM microstructure due to rapid cooling of the molten metal, into an a/b phase mixture is examined. It
was demonstrated that duplex annealing at temperatures below the b transus temperature of the alloy
would lead to such a microstructure while retaining the mesostructure, whose nature depends on the
Keywords:
Mechanical properties
process parameter combinations utilized. Near-doubling of the fracture toughness with only a ~20%
Titanium alloy reduction in sy was noted upon heat treatment. While the strength becomes isotropic after heat
Fatigue treatment, significant anisotropy in the fracture toughness of the heat-treated alloy with columnar prior
SLM b structure was noted. While the steady state fatigue crack growth (FCG) rates are comparable to cor-
Heat-treatment responding values of the same alloy, but manufactured using conventional means, the threshold for
fatigue crack initiation (DK0) increases by 34%e56%. The enhancement in DK0 was found to be a result of
the transition in the near-threshold crack growth, from trans-to inter-granular and caused by the a/b
basket weave microstructure, which imparts a high crack path tortuosity. Overall, this study demon-
strates that post-processing heat-treatment can improve the damage tolerance of SLM Ti64 by increasing
both KIc and DK0.
© 2019 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

1. Introduction phase is atypical in the specimens that are manufactured using

Additive manufacturing (AM) of metallic components, by using
either lasers or e-beams for fusing selected locations of power beds,
offers a number of advantages, particularly from the manufacturing
perspective. Consequently, this emerging field is attracting
considerable current research interest, especially from the metal-
lurgical stand point of view. Since the molten pool at any instance is
small in volume, it gets rapidly quenched. This, in turn, results in a
metastable microstructure with enhanced solid solubility of the
solute elements (when present) and highly refined microstructural
features such as grain size. In the case of Tie6Ale4V (Ti64 here
afterwards), the as-selectively laser melted (SLM) alloy's micro-
structure consists of acicular a0 martensitic phase, whereas such a
* Corresponding author.
E-mail address: uram@ntu.edu.sg (U. Ramamurty).
conventional means of casting followed by thermo-mechanical
processing. Additionally, the line-by-line, layer-by-layer method
of part fabrication via SLM imparts a distinct mesostructure to
them. Together, the combinations of micro- and meso-structural
features can lead to unique combinations of mechanical proper-
ties for 3D printed alloy coupons [1].
A particular issue, as far as SLM Ti64 is concerned, is the pres-
ence of the columnar prior b grains, whose height can span the
entire coupon in the build direction [2e4]. In a recent paper [5], we
demonstrated that it is possible to eliminate it, and obtain equiaxed
grain structure without resorting to additional alloying elements,
via a judicious combination of layer thickness, t, and scan rotation
between successive layers, f. Detailed mechanical property char-
acterization showed that all the alloy coupons, produced with four
different t - f combinations, were found to exhibit high yield
strength, sy, which was attributed to the fine martensitic a0 lath
microstructure, while possessing a reasonably good mode I fracture

https://doi.org/10.1016/j.actamat.2019.03.003
1359-6454/© 2019 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
46 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
pffiffiffiffiffiffi
toughness, KIc, of ~50 MPa m . The stability of a0 , which is a
metastable phase, in service conditions, especially at high tem-
peratures, is a major concern and hence Ti alloys with a0 in their
microstructures are not generally favored. Keeping this in view, in
this study we explore various heat treatment schedules that would
not only transform a’ into a more stable a/b phase mixture, but also
enhances the ductility and KIc without a substantial compromise on
sy. Note that an a/b microstructure in Ti64 produced via SLM can be
achieved by adapting several different 'in-situ tailoring' methods
such varying the focal offset distance (FOD), maintaining a close
hatch spacing (so that melt pools overlap multiple times), and
preheating of the powder bed [6,7]. While these can improve the
ductility and produce lead to Ti64 parts whose properties are
comparable to those of wrought Ti64, an overall reduction in the
process efficiency is a major drawback of them. For instance, the
requirement of a fine control of the thermal gradient across the
layers imposes a restriction on the size of the built parts [8]. Like-
wise, reducing the hatch spacing increases the time required for
part production.
The other possible way to impart the desired microstructure to
SLM Ti64 is by employing a suitable post-processing heat-treat-
ment. Though it will indeed add an extra step to the manufacturing
process, part size will no longer be a major factor. Nor it will reduce
the production efficiency [4] since a post-SLM anneal may be
imperative, so as to relieve the built-in residual stresses, in many
cases. While several studies have been performed in this direction,
they have mostly limited their efforts to the examination of the
microstructures of the heat treated samples [4,9e11]. In particular,
a comprehensive understanding of the structure - property corre-
lations, especially the effect of heat treatment on the damage
tolerance characteristics, in terms of fracture toughness and fatigue
crack growth (FCG) resistance, is yet to be developed. While a few
studies do report the effect of post-processing on these properties
of SLM Ti64 [12e14], they are not comprehensive in nature; either
only one SLM processing condition is investigated or property
evaluation was not detailed. Importantly, an emphasis on corre-
lating the observed mechanical response to the underlying micro-
structure, which would pave the way for further optimization of
property combinations via microstructural design, is often missing.
Keeping this paucity in view, a detailed investigation into the effect
of the heat treatment on the micro- and meso-structures of SLM
Ti64, and, in turn, effect of a selected annealing schedule on the
mechanical response of the alloy processed using four different
combinations fo SLM parameters that result in mesostructures
ranging from columnar to equiaxed prior b grain structures was
conducted in this study.
2. Materials and experiment
2.1. Coupon fabrication via SLM and post-fabrication heat
treatments
All the samples examined in this work were fabricated by using
the ELI grade Ti64 powder. SLM was performed in an EOSINT M 280
SLM machine equipped with a Yb: YAG fiber laser. During fabrica-
tion, an inert atmosphere was maintained in the chamber by
maintaining a constant flow of Ar gas; via this, the oxygen content
in the chamber was maintained below 0.1 ppm. Coupons that are
14 mm thick and 64  64 mm2 cross-section were produced by
employing four different t-f combinations: t ¼ 30 or 60 mm and
f ¼ 67 or 90 . For coupons produced with t ¼ 30 mm, the scan
spacing (l) was 140 mm, whereas it was 120 mm for t ¼ 60 mm. The
samples are designated as 3090, 3067, 6090 and 6067; here, the
first two digits refer to t whereas the next to f. For example, 3090
indicates that t ¼ 30 and f ¼ 90 .
The fabricated coupons were subjected to four different heat
treatment schedules (labeled HT1, HT2, HT3, and HT4) which are
schematically illustrated in Fig. 1. As seen from it, the maximum
annealing temperatures, Ta, in HT1 and HT2 are below the b transus
temperature (Tb ¼ 995  C), such that the prior b mesostructure is
retained [5]. In contrast, Ta in HT3 and HT4 is above Tb; as a result,
the prior b mesostructure present in the as-SLM samples gets
transformed (see section 3 for details). While HT1 and HT 3 employ
a single step annealing, HT2 and HT4 utilize a two-step (or duplex)
process. The choice of Ta either being above Tb or below it is made so
as to evaluate the relationship between final aþb microstructure
with the initial a0 microstructure and prior b mesostructure. The
cooling rates were selected so as to analyze the effect of the ho-
mogenizing step on the partitioning of the a and b phase by
decomposition of a’.
2.2. Microstructural and mechanical property characterization
For microstructural analyses of the heat-treated coupons, opti-
cal and scanning electron microscopies (SEM) were employed on
samples that were mirror polished and etched using the Kroll's
reagent (100 ml distilled water, 5 ml nitric acid, and 2 ml HF). Op-
tical images were taken from the top as well as side surfaces of the
samples to generate 3D representative microstructures. The a lath-
thickness, la, in all the samples was measured from the SEM images
using at least four images for each sample and ImageJ, a commer-
cially available image analysis software. ImageJ was also used to
determine b volume fractions, Vb, using high magnification SEM
images. For estimating Vb, SEM images were first converted in to
RGB stack type and then in to gray scale image by thresholding to
generate clear contrast between a and b phase. The presence of b
phase in the microstructure was confirmed through wavelength
dispersive X-ray spectroscopic (WDS) compositional analysis in an
electron probe microanalyzer (EPMA).
For the texture analysis of the microstructures both before and
after the heat-treatment, electron backscatter diffraction (EBSD)
scans were carried out electropolished samples. In each sample, an
area ~400  400 mm2 was scanned using a step size of 0.3 mm.
Texture analysis was performed on both the top (B) and side (S)
surfaces with respect to the build direction of SLM. The data
generated was analyzed by using a commercially available
software.
For examining the mechanical behavior of heat-treated SLM
coupons, tensile stress-strain responses, fracture toughness, and
FCG resistance properties were evaluated. The tensile tests were
performed on dog-bone shaped specimens with 6 mm gauge
Fig. 1. Schematic illustration of the four different heat treatment schedules utilized in
this study.
 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59 47

length and 2 (width) by 0.5 (thickness) mm2 cross-section. da/dN vs. DK data generated was analyzed using the Paris equation:
Displacement controlled tensile tests were performed at a nomi- da/dN ¼ C(DK)m, where C and m are material properties and are
nal rate of 0.001 mm/s, according to the ASTM standard D1708 [15]. referred to as Paris constant and exponent, respectively. Standard
The loading direction is either parallel or perpendicular to the build procedures described in the standard ASTM 647-15 were utilized
direction; this allowed us to assess the degree of anisotropy in for estimating m from the experimental data generated. Post-
properties. Hereafter, we refer to these either as ‘B’ or ‘S’ respec- mortem fractographic analyses were performed on all the tensile
tively, as abbreviations of 'build' and 'scan' directions. Note that the tested samples as well as the quasi-static and fatigue fractured
latter is orthogonal to the build direction. samples so as to ascertain the dominant failure mechanisms.
Experiments to evaluate KIc and FCG characteristics were con-
ducted on Chevron notched, compact-tension specimens, C(T),
3. Results
electrical discharge machined (EDM) from the SLM blocks, with a
thickness, b, of 12 mm and width, W, of 24 mm. (Since these di-
3.1. Effect of the heat treatment on the microstructure
mensions are approximately half of the standard specimen sizes,
such specimens are often referred to as half C(T)). In all the cases,
The four different heat treatment schedules employed in this
two samples were tested for measuring fracture toughness and
study imparted a wide range of micro- and meso-structures to Ti64.
fatigue crack growth characteristics and the average values are
The as-built coupons' microstructures and mechanical properties
reported. Prior to testing, both the sides of the samples were mirror
were discussed in detail by us in an earlier paper [5] and hence will
polished, so as to monitor the crack growth using a traveling mi-
not be repeated here, unless otherwise necessary. The micro-
croscope (0.01 mm resolution at 10X magnification). The samples
structures resulting from different heat treatment schedules are
were fatigue pre-cracked, for up to a/W ~0.45e0.55, where a is the
described here, using 3090 as the representative example. In the as-
crack length and W is the width of the specimen, using a servo-
SLM condition, it contains long columnar prior b grains, which are
hydraulic testing machine. A sinusoidal wave form with a fre-
square in cross-section; the sides of the square are exactly the same
quency of 10 Hz and at a load ratio, R (defined as the ratio of
as the scan spacing employed (140 mm) [5]. Representative 3D
minimum to maximum load of the fatigue cycle), of 0.1, as pre-
microstructures of this alloy after HT1 and HT2 are displayed in
scribed in the ASTM standards E399-12 [16] and ASTM 647-15 [17],
Fig. 2a and b, respectively. Since annealing below Tb does not alter
was employed for cycling the load. After the pre-cracking, the
the prior b grains [11], their signature columnar structure remains
samples were loaded in quasi-static mode until fracture at a
intact. However, HT2 leads to the coarsening of the a laths since Ta
displacement rate of 0.01 mm/s in order to determine KIc.
is closer to Tb as compared to that in HT1. A higher magnification
The load shedding method, prescribed in ASTM 647-15, was
image, displayed in Fig. 3a, shows needle shaped a laths with b
utilized to determine the threshold for fatigue crack initiation, DK0,
phase along the grain boundary in alloy subjected to HT1; the shape
during FCG testing of the pre-cracked C(T) specimens. Here, the
of the a laths is more lenticular in the case of HT2 (Fig. 3b). A similar
stress intensity factor range (DK) was reduced by ~10% after each
microstructure was noted by Vrancken et al. [18] after the heat-
crack length increment of 0.2 mm till the crack growth rate per
treatment of SLM Ti64 below Tb.
cycle, da/dN, is  2  109 m/cycle; the stress intensity factor range,
For Ta > Tb, however, the columnar prior b grain structure is
DK, at which this was achieved was designated as DK0. Subse-
completely erased by the heat treatment, as seen from Fig. 2c and d,
quently, DK was increased by ~10% after each 0.2 mm fatigue crack
which show the mesostructures after HT3 and HT4, respectively.
extension until failure. The steady-state crack growth regime of the
This leads to equiaxed prior b grains that are significantly coarser

Fig. 2. Representative 3D microstructures of alloy 3090 after being subjected to heat treatment schedules (a) HT1, (b) HT2, (c) HT3, and (d) HT4.
48 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
Fig. 3. Representative microstructures (Obtained using SEM) of alloy 3090 after being subjected to heat treatment schedules (a) HT1, (b) HT2, (c) HT3, and (d) HT4.
with >500 mm sizes, irrespective whether the cooling was per-
formed in single or duplex steps. This observation is consistent with
that reported by Lütjering [19], who found that the holding time at
Ta or the rate of cooling from Ta to room temperature do not exert
any pronounced effect on the prior b grain size as long as Ta > Tb.
The a lath structure, however, does depend on whether the
cooling from Ta is performed in one step or two. The relatively fast
cooling in the single step cooling process (HT3) leads to the for-
mation of a fully a0 lath microstructure with the basket weave
structure (Fig. 3c). However, the morphology of this martensite is
different (and hence referred to as secondary a’) as compared to the
needle-shaped martensite laths observed in the as-built SLM Ti64.
The homogenization at 700  C in the case of the heat treatment
with duplex cooling (HT4) results in an equilibrium microstructure
(Fig. 3d) with large colonies of the a lamellae inside the prior b
grains and b phase along the lamellae boundaries.
The mechanism of precipitation of the b phase within the col-
onies during the annealing treatments HT1 and HT2 is different
from that in HT3 and HT4. When Ta is below Tb, the supersaturated
a’ transforms into a by rejecting alloying element V out of the
transformed product; the resulting high concentration of V along
the a lath boundary, leads to the nucleation of the b phase [20].
(Note that V is a b stabilizer due to its BCC crystal structure.)
However, in HT3 and HT4, the a laths nucleate at the prior b grain
boundaries are grow radially inwards of the grain [21].
The four different heat treatment schedules employed influence
la, whose variation in different specimens in terms of the average
lath thickness, la , is plotted in Fig. 4a. From it, we note that la in
HT4 sample is substantially higher than those estimated for HT1,
HT2, and HT3 samples. Within the latter three, la in the HT2 sample
is relatively higher as compared to HT1, indicating a higher fraction
of the coarse laths in it; this is illustrated via Fig. 4b where the
distributions in la in 3090 subjected to HT1 and HT2 are plotted.
This is because lath coarsening is favored when Ta is closer to Tb
[18,22]. From Fig. 4a, we see that la in SLM samples built with
t ¼ 30 mm is slightly higher than those manufactured with
t ¼ 60 mm. This difference is pronounced in the case of HT3 and HT4
samples, probably because of the smaller prior b grain size in the
case of t ¼ 60 mm, which is related to l, in the as-built SLM micro-
structure. (Recall that l ¼ 120 mm for t ¼ 60 mm whereas it is 140 mm
for t ¼ 30 mm [5].) Smaller prior b grains result in a smaller la
because the b phase transforms into a laths by the nucleation of a/a’
laths from the prior b boundary [21].
The difference in Ta of HT1 and HT2 leads to different Vb in the
microstructure because the concentration of V that is rejected along
the a lath boundary is larger at higher temperatures. When Ta is
closer to T (as in HT2), a higher equilibrium Vb can be expected.
Fig. 4c and d shows that the b phase decorates the lath boundary in
the HT1 (14%) and HT2 (22.5%) microstructures, which was
confirmed by WDS (Fig. 5). The compositional analysis also shows a
higher concentration of V along the a lath boundaries which is an
evidence of the presence of b phase, whereas a higher concentra-
tion of Al is noted in the interiors of the a laths.
3.2. Effect of the heat treatment on the texture
Texture analyses were performed to investigate the crystallo-
graphic aspects related to the following microstructural features of
SLM Ti64: prior b mesostructure, basket wave structure, colonies,
and laths. The Burgers orientation relationship (BOR) between the a
laths and the BCC b matrix [23] is well known. It is based on two
parallel planes (0001)a jj {110}b and directions <1120>a jj <111>b in
the respective phases. Owing to symmetry in the parent and
product crystals, a total of 12 different variants for the a/a0 nucle-
ation from the b matrix is possible. The high cooling rate that is
associated with the SLM process provides a sufficient driving force
for the formation of a’ laths with almost all the possible variants.
This, in turn, results in the formation of laths with several different
orientations leading to a basket weave microstructure. This is
illustrated via the inverse pole figure (IPF) map of the microstruc-
ture of as-SLM 3067 sample, displayed in Fig. 6a. However, it has
been reported that some variants are statistically more favourable
 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59 49

Fig. 4. (a) Comparison of the average lath thickness' in the four alloy coupons that were subjected to different heat treatment schedules. (b) Distributions in the lath thickness' and
(c) and (d) the b-phase distribution, in 3090 after annealing per HT1 and HT2 schedules, respectively.

Fig. 5. (a) Backscattered electron micrograph obtained from 3090 after being subjected to HT2. Figures (b), (c), and (d) show the elemental distribution maps of Ti, Al, and V,
respectively.

compared to others [24]. The different texture variants can be
identified with the aid of the peak intensities in the pole figure at
different locations. The (0001) pole figure of 3067, displayed in
Fig. 6b, shows that the few peaks have a higher intensity than the
others. The maximum peak intensity, which is also referred to as
the texture strength of the sample, in this pole figure is 7.9. The
intensity peaks along the boundary of the pole figure correspond to
the {1120} planes as indicated in Fig. 6b. The laths corresponding to
these planes have a prismatic orientation.
As mentioned already, since Ta is below Tb in both HT1 and HT2,
50 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59

Fig. 6. (a) Representative inverse pole figure (IPF) map, obtained using electron back scattered diffraction (EBSD), of 3067 in the as-SLM condition. Black lines are drawn to guide the
eye in delineating the colonies. (b) Texture distribution represented by the (0001) pole figure.

the prior b mesostructure remains intact in the SLM Ti64 samples
even after these heat-treatments. Hence, the IPF maps of the
sample 3067 after HT1 and HT2 (Fig. 7a and b, respectively) show
similar prior b structure as that seen in Fig. 6a. The mechanism
responsible for lath coarsening during the heat treatments HT1 and
HT2 can be analyzed using the texture data. The (0001) pole figure
of 3067 subjected to HT1 (Fig. 8a) shows similar peak intensities for
nearly-all the variant planes. Although the number of variants re-
mains the same, the texture strength is reduced by almost half. The
pole figure of 3067 after HT2 (Fig. 8b) shows that a higher Ta
markedly reduces the number of variants. This observation implies
that the lath coarsening is due to the bigger a laths with the pris-
matic orientation {1120} growing at the expense of smaller ones
with the basal texture [25]. Consequently, a higher texture strength
(6.9) was noted for the HT2 sample than in HT1(4.8).
The completely transformed prior b structure due to the heat
treatment at Ta > Tb (HT3 and HT4) can be clearly seen from the IPF
maps displayed in Fig. 7c and d, respectively. Notably, the resulting
microstructures do not depend on the respective structures in the
as-built coupons. As discussed in the previous section, fast cooling
during HT3 results in a microstructure with 'interwoven' a0 laths.
(The presence of a0 in the microstructure even after annealing is
due to the relatively high cooling rate associated with the air-
cooling process employed.) Additionally, the presence of a coarse
a phase on both the sides of the prior b boundaries can be noted;
this phase is often referred to as massive a, and was reported to
consist of an ultrafine lamellar mixture of a and b phases [26,27].
Importantly, this phase's presence in the microstructure of Ti64 is
considered detrimental from the mechanical performance point of
view, especially fatigue resistance [18,28,29]. A similar massive
transformation has been observed in the as-fabricated Ti64, man-
ufactured using either the electron beam melting (EBM) or the
shaped metal deposition (SMD) techniques; the reason for this is
the high energy inputs utilize, which causes the overall cooling rate

Fig. 7. Representative IPF maps after heat treatment. Figures (a) and (b) are from 3067 subjected to HT1 and HT2, respectively whereas (c) and (d) are from 3030 after HT3 and HT4,
respectively. In all cases, the build (B) direction is normal to the plane of the micrograph.
 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
Fig. 8. (0001) pole figures of 3067 subjected to (a) HT1 and (b) HT2, and 3090 subjected to (c) HT3 and (d) HT4. In all cases, texture analysis was performed on the B plane.
to lower than 420  C/s [26,30].
The large prior b grains and the massive a phase along the grain
boundaries impart a substantially large texture strength (21.5) to
the HT3 sample (Fig. 8c). The other possible contributor to this
strong texture is the preferred variant selection during the trans-
formation of b to a’ phase, as air cooling after annealing provides a
relatively smaller driving force for such a transformation (as
compared to that in SLM).
The homogenization step during cooling in the heat treatment
schedule HT4 (Fig. 7d) results in an equilibrium microstructure
having colonies in which all the laths have the same orientation.
Such a microstructure is often referred to as the lamellar structure.
Here, b nucleates at the boundaries of the a lamellae, and its
orientation is determined by BOR. The (0001) pole figure of the
sample (Fig. 8d) shows a strong fiber texture along the prismatic
direction, with a strength of 38, due to contributing factors such as
large prior b grains and colonies with thick laths.
Since the objective of the current study is to examine the pos-
sibility of further improving the overall performance of SLM Ti64,
we have selected HT2 for mechanical property studies. This was
done on the basis of the extensive knowledge on the microstructure
- mechanical property relations in TI64 that is available in litera-
ture, with the following being the key considerations. (i) The
massive a phase formed due to HT3 and HT4 will adversely affect
the tensile strength because of the localization of deformation
along the grain boundary regions [26,30]. Moreover, these samples
not only lost the SLM prior b structure, but also contain highly
coarse prior b grains; such coarse microstructures are generally
undesirable. The microstructure also contains colonies of the laths
with similar orientation, which often leads to relatively low fatigue
crack growth resistance [21,31]. These considerations eliminated
the further pursuit of HT3 and HT4 in this study. (ii) Both the
remaining heat treatment schedules, HT1 and HT2, leave the prior b
51
structure intact. Since a microstructure with a coarse lath structure
is preferable–because thicker laths can lead to higher crack tortu-
osity that could impart crack growth resistance, HT2, which leads to
such a microstructure, was chosen [31].
3.3. Effect of the heat treatment schedule HT2 on the prior b
mesostructures
The four different combinations of t and f used for SLM Ti64
result in mesostructures that range from columnar to equiaxed
prior b grains [5]. Fig. 9a shows the 3D representative IPF map of
the sample 3090 after HT2. As expected, the columnar prior b
structure remains intact after the heat-treatment. Within each
prior b grain, laths with multiple orientations can be seen. How-
ever, thicker laths with similar orientation are more common than
smaller laths, especially on the side surface (S plane). Consequently,
the S plane has a higher texture strength (12) as compared to the B
plane (7); see respective (0001) pole figures in Fig. 10c and a. Most
of the thicker laths in the S plane are at 30 to 45 to the building (B)
direction. The texture of these laths exhibits a peak intensity near
the prismatic planes {1120} (Fig. 10c).
When f is changed from 90 to 67, while maintaining
t ¼ 30 mm, the columnar prior b grain structure breaks down (see
Fig. 9b). This, in turn, leads to similar texture strengths in both the B
(6.9) and S planes (5.1); see Figs. 8b and 10e, respectively. A com-
parison of the pole figures of S3067 (Fig. 10e) and S3090 (Fig. 10b),
both after HT2, indicates a higher number of texture variants in the
former. The B plane of 6090 (Fig. 9c) stills exhibits the square prior b
grain cross-sections in that plane, although they columnar struc-
ture breaks down in the S plane due to formation of the melt pool
boundaries.
Fig. 9d shows that 6067 has equiaxed grains in both B and S
planes. The respective pole figures, displayed in Fig. 10b and d,
52 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
Fig. 9. Representative 3D IPF maps of (a) 3090, (b) 3067, (c) 6090 and (d) 6067, subjected to the heat treatment schedule HT2.
indicate texture strengths of 5.9 and 6.2, respectively, confirming
microstructural isotropy. However, the pole figure obtained on the
B plane indicates a higher number of texture variants as compared
to that obtained from the S plane. In latter, the peak texture in-
tensity is along the prismatic planes (2110), (1210) and (2110) and
most of the laths make 30 to 45 with the build direction (Fig. 9d).
3.4. Mechanical properties
Representative tensile stress - strain responses, measured on
different coupons after HT2, with the loading axis being either
parallel or perpendicular to the build direction, are displayed in
Fig. S1 of the supplementary information (SI). Tensile properties
such as sy, ultimate tensile strength, su, and strain to failure, ef,
extracted from such plots are summarized in Table 1. The relative
changes in these properties (in %) with respect to those measured
on as-SLM samples (reported by us in Ref. [5]) are also given. The
following are the key observations made from the data given in
Table 1. (i) Upon heat treatment, and as expected, both sy and su
decrease in all the cases. While the overall range of these reductions
is relatively wide (7%e23%), majority of data is between 15% and
20%. Interestingly, 3090 sample with the columnar microstructure
shows the least reduction, especially in the S orientation. (ii) While
sy ranges between 873 and 1029 MPa, su varies from 947 to
1079 MPa. These strength values are still superior to the respective
values of conventionally manufactured alloys with similar grain
sizes [19,32,33]. (iii) The amount of strain hardening in all samples
is relatively minor, as gauged from the difference between su and
sy (range: 47e93 MPa). It is the lowest in 3090 tested in the B
orientation; sy is the highest in this case, exceeding 1000 MPa. (iii)
On comparing sy and su measured in B and S orientations, we note
that 3067, 6090, and 6067 remain nearly-isotropic even after the
heat treatment. Even in 3090, which has columnar prior b grains,
the anisotropy in sy is only ~5%. (iv) The strength reductions that
are seen upon annealing are more-than-adequately offset by
ductility enhancements, as gauged by ef. In some cases, the im-
provements are more than 50%. Fractographic observations do
indeed indicate to 'cup and cone' fracture features (not shown
here), confirming the ductile nature of the heat treated SLM Ti64.
The fracture toughness values measured on all the heat treated
samples are also listed in Table 1. Note that these are labeled as
conditional fracture toughness', Kq, as the specimen thickness of
the half-C(T) specimen that was utilized is insufficient to satisfy the
plane strain conditions as per ASTM E399-12 [16]. (For as-SLM
samples, those conditions were satisfied by the same-sized sam-
ples utilized to evaluate KIc. After heat treatment, however, the
combined effect of a reduction in sy and increase in the fracture
toughness made them inadequate.)1 As seen from Table 1, sub-
stantial enhancements in the fracture toughness of SLM Ti64 accrue
as a result of the heat treatment; in a few cases, the toughness more
than doubled. This is significant, especially since the KIc values of
pffiffiffiffiffi
as-SLM samples (ranging between 48 and 58 MPa m [5]), them-
selves, were comparable to those of the conventionally manufac-
tured Ti64 [5]. While 3067 and 6067 are nearly-isotropic in their
fracture responses, the coupons built with 90 scan rotation (3090
and 6090) exhibit non-negligible anisotropy. This is in contrast to
the as-built case, wherein KIc in all the coupons built with different
1
ASTM E399 prescribes that the thickness (and uncracked ligament length)
should be at least 25 times the plane strain plastic zone size (rp). In the current
context, the largest value of rp is 1.3 mm (for 6067 whose Kq ¼ 101 MPa√m, and
sy ¼ 883 MPa), which is about a tenth of the thickness of the sample (12 mm).
Hence, it is likely the Kq values that we reported are far-closer to plane strain
condition than plane stress. Munz et al. [55] have investigated the effect of thick-
ness on the fracture toughness of Ti64 and report that it is possible to determine
the plane strain fracture toughness if either extensive plastic deformation or stable
crack growth at the crack tip do not occur. They report that the R-curve is inde-
pendent of thickness in the investigated range of 2 < b < 20 mm and hence Kq is also
independent of thickness within this range. Moreover, their work reveals that the
divergence between the maximum toughness (on account of the R-curve behavior),
determined by using the maximum load (Pmax, where after unstable crack growth
occurs) of the load-displacement curve and Kq diverge by only about ~10% (see
Fig. 8 in their paper), at maximum, for specimens that are between 10 and 20 mm
thick (see Fig. 8 in their paper). Representative example of the load vs. displace-
ment plots, which were used to determine Kq by the secant method in our study,
are displayed in Fig. S3. In both cases, minimal nonlinearity before Pmax is noted. As
a result, the secant method also yields the Pmax as the load with which Kq needs to
be computed. All the above observations clarify indicate that it is reasonable to
compare Kq values of the heat treated SLM Ti64 samples with the KIc data obtained
on specimens in the as-processed state.
 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59 53

Fig. 10. (0001) pole figures after heat treatment HT2 of 3090 in (a) B and (c) S orientations, 6067 in (b) B and (d) S orientations, and (e) 3067 in S orientation.

Table 1
Summary of the mechanical properties of heat-treated SLM Ti64. The data in parenthesis indicates the relative change due to the heat treatment as compared to the respective
value in the as-SLM state. See Ref. [5] for the properties of the as-SLM alloy coupons. Red and blue colors are used to highlight property deterioration or improvement,
respectively.

Sample sy (MPa) su (MPa) ef (%) Kq (MPa√mÞ DK0 (MPa√mÞ m rmax (mm) rc (mm) la (mm)
3090 B 1029±11 (11%) 1079±8 (13%) 11.6±1:7 (53%) 106 (104%) 8 (43%) 3.9 (54%) 8.3 1.60 0.87
S 944±13 (8%) 1016±16 (-7%) 12.5±0.6 (60%) 77 (40%) 8.1 (42%) 3.5 (6%) 9.6 1.95 1.01
3067 B 875±25 (-22%) 957±19 (-19%) 12±2:4 (48%) 96 (100%) 7.1 (34%) 3.7 (4%) 8.6 1.75 0.8
S 873±17 (-22%) 947±15 (21%) 11.8±0.5 (17%) 93 (72%) 8.3 (43%) 3.4 (10%) 11.8 2.40 0.77
6090 B 881±12 (-23%) 974±12 (-20%) 13.1±2:6 (34%) 97 (90%) 8.1 (40%) 3.7 (29%) 11.1 2.24 1.12
S 901±22 (-19%) 975±26 (18%) 15.8±1.9 (63%) 83 (57%) 8.3 (43%) 4 (38%) 11.1 2.25 1.11
6067 B 883±10 (-20%) 956±7 (-17%) 16.6±0.7 (33%) 101 (74%) 8.4 (56%) 3.7 (5%) 11.9 2.40 0.99
S 874±8 (-18%) 963±12 (-15%) 13.9±0:2 (9%) 95 (64%) 7.9 (39%) 3.2 (8%) 10.7 2.17 1.07

combinations of t and f was found to be relatively insensitive to the
specimen orientation with respect to the build direction.
The values of Kq of the heat treated SLM Ti4 of the present study
are comparable with those reported for forged Ti64
pffiffiffiffiffi
(88e110 MPa m) and cast and hot isostatically pressed Ti64 with
pffiffiffiffiffi
grain sizes of the order of 2 mm (97e112 MPa m). However, they
are much higher than the Kq of the cast and annealed Ti64
pffiffiffiffiffi
(65e90 MPa m) [32,34,35]. They are also higher than those
54 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
reported for heat-treated SLM Ti64, for which only a few studies
have been performed thus far. Cain et al. [13] report a KIc of
pffiffiffiffiffi
~49 MPa m for SLM Ti64 after it was subjected to a single step heat
treatment. Dhansay et al. [12] investigated fracture toughness of
duplex heat-treated SLM Ti64 and found near isotropic value (80
pffiffiffiffiffi
and 85 MPa m) in both B and S directions. Seifi et al. [35] report Kq
pffiffiffiffiffi
ranging between 65 and 80 MPa m with minimal anisotropy for
Ti64 fabricated using the electron beam melting technique,
wherein the build platform was maintained at a temperature of
750  C, which, in turn, leads to a basket weave microstructure
similar to that observed in the present study.
Results of the FCG tests on heat-treated SLM Ti64 are displayed
in Fig. 11 as da/dN vs. DK plots. Values of m and DK0, extracted from
these plots are summarized in Table 1. As seen, m ranges between
3.2 and 4, which is similar to those reported by Cain et al. [13] in B
(3.8) and S (3.1) directions for the SLM Ti64 subjected to a single
step heat-treatment with Ta < Tb. In all the cases, cracks grow at
broadly similar rates in both B and S directions. Furthermore, the
steady state crack growth rates appear to be unaffected by the heat
treatment for the coupons fabricated with f ¼ 67 showing a
marginal variation in m after the heat treatment as compared to
that before heat treatment. However, in the case of samples
Fig. 11. Variations of the fatigue crack growth rate per cycle, da/dN, plotted as a function of the applied stress intensity factor range, DK, in samples (a) B3090 and S3090, (b) B3067
and S3067, (c) B6067 and S6067, and (d) B3090 before and after the heat-treatment.
manufactured with f ¼ 90 , m increases substantially in three cases
except the S direction of 3090 where again the change is only
marginal. The highest increase was noted in the B direction of
coupon 3090, for which, FCG data before and after heat treatment
are compared in Fig. 11d. From it, we note annealing leads to a
substantial increase in m (by 54%). (Here, it is worth recalling that in
the as-SLM condition, m was 30% higher in S direction as compared
to B direction for 3090.) Overall, it appears that the heat treatment
not only reduced the anisotropy in the crack growth rates but
reduced the range of m (amongst the four different coupons
considered) from 2.53 to 3.55 in the as-fabricated samples to 3.2e4
in the heat-treated samples.
Values of DK0, listed in Table 1, indicate that it ranges between
pffiffiffiffiffi
7.1 and 8.4 MPa m. Three observations are noteworthy. (i) The
overall range of DK0 is small, suggesting that the prior b meso-
structure exerts no significant influence on DK0, neither before
pffiffiffiffiffi
(range of DK0: 5.3e5.8 MPa m) nor after heat treatment. (ii) Heat
treatment, however, enhances DK0 of all the samples; the increases
range between 34% and 56%. (iii) No significant anisotropy in DK0
could be seen, i.e., the values are similar in both S and B directions.
For comparing with the literature data, we note that not many
studies, which report DK0 of SLM Ti64 after heat treatment, are
 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
available. Leuders et al. [36] report that the hot isostatic pressing
pffiffiffiffiffi
(HIP) above Tb improves DK0 from a very low value of ~1.7 MPa m
pffiffiffiffiffi
in the as-SLM condition to 6.1 MPa m. Galarraga et al. [37] report a
pffiffiffiffiffi
DK0 ~4.2 MPa m for Ti64 manufactured by e-beam melting, which
also produces an a/b microstructure because of the high energy
input in this method; post-fabrication annealing with Ta > Tb
pffiffiffiffiffi
further improves it to 6 MPa m. Seifi et al. [38] report a DK0 of
pffiffiffiffiffi
5.7 MPa m for Ti64 manufactured with e-beam melting of a pre-
heated powder bed (750  C) and attribute it to the in-situ decom-
position of a’; they also suggest that DK0 decreases with a lath
coarsening. For additively manufactured Ti64 employing different
powder bed fusion methods, Lewandowski et al. [39] report DK0
pffiffiffiffiffi
values ranging between 3.8 and 6.3 MPa m. As can be seen, the
pffiffiffiffiffi
values of DK0 obtained in the present study (7.1e8.4 MPa m) are
higher than all those reported thus far. These are also higher than
pffiffiffiffiffi
DK0  6.8 MPa m reported for Ti64 with an a/b lamellar micro-
structure and manufactured using conventional methods [34,40].
4. Discussion
4.1. Strength, ductility, and toughness
The high cooling rates that are intrinsic to the SLM process result
in a Ti64 with a basket weave microstructure of fine a0 laths
[5,7,25]. Furthermore, the high dislocation density inside the a0
laths hinders dislocation mobility and hence makes them strong.
Together, these two factors enhance the strength of as-SLM Ti64
and adversely affect its ductility. The presence of a mesoscopic prior
b mesostructure also affects ef, due to the presence of relatively
weak a phase along the prior b boundaries. This situation gets
exacerbated in alloys with columnar prior b grains, when the
loading direction is perpendicular to the prior b columns [41].
Hence, the tensile properties, especially ductility, of the as-built
Ti64 are sensitive to prior b structure whereas the a’ lath thick-
ness or their relative orientation are unaffected by the process
parameter combinations. One way to alleviate the problem of the
anisotropy in ductility in as-SLM Ti64 is by imparting an equiaxed
mesostructure. Indeed, we demonstrated in our previous study that
ef of SLM Ti64 produced with f ¼ 67, which has an equiaxed prior b
grain structure, is substantially higher than that produced with
f ¼ 90 [5]. Heat treatment, it appears, eliminates such an influence
of the prior b mesostructure on ef, with all the different samples of
the present study exhibiting 12%e16% ef, which are comparable to
those of the wrought Ti64. Here, it is important to keep in mind that
multiple thermo-mechanical processing steps are often required
for achieving such ductility in wrought Ti64 manufactured using
the conventional manufacturing methods [21,32].
The post-SLM annealing of Ti64 not only allows for the trans-
formation of a’ into a/b [9,11,18,42e44], but also for the coarsening
of a laths. However, heating close to T and for a long period can
increase the colony size and eliminate the basket weave structure,
leading to a significant reduction in sy [25]. Thus, a trade-off be-
tween the basket weave and coarse colony microstructures needs
to be considered for obtaining an alloy with high strength and
ductility combinations [44]. The duplex heat-treatment process
that was employed in the present study results in a microstructure
with coarse a laths in a basket weave configuration; this results in
an alloy with sy above 850 MPa and ef up to 16.6%. Here, it is
interesting to note these properties are above the 10% ef and sy 795
and 825 MPa, prescribed by ASTM for the surgical implants and
aerospace applications respectively [45,46].
Along with the lath thickness and the colony size, texture could
also play an important role in determining ef of Ti alloys. During
annealing, a’ transforms into a with the b phase present at the lath
boundaries. During this transformation process, bigger and
55
favorably oriented laths grow at the expense of the smaller ones
[25], leading to a reduction in the strength of the texture variants,
as seen in Figs. 6b and 8b. The latter figure also indicates that laths
with prismatic orientation make a 30e45 angle with the build
direction. Similarly, the laths in the IPF map of the S plane (Fig. 9)
also make a 30e45 angle with the build direction. Since prismatic
slip is easier than basal slip in Ti64 (c/a < 1.633), the enhanced
ductility observed in both these samples is possibly due to a large
population of laths with a prismatic orientation {1120}. Likewise,
3067 in the B orientation contains laths with prismatic orientation
and exhibits a 48% improvement in ductility after the heat-
treatment. Another example is the 6067 tested in S orientation,
which again exhibits a strong prismatic texture (Fig. 10d) and
hence leads to a high ef of 16.6% after the heat-treatment. Coupon
3090 tested in the S direction has an ef of 12.5%, even though the
peak intensity near the basal plane (Fig. 10c) occurs at 15e30 to
the build direction. This is because the presence of other texture
variants, whose orientation is favourable for slip. The higher
strength of 3090 in the B orientation is also possibly because of the
high texture strength (12) that arises due to the columnar prior b
grains.
Turning attention to the fracture toughness, the data available in
published literature indicates that KIc of SLM Ti64 is either lower or
comparable to that of the wrought alloys [5,12,13,32]. In the con-
texts where it was found to be substantially lower, the presence of
hard and relatively-less ductile a’ phase in the microstructure was
attributed for the low KIc. Thus, the substantial enhancement in the
fracture toughness observed in the present study upon heat
treatment could be due to the formation of a/b Widmansta €tten
microstructure, which is considerably more ductile, upon anneal-
ing. Furthermore, coarsening of the laths during heat treatment can
also enhance the fracture toughness by increasing the crack tor-
tuosity [21,31,47].
In some SLM alloys, such AleSi, the mesoscopic structural fea-
tures, which form along the contours of the melt pool boundaries of
the laser tracks, impart high crack tortuosity. This, in turn, can
improve KIc in a substantial manner [1]. In SLM Ti64 of the current
study, the mesostructure consists of the prior b grains formed along
the laser tracks and could influence KIc. These grain boundaries are
decorated with the a phase, due to relatively slower cooling at the
center of the laser track. It is thought that such a mesostructure can
have an adverse effect, especially when aligned along the crack
growth direction since it may offer low resistance to crack growth
[48]. In the present study, we evaluated the fracture toughness of
heat-treated SLM Ti64 with prior b mesostructure that ranges from
highly columnar to near equiaxed structures. In the case of the alloy
with the columnar structure (3090), Kq was found to be 27% lower
in the S orientation, i.e., the configuration in which mode I crack
growth occurs parallel to the columnar prior b grains, as compared
to B orientation where the growing crack has to cut-through the
columns. This is apparent from the fractographs of 3090, wherein
the fracture surface of 3090 tested in B orientation (Fig. 12a) is
considerably more corrugated as compared to that tested in S di-
rection (Fig. 12b). (In contrast, the near equiaxed prior b meso-
structure in 6067 alloy results in similar Kq in both B and S
directions.). Thus, it appears that the crack tortuosity, aided by the
mesoscopic columnar structure, does indeed affect the fracture
toughness of SLM Ti64 after heat treatment. In contrast, the prior b
structure did not have a substantial effect on KIc of the as built SLM
samples. A comparison of the fractographs obtained from the
fracture toughness tested sample of 3090 in B orientation, before
(Fig. 12c) and after heat treatment (Fig. 12a), shows the latter to be
more tortuous, possibly because of a stronger metallurgical
bonding between the layers and lath coarsening due to heat-
treatment.
56 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
Fig. 12. Representative low magnification fractographs of samples (a) B3090 and (b) S3090, both after the heat-treatment, and (c) B3090 before the heat-treatment.
4.2. Fatigue crack growth
Data displayed in Table 1 shows that annealing leads to a nar-
rower m range and the mitigation of anisotropy that was significant
in the as-fabricated SLM Ti64, which was attributed to the presence
of the a phase along these prior b grain boundaries [5]. It is well
known that the grain boundary a phase provides an easy path for
crack growth due to the strain localization within it, especially
when the interior of the grain contains a0 phase, which is much
harder [5,13,49,50]. However, after the heat-treatment, the matrix
also transforms into an a/b microstructure. Thus plastic strain
localization, which would facilitate faster crack growth under cyclic
loading conditions, is minimized. Since the heat-treatment elimi-
nates the grain boundary a, it, in effect, removes the role of mes-
ostructure on the FCG behavior. Indeed, similar m in both S and B
orientations of heat-treated samples confirm that the prior b
mesostructure no longer exerts a significant effect on steady state
FCG characteristics of SLM Ti64 after being subjected to HT2.
In the case of 3090 tested in B orientation, m increases from ~2.5
to 3.9, indicating a substantial reduction in the FCG resistance upon
heat treatment. Note that this reduction occurs while both ductility
and fracture toughness increase substantially as compared to the
respective properties in the as-SLM state. In contrast, a substantial
improvement in the near-threshold FCG resistance, as measured by
DK0, upon heat treatment was noted. These contrasting behaviors
are exemplified by the da/dN vs. DK plots, displayed in Fig. 12d, of
3090 sample in B orientation before and after heat treatment. This
figure shows that a crossover between the crack growth data occurs
pffiffiffiffiffi
at DK  12 MPa m, which reflects the effect of heat treatment on
DK0 and m. Such a transition in the mechanism of FCG occurs when
the plastic zone size is comparable to the microstructural feature
size [51,52]. If the material under investigation is assumed to be
elastic-perfectly plastic, which is the case for Ti64 as it does not
exhibit significant levels of work hardening, the maximum and
cyclic plastic zone sizes (rmax and rc respectively) near the threshold
under plane strain conditions and within the continuum mechanics
 2  2
framework, are given by: rmax ¼ 31p ð1RÞ DK0 and rc ¼ 31p D2sKy0 .
sy
Values of rmax and rc, estimated using these relations, for each
specimen are listed in Table 1; from it we note that they range
between 8.3 to 11.9 mm and 1.6e2.4 mm respectively. These length
scales are in the same order of magnitude as the average colony size
(26 ± 10 mm) and la, is also listed in Table 1, within the micro-
structures of the alloys. It is interesting to note that in most cases rc
is approximately two times la . This observation clearly indicates
that it is the lath size that controls the near-threshold FCG behavior.
All the heat-treated samples exhibit similar DK0, which ranges
pffiffiffiffiffi
between 7.1 and 8.4 MPa m. Since DK0 tends to be highly sensitive
to the microstructural features, such a close range of experimental
DK0 values indicates that the interaction between the fatigue cracks
and the microstructures near the threshold of the heat-treated Ti64
with a/b lamellar structure examined in this study is similar. Hence,
such crack-microstructure interactions are illustrated using the
following micrographs [51,53]. Near the threshold, crack deflection
along the lath boundaries and through the b phase and along the
boundary of the a laths is favored, as illustrated in Fig. 13a. Such
deflections reduce the mode I crack driving force significantly,
leading to the arrest of the crack completely. At a higher DK
pffiffiffiffiffi
(~12 MPa m), crack deflection can also take place along colony
boundaries, as seen in Fig. 13b; this is because of the basket weave
 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
Fig. 13. Interactions of the fatigue cracks with the microstructures, illustrating (a) crack deflection along the lath boundaries near the threshold stress intensity factor range, (b)
crack deflection by the colonies of the laths at higher DK, and (c), trans-colony crack propagation in the Paris regime.
microstructure in the heat treated SLM Ti64, wherein some groups
of laths are oriented similarly and hence can be considered as a
colony (see Fig. 7b). Recall that the size of these colonies are of the
same order of the rmax; thus, when DK is higher than DK0 (say about
pffiffiffiffiffi
10e12 MPa m), crack deflections along the colony boundaries
occurs because of the orientation differences in the laths across
colonies [51,54]. Well into the Paris regime, where DK is sufficiently
large, the size of the cyclic plastic zone is on the order of tens of
microns or larger and hence exceeds the colony size. Consequently,
cracks cut across the colonies (Fig. 13c) and their growth rate be-
comes insensitive to the microstructural features.
The above results illustrate that SLM Ti64 with a basket weave a/
b microstructure containing optimum a lath thickness and colony
size can impart significantly higher fatigue resistance to the SLM
Ti64, especially in terms of DK0. Although the cracks can grow at a
much faster rate in the Paris regime, due to an increased m, the
substantial enhancements observed in the fracture toughness upon
heat treatment can offset those, i.e., the overall number of cycles to
failure, Nf, made using the fracture mechanics approach (wherein
an initial crack length is assumed and then Nf is estimated on the
basis of the Paris law and KIc) may not get altered. In such a sce-
nario, the marked increase in DK0 offers the following specific
advantage in the context of SLM alloys. Since SLM is a powder
metallurgy process, porosity is an inevitability. Pores, especially
those at or close to the surface, can reduce the fatigue lives pre-
cipitously. Indeed, a major drawback, which is yet to be overcome,
of SLM alloys manufactured using powder bed fusion technologies
is their low fatigue resistance. Consequently, a major issue for
research conducted in the AM industry is methods to overcome
this, and, in the process, make the certification of the components
possible. Since the elimination of porosity completely may not be
possible –unless secondary processing steps such as HIPing or
thermo-mechanical processing are performed, damage tolerant
design based on fracture mechanics are one way to circumvent the
problem. In this approach, critical components are designed for safe
stress levels assuming the existence of a defect, whose size is of the
57
order of the non-destructive testing technique's resolution, located
at critical spot of the component body. The designed levels of far
field stresses are such that the condition DK is always less than DK0.
Thus, the DK0 achieved in this study can be utilized the design fa-
tigue resistant SLM components.
5. Summary and conclusions
The possibility of enhancing the fracture toughness and fatigue
crack growth resistance of SLM Ti64, without a significant com-
pramize on the tensile strength, via annealing heat-treatments was
examined. Towards this end, microstructures obtained after four
different heat treatment schedules were characterized in detail. On
this basis, a schedule, wherein the maximum annealing tempera-
ture is below Tb transus temperature, that contains two step cooling
is utilized to examine the mechanical properties of SLM Ti64
manufactured with four different combinations of SLM parameters.
On the basis of these studies, the following conclusions can be
drawn. Annealing the SLM Ti64 at temperatures above Tb, erases the
mesoscopic prior b grain structure, which uniquely depends on the
SLM process parameter combinations employed, and a coarse
microstructure. On the other hand, a two-step heat treatment
schedule with Ta<Tb results in an a/b basket weave microstructure
with coarser a laths and preservation of the prior b mesostructure.
Such a post-SLM heat-treatment mitigates the anisotropy in
properties, enhances the ductility, fracture toughness, and fatigue
crack growth resistance, while reducing the yield and ultimate
tensile strengths by ~20%, of the SLM Ti64 as compared to respec-
tive properties of the alloy in the as-SLM condition. Importantly,
these properties were significantly better than those of the
wrought Ti64 with similar grain sizes. Furthermore, the tensile
behavior and the steady state FCG behavior of the heat-treated
samples were found to be independent of the prior b meso-
structure whereas the fracture toughness is dependent. These are
opposite to those observed on the as-built Ti64; a transition in the
crack growth mechanism, from inter-to trans-granular, due the
58 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
heat-treatment was responsible for this reversal.
Acknowledgements
The research work reported in this paper was funded by the
Boeing Company (PC36035). We are grateful Dr. Om Prakash for
many fruitful discussions.
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.actamat.2019.03.003.
References
[1] J. Suryawanshi, K.G. Prashanth, S. Scudino, J. Eckert, O. Prakash, U. Ramamurty,
Simultaneous enhancements of strength and toughness in an Al-12Si alloy
synthesized using selective laser melting, Acta Mater. 115 (2016) 285e294,
https://doi.org/10.1016/j.actamat.2016.06.009.
[2] Y.J. Liu, H.L. Wang, S.J. Li, S.G. Wang, W.J. Wang, W.T. Hou, Y.L. Hao, R. Yang,
L.C. Zhang, Compressive and fatigue behavior of beta-type titanium porous
structures fabricated by electron beam melting, Acta Mater. 126 (2017)
58e66, https://doi.org/10.1016/j.actamat.2016.12.052.
[3] Q. Huang, N. Hu, X. Yang, R. Zhang, Q. Feng, Microstructure and inclusion of
Tie6Ale4V fabricated by selective laser melting, Front. Mater. Sci. 10 (2016)
428e431, https://doi.org/10.1007/s11706-016-0354-8.
[4] D. Agius, K. Kourousis, C. Wallbrink, A review of the as-built SLM Ti-6Al-4V
mechanical properties towards achieving fatigue resistant designs, Metals 8
(2018) 75, https://doi.org/10.3390/met8010075.
[5] P. Kumar, O. Prakash, U. Ramamurty, Micro-and meso-structures and their
influence on mechanical properties of selectively laser melted Ti-6Al-4V, Acta
Mater. 154 (2018) 246e260, https://doi.org/10.1016/j.actamat.2018.05.044.
[6] M. Simonelli, Y.Y. Tse, C. Tuck, The formation of a þ b microstructure in as-
fabricated selective laser melting of Tie6Ale4V, J. Mater. Res. 29 (2014)
2028e2035, https://doi.org/10.1557/jmr.2014.166.
[7] W. Xu, E.W. Lui, A. Pateras, M. Qian, M. Brandt, In situ tailoring microstructure
in additively manufactured Ti-6Al-4V for superior mechanical performance,
Acta Mater. 125 (2017) 390e400, https://doi.org/10.1016/
j.actamat.2016.12.027.
[8] W. Xu, M. Brandt, S. Sun, J. Elambasseril, Q. Liu, K. Latham, K. Xia, M. Qian,
Additive manufacturing of strong and ductile Ti-6Al-4V by selective laser
melting via in situ martensite decomposition, Acta Mater. 85 (2015) 74e84,
https://doi.org/10.1016/j.actamat.2014.11.028.
[9] G. Nicoletto, S. Maisano, M. Antolotti, F. Dall'Aglio, Influence of post fabrication
heat treatments on the fatigue behavior of Ti-6Al-4V produced by selective
laser melting, Procedia Struct. Integr. 7 (2017) 133e140, https://doi.org/
10.1016/j.prostr.2017.11.070.
[10] 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. Alloy. Comp. 541 (2012) 177e185, https://doi.org/10.1016/
j.jallcom.2012.07.022.
[11] 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. 42A (2011) 3190e3199, https://doi.org/10.1007/s11661-011-0731-y.
[12] D.N. Mohamed, T. Robert, B. Thorsten, Fatigue and fracture toughness of Ti-
6Al-4V titanium alloy manufactured by selective laser melting, Adv. Mater.
Res. 1019 (2014) 248e253, https://doi.org/10.4028/www.scientific.net/
AMR.1019.248.
[13] 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.
[14] A. Riemer, H.A. Richard, Crack propagation in additive manufactured materials
and structures, Procedia Struct. Integr. 2 (2016) 1229e1236, https://doi.org/
10.1016/j.prostr.2016.06.157.
[15] ASTM D170813, Standard test method for tensile properties of plastics by
use of microtensile specimens, Am. Soc. Test. Mater. 08 (2014) 5, https://
doi.org/10.1520/D1708-13.
[16] ASTM E399 12, Standard test method for linear-elastic plane-strain fracture
toughness KIC of metallic materials, ASTM Int 3 (2012) 01, https://doi.org/
10.1520/E0399-12E03.
[17] ASTM E647-15, Standard test method for measurement of fatigue crack
growth rates, ASTM Int 3 (2016) 01, https://doi.org/10.1520/E0647.
[18] 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. Alloy. Comp. 541 (2012) 177e185, https://doi.org/10.1016/
j.jallcom.2012.07.022.
[19] G. Lütjering, Influence of processing on microstructure and mechanical
properties of (aþb) titanium alloys, Mater. Sci. Eng. 243 (1998) 32e45, https://
doi.org/10.1016/S0921-5093(97)00778-8.
[20] X. Tan, Y. Kok, W.Q. Toh, Y.J. Tan, M. Descoins, D. Mangelinck, S.B. Tor,
K.F. Leong, C.K. Chua, Revealing martensitic transformation and a/b interface
evolution in electron beam melting three-dimensional-printed Ti-6Al-4V, Sci.
Rep. 6 (2016) 1e10, https://doi.org/10.1038/srep26039.
[21] G. Lütjering, J. Williams, Titanium, second ed., Springer, Berlin, 2007.
[22] X. Yan, S. Yin, C. Chen, C. Huang, R. Bolot, R. Lupoi, M. Kuang, W. Ma, C. Coddet,
H. Liao, M. Liu, T. Eli, Effect of heat treatment on the phase transformation and
mechanical properties of Ti6Al4V fabricated by selective laser melting, J. Alloy.
Comp. 764 (2018) 1056e1071, https://doi.org/10.1016/j.jallcom.2018.06.076.
[23] E. Leey, R. Banerjee, S. Kary, D. Bhattacharyyay, H.L. Frasery, Selection of a
variants during microstructural evolution in a/b titanium alloys, Philos. Mag.
A 87 (2007) 3615e3627, https://doi.org/10.1080/14786430701373672.
[24] M. Simonelli, Y.Y. Tse, C. Tuck, Further understanding of Ti-6Al-4V selective
laser melting using texture analysis, in: 23rd, Annu. Int. Solid Free, Fabr.
Symp., 2012, pp. 480e491. https://sffsymposium.engr.utexas.edu/
Manuscripts/2012/2012-37-Simonelli.pdf. (Accessed 10 August 2017).
[25] G.M. Ter Haar, T.H. Becker, Selective laser melting produced Ti-6Al-4V: post-
process heat treatments to achieve superior tensile properties, Materials 11
(2018) 1e15, https://doi.org/10.3390/ma11010146.
[26] S.L. Lu, M. Qian, H.P. Tang, M. Yan, J. Wang, D.H. StJohn, Massive trans-
formation in Ti-6Al-4V additively manufactured by selective electron beam
melting, Acta Mater. 104 (2016) 303e311, https://doi.org/10.1016/
j.actamat.2015.11.011.
[27] B. Baufeld, O. Van Der Biest, S. Dillien, Texture and crystal orientation in Ti-
6Al-4V builds fabricated by shaped metal deposition, Metall. Mater. Trans. A
Phys. Metall. Mater. Sci. 41 (2010) 1917e1927, https://doi.org/10.1007/
s11661-010-0255-x.
[28] X.Y. Zhang, G. Fang, S. Leeflang, A.J. Bo €ttger, A.A. Zadpoor, J. Zhou, Effect of
subtransus heat treatment on the microstructure and mechanical properties
of additively manufactured Ti-6Al-4V alloy, J. Alloy. Comp. 735 (2018)
1562e1575, https://doi.org/10.1016/j.jallcom.2017.11.263.
[29] 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.
[30] Z. Liu, S.L. Lu, H.P. Tang, M. Qian, L. Zhan, Characterization and decomposi-
tional crystallography of the massive phase grains in an additively-
manufactured Ti-6Al-4V alloy, Mater. Char. 127 (2017) 146e152, https://
doi.org/10.1016/j.matchar.2017.01.012.
[31] Y. Liu, J. Zhang, S.J. Li, W.T. Hou, H. Wang, Q.S. Xu, Y.L. Hao, R. Yang, Effect of
HIP treatment on fatigue crack growth behavior of Ti-6Al-4V alloy fabricated
by electron beam melting, Acta Metall. Sin. (English Lett. 30 (2017)
1163e1168, https://doi.org/10.1007/s40195-017-0665-5.
[32] R.C. Rice, Metallic Materials Properties Development and Standardization,
Virginia, 2003.
[33] G. Singh, I. Sen, K. Gopinath, U. Ramamurty, Influence of minor addition of
boron on tensile and fatigue properties of wrought Tie6Ale4V alloy, Mater.
Sci. Eng. 540 (2012) 142e151, https://doi.org/10.1016/j.msea.2012.01.119.
[34] B.L. Boyce, R.O. Ritchie, Effect of load ratio and maximum stress intensity on
the fatigue threshold in Ti-6Al-4V, Eng. Fract. Mech. 68 (2001) 129e147,
https://doi.org/10.1016/S0013-7944(00)00099-0.
[35] M. Seifi, M. Dahar, R. Aman, O. Harrysson, J. Beuth, J.J. Lewandowski, Evalu-
ation of orientation dependence of fracture toughness and fatigue crack
propagation behavior of as-deposited ARCAM EBM Ti-6Al-4V, JOM (J. Occup.
Med.) 67 (2015) 597e607, https://doi.org/10.1007/s11837-015-1298-7.
[36] S. Leuders, M. Thone, A. Riemer, T. Niendorf, T. Troster, H.A. Richard,
H.J. Maier, On the mechanical behaviour of titanium alloy TiAl6V4 manufac-
tured by selective laser melting: fatigue resistance and crack growth perfor-
mance, Int. J. Fatigue 48 (2013) 300e307, https://doi.org/10.1016/
j.ijfatigue.2012.11.011.
[37] H. Galarraga, R.J. Warren, D.A. Lados, R.R. Dehoff, M.M. Kirka, Fatigue crack
growth mechanisms at the microstructure scale in as-fabricated and heat
treated Ti-6Al-4V ELI manufactured by electron beam melting (EBM), Eng.
Fract. Mech. 176 (2017) 263e280, https://doi.org/10.1016/
j.engfracmech.2017.03.024.
[38] M. Seifi, D. Christiansen, J. Beuth, O. Harrysson, J.J. Lewandowski, Process
mapping, fracture and fatigue behavior of Ti-6Al-4V produced by EBM addi-
tive manufacturing, Proc. 13th World Conf. Titan. (2016) 1373e1377, https://
doi.org/10.1002/9781119296126.ch232.
[39] J.J. Lewandowski, M. Seifi, Metal additive manufacturing: a review of me-
chanical properties, Annu. Rev. Mater. Res. 46 (2016) 151e186, https://
doi.org/10.1146/annurev-matsci-070115-032024.
[40] R.K. Nalla, B.L. Boyce, J.P. Campbell, J.O. Peters, R.O. Ritchie, Influence of
microstructure on high-cycle fatigue of Ti-6Al-4V: Bimodal vs. lamellar
structures, Metall. Mater. Trans. A Phys. Metall. Mater. Sci. 33 (2002)
899e918, https://doi.org/10.1007/s11661-002-0160-z.
[41] B.E. Carroll, T.A. Palmer, A.M. Beese, Anisotropic tensile behavior of Ti-6Al-4V
components fabricated with directed energy deposition additive
manufacturing, Acta Mater. 87 (2015) 309e320, https://doi.org/10.1016/
j.actamat.2014.12.054.
[42] E. Sallica-Leva, R. Caram, A.L. Jardini, J.B. Fogagnolo, Ductility improvement
due to martensite a’ decomposition in porous Ti-6Al-4V parts produced by
selective laser melting for orthopedic implants, J. Mech. Behav. Biomed.
Mater. 54 (2016) 149e158, https://doi.org/10.1016/j.jmbbm.2015.09.020.
[43] P. Barriobero-Vila, J. Gussone, J. Haubrich, S. Sandlobes, J.C. Da Silva,
P. Cloetens, N. Schell, G. Requena, Inducing stable aþb microstructures during
 P. Kumar, U. Ramamurty / Acta Materialia 169 (2019) 45e59
selective laser melting of Ti-6Al-4V using intensified intrinsic heat treatments,
Materials 10 (2017) 1e14, https://doi.org/10.3390/ma10030268.
[44] M. Tho €ne, S. Leuders, A. Riemer, T. Tro € ster, H.A. Richard, Influence of heat-
treatment on selective laser melting products e e.g. Ti6Al4V, in: Solid Free,
Fabr. Proc., 2012, pp. 492e498. https://sffsymposium.engr.utexas.edu/
Manuscripts/2012/2012-38-Thoene.pdf. accessed June 20, 2018.
[45] ASTM F136-13, Standard specification for wrought Titanium-6 Aluminum-4
Vanadium ELI ( extra low interstitial ) alloy for surgical implant applications
(UNS), ASTM Int 13 (2012) 1e5, https://doi.org/10.1520/F0136-12.2, 01.
[46] I. Inagaki, T. Tsutomu, S. Yoshihisa, A. Nozomu, Application and Features of
Titanium for the Aerospace Industry, 2014.
[47] C.T. Liu, J.H. Schneibel, P.J. Maziasz, J.L. Wright, D.S. Easton, Tensile properties
and fracture toughness of TiAl alloys with controlled microstructures, In-
termetallics 4 (1996) 429e440, https://doi.org/10.1016/0966-9795(96)00047-
7.
[48] J. Suryawanshi, K.G. Prashanth, U. Ramamurty, Mechanical behavior of se-
lective laser melted 316L stainless steel, Mater. Sci. Eng. 696 (2017) 113e121,
https://doi.org/10.1016/j.msea.2017.04.058.
[49] Z.H. Jiao, R.D. Xu, H.C. Yu, X.R. Wu, Evaluation on tensile and fatigue crack
59
growth performances of Ti6Al4V alloy produced by selective laser melting,
Procedia Struct. Integr. 7 (2017) 124e132, https://doi.org/10.1016/
j.prostr.2017.11.069.
[50] C.D. Rans, J. Michielssen, M. Walker, W. Wang, L. Hoen-Velterop, Beyond the
orthogonal: on the influence of build orientation on fatigue crack growth in
SLM Ti-6Al-4V, Int. J. Fatigue 116 (2018) 344e354, https://doi.org/10.2514/
6.2018-1643.
[51] P.E. Irving, C.J. Beevers, Microstructural influences on fatigue crack growth in
Ti–6A1–4V, Mater. Sci. Eng. 14 (1974) 229e238.
[52] S. Suresh, Fatigue of Materials, Cambridge University Press, 1998.
[53] G.R. Yoder, L.A. Cooley, T.W. Crooker, Observations on microstructurally
sensitive fatigue crack growth in a widmansta €tten Ti-6Al-4V alloy, Metall.
Trans. A. 8 (1977) 1737e1743, https://doi.org/10.1007/BF02646877.
[54] R.J. COOKE, C.J. BEEVERS, The effect of load ratio on the threshold stresses for
fatigue crack growth in medium carbon steel, Eng. Fract. Mech. 5 (1973)
1061e1071.
[55] R. Munz, S. Size, Effect of specimen size on fracture toughness of a Titanium
alloy, Am. Soc. Test. Mater. ASTM STP 5 (1976) 219e234. https://doi.org/10.
1520/STP33948S.