Materials Science & Engineering A 813 (2021) 141111

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Materials Science & Engineering A

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

Impact of high temperature stress relieving on final properties of Inconel

718 processed by laser powder bed fusion
Konrad Gruber a, *, Robert Dziedzic a, Bogumiła Kuźnicka a, Bartosz Madejski b, Maciej Malicki b
a
Wrocław University of Science and Technology, Faculty of Mechanical Engineering, Centre for Advanced Manufacturing Technologies (CAMT-FPC), Ul. Łukasiewicza
5, 50-371, Wrocław, Poland
b
Łukasiewicz Research Network, Institute of Aviation, Al. Krakowska 110/114, 02-256, Warsaw, Poland

A R T I C L E I N F O A B S T R A C T

Keywords: During manufacture of Inconel 718 (IN718) parts with complex geometry and high dimensional accuracy by
Laser powder bed fusion laser powder bed fusion (LPBF), effective stress relieving is required before cutting off the parts from the build
Inconel 718 platform, in order to prevent distortion. The residual stress can be removed completely only by full recrystal­
Stress relief
lization of structure, induced by annealing at the temperature close to that used in hot isostatic pressing (HIP).
Microstructure
Tensile properties
This work was aimed at investigating the effect of stress-relieving at 1150 ◦ C for 6 h on properties of LPBF-ed
IN718, obtained after each of successive thermal processing steps: optional HIP, solution annealing and dou­
ble aging, in relation to analogous research performed with use of the thermal processing parameters recom­
mended by ASTM standards. In addition, the effect of heating and cooling rates during individual heat-treatment
steps on dissolution and precipitation of secondary phases was investigated. It was shown that an advantage of
stress relieving at 1150 ◦ C in comparison to the standard annealing at 1065 ◦ C is higher effectiveness of stress
elimination, higher resistance to liquid-film formation during heating-up, lack of delta phase, significantly higher
elongation (48%) and area reduction (30%) of IN718 in final (without HIP) aged condition. Although the high-
temperature stress relieving and HIP treatments resulted in coarse-grained microstructures, the tensile strength
values determined at room and elevated temperatures (425 ◦ C and 650 ◦ C) were higher than the nominal values
of wrought IN718 with similar grain size and much higher than those of cast and HIP-ed IN718.

1. Introduction 1.1. Residual stresses and distortion in the LPBF manufactured parts

A characteristic feature of the laser powder bed fusion (LPBF) tech­
nology is multi-layer deposition of selectively melted powder with use of
a laser beam moving according to the accepted scan strategy within the
contour determined by the CAD model. This technology arouses
immense interest of the industry, since gives possibilities of
manufacturing complex parts with variable cross-sections and of quick
prototyping. In spite of a considerable progress in its development, a
number of problems related to manufacture of parts with complex
shapes still exists, impeding wide application of the technology in the
industry. The particularly difficult problem is high level of thermal
stresses induced in the manufactured part during the process, as well as
residual stresses remaining after completion of the process and when the
finished part reached its equilibrium state.
Residual stresses are consequences of a steep temperature gradient,
very high cooling rates (105–106 K/s) [1] and thermal strain [2]. Dis­
tribution of residual stresses varies within a layer and between layers.
The complex nature of residual stress strongly related to processing
parameters such as laser power, scanning speed and scanning strategy,
depends also on material properties, geometry and size of the manu­
factured part. Large and anisotropic residual stresses can cause distor­
tion, delamination and cracking during manufacture. Therefore, one of
optimization criteria of the LPBF process is maximum reduction of re­
sidual stresses to prevent thermal cracking and distortion during the
process.
Complexity of concurrent influence of the above-mentioned factors
on residual stress results in discrepancies between the published results
concerning this influence. Numerical estimations [3] showed that
reduction of heat input (decreased laser power and increased scanning

* Corresponding author.
E-mail address: konrad.gruber@pwr.edu.pl (K. Gruber).

https://doi.org/10.1016/j.msea.2021.141111
Received 7 January 2021; Received in revised form 8 March 2021; Accepted 13 March 2021
Available online 19 March 2021
0921-5093/© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
K. Gruber et al.
speed) and of layer thickness results in lower thermal strain and,
consequently, in lower residual stress. However, experimental findings
show the reverse relationship, i.e., residual stress reduction with
increasing heat input [4] and increasing layer thickness [5,6]. To miti­
gate residual stresses, it is desirable to use short scan vectors [7] with
optimum orientation in a particular direction [8] especially the chess­
board scanning strategy with properly selected sequence of scanning the
“islands” [9]. An effective method of reducing residual stresses is pre­
heating the build platform [10]. The fact that higher temperature of the
build platform results in lower level of residual stresses is confirmed by
both experimental analysis and simulations [2].
The additional factor reducing residual stresses are support struc­
tures used in the LPBF technology in order to support the parts being
built. Because of poor thermal conductivity of loose powder in the bed,
support structures facilitate heat dissipation and, in consequence,
reduce the level of thermal stresses [11], thus reducing the risks of
distortion and cracking. Their effectiveness depends on geometry and
size of the built part, as well as on the used material. Therefore, the
optimally designed support structure makes it possible to avoid distor­
tion during the process [12]. However, cutting-off the parts from the
build platform, whether they were made with a support or with no
support, induces relaxation of stresses by distortion [11], especially of
the parts with low structural stiffness [13].
Irrespective of the large number of research works cited in review
articles [1,2,14] it seems that complexity of the LPBF process excludes
sufficiently exact estimation of process-induced stress magnitudes and
distributions, as well as distortion, by computational methods. In turn,
measurements of residual stresses in the LPBF processed parts are
troublesome, in many cases require using more than one measuring
technique and their accuracy is limited [15]. Besides, contradictory
opinions exist in literature with regard to influence of geometry and size
of the manufactured part on the resulting residual stresses [2].
In view of the above facts, it is well-grounded to assume that, when
manufacturing parts with complex geometry and variable cross-sections,
removing parts from the platform without a properly selected stress-
relief annealing is risky to the degree dependent of the material and
geometry of the manufactured part.
1.2. Mitigation of residual stress in the LPBF IN718 parts
The IN718 alloy is a material used in aerospace industry, because of
its satisfactory combination of strength and ductility [16]. Its techno­
logical properties like very good weldability and casting properties [17],
and thermo-physical properties [18,19] classify this alloy as easily
processable by LPBF, i.e., with low susceptibility to forming defects
(pores and cracks) in comparison to high strength aluminum alloys or
magnesium alloys [1]. Nevertheless, in order to mitigate thermal
distortion of IN718 parts during LPBF, heat input should be minimized
by decreasing laser power or by increasing scanning speed, as well as by
a reduction of layer thickness. Since high scanning speed at low thermal
diffusivity increases thermal strain, IN718 with lower (in comparison to
e.g., 316 stainless steel and Ti6Al4V alloy) thermal conductivity [18]
and thermal diffusivity [19], and with similar heat capacity is more
susceptible to higher peak temperature, larger pool volume and higher
thermal strain [20].
The results of computational analysis of residual stresses summa­
rized in the review article [1] showed that the maximum computed
residual stresses in thin walls achieve level of 1.5 yield strength for
IN718 in relation to 1.0 YS for the Ti6Al4V alloy and 0.6–0.9 YS for 304
stainless steel. The experiments of Dunbar et al. [21] demonstrated that
IN718 parts distort 50% more than Ti6Al4V parts for the same geometry
and experiment condition. It results from here that, in manufacture of
complex, thin-walled parts of IN718, preventing a distortion is the main
criterion of process parameter selection, apart from porosity.
There is a big interest of researchers representing different disci­
plines in behavior of the IN718 alloy during the LPBF process [14]. The
2
Materials Science & Engineering A 813 (2021) 141111
common feature of the papers is focusing on examination of specimens
with a given geometry consistent with the CAD model or mechanically
cut-out (shaped) from a block made by LPBF [22]. However, the LPBF
technology is finally intended for manufacture of parts with complicated
geometry and variable cross-sections (thin-walled), hardly possible or
impossible to be made by traditional technologies. From the viewpoint
of product quality, the requirements related to optimization of process
parameters are completed with rigid requirements related to accuracy of
imitating the assumed geometry, which can be ignored in the case of
manufacturing specimens with simple shapes and small sizes. Mean­
while, stress-relief annealing is of significant importance as the first
stage of post-processing heat treatment, since it can induce irreversible
changes in the as-built microstructure (changes of phase fraction,
recrystallization and grain growth or carbides coarsening), which
significantly affect selection and expected results of subsequent
heat-treatment operations.
For IN718 parts fabricated by LPBF, the standard ASTM F3055− 14a
recommends stress-relief annealing temperature within 1065 ◦ C ± 15 ◦ C
for 1.5 h, leaving however to the manufacturer the decision on matching
annealing temperature and time with overall dimensions and shape of
the part, dimensional accuracy requirements and type of the PBF-LB/M
machine. According to Dunbar et al. [21] experiments, two identical
IN718 parts made by different manufacturers can be distorted in the z
direction with a 10.6% difference. Mercelis and Kruth [23] reported that
stress level in the 316 L manufactured components on the build platform
reaches the material yield point. Even if the stress level in the compo­
nent removed from the platform is significantly lower, it can deform
during its cutting-off. Therefore, in the authors’ opinion, application of
high-temperature annealing of IN718 parts, guaranteeing complete
elimination of residual stresses to avoid distortion during their removing
from the platform, is of particular importance for manufacture of parts
with high shape and dimensional accuracy.
This work was aimed at investigating the effect of high-temperature
stress relieving, i.e., annealing carried-out at a temperature above the
recrystallization temperature, on the LPBF IN718 properties obtained
after subsequent thermal processing steps: optional high isostatic
pressing, solution treatment and aging, in relation to analogous research
performed with use of the thermal processing parameters recommended
by ASTM standards.
At the first stage, distortion susceptibility tests of the LPBF-ed
cantilever specimens during cutting them off from the build platform
without annealing and after two variants of stress relieving were carried-
out. The purpose was to determine the level of macroscopic (i.e., Type I)
residual stresses induced by volumetric shrinkage of melted layers
during their solidification and thermal contraction of the previously
solidified layers, as well as effectiveness of employed stress relieving
variants.
At the second stage, examinations were carried-out on cylindrical
specimens that, after two variants of stress relieving on the platform,
were subjected to the subsequent heat treatment steps. Microstructure
was checked and hardness measured between the steps, and tensile
properties at room and elevated temperatures were determined after
ageing.
It was shown how much significant is, beside temperature and
soaking time, the effect of heating and cooling rates during stress-relief
and solution treatments on phase transformations in the LPBF IN718
specimens, which is useful for designing and optimizing the heat treat­
ment strategy but, according to the authors’ knowledge, has not be taken
into consideration before.
2. Materials and methods
2.1. Feedstock
During the LPBF process, powder distributed by a recoater should
flow evenly over the preceding solidified layer. Therefore, the powder
K. Gruber et al.
characteristics deciding such behavior and thus its usefulness for
manufacture of high-quality parts with known and expectable properties
[24] are so important. The argon atomized powder of IN718, supplied by
SLM Solutions, was composed of mostly spherical (according to ASTM
B243-11) grains with smooth surfaces, sporadically accompanied by
satellite particles, and a small part of irregularly shaped grains (Fig. 1).
Chemical composition of the powder (Table 1) was within the range
determined by ASTM B637 for the IN718 alloy.
Particle size distribution (PSD) was determined by laser light
diffraction with the instrument combined of a HELOS/BR sensor and a
RODOS/T4 dispersing unit. As results from the cumulative distribution
curves shown in Fig. 1a, size of 85% of powder particles ranged within
20–50 μm and the mean particle size x50 was 33.4 μm, which meets
requirements of the LPBF technology [25].
2.2. Process parameters
All kinds of specimens were made on the PBF-LB/M machine, SLM
Solutions 280 2.0, equipped with an IPG 1070 nm continuous-wave fiber
laser. High-purity argon was used as protective atmosphere. The set of
process parameters (see Table 2) was accepted according to the machine
manufacturer in order to produce IN718 specimens with high dimen­
sional accuracy and relative density over 99.95%. Specimens were built
on a IN625 build platform (100 × 100 × 25 mm3). In the light of the
results cited in the previous paragraph, the process parameters specified
in Tables 2 and i.e., low heat input, small layer thickness, build platform
preheat and scanning strategy with short hatch rotation (Fig. 2), should
prevent thermal distortion of specimens during building.
2.3. Specimens and scope of examinations
Three kinds of specimens were prepared, whose shape, dimensions
and build orientation are presented in Table 3. Cantilever beams for
distortion measurement were made in horizontal position at 0◦ , 45◦ and
90◦ in relation to the x axis (Fig. 3a). Specimens for microstructure ex­
amination, for hardness measurements and for tensile testing were
prepared in the form of cylinders in perpendicular position to the build
platform. Final dimensions of gauge lengths of tensile specimens were
obtained by turning and peripheral grinding according to ASTM E8-04.
Scope of the examinations included:
1. Measurements of maximum z-displacement of one-end fixed speci­
mens with low structural stiffness after cutting them from the plat­
form (see Fig. 3b), without previous stress-relief annealing and after
stress relieving together with the build platform. This test was aimed
at evaluating maximum stresses left in LPBF-ed specimens with use
Fig. 1. Characteristics of IN718 powder: a) particle size distribution, b) particle shape.
3
Materials Science & Engineering A 813 (2021) 141111
of process parameters specified in Table 2, in the as-built condition
and after stress-relieving together with the platform at 1150 ◦ C (i.e.,
above recrystallization temperature) and at 1065 ◦ C as recom­
mended by ASTM F3055-14a.
2. Determination of influence of the suggested stress-relieving param­
eters on tensile properties at ambient temperature and at elevated
temperatures, as well as on hardness and microstructure of cylin­
drical specimens subjected to solution annealing after removing from
the platform and then turned, ground, and finally aged acc. to AMS
5383. Properties of the specimens stress-relieved on the platform
with use of the parameters recommended by ASTM F3055-14a, so­
lution annealed acc. to AMS 5664E, and aged acc. to AMS 5383 were
accepted the reference level for the obtained results
Parameters of the used heat-treatment variants with their acronym
designations and heating/cooling rates are compiled in Table 4 and in
Fig. 4. Results of microstructure observations in the stress-relieved
condition, presented in a further part of the paper, inspired the au­
thors to subject two series of specimens to the HIP (Hot Isostatic
Pressing) process between the stress relieving and solution annealing
operations. The process parameters are given in Table 4 and in Fig. 4b.
Heat treatment was carried-out in a vacuum furnace TAV H3S 1600.
Three kinds of cooling were applied: furnace cooling (FC) at residual
pressure 140 Pa, argon cooling (AC) at absolute pressure 1 MPa with fan-
forced gas circulation and, argon cooling (AC) at absolute pressure 0.1
MPa with fan-forced gas circulation. The HIP treatment was carried-out
in a graphite furnace VHT 822-GR.
After spark-cutting from the platform, displacement of free ends of
the cantilever beams in the z axis direction was measured using a co­
ordinate measuring machine (CMM). Static tensile tests were carried-out
according to ASTM E8/E8M-16a and ASTM E21-09 on a servo-hydraulic
machine MTS 318.10 equipped with an extensometer MTS 63253F-14,
and a furnace INSTRON SFL SF1770. Hardness measurements were
performed using a Zwick/Roell Vickers hardness tester at the loads of
4.9 N and 98.1 N. Microstructure examination was carried-out with a
Keyence VHX6000 digital microscope, an Olympus LEXT OLS4000
confocal laser scanning microscope (CLSM), and a Zeiss EVO MA25
scanning electron microscope equipped with the EDS detector. Metal­
lographic polished sections on longitudinal and perpendicular cross-
sections of the specimens were etched using the waterless Kalling’s re­
agent to reveal general microstructure and the Glyceregia reagent to
outline carbides. The average grain size in the heat treated specimens
was determined acc. to ASTM E112–13 by the Heyn intercept method
excluding twin boundaries.
Electron backscatter diffraction (EBSD) measurements and analysis
were performed using a fully automated TEAM™ EBSD analysis system
K. Gruber et al. Materials Science & Engineering A 813 (2021) 141111

Table 1
Chemical composition of IN718 powder (acc. to SLM Solutions Certificate).
Element Ni Cr Fe Ta + Nb Mo Ti Al Si C Co B Mn Cu P S O N

wt% 52.83 18.97 18.16 5.05 2.99 0.96 0.46 0.35 0.045 0.03 0.003 < 0.03 < 0.03 < 0.015 < 0.015 0.01 166 ppm

of the specimens in the z axis direction. Note that differences between

Table 2
deflections of the specimens with different orientation of their long axes
Process parameters.
in respect to the recoater direction (x axis) are small at 0.05–0.11 mm,
Parameter value Scanning strategy (see Fig. 2) due to the applied strategy of scanning with short hatch rotation. Stress
Laser power, P 300 W Stripe length 7 mm relieving at 1150 ◦ C for 6 h resulted in complete elimination of the
Scanning speed, v 1300 mm/s Shift factor 11 distortion. The annealing recommended by ASTM, 1065 ◦ C for 1.5 h,
Focal beam diameter, D 100 μm Initial hatch angle 45◦ appeared also to be very effective, although the recorded small dis­
Layer thickness, g 30 μm Hatch rotation angle 67◦
Hatch distance, h 120 μm Window limitation 135◦ (±67.5◦ )
placements did not guarantee that distortions of slender specimens were
Build platform preheat 200 ◦ C Number of borders 2 completely eliminated. They suggested however, that the residual stress
Calculated value Type II (micro-stress) was not completely released. This is consistent
Linear energy density, EL = P/v 0.23 J/mm with the results of Cao et al. [26], who found, by EBSD measurements,
Volume energy density, EV = P/(v∙g h) 64 J/mm3
presence of residual plastic strains inside columnar grains after 1-h
annealing at 1080 ◦ C.
interfaced to a Zeiss Sigma 500VP scanning electron microscope. The On the grounds of the measured deflections, residual stresses were
mapping areas of 900 μm × 700 μm were indexed with the step size of 3 calculated from the common formula σmax = F⋅l/W, using the formula
μm. For each specimen, 3 EBSD (electron backscatter diffraction) maps wzmax = F⋅l3/3 EJ for maximum deflection of a cantilever beam loaded at
were acquired. its end by the force F (see Fig. 3), where moment of inertia J = 27 mm4
A Rigaku Ultima IV X-ray diffractometer was used to determine and cross-section modulus W = 18 mm3. Considering the range of
phase composition of the specimens. Monochromatic radiation of the Young’s modulus values given in literature for horizontally LPBF-ed
tube with copper anode (λ = 1.54 Å) was applied. Diffraction lines were specimens, like 193 GPa [27], 195 GPa [28], 200 GPa [29] and 203
recorded within the 2θ value from 30◦ to 100◦ by the step method with GPa [30], the value E = 200 GPa was accepted. It should be stressed that
the 2θ step equal to 0.02◦ and the irradiation time equal to 4 s. the above E values are significantly higher than those obtained for
Detection and visualization of three-dimensional distribution of vertical specimens subjected to tension in parallel to the build direction.
pores in the specimens was carried-out by computed tomography with This difference results from crystallographic texture, specific cellular
the GE phoenix v|tome|x s240 system. Resolution of data for the IN718 substructure of columnar grains created by the dislocation network
specimens was 9 μm at the tube voltage of 160 kV and current of 60 μA.
The examinations confirmed that relative density of the specimens was
Table 3
higher than 99.96%. Single pores only were found in the manufactured Shape, dimensions, and destination of LPBF specimens.
specimens, which corresponded to porosity below 0.04%.
Destination Shape ( Dimensions of gauge length Build
Fig. 3a) orientation
3. Results and discussion
Distortion Cantilever l × b × h = 60 mm × 12 mm Horizontal
measurement beam × 3 mm
3.1. Distortion and residual stress Microstructure Cylindrical Diameter 7.5 mm × 71 mm Vertical
examination
Results of tip-displacement measurements of the cantilever speci­ Tensile test Cylindrical Diameter 4 mm, gauge Vertical
mens are shown in Table 5. Cutting-off the specimens in the as-built length 19 mm, screw thread
250-20 UNC
condition results in stress releasing and in the significant deflections

Fig. 2. Schematic presentation of stripe-scan patterns with 67◦ rotation between consecutively built layers.

4
K. Gruber et al.
Fig. 3. Position of cantilever specimens on the build platform: (a) before and (b) after cutting them from the platform.
Table 4
Variants of post-processing heat treatment (HT).
Heat treatment step Heat treatment variant
H1 and H1+HIP H2 and H2+HIP
Stress relieving SR1150; SR1065 1150 ◦ C/6 h 1065 ◦ C/1.5 h
Hot isostatic pressing HIP 1150 ◦ C/4 h/100 MPa
Solution annealing SA1100; SA1065 1100 ◦ C/1 h 1065 ◦ C/1 h
Double aging DA 720 ◦ C/8 h + 620 ◦ C/10 h
[29], and residual stress distribution since residual stresses add up to
tensile stresses during the tensile test. As results from the calculations,
maximum deflection of free-end of the beam (Table 5) corresponds with
high level of maximum tensile stresses at bending in the as-built con­
dition, ranging between 785 and 865 MPa. Such a high stress level
reaches the yield strength determined for horizontal as-built specimens
by Zhang et al. [31] and Watring et al. [28], and is 1.6 times higher than
the yield strength determined for vertical specimens by Aydinöz et al.
[32]. Residual stresses are reduced by stress-relief annealing at 1065 ◦ C
to ±18 MPa and completely removed by annealing at 1150 ◦ C.
3.2. Microstructure and hardness in as-built and heat treated condition
Chemical composition of the IN718 alloy was developed from the
viewpoint of its application in the precipitation strengthened state for
the parts withstanding loads at elevated temperatures. The strengthened
state is obtained by dissolving secondary phases in solid solution γ (RSC)
during solution annealing and the following double aging with
controlled, very slow cooling (as shown in Fig. 4a). In the aged condi­
tion, two kinds of secondary strengthening phases coherent with the γ
matrix exist: γ’ [Ni3(Al,Ti)], equilibrium (fcc) phase and γ’’ [Ni3(Nb,Al,
Ti)], metastable (bct) phase. The γ’’ phase is the main strengthening
phase that above 650 ◦ C transforms to the equilibrium orthorombic
phase, δ (Ni3Nb). Precipitations of the γ′ -phase play a minor role in
IN718 strengthening and dissolve in the matrix at temperatures above
1000 ◦ C [33].
3.3. As-built microstructure and hardness
Microstructure of LPBF-ed IN718 in the as-built condition is shown in
Fig. 5. As can be seen, the microstructure features connected with the
process parameters, like columnar γ grains elongated to the build di­
rection (Fig. 5a), traversing the fusion lines i.e., solute banding lines that
outline the shape of track interfaces in individual layers, additionally
confirm the specific morphology of the layer-by-layer solidified micro­
structure of LPBF-ed IN718 [34]. Irregular arrangement of solute-rich
bands of individual tracks, shown in the cross-sections xz (Fig. 5a) and
xy (Fig. 5b), is adequate to the applied scanning strategy using rotation
of the scanning vector between subsequently built layers (see Fig. 2).
However, it should be stressed that the IN718 microstructures in the
5
Materials Science & Engineering A 813 (2021) 141111
as-built condition reviewed by Hosseini et al. [14] are different on
different levels of the length-scale because of strong dependence of
qualitative and quantitative features of microstructure on the processing
parameters. This influences phase transformation kinetics in LPBF-ed
IN718 during post-processing heat treatment and so it is highly desir­
able to collect data concerning the relationships between the process
and the as-built microstructure.
The substructure of columnar γ-phase grains (Fig. 6) is built of
“packets” of the parallel dendritic cells with small misorientation angles
(2◦ < θ < 5◦ ). The high-density dislocation structure of these very low-
angle boundaries (VLAGBs) creates a rigid three-dimensional network,
which was repeatedly confirmed by TEM examination, e.g. Refs. [29,35,
36]. As was shown by EBSD analysis, the part of the VLAGBs is large
(Fig. 7) in comparison to the fraction of low-angle boundaries (LAGBs)
with misorientation angles (5◦ < θ < 15◦ ), occurring between packets of
dendritic cells.
As was indicated with arrows in Fig. 6b, the intercellular boundaries
are decorated by carbides and particles of Laves phase. Their presence is
a result of cellular-dendritic growth of γ-phase grains and micro­
segregation of alloying elements with the partition coefficient k < 1, i.e.,
Nb, Ti and Mo (see Table 6) stabilizing the liquid film in the intercellular
spaces. Partition of these elements to the liquid causes also rapid
changes of the solidification front rate and, in consequence, creation of
solute banding lines (Figs. 5 and 6a). Concentration of the above-
mentioned elements in residual liquid metal results in its non-
equilibrium solidification by the eutectic transformation, accompanied
by volumetric shrinkage of 2% [17] and thermal contraction (when vol
% of solid ~ 0.9) generating dislocation structure of cell walls. Apart
from γ phase and carbides type (Nb,Ti)C, the brittle intermetallic Laves
phase (Ni,Cr,Fe)2(Nb,Mo,Ti) is also a product of the eutectic trans­
formation. Sizes, shapes, and number of particles of this phase as com­
ponents of the eutectic mixture are strongly dependent on process
parameters, first of all on the laser power and scanning speed [37], so
effectiveness of its dissolving during solution annealing is various.
In comparison to the examinations of the LPBF-ed IN718 alloy,
previously carried-out by the authors of this paper [27], a change of
scanning strategy and significant reduction of energy density (linear
below 0.30 J/mm and volumetric below 100 J/mm3) resulted in over
two times smaller primary spacings between dendritic cells, ranging
between 0.5 and 1.5 μm (see Fig. 6). In consequence, particles of Laves
phase were smaller (see Fig. 6b), easily distinguished in the BSE/SEM
image by their characteristic shapes with concave boundaries (see
Fig. 6). The eutectic (Nb,Ti)C carbides became smaller as well.
Hardness of the specimens in as-built condition is given in Table 7.
The obtained range from 314 to 326 HV0.5 is consistent with that pre­
sented e.g., by Holland et al. [39] and Fayed et al. [40], and in the re­
view paper [14]. This hardness is higher than that within 150–250 HV
generally obtained for the solution annealed condition and lower than
that within 400–500 HV obtained for the aged condition. It suggests that
strengthening of the alloy in as-built condition, measured by its hardness
K. Gruber et al. Materials Science & Engineering A 813 (2021) 141111

Fig. 4. Thermal histories of two variants (H1 and H2) of post-processing heat treatment (a), and of HIP process (b).

respectively 32 and 14%. It results in higher yield strength but lower

Table 5
elongation in comparison to solutioned state of the alloy, and in lower
Displacement wz of free ends of the LPBF cantilever specimens depending on
yield strength but higher elongation in comparison to its aged state [29].
their orientation in respect to x and y axes, after cutting-off from the platform.
Because of fine particle size and low volumetric fraction of the Laves
Condition Orientation of cantilever specimen in respect to x axis (recoater phase and carbides in the as-built microstructure, neither peaks from
direction)
them nor those coming from the δ phase were recorded on the XRD
0◦ 90◦ A-45◦ B-45◦ diffractograms (Fig. 8). The difference between the intensity ratios I200/
a
Displacement wz [mm] I111 (Table 8) for the as-built condition and for the powder sample with
As-builta 3.24 ± 0.14 3.35 ± 0.15 3.33 ± 0.04 3.30 ± 0.06 random orientation of grains indicates a weak texture, i.e., a slightly
SR1150 0.00 0.00 0.02 0.00 larger part of grains with their (002) planes parallel to xz surface of the
SR1065 − 0.07 0.04 0.00 0.07 specimen in the y direction. The relatively weak alignment of [002] with
a
Average value for three specimens. the y direction is also confirmed by the fact that red color does not
prevail on the inverse pole figures (IPF) maps shown in Fig. 9a.
Weak texture of the γ phase results from the accepted scanning
increase, is caused by the dislocation network inside the columnar
strategy (short scanning vectors in connection with their rotation on the
grains, accompanied by intercellular microsegregation of Nb, Ti and Mo,
subsequent scanning planes) and from the fact that the dendritic cells
as well as by presence of the Laves and δ phases. As can be seen in Fig. 7,
grow in the direction of the laser beam movement. This explains the
the number fraction of VLAGBs and LAGBs with dislocation structure is
reason why no differences were found between relative intensities

6
K. Gruber et al. Materials Science & Engineering A 813 (2021) 141111

Fig. 5. CLSM micrographs of LPBF IN718 in as-built condition: a) columnar grains traversing solute banding lines that outline of tracks (arrow), b) visible array of
intersecting tracks separated by solute-rich bands (arrow).

Fig. 6. BSD/SEM images of microstructure in as-built condition (xz plane): a) arrays of parallel dendritic cells inside columnar grains; red arrows show solute
banding lines, b) particles of eutectic Laves phase in spaces between dendritic cells (yellow arrows) and primary carbides (white arrows). (For interpretation of the
references to color in this figure legend, the reader is referred to the Web version of this article.)

Fig. 7. Distribution of misorientation angles of grain boundaries for the specimens in as-built, SR1150, and SR1060 condition (EBSD analysis).

7
K. Gruber et al. Materials Science & Engineering A 813 (2021) 141111

Table 6 parameters do not guarantee that deformation of thin-walled parts

Average values of partition coefficients of solute elements for the IN718 alloy would be avoided in furnaces with other cooling-down characteristics
[38]. than those applied in this work (Fig. 4a and b).
Element Nb Ti Mo Al Ni Fe Cr Si Microstructures of IN718 after relieving SR1150 and SR1065 are
k 0.50 0.67 0.82 0.95 1.00 1.06 1.11 1.58
shown in Fig. 10. As can be seen in Fig. 10a,c and in the EBSD orien­
tation map in Fig. 9b, an increase in the annealing temperature and time
resulted in almost complete recrystallization and homogenization of the
alloy. This is also confirmed (see Fig. 7) by a drastic drop (from 32% to
Table 7
~ 2%) in the VLAGBs number fraction and an increase (from 3% to 62%)
Hardness measurements of specimens in as-built condition and after subsequent
post-processing steps.
in a fraction of coherent twin boundaries Σ3 characterized by 60◦
misorientation around <111> directions [43].
Condition Hardness HV0.5
After relief-annealing SR1065, a significant part of non-recrystallized
xz plane xy plane Average grains with maintained intercellular microsegregation was left (Fig. 10b,
As-built 326 ± 12 314 ± 15 320 d). This is evidenced by a small increase (from 3% to 12%) in the twin
SR1150 424 ±9 419 ± 13 422 boundaries fraction and a small decrease (from 32% to 24%) in the
SR1065 412 ±4 417 ± 8 414 VLAGBs fraction (Fig. 7). These results are consistent with the distortion
SR1150 + SA1100 198 ±8 197 9 198
measurements shown in Section 3.1 and with the residual strain mea­
±
SR1065 + SA1065 247 ±8 245 ± 3 246
SR1150 + HIP 378 ±9 355 ± 9 367 surements presented by Cao et al. [26]. They indicate that the recovery
SR1065 + HIP 380 ± 13 371 ± 11 376 process preceding recrystallization is slow at 1065 ◦ C, since coalescence
SR1150 + HIP + SA1100 190 ±7 191 ± 5 191 of dendritic cells is impeded by slow back-diffusion of Nb, Ti and Mo in
SR1065 + HIP + SA1065 204 ±5 201 ± 7 203 γ-phase, which slows down dissolution of the Laves phase [44]. There­
fore, homogenization temperature of LPBF IN718 should be higher than
obtained from the xy planes (perpendicular to the build direction) and 1100 ◦ C.
powder samples in the case of using similar process parameters [30]. After relieving SR1150, all secondary phases except equilibrium
primary carbides (Nb,Ti)C were completely dissolved (Fig. 10a,c). They
are clearly coarser in comparison to those in the as-built condition. Their
3.4. Microstructure and hardness after stress relieving arrangement along high-angle grain boundaries and former sub-
boundaries indicates that they are primary carbides whose growth is
In order to avoid deformations of the geometrically complex part possible due to diffusion of niobium from the dissolving Laves phase
fabricated by LPBF during its removing from the build platform, this particles. This is confirmed by the presence of titanium in the (Nb,Ti)C
operation must be preceded by stress-relief annealing. However,
importance of proper selection of these annealing parameters is under­
Table 8
estimated in the related literature. The relief-annealing parameters
Intensity ratios of diffraction lines for Bragg-Brentano geometry (penetration
cannot be directly carried-over from the relieving practice of castings or
depth > 10 μm).
forgings, since the different distribution of residual stresses and specific
Specimen, condition I200/I111 I220/I111 I311/I111 I222/I111
microstructure of LPBF-ed parts (microsegregation, dislocation structure
and texture) necessitate corrections of annealing temperature and time, Standard γ-Ni (table) 0.32 0.14 0.09 0.03
as well as of heating and cooling rates [27,41,42]. This is considered by Powder 0.33 0.14 0.26 0.07
As-built 0.95 0.14 0.18 0.05
the ASTM standard that, for LPBF-ed IN718 parts, recommends SR1150 0.31 0.27 0.11 0.08
stress-relief annealing at 1065 ◦ C with no special recommendation for SR1150 + SA1100 0.19 0.11 0.11 0.06
the cooling medium. However, the distortion measurements given in H1 0.19 0.20 0.11 0.05
Section 3.1 showed that, in spite of very slow furnace cooling, the above

Fig. 8. XRD patterns for IN718 powder and LPBF fabricated specimens in as-built state and after different steps of post-processing heat treatment (variant H1),
obtained for xz plane.

8
K. Gruber et al. Materials Science & Engineering A 813 (2021) 141111

Fig. 9. The EBSD orientation maps (IPF) of LPBF-ed specimens in conditions: a) as-built, b) SR1150, c) SR1065.

Fig. 10. Microstructures of the LPBF IN718 after stress relieving: a) and c) – SR1150; b) and d) – SR1065. Yellow arrows: not recrystallized grains, red arrows:
recrystallized grains, black arrows: twin boundaries, green arrows: places prone to liquation (CLSM images). (For interpretation of the references to color in this
figure legend, the reader is referred to the Web version of this article.)

carbides, found by EDS analysis, see Fig. 11. Volumetric fraction of
carbides equal to (0.55 ± 0.1)%, determined by image analysis, is
consistent with the fractions of carbides in equilibrium state, determined
for IN718 according to the CALPHAD model [45]. The presence of
coarse carbides is also confirmed by appearance of additional peak in the
diffraction pattern obtained for IN718 after SR1150 treatment (Fig. 8).
The average grain size of the γ-phase after SR1150 amounted to (95
± 14) μm. Considering high stability of the alloy grain size during
annealing at 1180 ◦ C for 1 h–12 h found by Zhao et al. [45], remaining
within (130 ± 50) μm, it can be concluded that the 6-h annealing time

9
K. Gruber et al.
Fig. 11. EDS/SEM analysis of the areas containing bright (visible in Fig. 10a,c)
differing with the particle shape. SR1150; xz plane.
accepted in this work did not influence the grain growth. However, the
suggested stress-relieving parameters gave similar results of homoge­
nization as those obtained in Ref. [45], but with maintained smaller
grain size.
After SR1150, the high number fraction equal to 62% of twin
boundaries in comparison to 25% after hot rolling [46] suggests that the
main role of twinning during stress-relief annealing is supporting the
recrystallization process. This means that, when the driving force is
insufficient for quick migration of the HAGBs, reduction of total grain
boundary energy overcomes increase of total surface of grain boundaries
by creating twin boundaries whose energy is ~20 times smaller than the
ordinary HAGB energy in nickel [47]. This is possible due to low
stacking fault energy of nickel.
Hardness of as-built IN718 amounts to 320 HV0.5 (Table 7), which
corresponds to hardness of the wrought alloy subjected to solution
treatment followed by 30–35% cold working [48]. So, it can be recog­
nized that average dislocation density in LPBF-ed IN718 in as-built
strain hardened condition must be high at about (0.8–2.4)⋅1014 m− 2
[29], in comparison to typical density in the annealed state ~1011 m− 2
and that in the heavily deformed state ~10− 16 m− 2 [47]. In spite of this
consistency, recrystallization of LPBF-ed IN718 requires higher tem­
perature, incubation time and completion time in comparison to
cold-worked IN718. As it was mentioned before, the reason is slow
dissolution of phases and slow back-diffusion of Nb, Ti and Mo
hampering migration of grain boundaries. The not deformed HAGBs of
γ-phase in the LPBF-ed alloy with their energy lowered by solute atoms
Fig. 12. Hardness of LPBF-ed IN718 depending on cooling rate from a temperature between 1065 and 1150 ◦ C–500 ◦ C in relation to hardness of hot-extruded alloy
homogenized at 1100 ◦ C for 1 h. Developed on the grounds of the results of Geng et al. [49] (black points).
10
Materials Science & Engineering A 813 (2021) 141111
and pinned by undissolved particles migrate much more slowly than the
more densely distributed deformation-induced HAGBs in deformed
γ-phase.
Results of hardness measurements taken between individual heat
treatment steps are given in Table 7. In spite of the significantly different
annealing parameters, the stress-relieved specimens showed similar in­
crease of hardness in relation to that in as-built condition. This indicates
that hardness of the alloy is mostly influenced by dispersion degree of
strengthening phases γ’’/γ′ , determined by cooling rate.
As can be seen from the relationship in Fig. 12, determined experi­
mentally by Geng et al. [49], peak hardness of 410 HV0.5 corresponds to
cooling rate 5 ◦ C/min. The furnace cooling from 1150 ◦ C or 1065 ◦ C
down to 500 ◦ C, used in this research, corresponds to cooling rate of
6 ◦ C/min and 6.3 ◦ C/min, respectively. This means that slow
cooling-down with the furnace, advantageous from the stress-relieving
viewpoint, results in high hardness of the alloy, unfavorable for its
machinability and ability to obtain an acceptable surface finish. Course
of the hardness curve in Fig. 12 suggests that, in order to obtain the
favorable for machinability hardness below 320 HV0.5 [50], cooling
rate after stress-relief annealing should be higher than 23 ◦ C/min (as
marked with the yellow dashed line). Such cooling of a part with com­
plex geometry and low thermal conductivity of IN718 (8.9–28.3 W/m⋅K
within 25–1100 ◦ C [18]) can result in its deformation during cutting-off
from the platform, caused by residual stresses.
Therefore, in the case of manufacturing a part with complex geom­
etry, the only solution to avoid its deformation is furnace cooling before
removing from the platform, and next: cutting-off from the platform,
solution treatment preceded by HIP or not, surface finishing and ageing.
3.5. The stress relief, solution annealed and double aged condition
Solution annealing treatment SA1100 decreased the alloy hardness
down to 238 HV0.5 in relation to 422 HV0.5 after SR1150 (see Table 7).
In the diffractogram (Fig. 8) obtained for SR1150 + SA1100, the peaks
from carbides and δ phase disappeared. This indicates that most of the
small size carbides were dissolved (following the rule of Ostwald
ripening) and the growing carbides particles could not be detected by
XRD. The remaining coarsened primary carbides type (Nb,Ti)C and
sparse titanium carbonitrides solidified on aluminum nitrides or oxides
are shown in Fig. 13. Widening of the peaks from γ phase for the solu­
tioned and solutioned + aged conditions on the diffractograms is caused
by increased Nb concentration in solid solution as a result of dissolution
K. Gruber et al.
of γ′ and γ’’ phases precipitated during furnace cooling after stress-
annealing, as well as of partial dissolution of carbides. Solution
annealing SA1065 following after SR1065 reduced the hardness from
414 HV0.5 (Table 7) to 260 HV0.5.
During the solution treatments SA1100 and SA1065, apart from
dissolution of secondary phases, local changes occurred in micro-areas
at grain boundaries, marked by arrows in Fig. 14a,c. These changes, in
form of colonies of fine-grained eutectic mixture (Fig. 14c, black arrows)
and thin layer-shaped phase between grain boundaries of solid solution γ
(black arrows), appeared after solution annealing at 1065 ◦ C. In the case
of solution annealing at 1100 ◦ C, small intensity thin layer-shaped phase
(Fig. 14a) was only found.
Considering the researches [51,52] on the mechanism of intergran­
ular liquation in wrought and cast IN718, it is well grounded to state that
the observed microstructure changes are results of local formation of
liquid film on grains boundaries during heating-up and its solidification
during cooling-down the alloy. According to Radhakrishnan and
Thompson [51], liquid is formed by constitutional liquation of NbC
during rapid heating at temperatures above that of the pseudo-ternary
eutectic (γ + NbC + Laves) but below that of the equilibrium transi­
tion (γ + NbC ~ L + γ + NbC) for nominal composition of IN718.
Constitutional liquation may occur by partial or complete dissolution of
carbides during rapid heating-up to the pseudo-ternary eutectic tem­
perature and subsequent liquation of the solute enriched regions. If
carbide particles are located on the γ-phase grain boundary, the liquid
can spread along this boundary [52].
In the presented research, the as-built specimens were heated-up
during stress-relieving very slowly at 3.8 ◦ C/min and 3.5 ◦ C/min to
1150 ◦ C and 1065 ◦ C, respectively, and next held isothermally for 6 h
and 1.5 h. Thus, according to expectations, microstructure of the stress-
relieved specimens was free from liquation and resolidification traces
(see Fig. 10). However, during solution treatment, heating rate was
increased to 18 ◦ C/min and the soaking time was reduced to 1 h. Even if
the used parameters cannot be regarded as rapid heating and very short
soaking time, the grain boundary liquation still occurred. This indicates
a basic influence of distribution and diffusion of niobium (volume and
grain boundary diffusion) on phase transformations during heating-up
the IN718 alloy. Because of low Nb diffusion coefficient in γ matrix
(6.6 10− 11 cm2/s at 1140 ◦ C [53]), places conducive to local melting by
constitutional liquation during solution reheating remained after stress
relieving in both kinds of microstructures (Fig. 10). In the microstruc­
tures relieved at 1150 ◦ C they are (indicated by green arrows in Fig. 10a,
c) mobile interfaces between residual non-recrystallized and recrystal­
lized grains. They are enriched in niobium, since during annealing at so
high temperature only diffusion of Nb atoms (coming from the dis­
solving Nb-rich phases) along the grain boundaries (much faster than
volume diffusion) could induce migration of grain boundaries away
from their curvature centers [54]. In the case of relieving at 1065 ◦ C,
they are places with high concentration of carbides and strengthening
phases γ’/γ’’ nearby and on grain boundaries (pointed in Fig. 10b,d with
green arrows), left after incomplete homogenization of the alloy. In
Fig. 13. EDS/SEM analysis of the area containing particles with two charac­
teristic shapes. The IN718 alloy in the SR1150 + SA 1100 condition; xz plane.
11
Materials Science & Engineering A 813 (2021) 141111
these places susceptible to local melting during heating-up, the
remaining liquid could reach chemical composition close to the pseu­
doternary eutectic.
From the viewpoint of mechanical properties, “scars” left by liqua­
tion and resolidification at grain boundaries can reduce ductility of the
alloy. Constitutional liquation can result in intergranular microcracks
and voids in vicinity of the coarse carbide particles and, in our opinion,
these cracks and voids are responsible for a significant loss of ductility of
LPBF IN718 reported by Fayed et al. [22]. So, it was found appropriate
to supplement stress relieving with the HIP operation, whose combined
action of high pressure and high temperature should not only reduce
porosity, but also eliminate microstructure non-homogeneities left after
relieving, susceptible to liquation during heating-up. The applied HIP
parameters were 1150 ◦ C/100 MPa for 4 h, according to Tillmann et al.
[55] the most effective in closing all the internal material discontinuities
except pores filled with argon. In the HIP process, slow furnace cooling
at 10.2 ◦ C/min to 500 ◦ C resulted in hardness higher than 350 HV0.5
(see Table 7) and much higher than that obtained by Aydinӧz et al. [32]
and Tillmann et al. [55] for HIP-ed and freely furnace-cooled specimens,
amounted to i.e., 259 HV0.1, 230 HV1. This is connected with the steep
drop of the hardness curve in Fig. 12 in the range of cooling rate between
6 and 60 ◦ C/min, as confirmed by Zhao et al. [56]. Further, it motivates
acceptation of the following sequence of post-process heat-treatment
and finishing operations: stress relieving, HIP, solution annealing, sur­
face machining and aging.
Microstructure of the alloy after heat-treatment followed by HIP is
shown in Fig. 14b for the variant H1+HIP and in Fig. 14d for the variant
H2+HIP. Including HIP in both heat-treatment variants caused complete
homogenization of microstructure and made them identical with regard
to grain size of the matrix, as well as to quantity and arrangement of
carbide particles. No places indicating liquation of grain boundaries
were found, like those occurred during solution annealing. Insofar as
microstructure changes caused by HIP are unnoticeable in the H1+HIP
variant, the changes in the H2+HIP variant are significant because of
recrystallization and homogenization of the alloy.
3.6. Tensile test results
Tensile test was carried-out at room temperature, as well as at 425 ◦ C
and 650 ◦ C, using specimens in four states of post-build heat treatment.
Results are given in Table 9. Considering the results at ambient tem­
perature, in comparison to those in the H2 state, the specimens in the H1
state show 6% higher yield stress, increased YS/UTS ratio, 48% lower
elongation and 30% lower area reduction. These differences are results
of non-recrystallized H2 microstructure with maintained residual
microsegregation after solution annealing (Figs. 14c) and 12% higher
effectiveness of precipitation strengthening by the γ’/γ’’ phases. Higher
hardness for the H2 state, amounting to (497 ± 31) HV0.5 on the xy
plane and (479 ± 17) HV0.5) on the xz plane, is grounded by higher
concentration of niobium dissolved in the γ matrix at the solution
annealing temperature due to small amount of NbC carbides and
maintained large portion of low-angle grain boundaries. Application of
HIP results in microstructure recrystallization and homogenization
(Fig. 14d), thus equalizing its parameters like grain size, distribution of
grain misorientation, amount of carbides and hardness with those of the
conditions H1 and H1+HIP, as is shown in Table 9.
The tensile properties for the H1 and H1+HIP states, determined at
room temperature are very similar (Table 9). This is unsurprising,
considering that these properties are influenced by the factors like
identical stress-relief annealing parameters, nearly zero porosity of the
specimens and high toughness of the alloy decreasing material suscep­
tibility to brittle cracking initiated on the build defects type lack of
fusion or gas pores. Similar behavior of the specimens is also maintained
in the tensile test at 425 ◦ C (Table 9), i.e., about 10% lower Young’s
modulus, as well as 12% and 18% lower respectively YS and UTS, at
statistically insignificant changes of plastic properties.
K. Gruber et al. Materials Science & Engineering A 813 (2021) 141111

Fig. 14. SEM images of IN718 microstructure after heat treatment variants: a) SR1150 + SA1100, b) SR1150 + HIP + SA1100 + DA (H1+HIP), c) SR1065+ SA1065,
d) SR1065 + HIP + SA1065 + DA (H2+HIP).

Table 9
Tensile test results.
Temperature Heat treatment variant Young’s modulus Yield strength YS 0.2% Tensile strength UTS Permanent elongation Reduction of area YS/UTS
◦
C A4 Z

GPa MPa MPa % % %

RT H1 208 ± 10 1142 ± 26 1388 ± 10 24.8 ± 2.3 36.5 ± 5.8 0.82

H2 200 ± 10 1206 ± 10 1364 ± 28 12.8 ± 2.6 25.7 ± 5.7 0.88
H1+HIP 202 ±6 1143 ± 10 1391 ± 10 24.9 ± 2.2 36.8 ± 5.8 0.82
425 H1 194 ± 20 993 ± 17 1160 ± 10 23.6 ± 5.8 39.5 ± 4.1 0.86
H1+HIP 172 ±9 1014 ± 4 1170 ± 10 23.6 ± 5.8 39.5 ± 4.1 0.87
650 H1+HIP 161 ±4 881 ± 42 1057 ± 25 24.5 ± 4.7 25.1 ± 5.0 0.83
H2+HIP 163 ± 20 857 ± 17 1052 ± 10 27.6 ± 5.8 26.2 ± 4.1 0.81

The above results inspired the authors to carry out tensile tests at the
Table 10
IN718 ceiling temperature of 650 ◦ C, above that the main strengthening
Grain size, carbides fraction, and hardness of LPBF-ed IN718 in different post-
phase γ′′ rapidly overages [57]. For comparison, both specimens in the
processing heat treatment condition.
H1+HIP and H2+HIP states were subjected to tensile tests at this tem­
perature. It was found for the H1+HIP specimens that tensile strength Heat treatment variant

decreased by ~20% in comparison to the value at room temperature, but H1 H1+HIP H2+HIP
area reduction decreased by 36%, which guaranteed more uniform Average grain diameter d and ASTM grain size number G*
elongation of the tested specimens. It can be noticed that the tensile
Plane d [μm] G d [μm] G d [μm] G
properties at 650 ◦ C after post-processing heat treatment H1+HIP and
H2+HIP are identical. This means that, by its recrystallizing and ho­ xz 104 ± 17 3.6 ± 0.5 90 ± 7 4.0 ± 0,2 92 ± 19 4.0 ± 0.6
xy 86 ± 11 4.1 ± 0.4 77 ± 7 4.4 ± 0.2 75 ± 7 4.5 ± 0.3
mogenizing action, HIP causes that the solution treatments at 1100 ◦ C *G = (6.643856 log10 l) - 3.288; l – intercept length (twin boundaries Σ3 not
and 1065 ◦ C, followed by air cooling, give identical effect after ageing, considered)
measured by increased hardness and volumetric fraction of undissolved Volumetric fraction of carbides [%]
carbides NbC and (Nb,Ti)C (see Table 10). xz 0.5 ± 0.2 0.5 ± 0.2 0.5 ± 0.2
xy 0.5 ± 0.2 0.6 ± 0.2 0.6 ± 0.1
So, the conclusion raises that microstructure evolution during heat
Hardness HV10
treatment steps (H1+HIP and H2+HIP) is strongly dominated by high- xz 438 ± 29 436 ± 33 438 ± 30
temperature HIP treatment and thus the preceding stress relieving xy 427 ± 31 434 ± 20 435 ± 26
does not affect it significantly. Exclusion of HIP makes this effect very (Hardness H2 variant: xz plane: 479 ± 17 HV0.5; xy plane: 497 ± 11 HV0.5)
strong. However, it does not change the fact that, in the case of complex-
shaped parts, selection of stress-relief annealing parameters to prevent
distortion during removing from the build platform is crucial,

12
K. Gruber et al.
irrespective whether HIP will be employed or not.
The data in Table 10 indicate that the high-temperature stress-
relieving and HIP processes lead to coarse-grained microstructures
(Fig. 15) with ASTM grain size between 3.6 and 4.5 (average grain di­
ameters d = 75–104 μm). As it was reported by Liu et al. [58], the IN718
yield strength and flow stress for a given strain decrease with increasing
grain size, while the effect of grain size on Young’s modulus is negli­
gible. However, this effect is quantitatively consistent with the tensile
curves empirically determined for the solution-annealed state only.
According to the Hall-Petch equation (σy = 325 MPa + 750 MPa
μm0.5⋅d− 0.5) for d = 75–104 μm, the σy value ranges between 412 and
399 MPa. In the aged condition, precipitation strengthening dominates
the grain-boundary strengthening to the extent dependent on quantity of
niobium dissolved in solid solution γ, i.e., on effectiveness of supersat­
uration. In the as-built and the non-recrystallized conditions (Fig. 9a,c),
when the grain aspect ratio is about 0.2 and dislocation density is high
[29] due to high fraction of low-angle grain boundaries of dislocations
cell (Fig. 7a,c), the Hall-Petch equation gives understated values. This
makes it difficult to compare the results obtained in the presented
research with those reported in the related literature. It is also confusing
to use the notion of grain size measured using different microscopy and
EBSD techniques which can include in the evaluation of grain diameters
both low-angle grain boundaries as well as twin boundaries [46,59].
Considering the above, the tensile test results obtained in this
research are shown in Fig. 16 in comparison to the tension curves
showing the influence of both grain size and testing temperature on the
nominal tensile strength of wrought IN718 [16]. As can be seen in this
figure, the obtained results are more consistent with the curve corre­
sponding to the solution-treated and aged condition with grain size
ASTM 8 than with grain size ASTM 4–6.
On one hand, an advantage of the recrystallized microstructure ob­
tained after each of the three heat-treatment variants is missing δ-phase
and high homogenization degree of chemical composition. On the other
hand, the large fraction of coherent thin boundaries can significantly
affect fatigue properties of LPBF-ed IN718, since the regions close to Σ3
twin boundaries in subsurface grains are privileged sites for location of
cyclic strain and initiation of fatigue cracks [62]. From the grain
boundary engineering viewpoint however, by improving distribution
and connectivity of these special boundaries [39], a chance exists to
improve some properties of the LPBF IN718 alloy, like resistance to
intercrystalline and stress corrosion at elevated temperatures [63].
4. Conclusions
The examinations presented in this paper facilitated complex eval­
uation of the multi-operation, additive manufacturing process of IN718
parts by LPBF, which includes building the parts on a platform and the
multistage post-processing heat treatment. A new approach, in relation
to those presented in the subject literature, was the assumption that, in
Fig. 15. Light microscope images of IN718 microstructure after heat treatment variants: a) H1; grain size ASTM 3.5–4, b) H1+HIP; ASTM 4–4.4; H2+HIP;
ASTM 4–4.5.
13
Materials Science & Engineering A 813 (2021) 141111
manufacture of parts with complex geometry and required high
dimensional accuracy, the main strategy criterion is mitigation of
distortion during the process and complete elimination of macro- and
micro-residual stresses during high-temperature stress-relief annealing
before removing the parts from the platform.
It was found that application of higher temperature than the
recrystallization temperature in the first operation of post-processing
heat treatment significantly affects results of the following heat-
treatment steps. In addition, the effect of heating and cooling rates
during individual heat-treatment steps on dissolution and precipitation
of phases was explained.
The conclusions are as follows:
1. In spite of application of the LPBF parameters strongly reducing
thermal stresses and distortion (i.e., preheating of build platform,
low heat input, short vector and hatch rotation strategy), the residual
tensile stresses estimated in cantilever specimen tests reached or 1.6
times exceeded the yield strength reported in the literature for hor­
izontal and vertical specimens in the as-built condition. The sug­
gested high-temperature stress relieving at 1150 ◦ C for 6 h at cooling
rate 6 ◦ C/min to 500 ◦ C reduced the macro- and micro-residual
stresses completely, while the standard stress relieving at 1065 ◦ C
for 1.5 h at the same cooling rate reduced almost completely the
macro-stress only.
2. In manufacture of complex IN718 parts with high dimensional ac­
curacy, it is advised to carry out effective stress relieving prior to
removing parts from the build platform. The SR1150 variant is more
effective than the SR1065 variant, since it generates a recrystallized,
stable and isotropic microstructure. Whereas the SR1065 variant
leaves microstructure non-recrystallized with maintained cellular
dislocation structure inside columnar grains. Slow cooling results in
hardness above 400 HV0.5 that must be considered at scheduling the
sequence of successive operations, including the surface finishing
operation.
3. After SR1150 treatment, IN718 microstructure is free from solute
microsegregation as well as from δ and Laves phases, but non-
homogeneous due to grain boundary diffusion of Nb that accom­
panies coarsening of carbides. Carbides at grain boundaries and
enrichment of grain boundaries in Nb induce liquid film formation
on grains boundaries, while heating rate during SA1150 is higher
than 18 ◦ C/min. Microstructure after SR1065 is free from δ and Laves
phases, but with maintained strong solute microsegregation, espe­
cially at columnar grain boundaries and track interfaces. For this
reason, the microstructure is susceptible to liquation during SA1065
carried-out with too high heating rate. Both colonies of fine-grained
eutectic mixture and the thin layer-shaped phase along grain
boundaries are a result of liquation and influence tensile properties
after final aging. Effectiveness of solution annealing evaluated on the
grounds of hardness is smaller from that possible to be reached for
K. Gruber et al.
Fig. 16. Tensile strength at ambient and elevated temperature of LPBF-ed IN718 after different post-processing heat treatment (i.e. recrystallized and aged) [59–61]
in comparison to relationships between nominal tensile strength of wrought IN718 and temperature and grain size (curves elaborated on the ground of [16]).
IN718 (i.e., when hardness is lower than 200 HV0.5) in the case of
SA1150 and much smaller in the case of SA1065.
4. After complete post-processing heat treatment (without HIP), tensile
properties of the specimens in H1 state were different from those of
the specimens in H2 state by 6% lower yield strength, lower YS/UTS
ratio, 48% higher elongation and 30% higher area reduction.
5. HIP treatment applied between the SR and the SA treatments caused
recrystallization of microstructure and thus its parameters (grain
size, distribution of grain misorientation, amount of carbides and
hardness) became identical for different SR and SA temperatures.
After cooling-down at the rate 10.2 ◦ C/min, hardness of the alloy
reached over 350 HV0.5, so it had to be followed by the SA treatment
to dissolve the phases γ’/γ’’ before aging and to improve machin­
ability. As a result, application of the sequence SR1150 + HIP +
S1100 and SR1065 + HIP + S1065 reduced hardness below 200
HV0.5 in both variants.
6. Even if the high-temperature SR and HIP treatments result in coarse-
grained microstructures with ASTM grain size between 3.6 and 4.5,
tensile strength values determined at room temperature, 425 ◦ C, and
650 ◦ C are closer to the nominal tensile strength values of wrought
IN718 in solution treated and aged conditions with grain size ASTM 8
than with ASTM 4–6 and much higher than those of cast and HIP-ped
IN718 alloy.
7. Microstructure evolution during post-processing heat treatment
steps (H1+HIP and H2+HIP) is strongly dominated by HIP treatment
and thus variants of both prior stress relieving and post solution
treatment finally lead to similar microstructures, hardness and ten­
sile properties, comparable with those after the heat treatment
variant H1. When HIP is designed in heat treatment schedule, the
high-temperature stress relieving can be employed to avoid distor­
tion of parts after removing from the platform with no risk of
worsening the final properties.
CRediT authorship contribution statement
Konrad Gruber: Conceptualization, Visualization, Formal analysis,
Writing – original draft. Robert Dziedzic: Methodology, Data curation,
Writing – review & editing. Bogumiła Kuźnicka: Supervision, Writing –
review & editing. Bartosz Madejski: Investigation, Resources. Maciej
Malicki: Investigation, Resources.
Declaration of competing interest
The authors declare that they have no known competing financial
14
Materials Science & Engineering A 813 (2021) 141111
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
This work was supported by the National Centre for Research and
Development in Poland (Grant No. TECHMATSTRATEG1/347514/7/
NCBR/2017).
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