Materials Science & Engineering A 689 (2017) 1–10

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Materials Science & Engineering A

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

Effect of heat treatment and hot isostatic pressing on the microstructure MARK
and mechanical properties of Inconel 625 alloy processed by laser powder
bed fusion
⁎
Alena Kreitcberga, Vladimir Brailovskia, , Sylvain Turenneb
a
École de technologie supérieure, 110 Notre-Dame Street West, Montreal, Quebec H3C 1K3 Canada
b
École Polytechnique de Montréal, 2900 boul. Édouard-Montpetit, Montreal, Quebec H3T 1J4 Canada

A R T I C L E I N F O A BS T RAC T

Keywords: The effect of different heat treatments and hot isostatic pressing on the microstructure and mechanical
Nickel based superalloys properties of laser powder bed fusion IN625 alloy was studied. The heat treatments were: stress relief annealing,
Additive manufacturing recrystallization annealing and low-temperature solution treatment. The resulting microstructure and crystal-
Selective laser melting lographic textures were studied using optical and scanning electron microscopy. The mechanical properties of
Inconel
the as-built and post-treated IN625 alloy were obtained after tensile testing at room temperature and at 760 °C
Tensile testing
(1400 °F), and compared to those of an annealed wrought alloy of the same composition.
Microstructure

1. Introduction
Laser powder bed fusion (L-PBF) technology allows the production
of parts on demand with complex geometry and is applicable to
different classes of metallic materials including Ti, Ni, Co, Al and Fe-
based alloys [1–5].
The L-PBF processing of metallic parts involves three main phases:
(1) preparation phase, (2) L-PBF of metallic powders and (3) post-
treatment. The first phase involves the orientation of a 3D CAD part
model with respect to the building platform, data conversion into an
STL format, and model slicing. The L-PBF of metallic powders (second
phase) comprises layer-by-layer powder consolidation, a complex
thermal processing involving localized melting, solidification and cool-
ing of spread powder particles. This non-equilibrium laser processing
triggered by a high localized heat input, and involving short interaction
times, determines the material integrity and homogeneity, microstruc-
ture and mechanical properties, which are different from those result-
ing from conventional manufacturing processes [6–11]. Therefore, the
final phase, post-treatment, serves to attenuate the negative conse-
quences of the layer-by-layer selective laser powder consolidation, such
as high level of internal stresses and anisotropy of mechanical proper-
ties, while preserving the capacity to produce components with
complex geometry.
This post-treatment phase is especially important for high-perfor-
mance components used in the aeronautics, nuclear, chemical and
petrochemical industries. One of the most promising alloys used in
these fields is Inconel 625 due to its high corrosion resistance and
mechanical properties at elevated temperatures [12,13]. Since, accord-
ing to [1], the mechanical properties of L-PBF IN625 components are
highly anisotropic, significant effort must be made to optimize post-L-
PBF operations with the objective of decreasing the level of anisotropy
while preserving the high mechanical properties of this alloy under
service conditions.
Four post-treatment schedules can be recommended for L-PBF
IN625: 1) stress relief (SR) annealing, 2) recrystallization annealing
(RA), 3) solution treatment (ST) and 4) hot isostatic pressing (HIP).
– Stress relief annealing is recommended for L-PBF parts to reduce
residual stresses and therefore decrease distortions before cutting
the parts from the building platform, but without significantly
affecting the grain structure. For nickel alloys, stress relief tempera-
tures range from 650 to 870 °C, but this operation runs the risk of
experiencing carbide precipitation phenomena and other phase
formation [14,15].
– Recrystallization annealing of L-PBF parts is intended to produce a
recrystallized grain structure and reduce the anisotropy of mechan-
ical properties. For nickel alloys, the recrystallization annealing
requires temperatures ranging from 930 to 1040 °C [15–17].
– For nickel alloys, a solution treatment at 1040–1200 °C serves to
dissolve carbides and δ-phase precipitates before age-hardening
treatment [14,15].
– Hot isostatic pressing (1120–1240 °C, 100–165 MPa, 3–4 h) allows

⁎
Correspondence to: Mechanical Engineering Department, Ecole de technologie superieure, 1100, Notre-Dame Street West, Montreal, Quebec H3C 1K3, Canada.
E-mail addresses: alena.kreitcberg.1@ens.etsmtl.ca (A. Kreitcberg), vladimir.brailovski@etsmtl.ca (V. Brailovski), sylvain.turenne@polymtl.ca (S. Turenne).

http://dx.doi.org/10.1016/j.msea.2017.02.038
Received 1 December 2016; Received in revised form 17 January 2017; Accepted 11 February 2017
Available online 14 February 2017
0921-5093/ © 2017 Elsevier B.V. All rights reserved.
A. Kreitcberg et al.
the reduction of the microporosity and a decrease in anisotropy of
the alloy's mechanical properties [18,19].
The initial (as-built) microstructure, level and distribution of
residual stresses in L-PBF-processed parts influence the precipitation
kinetics and grain structure evolution triggered by post-L-PBF thermal
treatments and HIP, and, therefore, impact the resulting mechanical
properties. To date, the effects of thermal treatments and HIP on the
anisotropy of the mechanical properties of L-PBF-processed IN625
alloy have undergone much less intense study than those of other
nickel-based superalloys, such as IN718 [1]. Thus, the main purpose of
the experiments described in this paper was to study the structural
changes occurring during thermal and HIP post-L-PBF treatments of
the IN625 alloy and assess their influence on the mechanical properties
of this material. The experimental results should allow the optimization
of the post-treatment schedule of L-PBF-processed IN625 alloy com-
ponents, with the main objective being to improve the homogeneity of
their microstructure and mechanical properties. Note that in this work,
the exact heat and HIP-treatment conditions are omitted and the stress
values measured are normalized to protect proprietary partner infor-
mation.
2. Material and methods
An EOSINT M290 (EOS GmbH, Munich Germany) selective laser
melting machine equipped with a Ytterbium 400 W fiber laser and an
EOS IN625 Performance Setup were used to manufacture two types of
specimens: 10×10×10 mm3 cubic specimens for microstructure eva-
luation and 85×18×3 mm3 rectangular prismatic coupons with three
build orientations (ZX/vertical, XZ/horizontal and 45°/inclined), for
mechanical testing (Fig. 1a).
Next, directly after L-PBF, some specimens were cut from the
platform to evaluate the as-built microstructure and mechanical
properties. The specimens remaining on the building platform were
subjected to stress relief annealing (SR) [15,20]. Then, all the SR-
annealed specimens were cut from the platform, and the rectangular
prismatic coupons were machined to obtain dumbbell-shaped tensile
testing specimens shown in Fig. 1b. Some specimens were then
reserved for future study. The other specimens were subjected to three
post-treatments: recrystallization annealing (RA), solution treatment
(ST) [15,20], and HIP [18,19,21]. All the treatments were conducted
under argon atmosphere. After post-treatment, RA and ST specimens
were water-quenched, SR specimens were air-cooled and HIP speci-
mens were furnace-cooled.
It was hypothesized that the RA and ST post-treatments would
reduce the anisotropy of the as-built alloy's mechanical properties, but
to a different extent, whereas HIP post-treatment would additionally
strengthen the material by eliminating the L-PBF-generated micro-
porosity [16,17]. All the concurrent thermomechanical treatment
schedules are schematically presented in Fig. 2. For reference,
annealed wrought IN625 alloy (ASTM B443) with a grain size of
20 µm provided by McMaster Corp. was also mechanically tested in the
Fig. 1. (a) Specimen orientations during processing; (b) Tensile specimens (dimensions in mm).
2
Materials Science & Engineering A 689 (2017) 1–10
Under Ar atmosphere
Temperature
HIP [21]
Hot isostatic pressing
ST [15]
Solution
treatment
RA [20]
Recrystallized
natu
annealing
SR [20]
ral c
Stress-relief
oo
air-forc
water-quenchin
annealing
ling
ed
coolin
g
g
SLM
as-built
Time
Fig. 2. Specimens designation and corresponding thermomechanical treatment (TMT)
routes.
framework of this study.
For microstructure analysis, an optical microscope (OM, Olympus
3D laser microscope) and scanning electron microscope (SEM, Hitachi
SU8230) equipped with an electron backscatter diffraction (EBSD) unit
were used. The horizontal (XY) and vertical reference (ZX) faces of the
cubic specimens were polished manually (1 µm grit size), and then by
using a vibrometer and colloidal silica (0.05 µm grit size). For OM, the
specimens were electro-etched for 1–4 min under 2–5 V potential in a
70 mL HPO3+30 mL water solution. Grain size was measured accord-
ing to ASTM E112−13 (linear intercept method, 700–1000 grains for
statistics), using OM images for the horizontal plane (XY). The texture
evolution was characterized using EBSD, orientation contrast imaging
and integrated ARGUS FES/BSE imaging. Specimens were tilted by
70° and scanned at 20 kV, with a 1–2 µm step. This analysis was
performed using 1×1 mm2 and 0.5×1 mm2 mapping areas for hor-
izontal and vertical planes, respectively. Inverse pole figures were
calculated using a 1×1 mm2 area to eliminate local heterogeneities of
the specimens.
The dumbbell-shaped specimens (Fig. 1b) with a 2×4 mm2 gauge
section were tested in tension at room temperature (RT) and at 760 °C
(1400 °F). The tensile tests were performed under a constant strain
rate of 10−3 s−1 using an MTS 810 system. For RT testing, this system
was coupled with an MTS 634.12 contact extensometer (initial gauge
length of 20 mm). For high-temperature testing, the specimens were
heated up to 760 °C with a 1 °C/s rate, using an infrared radiant
heating chamber (Fig. 3a), and then maintained for 10 min at this
temperature before testing. The thermal field uniformity was assessed
using three K-type thermocouples distributed along the specimen
gauge length and placed in contact with the specimen, the central
thermocouple being used for temperature control (Fig. 3b). The high-
temperature testing was performed under Ar atmosphere with a flow
rate of 5–18 L/h.
Three specimens were tested for each build orientation. The relative
orientation dependence of mechanical properties as a function of the
A. Kreitcberg et al. Materials Science & Engineering A 689 (2017) 1–10

3. Results

3.1. Microstructure analysis

For the as-built alloy, Fig. 4a and b show overlapped, bowl-shaped

melt pool contours in the vertical plane and stripe patterns in the
horizontal plane, with the latter reflecting the EOS laser scanning
strategy involving a 67° hatch rotation between two successively built
layers. The melt pool width is found to be equal to the hatch spacing
(around 120 µm), while the average layer thickness corresponds to
~50 µm. The melt pool boundaries become visible due to the presence
of the preferentially etched Ni3Nb phase (Fig. 4b). After SR, the melt
pool contours are still observable (Fig. 4c), while after RA, they are no
longer distinguishable (Fig. 4d).
In Fig. 5, the grain structure evolution is presented for different
post-treatment operations. In the case of as-built specimens, a
significant quantity of Ni3Nb phase, which is subjected to preferable
Fig. 3. (a) Schematic representation of the 760 °C tensile testing setup; (b) thermo-
etching, prevents the grain boundary observation, and therefore, OM
couples positioning.
images of the as-built specimens are not given in Fig. 5.
Contrarily to OM, EBSD analysis allows the grain structure to be
build direction (L-PBF anisotropy) was calculated as follows:
revealed for both the as-built and the SR-processed specimens (Fig. 6a,
(x max − x min ) b). For both cases, grains are aligned along the Z direction (build
Δx = ⋅100% direction, vertical plane). A combination of local laser heating of the
x max
upper levels of the powder bed with significant heat dissipation towards
where x represents either the yield stress (YS), the ultimate tensile the build platform results in a high temperature gradient along the
strength (UTS), or the elongation (δ). build direction. Therefore, in the vertical plane, the grains grow from
the build platform towards the melt pool boundary/solid interface
(columnar grain structure), and their length is significantly greater
than the thickness of one powder layer and the depth of the melt pool.

Fig. 4. Cross section views of the as-built (a, b), SR (c) and RA (d) post-processed specimens.

3
A. Kreitcberg et al.
Fig. 5. Microstructure after SR (a), RA (b), ST (c), HIP (d).
Conversely, in the horizontal plane, grains are mostly equiaxed, and
their size varies from 3 to 100 µm for both the as-built and the SR-
processed specimens. However, a mean grain size of the as-built
specimens differs slightly from that of their SR-counterparts: ~25
versus ~20 µm, respectively.
EBSD-based grain/subgrain misorientation angle measurements
performed on as-built, SR- and RA-treated specimens (Fig. 7) demon-
strate that the as-built specimens possess a bimodal structural element
misorientation distribution, with the first peak located at > 10° and the
second at 50°, which clearly reflects the presence of a mixed grain/
subgrain structure in the as-built material. However, after SR, the
fraction of low-angle grain boundaries (subgrains) decreases, while the
fraction of high-angle grain boundaries (grains) increases, thus in-
dicating that a large quantity of subgrains coalesce to form grains.
After RA treatment, the amount of grain boundaries with 15–30°
misorientation increases due to the recrystallization-related grain/
subgrain boundary rearrangement and migration (Fig. 7). These
measurements are confirmed by the EBSD observations (Fig. 6c)
showing that the microstructure underwent certain grain rearrange-
ments, accompanied by the formation in the horizontal plane of a
cellular-type grain structure, similar to that observed in [22]. Larger
grains are surrounded by smaller grains with mostly < 100 > orienta-
tion, while the average grain size remains unchanged, compared to
what is seen in SR treatment. However, the grains are still elongated in
the vertical plane, indicating that recrystallization process is not
completed at this temperature.
Low-temperature solution annealing (ST) significantly promotes
recrystallization. In the vertical plane, equiaxed grains start to appear
with annealing twins, indicating a recrystallization process, while
elongated grains are still present in the vertical plane, but to a much
smaller extent than after RA treatment (compare Fig. 5b, c and Fig. 6c,
d). The average grain size measured in the horizontal plane is still low
(~25 µm); there is still an area with a high concentration of small
grains remaining in the cellular grain structure after ST treatment.
The OM and EBSD images (Fig. 5, Fig. 6) show that HIP treatment
accelerates both the recrystallization and grain growth phenomena as
seen in the horizontal and vertical planes of the metallographic
specimens. The grains are equiaxed with annealing twins representing
4
Materials Science & Engineering A 689 (2017) 1–10
a low-stacking fault free energy fcc-matrix. The grain size varies from
10 to 200 µm and from 10 to 300 µm in the horizontal and vertical
planes, respectively. Hence, the average grain size without taking into
consideration the twin boundaries is close to 40 and 50 µm in the
horizontal and vertical planes, respectively, which is quite different not
only from the as-built columnar grain morphology, but also from the
grain structures resulting from all heat treatments in this study: SR, RA
and ST.
The results of a texture examination performed in the vertical and
horizontal planes after all treatments are presented in Fig. 6. For the
as-built specimens, the EBSD maps consist mostly of red zones
corresponding to a < 100 > texture along the build direction. The
inverse pole figures shown in Fig. 6f-i were calculated using a 1×1 mm2
area to eliminate any local heterogeneities of the specimens. The
maximum pole density is located near the < 100 > orientation,
Fig. 6f. Furthermore, the rotation of grains around this direction is
considered to be random, reflecting the presence of a fiber-like texture.
After SR and RA treatments, according to inverse pole figures (IPFs),
the preferred < 100 > texture becomes weaker (Fig. 6g and h), and
after ST, due to partial recrystallization, the texture weakens further,
and the < 100 > orientation spreads to a < 110 > orientation (Fig. 6i).
Finally, after HIP, the EBSD map shows that there is no more preferred
grain orientation (random texture); the IPF densities are more homo-
geneous on the standard triangle, with the maximum pole density
being 1.17, and minimum being 0.85 (Fig. 6j).
3.2. Mechanical properties
3.2.1. Room temperature testing
Typical RT stress-strain tensile diagrams of the annealed-wrought,
as-built, heat-treated and subjected to HIP IN625 specimens are shown
in Fig. 8. Three tests were carried out for each build orientation, and
the more representative diagrams for each orientation (horizontal,
vertical and at 45ᵒ) are shown here.
For the as-built specimens, the highest strength characteristics (YS
and UTS) are shown by the 45°-oriented specimens. Conversely, the
lowest YS is shown by the vertical specimens (Fig. 8b), but they are 1.5
times greater than those of the annealed-wrought specimens. The
A. Kreitcberg et al. Materials Science & Engineering A 689 (2017) 1–10

Fig. 6. EBSD maps of the as-built specimens (a) and after SR (b), RA (c), ST (d), and HIP (e); the corresponding inverse pole figures (f-j) (Color crystalline orientation code is inserted).
(For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.).

0,025 as-built decrease the relative orientation dependence of mechanical response to

SR
6%, 5% and 3% respectively, due to the gradual formation of an
0,020 RA
equiaxed microstructure. Nevertheless, among all the specimens
tested, the as-built specimens exhibit the highest yield stress and
0,015
ultimate tensile strength, but the lowest elongation (Fig. 9). Conversely,
Fraction

HIP results in the highest elongation (60%) and the lowest yield stress
0,010
and ultimate tensile strength. Heat-treated specimens (SR, RA and ST)
have an intermediate level of elongation and strength characteristics,
0,005
and the higher the heat treatment temperature, the lower the strength
0
and the higher the elongation.
0 10 20 30 40 50 60 To sum up, compared to the as-built specimens, the strength of the
Misorientation angle, degree
SR, RA, ST, and HIP-processed specimens continuously decreases in
Fig. 7. Grain/subgrain misorientation angle distribution. this order, while their maximum elongation to failure increases.
Finally, the strength of the HIP-treated specimens is comparable to
horizontal specimens occupy an intermediate position in terms of that of their annealed wrought counterparts, while their elongation to
strength, but their elongation to failure is the weakest (27%). Thus, the failure is even slightly higher.
maximum difference in strength is found between the vertical and the
45°-oriented specimens.
3.2.2. Elevated temperature testing (760 °C)
After SR treatment, the anisotropy of the mechanical properties is
Typical tensile stress-strain diagrams obtained at 760 °C for the
still present, and even slightly greater: the difference between the 45°-
annealed-wrought and the as-built and post-treated (SR, RA, ST and
and vertically-oriented specimens corresponds to 12% of the relative
HIP) L-PBF-processed specimens are shown in Fig. 10. Identically to
orientation dependence (Fig. 8c). The RA, ST and HIP treatments
the RT testing schedule, three specimens were used for each orienta-

5
A. Kreitcberg et al. Materials Science & Engineering A 689 (2017) 1–10

Fig. 8. Tensile stress-strain diagrams (RT): annealed-wrought (a), L-PBF as-built (b) and post-treated: SR (c), RA (d), ST (e) and HIP (f).

tion (horizontal, vertical and 45°), and the representative stress-strain After SR treatment, the YS and UTS of the vertical and horizontal
diagrams are shown here for each orientation. specimens are even slightly higher, compared to the as-built state, the
For all the tested specimens, initial strain hardening is followed by a elongation increases by up to 37% for the vertical orientation, and by
decrease in flow stress (termed ″work softening″) (Fig. 10), with the up to 10–12%, for the horizontal orientation and 45ᵒ orientation
latter phenomenon being more pronounced for the annealed-wrought, specimens. Relative orientation dependence of strength characteristics
as-built, SR and RA-treated specimens (Fig. 10a-d). decreases (9%), while that of elongation is still very high.
For the as-built specimens, the lowest yield stress and ultimate The mechanical properties after RA treatment are comparable to
tensile strength are still observed for the vertically-oriented specimens, those of the SR-treated specimens. The relative orientation dependence
and the highest strengths for the 45°-oriented specimens. Therefore, of elongation to failure is still high (~70%). After ST and HIP
the strength decreases in the following order: 45°→horizontal→verti- treatments, the difference between the differently-oriented specimens
cal, which represents the same trend as for the RT tensile tests. The is almost no longer observable: the relative orientation dependence of
relative orientation dependence of strength (12%) is the same as that strength and elongation decreases down to 3% and to 2%, respectively.
measured at RT. It can be seen that UTS and YS of the as-built Nevertheless, among all the L-PBF specimens tested, the SR-
specimens are ~1.2 times greater than that of their annealed-wrought processed specimens exhibit the highest strength characteristics: yield
counterparts. Conversely, compared to the RT tests, elongation to stress and ultimate tensile strength (Fig. 11). Conversely, among all the
failure of the as-built specimens is 3–10 times lower than that of the specimens tested, HIP treatment results in the lowest yield stress and
annealed-wrought specimens, and that the relative orientation depen- ultimate tensile strength; however, this treatment offers the highest
dence of elongation to failure is significant: the as-built vertical elongation to failure for all build orientations (21–25%), while ST
specimens exhibit the highest elongation (22%) compared to their results in an intermediate level of elongation to failure and strength
counterparts for other orientations (6–7%). characteristics.

1 Vertical Horizontal 45 ° 100

UTS 90
UTS
0.8 80

70
Normalized stress

0.6 δ 60
δ
Elongation, %

YS
50

0.4 YS 40

30

0.2 20

10

0 0
d- ilt SR RA ST HIP ilt SR RA ST HIP i lt SR RA P
ale -bu -bu -bu ST HI
ne ht as as as
a n r o ug
w

Fig. 9. Room temperature mechanical properties.

6
A. Kreitcberg et al. Materials Science & Engineering A 689 (2017) 1–10

Fig. 10. Tensile stress-strain diagrams obtained at 760 °C: annealed-wrought (a), as-built (b) specimens and after SR (c), RA (d), ST (e) and HIP (f) treatments.

Finally, the mechanical strength characteristics of the L-PBF speci- (Fig. 13a and b). For the horizontal specimens, the tensile surface
mens are greater than or comparable to those of their annealed- shows a brittle intergranular fracture (Fig. 13a), while the vertical
wrought counterparts, while their elongation to failure is significantly specimens present very deep upper open pores with dimpled features,
lower (Fig. 11). and the fracture mode is mainly intergranular, with some zones of
transgranular overload fracture (Fig. 13b).
3.2.3. Fracture surface Thus, the significant decrease in elongation of the horizontal
Tensile fracture surface analyses were performed for the SR- specimens tested at 760 °C compared to those tested at RT is
processed horizontal (XZ) and vertical (ZX) specimens, which exhibited accompanied by changes in their fracture patterns: from a mixture of
the highest difference in elongation to failure. After RT tensile testing cleavage and dimpled surfaces to mostly intergranular fracture. After
for both vertical and horizontal specimens, the fracture surface images HIP, the fracture surface is characterized by ductile intergranular
are quite similar and characterized by a mixture of smooth zones of fracture with visible triple points for both the horizontal and vertical
cleavage and dimpled patterns (Fig. 12). However, for the horizontal specimens (Fig. 13c and d) due to the grain boundaries weakening at
specimens, the fracture surface consists of a larger area of relatively elevated temperatures [23,24].
flat, layered patterns (Fig. 12b), while the vertical specimen's fracture
surface is mostly dimpled (Fig. 12c and d). 4. Discussion
After HIP treatment, the fracture surface of both the horizontal and
vertical specimens is characterized by typical ductile dimples resulting 4.1. Grain structure and texture
from coalescence of microvoids (Fig. 12e and f). A significant amount
of fine dimples indicates the extent of uniform plastic deformation. The particular thermo-kinetic phenomena occurring during L-PBF
Contrary to the RT tensile tests, after 760ᵒC, the surface fractures of processing impacts the phase development and grain morphology,
the horizontal and vertical specimens are more different after SR which differ notably from what is observed during conventional hot-

0.6
Vertical Horizontal 45° 100

90

80
δ
0.4 70
Normalized stress

UTS
60
Elongation, %

UTS
YS

50

YS
40
0.2
δ 30

20

10

0 d-
0
ale i lt SR RA ST HIP i lt SR RA ST HIP i lt SR RA ST HIP
ne ht -bu -bu -b u
an roug as as as
w

Fig. 11. Mechanical properties of the IN625 specimens at 760 ᵒC (the stress scale is identical to that of Fig. 9).

7
A. Kreitcberg et al. Materials Science & Engineering A 689 (2017) 1–10

Fig. 12. RT testing: fracture surface of the horizontal (a, c) and vertical (b, d) specimens; after SR (a-d) and HIP (e, f).

working processing. It is shown that the L-PBF processing is respon-
sible for the formation of elongated grains in the direction parallel to
the build direction. For the as-built specimens, the average grain size in
the horizontal plane is around 25 µm, while in the vertical plane, the
average grain size exceeds three-layer thickness (150 µm). The SR
treatment strongly decreases the fraction of low-angle grain bound-
aries, which is characteristic of a stress relief phenomenon. The average
grain size in the horizontal plane following SR treatment decreases to
20 µm. The grains are still elongated in the vertical direction.
The results of the RA treatment differ slightly from those of the SR
treatment: the grains are still elongated in the vertical direction, and
the average grain size in the horizontal plane remains almost un-
changed, compared to that after SR treatment, while the fraction of low
angle-boundaries continues to decrease. Note in this respect that in
work-hardened IN625 alloys, annealing at T≥980 °C already leads to
material recrystallization [16,25], while in our case, this process is
definitely delayed in temperature.
At a higher treatment temperature (ST), annealing twins are formed
in some grains as a consequence of twin formation at migrating grain
boundaries, and the average grain size in the horizontal plane increases
insignificantly, from 20 to 25 µm. The ST treatment should also trigger
precipitates dissolution [14]. This aspect is still under investigation.
Finally, the HIP treatment accelerates recrystallization and grain
growth phenomena: the average grain size increase up to 40–50 µm;
the grains become equiaxed and their sizes vary from 10 to 300 µm.
The as-built IN625 alloy is mainly composed of < 100 > grains
aligned in the build-direction. Generally, this texture is the most
favorable solidification texture for cubic materials because heat flow
is more significant in this direction through the liquid-solid interface
[26]. The < 100 > texture was found to be preferential for many alloys

Fig. 13. 760 °C testing: fracture surface of the horizontal (a, c) and vertical (b, d) specimens; after SR (a and b) and HIP (c and d).

8
A. Kreitcberg et al. Materials Science & Engineering A 689 (2017) 1–10

built using laser and electron beam PBF processes [27–30]. For the Ni- RT 760°C
based alloy, the < 100 > orientation provides the highest creep 1 80
δ
strength and the lowest Young modulus, compared to the < 110 > UTS
UTS UTS δ 70
and < 111 > orientations [31]. The thermal and HIP treatments of the 0.8

Normalized stress
δ 60
L-PBF-processed specimens of our study lead to the weakening of this

texture. After HIP, no preferred grain orientation is observed, and the
microstructure becomes isotropic.
4.2. Mechanical properties and failure
The grain shape, size and crystallographic texture of tensile speci-
mens depend on the build orientation of the specimens, and contribute
to the anisotropy of their mechanical response. The tensile tests
performed in this study show that vertical specimens exhibit the
highest elongation, but the lowest strengths, compared to their
differently-oriented counterparts mainly due to the texture effect,
which agrees with the literature data for L-PBF Ti-6Al-4V, Nimonic
263 and Co-Cr-Mo alloys [4,32,33]. On the other hand, the highest
strength characteristics are obtained for the 45°-oriented specimens.
The horizontal specimens occupy an intermediate position in terms of
strength, but their elongation to failure is ~1.3 times smaller than that
of the vertical specimens. However, the greater contribution of oriented
microstructures to ductility was found during tensile testing at an
elevated temperature (760 °C). Vertical specimens exhibit almost 4-
times higher elongation to failure than their horizontal and 45°-
oriented counterparts.
For the as-built IN625 specimens, flow curves at 760 °C showed
work hardening at the initial stage of deformation followed by work
softening until failure. Such a behavior can be explained by dynamic
structural changes occurring during deformation. For the nickel-based
alloy, these structural changes can be associated with the dynamic
recrystallization phenomenon occurring in alloys with low stacking
fault energy [34,35] and/or with γ″→δ transformation [17]. More
detailed microstructure studies of the deformed specimens are needed
to verify this hypothesis.
ST and HIP allow an improvement of ductility and a reduction of
the anisotropy of mechanical properties. After HIP, for example,
elongation to failure increases from 30% to 60% (RT) and from 10%
to 25% (760 °C, for all but the vertical specimens), while relative
orientation dependence decreases from 12% to 3%. It should be noted
however that after HIP, the elongation of the L-PBF IN625 alloy at
760 °C is almost half of that at RT: ∼25% compared to ∼50%.
Moreover, when the tests are carried out at 760 °C, the fracture mode
changes from transgranular to intergranular. It is hypothesized that
secondary carbide precipitation or/and porosity may result in the
intergranular crack propagation and elevated temperature embrittle-
ment of Ni-based alloys [36,37].
Even though the ST and HIP processing sequences lead to
comparable characteristics in terms of elongation and uniformity, the
overall mechanical strengths of the ST-processed specimens remain
higher than that of the HIP-processed specimens (Fig. 14).
Consequently, post-L-PBF ST treatment can be recommended for
applications requiring high static mechanical properties at room
temperature. However, since IN625 is primarily designed for high-
temperature applications, HIP appears to be the more favorable post-
treatment operation. Finally, even though the mechanical properties of
the L-PBF-built IN625 specimens at RT are comparable to those of
their annealed wrought counterparts, their elongation at an elevated
temperature (760 °C) is significantly lower and does not exceed 22%
after post-L-PBF HIP treatment (Fig. 14), it is probably due to the
specific grain boundary features (presence of carbides) in L-PBF alloy
as discussed above; further investigations will be carried out in our next
paper.
Elongation, %
δ
0.6 50
YS 40
YS
0.4 YS UTS
YS UTS UTS δ 30
YS YS
δ 20
0.2
10
0 0
d- ST P d-
ale HI ale ST HI
P
n ne gh t n ne ght
a r ou a rou
w w
Fig. 14. Mechanical properties of IN625 (mean values calculated for all orientations).
5. Conclusion
The microstructure and mechanical properties of the IN625 alloy
processed by selective laser melting were studied in the as-built state
and after the following post-L-PBF treatments: stress-relief annealing,
recrystallization annealing, solution treatment and HIP.
L-PBF processing of the IN625 alloy results in the formation of a
columnar microstructure with grains elongated along the build direc-
tion. The main texture component of the as-built IN625 specimens
corresponds to < 100 > .
Post-L-PBF heat treatments and HIP lead to the formation of an
isotropic equiaxed microstructure, but this is at the expense of grain
coarsening. The higher the heat treatment temperature, the larger the
grain size, and the lower the microstructure anisotropy.
The as-built IN625 specimens exhibit the highest tensile strength,
the lowest elongation and the highest relative orientation dependence
of mechanical properties, as compared to their post-treated counter-
parts. The vertical as-built specimens provide the lowest strength, but
the highest elongation to failure, while the 45°-oriented specimens
show the highest strength; the lowest elongation to failure is found for
horizontal specimens. The anisotropy in properties is mainly due to the
difference in the orientation of the columnar structure with respect to
the tensile test direction.
The low-temperature solution heat treatment and HIP treatment
allow an improvement in ductility and homogeneity, but they are
obtained at the expense of lower strength characteristics.
Finally, the overall mechanical strengths and elongation to failure
of the L-PBF-processed IN625 alloy obtained after tensile testing at
room temperature exceed or equal to those of the annealed wrought
alloy of the same composition. At an elevated temperature (760 °C), the
strength characteristics of the L-PBF-processed specimens are compar-
able to those of the annealed-wrought alloy, while its elongation to
failure is found to be significantly lower than that of the annealed
wrought alloy. Optimization of the post-L-PBF HIP treatment appears
to be a key to further improvement of the mechanical properties of
IN625 components built by selective laser melting.
Acknowledgements
The authors would like to express their appreciation for the
financial support provided by CRIAQ (Consortium de Recherche et
d′innovation en Aérospatiale au Québec (MANU721)) and by NSERC
(Natural Sciences and Engineering Research Council of Canada). Our
industrial partners (Pratt & Whitney Canada and Fusia) are gratefully
acknowledged for fruitful discussion of the results obtained and for
providing specimens used in this work.

9
A. Kreitcberg et al.
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