Materials and Design 198 (2021) 109228

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Materials and Design

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

A recrystallization heat-treatment to reduce deformation anisotropy of

additively manufactured Inconel 718
Nadia Kouraytem a,⁎, John Varga b, Behnam Amin-Ahmadi c, Hadi Mirmohammad b, Raphaël A. Chanut b,
Ashley D. Spear b, Owen T. Kingstedt b
a
Department of Mechanical and Aerospace Engineering, Utah State University, Logan, UT, USA
b
Department of Mechanical Engineering, University of Utah, Salt Lake City, UT, USA
c
Department of Mechanical Engineering, Colorado School of Mines, Golden, CO, USA

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

• Solutionizing heat-treatment is pro-

posed to decrease anisotropy in AM
IN718.
• Solutionizing heat-treatment resulted
in a higher yield strength compared to
as-built.
• Microscopy reveals the growth of hard-
ening nano-precipitates in the gamma
matrix.
• Findings will help provide a pathway of
transitioning AM from the lab to
industry.

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

Article history: The aim of the current study is to investigate the suitability of a solutionizing recrystallization (RC) heat-
Received 30 April 2020 treatment to improve the yield strength of laser powder-bed fusion (L-PBF) Inconel 718 (IN718), while decreas-
Received in revised form 26 August 2020 ing deformation anisotropy under uniaxial compression. Scanning electron microscopy measurements show an
Accepted 9 October 2020
increase in grain size, decrease in texture, and the formation of twins in the RC compared to the as-built (AB) and
Available online 15 October 2020
direct-age (DA) hardened conditions. Transmission electron microscopy measurements of the RC condition re-
Keywords:
vealed the formation of nano-precipitates in the gamma matrix. As a result, the compressive stress-strain behav-
Inconel 718 ior showed an increase in the yield strength of the RC specimens compared to the AB condition in the quasi-static
Microstructure and high-strain rate regimes despite having significantly larger grain sizes. Post-mortem in-plane ellipticity mea-
Heat-treatment surements show a statistically significant decrease in the deformation anisotropy of the RC specimens compared
Laser powder bed fusion to the AB and DA conditions. Overall, the solutionizing RC heat-treatment, when compared to the AB condition,
Split-Hopkinson pressure bar resulted in an increase in yield strength and decrease in deformation anisotropy, two desirable outcomes neces-
Compression sary to continue to provide path-ways to transitioning L-PBF parts from the research laboratory setting to com-
mercial implementation.
Crown Copyright © 2020 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction

Inconel 718 (IN718) is a precipitation-hardened nickel-based super

⁎ Corresponding author.
alloy. It has been widely adopted as a structural material in extreme ap-
E-mail addresses: nadia.kouraytem@usu.edu, nadia.kouraytem@utah.edu plications such as jet engines and space exploration due to its favorable
(N. Kouraytem). corrosion resistance and high strength at elevated temperatures

https://doi.org/10.1016/j.matdes.2020.109228
0264-1275/Crown Copyright © 2020 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al.
(>700 °C). In additive manufacturing research, IN718 has become a pre-
eminent alloy because of its exceptional weldability. IN718 owes its de-
sirable mechanical properties to precipitated phases distributed
throughout its microstructure. The predominant strengthening phases
in IN718 are the Ni3Nb body centered tetragonal γ′′ precipitateand the
Ni3(Al,Ti) face centered cubic (fcc) γ′ precipitate [1–3]. The γ′′ precipi-
tate is meta-stable, transforming to the stable Ni3Nb orthorhombic δ
phase over prolonged periods at elevated temperatures. The δ phase,
when properly distributed at grain boundaries, has been shown to re-
strict grain growth and improve resistance to grain boundary creep frac-
ture [4,5]. The commonly observed (Ni,Fe,Cr)2(Nb,Mo,Ti) Laves phase
occurs because of the poor diffusibility of Nb, and is easily formed due
to the segregated microstructures found in AM [6]. The Laves phase is
generally characterized as a brittle inter-metallic phase in the inter-
dendritic region that forms by segregation during solidification. The
presence of Laves phase is usually a favorable site for the initiation of
cracks and propagation which is found to detrimentally affect tensile
strength, fracture toughness, fatigue, and elongation by serving as
crack initiation sites during deformation. However, Sui et al. [7], re-
ported that small granular Laves phase improved yield strength by
impacting the γ′′ volume fraction, size, and precipitate distribution.
A wide range of post-build heat treatments have been developed
and applied to additively manufactured (AM) IN718 to tailor mechani-
cal behavior with objectives of manipulating phase precipitation
(e.g., [7–10]), controlling the presence of dislocation cells generated
during the build process (e.g., [11–13]), and altering grain size
(e.g., [14,15]). The most widely used two-steps heat treatments are
composed of a solutionizing step followed by a precipitation hardening
step. The temperature of the solid solutionizing step is chosen to be
above the solvus temperature of a certain phase that is not desired
(e.g., the Laves phase) and long enough to dissolve it, followed by a cer-
tain double-aging temperature to grow the desired phases to harden
the material (γ′ and γ′′). Sometimes this combination is referred to as
the solution treated and aged (STA). In the literature, STA temperatures
have been chosen between 970 °C and 1200 °C with a hold time of few
hours, and the aging temperature is set between 704 °C and 899 °C for
the first step then a lower temperature between 593 °C and 704 °C, as
reported by Tucho and Hansen [16].
Standardized heat treatments consisting of an annealing step and
aging step, intended for traditionally produced IN718 (e.g., cast or
wrought), have been applied to AM IN718 to improve material yield
strength and tensile strength e.g., [10,17–19]. For example, Trosch
et al. [18] investigated the effect of part orientation and STA for both
forged, cast, and SLM samples. The SLM produced IN718 samples exhib-
ited tensile properties superior to forged or cast IN718 when tested at
room temperature, and comparable to forged IN718 at elevated temper-
atures. Values of the yield strength in traditionally manufactured, stan-
dard heat-treated IN718 are around 758 MPa and 1034 MPa for cast
material and wrought material, respectively. While improved proper-
ties can be achieved using these standardized heat treatment ap-
proaches, they have been shown to be incapable of achieving the
optimal yield strength of AM IN718. A recent effort reported by
Gallmeyer et al. [11] presented a comparison of the microstructures
and mechanical behavior of AM IN718 after applying both traditional
(i.e., annealing + double aging step) and unconventional heat-
treatments such as 720 °C for 24 h. A promising direct-age (DA) hard-
ening heat-treatment consisting of subjecting the as-built part to
720 °C for 24 h was presented. This heat-treatment was designed to
precipitate hardening phases (i.e., γ′′ and γ′) while concurrently main-
taining dislocation cells. The resulting quasi-static tensile yield strength
of the DA-hardened IN718 was doubled compared to the as-built (AB)
condition, with a trade-off of 50% reduction in ductility in the DA con-
dition compared to the AB condition (from around 20% strain to about
10% strain). The same DA hardening heat-treatment was proven effec-
tive by Kouraytem et al. [20] in doubling the yield strength when test-
ing AM IN718 under quasi-static and high-strain rate compression.
2
Materials and Design 198 (2021) 109228
A common feature of direct aging heat treatments are process
temperatures below 1100 °C. Remaining below 1100 °C prevents re-
crystallization, thus maintaining the as-built grain morphology and
texture. It is well established that the thermal gradient developed dur-
ing L-PBF and the favorable solidification direction of fcc materials re-
sults in a 〈100〉 fiber texture and columnar grains aligned closely to
the build direction [20–22]. The combination of an established fiber
texture and columnar grain morphology results in anisotropic defor-
mation behavior, as recently elucidated by Kouraytem et al. [20] and
others (e.g., [10,23,24]). Therefore, in the context of large L-PBF build
volumes, alternative heat treatments (e.g., recrystallization heat treat-
ments) are needed to simultaneously reduce deformation anisotropy
without negatively affecting the mechanical properties when com-
pared to the AB condition.
Multiple research efforts have focused on studying the effect of solu-
tion heat treatments applied to AM IN718 with process temperatures at
or above 1100 °C (e.g., [14–16,25,26]). Heat treatments at these temper-
atures have been shown to induce recrystallization of AM IN718 and to
dissolve segregated phases (e.g., δ or Laves) into solution [5]. The disso-
lution of segregated phases is necessary to release trapped Nb, Ti, and Al,
to enable precipitation of desirable strengthening γ′ and γ′′ precipitates
[9,27] and to dissolve the grain growth inhibiting δ phase [5]. Chlebus
et al. [15] performed a 1 h 1100 °C heat treatment on L-PBF IN718
which resulted in a recrystallization and homogenization of the γ solid
solution with carbides observed at grain boundaries. Tensile testing of
the solution heat-treated and aged alloy showed a 72–95% increase in
yield strength and 30–46% in ultimate tensile strength compared to
the as-built condition. Tucho et al. [14] studied the effect of hold time
in comparatively more aggressive solution heat-treatments, utilizing
process temperatures of 1100 and 1250 °C for 1 or 7 h. The microstruc-
tures observed for the 1100 °C for 1 h treatment suggested recrystalliza-
tion had initiated but had not occurred completely throughout the
microstructure, with more aggressive heat treatments resulting in in-
creased grain coarsening with near complete recrystallization and dis-
solution of segregated phases. In the same study, mechanical behavior
was investigated using Vickers hardness testing. A 15% reduction in
hardness was observed when comparing the heat-treated specimens
to the as-built condition, which suggests the applied recrystallization
heat treatment resulted in a reduction in strength. The studies of
Tucho et al. [14] and Chlebus et al. [15]) provide conflicting results of
whether or not solution heat treatments are suitable for improving
AM IN718 mechanical performance.
The investigation of the mechanical properties of AM IN718 or sim-
ilar alloys have been limited to the quasi-static [22,25,28,29], fatigue
[30,31], and creep [13,17,32] regimes. In the high-strain-rate regime,
Asala et al. [33] showed strain-rate sensitivity of the wire-arc ATI
718Plus alloy that has a similar composition as IN718. In the quasi-
static regime, some investigators have also compared the yield strength
of AM IN718 to that of traditionally manufactured IN718, i.e., casting
and forging [18,34]. While the aforementioned efforts have provided
valuable investigations toward improving targeted material properties,
typically yield strength, there is notable scarcity of studies investigating
the high-strain-rate behavior of AM IN718 and deformation anisotropy.
In this study, a solutionizing recrystallization heat treatment is stud-
ied with the objective of reducing deformation anisotropy while im-
proving material compressive properties (specifically yield strength in
both the quasi-static and dynamic high-strain-rate regimes), compared
to as-built L-PBF IN718.
2. Materials and methods
2.1. Specimen extraction and heat treatments
All specimens included in the current study, a total of 45, were
sourced from the same parent L-PBF IN718 block. The large L-PBF vol-
ume was printed on a Concept Laser M2 Cusing machine using
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al.
manufacturer recommended process parameters with core parameters
of 160 W laser power, 680 mm/s laser scan speed, and 53 μm spot size.
The additively manufactured volume was printed using a checkerboard
scan strategy using a 5 mm by 5 mm island and virgin powder charac-
terized by a nominal composition and grain sizes +45–10 μm. Upon
completion of the build process, the block was removed from the
build plate in the as-built condition without applying a stress relieving
step. Using wire electrical discharge machining (EDM), two 6 mm diam-
eter cylinders were extracted, from each of the three principal direc-
tions, namely the build direction (BD), sweep direction (SD), and
transverse direction (TD), resulting in a total of six cylinders. One cylin-
der from each direction was set aside to remain in the as-built condition,
and the other one was reserved for a DA hardening heat treatment of
720 °C for 24 h [11]. Prior to applying the age-hardening heat treatment,
each cylinder was cut into 3.5 mm thick specimens using wire EDM. The
reserved as-built cylinders were similarly cut into 3.5 mm thick speci-
mens using wire EDM.
The remaining portion of the L-PBF block, minus the aforementioned
extracted cylinders reserved for the AB and DA heat treatment, was sub-
jected to the RC heat treatment. The RC heat treatment was also tested for
comparison to the AB and DA conditions. A solutionizing recrystallization
heat treatment of 1250 °C for 1 h, was selected to exceed the reported re-
crystallization temperature of 1100 °C while remaining below the melt-
ing temperature (1300 °C) of IN718 [35]. The RC heat treatment
consisted of a 625 °C/h ramp rate, a 1 h dwell at 1250 °C, and a 625 °C/h
ramp down rate. The hold time of the heat treatment matches that
of Tucho et al. [14], but otherwise differs significantly from Ref. [14]
due to the utilization of furnace cooling opposed to water quenching.
Furnace cooling (10.4 °C/min) was selected to allow for a cooling rate
fast enough to limit the precipitation of the delta phase, while also
ensuring passing through the γ′ and γ′′ precipitation region of the
transformation-time-temperature (TTT) diagram for IN718; see
Fig. 1 for the cooling path utilized. Initial precipitation of the δ
Fig. 1. A Transformation-time-temperature diagram of IN718 adapted from [37]. The red
curve corresponds to the cooling path for the RC heat treatment utilized in the current
study. (For interpretation of the references to colour in this figure legend, the reader is
referred to the web version of this article.)
3
Materials and Design 198 (2021) 109228
phase occurs at grain boundaries followed by the growth of thin
plates into the grains [5]. Intragranular nucleation has been observed
in the presence of the γ′′ precipitates [3,36]. The maximum precipita-
tion of the delta phase occurs around 900 °C, reaching an equilibrium
fraction within 20 h. With respect to the cooling rate used, the small
amount of time spent over the temperature range that the delta
phase precipitates during furnace cooling would result in a limited
delta phase presence as there is not sufficient time for significant pre-
cipitation to occur. As will be discussed in subsequent sections, the
observed δ phase was limited to grain boundaries. The precipitation
of the γ′ and γ′′ precipitates has been observed to occur homoge-
neously throughout the γ matrix [5]. The precipitated γ′ and γ′′ are
expected to be fine as it has been shown that precipitate coarsening
is linearly dependent on the cube root of aging time [3].
After the heat treatment was completed, a 6 mm cylinder was ex-
tracted from the SD and TD principal processing directions and two
were extracted from the BD, one from around the center of the block
and the other 9.4 mm from the edge (Fig. 2), using wire EDM. Each cyl-
inder was then cut into 3.5 mm thick specimens. Hence, the compres-
sion sample geometry is 6 mm diameter cylinders, 3.5 mm thick.
The number of mechanical tests preformed per condition was deter-
mined by the replicates required to achieve statistical significance in the
analysis of variance (ANOVA) presented in Section 3. Table 1 provides
an overview of the number of specimens examined.
2.2. Microstructure characterization
Specimens of each condition and orientation were prepared for
backscattered electron (BSE), electron backscatter diffraction (EBSD)
analysis, and energy dispersive spectroscopy (EDS) using mechanical
grinding and polishing. Between each grinding and polishing step, spec-
imens were thoroughly cleaned using water and an ultrasonic cleaner
for 1 min. The initial specimen surface finish (i.e., EDM recast layer),
was ground starting with 600 grit silicon-carbide paper down to 1200
grit. Using a combination of Kempad polishing pads, 6 and 1 μm dia-
mond suspension slurries and a 0.05 μm colloidal silica slurry, speci-
mens were manually polished using progressively finer slurries to
Fig. 2. Schematic representation of the location of the cylinders used to extract the
specimens used in the investigation. Equidistant samples were tested in the quasi-static
and dynamic regimes (number of samples specified in Table 1) and adjacent samples
were used for microstructural characterization. Figure not to scale.
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al.
Table 1
Number of samples used from each principal direction shown in Fig. 2 for experimental
testing.
Loading direction Quasi-static compression Dynamic compression
BD-center 4 6
BD-edge 7 5
TD 3 4
SD 3 5
achieve a high-quality surface finish satisfactory for EBSD and EDS
measurements.
The BSE, EBSD, and EDS measurements were captured using an FEI
Quanta 600 FEG scanning electron microscope equipped with an EBSD
detector. The EBSD measurements were made using an accelerating
voltage of 20 kV, spot size of 5 (approximately 2.3 nA current), and a
working distance of 12 mm. TSL OIM Analysis™ software was used to
post-process the EBSD data and produce the inverse pole figure maps,
pole figures, grain ellipticity, and grain boundary orientation distribu-
tion figures. TEAM software was used to perform EDS elemental analy-
sis. Line scans were taken over multiple particles and the matrix
material. To limit the effects of the EDS interrogating a volume, elemen-
tal results one micron on either side of the matrix particle interface were
omitted when determining the averaging composition of each particle.
2.3. Transmission electron microscopy
Three transmission electron microscope (TEM) samples (one ex-
tracted from each principal processing direction) were prepared by
grinding slices to a thickness of 90–100 μm; a mechanical punch was
then used to create discs with a diameter of 3 mm. A Fischione auto-
matic twin-jet electropolisher (Model 120) at 15 V and an electrolyte
of 10 vol% perchloric acid in methanol at −32 °C was then used to fur-
ther thin the TEM foils. Conventional bright-field (BF), dark field (DF),
selected area electron diffraction (SAED), and high-resolution transmis-
sion electron microscopy (HRTEM) characterizations were performed
using an FEI Talos TEM (FEG, 200 kV). Lattice dislocation densities of
cell interiors were measured in BF TEM micrographs by line intercept
method [38] using at least 50 dislocation cells. Entangled forests of dis-
locations along the cell boundaries were excluded from this calculation.
Average precipitate sizes, interparticle distances, and corresponding
standard deviations are reported using measurements of approximately
50 precipitates from several HRTEM, BF, and DF images taken from var-
ious regions throughout the build volume.
2.4. Mechanical testing
The mechanical behavior of specimens from each condition was in-
vestigated under uniaxial compression at quasi-static and dynamic
strain rates. For quasi-static strain-rate testing, specimens (sandwiched
between platens) were loaded in the Instron 5985 electromechanical
testing machine at a rate of 0.075 mm/min up to 1 mm crosshead dis-
placement, equivalent to around 15–18% strain. The stress-strain re-
sponse was compliance corrected to elastic modulus values measured
using the specimen density and wave propagation speed using the
same approach adopted in previous work [20].
For dynamic strain-rate testing, specimens were tested using a Split
Hopkinson Pressure Bar (SHPB) [39]. Details of the fundamental as-
sumptions and equations used to determine material behavior from
SHPB measurements can be found in text by Chen and Song [40], and
specific attributes of the SHPB apparatus used in this work can be
found in Ref. [20]. In these experiments, strain rates between 2200
and 2600 s−1 were achieved for the stress-strain curves shown. Over
this range, strain-rate effect were not observed, and thus the strain
rate for each curve is not reported. For each material condition and
4
Materials and Design 198 (2021) 109228
orientation, at least three replicates were performed to establish statis-
tical significance using an ANOVA that will be further discussed in
Section 3.3.
3. Results and discussion
3.1. As-built, direct-aged, and recrystallized microstructures
The authors previously characterized the meso- and nano-scale mi-
crostructure of the AB [20] and DA [11] L-PBF IN718. An overview of the
findings is provided here to aid in the comparison and interpretation of
mechanical test results. The AB and DA specimens exhibit similar micro-
structures at the meso-scale, displaying scan-strategy-influenced
(i.e., laser-path dependent) grain morphology and thermal-gradient
dictated columnar grain growth. Due to the similarity in microstructure
exhibited between the AB and DA conditions, a single BSE micrograph,
inverse pole figure map, grain boundary orientation distribution, and
pole figure is presented in Fig. 3 to represent the nominal meso-scale
microstructure of both conditions. A qualitative comparison of the mi-
crostructures achieved between the AB and DA, and the RC heat treat-
ment for specimens extracted from the transverse direction are
provided in Fig. 3. Figs. 3(a)-(d) provide representative BSE micrograph,
inverse pole figure map, grain boundary orientation distribution, and
pole figures of the [100], [110], and [111] directions characteristic of
both the AB and DA specimen conditions. Fig. 3(e)–(h) provide corre-
sponding images of the RC condition for comparison.
The representative BSE micrograph of the AB and DA conditions,
Fig. 3(a), exhibits features commonly observed in L-PBF IN718 (Fig. 3
(a)) [11,41]. As reported by Deng et al. [24], the cellular structure orien-
tation changes do not correspond to a change in grain orientations as
evidenced by the difference in length scale observed between the BSE
micrograph (Fig. 3(a)) and the EBSD inverse pole figure (Fig. 3(b)).
The BSE micrograph of the RC condition (Fig. 3(e)) clearly shows
that a drastically different microstructure has developed as a result of
the RC heat treatment. Segregated phases have been dissolved into so-
lution, and only a small quasi-random distribution of observable parti-
cles remains. The presence of undissolved inclusions pinning grain
boundaries are indicated by the arrows in Fig. 3(e). In IN718, grain
boundary migration is influenced by grain boundary pinning particles
and annealing twins [42]. Annealing twins form due to the elevated
heat treatment, reducing the stacking fault energy required to form a
twinned region [43]. The position of a few selected annealing twin re-
gions are encircled in Fig. 3(f). As shown by Jin et al. [44], the density
of annealing twins in nickel-based superalloys is inversely proportional
to grain size which explains the low density of annealing twins in the RC
condition, Fig. 3(f).
The inverse pole figure map shows the AB and DA columnar grain
morphology (Fig. 3(b)) that is absent in the RC condition (Fig. 3(f)),
where grains have become nominally equiaxed. In the AB and DA con-
ditions, the IPF maps showcase the columnar structure of the grains
that are aligned along the BD which in this case corresponds to the
[100] direction which suggests also a 〈100〉 fiber texture aligned with
the build direction as seen in the pole figures (Fig. 3(d)). It is also ob-
served that the RC heat treatment has consumed the low misorientaion
angle grain boundaries as compared to the AB condition (Fig. 3(c) for
the AB condition and Fig. 3(g) for the RC condition). The RC heat treat-
ment has resulted in a loss of the fiber texture, as demonstrated by the
more homogenized distribution of grain orientations (Fig. 3(h)).
High magnification micrographs exhibiting representative examples
of microstructure phases and their distributions in the AB and DA condi-
tion, as well as the RC condition are provided in Fig. 4. The intragranular
cellular substructure formed by micro-segregation is shown in Fig. 4(a).
The brightest features are the Laves phase whose irregular morphology
is shown in Fig. 4(b). The 1250 °C HT to achieve the recrystallized con-
dition dissolves the Laves phase into the matrix. During cooling the γ′
and γ′′ precipitates are predicted to precipitate according to the TTT
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al. Materials and Design 198 (2021) 109228

Fig. 3. Representative backscattered electron micrographs, inverse pole figure maps, grain misorientation, and pole figures representative of the as-built and direct-age hardened (a-d) and
the recrystallized (e-h) conditions. The direction normal to the viewing plane is indicated in the BSE and IPF maps. Arrows in (e) indicate precipitates located at grain boundaries. Encircled
regions in (f) are annealing twins. The reference direction for each IPF map is the sample normal, which is also the loading direction.

diagram (Fig. 1). Evidence of a dense precipitation network is shown in
Fig. 4(c) by the numerous sub-micron needle-like features. In section
3.2, HRTEM micrographs and diffraction patterns identify the precipita-
tion network to be composed of the γ′ and γ′′ precipitates.
The δ phase is predicted to be present within the microstructure
based on the cooling path utilized. Precipitation of the δ phase has
been shown to first occur at grain boundaries [45]. As shown in Fig. 5,
the needle-shaped delta phase is observed at a grain boundary. The
overall presence of the delta phase is limited, finding its existence on
just one grain boundary of the more than 30 surveyed. Intragranular δ
phase was not observed in any of the TEM micrographs discussed in
Section 3.2. The lack of intragranular δ phase in the microstructure is
inline with the work of Tucho et al. [14], who used a 1 h 1250 °C
solutionizing heat treatment followed by quenching.
Heat treatments exceeding the δ phase solvus temperature result in
rapid grain growth as the δ phase serves to pin grain boundaries. Grain
boundary growth is inhibited instead by less-soluble non-δ particles
[5,15]. The elemental composition of ten grain boundary particles
were investigated using EDS, see Fig. 6 for a representative line scan.
The grain boundary particles were determined to be MC-carbides due
to their predominant presence at grain boundaries, faceted morphology,
and high Niobium and Titanium content compared the matrix [46]. The
composition in weight percent for the matrix, and MC-particle are pro-
vided in Table 2.
In terms of the grain morphology and orientation, Fig. 7 presents
quantitative measurements of columnar grain growth in all preparation
conditions. The plot in Fig. 7(b) was generated using the EBSD data from
the AB and DA conditions, and Fig. 7(c) from the RC preparation condi-
tion. Multiple specimens from the BD, SD, and TD were analyzed to
show the average orientation spread of the major axis of the grains mea-
sured. In these plots, the orientation is taken with respect to the
specimen's scan horizontal axis as shown in the schematic of Fig. 7(a).
In the AB (and nominally the DA) condition, Fig. 7(b), peaks are ob-
served in the SD and TD lines around 80° approaching 90°. This approx-
imate alignment with the build direction is due to the thermal gradient
being not perfectly normal to the raster surface. Additionally, note the
peaks in the BD specimens at 45° and 135°, which are due to the laser
dependent grains that solidified due to the checkerboard strategy with

Fig. 4. Field emission SEM characterization of phases presence. a) Phase segregation traditionally observed in the AB and DA materials. b) A high resolution micrograph showing the
irregular morphology of the Laves phase. c) Evidence of the dense precipitation network that forms after applying the 1250 °C HT. Subsequent HRTEM images confirm the
precipitation network consists of the γ′ and γ′′ precipitates.

5
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al. Materials and Design 198 (2021) 109228

structures with the Laves phase segregating to the inter-dendritic re-

gions are observed [8,17,24,47–49].
The micrograph of the DA condition in Fig. 9(a), taken along the cell
cross-section, shows columnar morphology of the cells. The microstruc-
ture consists of 1.16 ± 0.10 nm dislocation cells consistent with the cell
size of the AB condition measured along the minor axis, confirming the
thermal stability of the dislocation cell structure at these times and tem-
peratures [11]. Similar to the AB condition, in the DA condition, the
Laves phase and metal oxides and carbides at the intercellular bound-
aries (indicated by the white arrows in Fig. 9(a)) were also observed.
However, the dislocation density within the interior of the cells has de-
creased to 2 ± 0.5 × 1014 m−2, which is nearly half of the AB condition.
Furthermore, as reported in Ref. [11], there is still Nb segregation along
the cell boundaries even after direct-aging at 720 °C for 24 h; therefore,
this aging temperature is also insufficient to diffuse the segregated Nb
back into the matrix.
Additionally, the high magnification BF micrograph and correspond-
ing SAED pattern in Fig. 9(b) taken along the [011]γ, γ′//[110]γ′′ zone axis
exhibits the superlattice reflections consistent with γ′ and γ′′ precipi-
tates however all superlattice reflections of γ′ overlap with those from
γ′′ (indicated with solid circles in the SAED pattern). Therefore,
HRTEM micrographs were used to identify lenticular γ′′ precipitates
and spherical γ′ precipitates. A quantitative analysis of the HRTEM im-
ages including Fig. 9(c) also confirms the existence of monolithic γ′′
(length: 25 ± 3 nm and width: 9.5 ± 1 nm) and γ′ (19 ± 4 nm), respec-
Fig. 5. Delta phase observed at grain boundaries. tively homogeneously distributed throughout the matrix. The interpar-
ticle distance between these precipitates is 12 ± 1 nm.
Fig. 10(a,b) shows a BF and HRTEM micrograph of the AM IN718
which the build volume was printed. These laser dependent patterns after applying the RC heat treatment. Both the entangled dislocations
are more pronounced at the top surface of the build volume, as little inherent to the cell walls and lattice dislocations in the cell interior
remelting and recrystallization has occurred compared to the bottom have been annihilated and all elemental segregation have been
of the build volume that underwent thermal cycling [20].
As shown in Fig. 7(c), the RC heat treatment resulted in the
homogenization of the crystal structure throughout the build volume.
The homogenization of the crystal structure is apparent due to the
larger-equiaxed grains, reduction in SD and TD major axis alignment
along the BD, and loss of texture as presented in the pole figures in
Fig. 3. Grain size was determined using the line intercept method ap-
plied to EBSD data collected in the planes normal to the three principle
processing directions following the ASTM E112–13 standard. In this
method, the number of grains that intercept a test line are count and
used to calculate the mean lineal intercept length which is used to deter-
mine the ASTM grain size number. The average grain size over the whole
build volume for RC specimens is 63.0 μm with a standard deviation of
43.2 μm, while in the AB and DA conditions is 22.1 μm with a standard
deviation of 10.4 μm. Fig. 7(c) compared to Fig. 7(b) shows a decrease
in intensities along the SD and TD specimens at the 80–90° mark, sug-
gesting a more uniform orientation of the grains with respect to specific
directions. Additionally, the texture of the microstructure was seen to be
vastly different than that of the original AB and DA specimens; however
because the whole block was recrystallized, a single pole figure set, such
as Fig. 3h, is representative of the entire RC build volume.

3.2. Nanoscale dislocation cell structure and precipitated phases

The cellular substructure of AB AM IN718 is shown in Fig. 8. The

plan-view of the cells are 2 ± 0.2 μm along the major axis and 1.2 ±
0.15 μm along the minor axis. Lattice dislocation densities within the
cell interiors were measured to be 4 ± 0.4 × 1014 m−2. The heteroge-
neous dark phases (indicated by the white arrows) at the intercellular
boundaries are metal carbides, metal oxides, and Laves phase, which
are characterized in detail in Ref. [11]. During rapid solidification in
the AM IN718 build process, metastable and Laves phases form due to
microsegregation of alloying elements [15]. As a result, fine cellular Fig. 6. Elemental composition line scan of a grain boundary carbide particle.

6
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al.
Table 2
Phase composition (wt%) in the particles observed in Fig. 3 (e) determined using EDS.
Phase Ni Fe Cr Ti Mo
Matrix 50.6 16.9 17.9 1.1 3.1
MC-particles 4.6 2.1 2.0 7.5 4.4
homogenized. The Laves phase and δ phase were also suppressed, as ex-
pected from the high temperature solution anneal (i.e. 1250 °C), how-
ever metal oxides and metal carbides are still present. Interestingly,
dense, homogeneously distributed γ′ and γ′′ nanoprecipitation is re-
vealed by diffraction contrast in Fig. 10(a) and confirmed by SAED pat-
tern and HRTEM micrograph in Fig. 10(b). It is reported that the slow
cooling from solutionized temperature can lead to the formation of γ′
and γ′′ nanoprecipitates [11]. Recently, it has been shown that the dis-
locations along the cell boundaries after the solution anneal can pro-
mote the heterogeneous nucleation of precipitates on boundaries [11];
however, the absence of such precipitates in AM IN718 after being re-
crystallized at 1250 °C for 1 h (Fig. 10) confirms that the dislocation
cells have been recovered mainly during holding at 1250 °C in the RC
condition. Quantification of HRTEM micrographs determine the
nanoprecipitation to consist of monolithic γ′′ (length: 35 ± 4 nm and
width: 12.5 ± 2 nm) and γ′ (22 ± 3 nm) precipitates separated by
31 ± 10 nm regions of γ matrix phase.
3.3. Mechanical properties
The quasi-static and dynamic stress-strain response of the RC condi-
tion are reported in Figs. 11 and 12, respectively. The curves provided
for the DA and AB represent the average stress-strain curve in all
three principal directions in a single preparation condition, and are
Fig. 7. Major axis orientation of grains in pre-mortem BD, SD and TD specimens as defined in the schematic (a), for the (b) AB (quantitatively representative of the DA heat treatment,
which did not undergo any recrystallization), and (c) RC conditions.
Materials and Design 198 (2021) 109228
intended to contextualize the mechanical performance of the RC heat
treatment. As mentioned previously, there is a dearth of studies which
Nb C have investigated the dynamic behavior of AM IN718. A recent excep-
4.4 1.4
tion is the work of Babamiri et al. [50], which studied the AB, stress-
66.7 4.8 relieved (SR), hot-isostatic pressed (HIP), and STA conditions. Their
curves have been included in Figs. 11 and 12. The curves by reference
[50] represent the compressive response of IN718 that was additively
manufactured using different processing parameters than the ones
used in this study therefore resulting in different initial material micro-
structure. The respective curves are used to exhibit the available litera-
ture for more builds and post-build heat treatments that can be applied
to alter the material response.
In the case of the RC heat treatment, the stress-strain response of the
material exhibits an increase in the yield strength (in both strain-rate
regimes) compared to the AB condition. The yield strength of the RC
material in the quasi-static regime (Fig. 11) increased from an average
of 771 MPa in the AB condition with a standard deviation of 34 MPa
(AB samples taken from the same block of material) to a range between
830 and 950 MPa, and in the dynamic regime (Fig. 12) from an average
about 800 MPa in the AB condition (samples taken from the same block
of material) to a range between 1000 and 1250 MPa in the RC condition.
Comparing the stress-strain response of the RC heat-treatment to the
DA heat treatment clearly shows the RC heat treatment does not opti-
mize the yield strength, but it does increase the yield strength relative
to the AB condition from the same block of material. The grain size of
the RC specimens is three times larger than that of the AB and DA con-
ditions. Thus, the increased yield strength is not attributed to grain
boundary strengthening (i.e., Hall-Petch) effects. Comparing the AB ma-
terial microstructure, specifically the dislocation network and cellular
structures, to the RC condition microstructure, where these features
are absent, it is concluded that the dislocation networks and cellular
structures are secondary contributors to strength in AM IN718 relative
7
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al.
Fig. 8. Conventional BF micrographs of the as-printed IN718 showing formation of
dislocation cells with the SAED pattern (taken from the region indicated by white circle)
along the [011]γ zone axis shown as an inset. The Laves phases and metal oxide/carbide
are indicated by arrows.
to the precipitation of the γ′ and γ′′ precipitates. The feature governing
the improved yield strength of the RC condition is nanoprecipiation of
the γ′′ and γ′, as captured in the TEM micrographs presented in
Section 3.2.
To identify the presence of statistical significance between loading
orientations within the mechanical test results obtained in the RC con-
dition, an ANOVA is performed, specifically on the values of the yield
strength of the specimens tested in both strain-rate regimes. Yield
strength values for each principal processing direction in the RC condi-
tion were grouped under quasi-static (n = 3) and dynamic (n = 4) re-
gimes to determine the effect of loading direction on the yield strength.
Note that one cylinder each was extracted from the SD and TD, while
two BD cylinders where extracted from the build volume (one located
at the edge of the volume BD-edge and the second one from its center
BD-center as shown in Fig. 2). The ANOVA found no statistically
significant differences among the yield strength values in the SD, TD,
and BD-edge in the RC condition for both the quasi-static and
Fig. 9. (a) Conventional BF micrograph of AM IN718 after direct aging at 720 °C for 24 h showing secondary particles (i.e., Laves phases) and metal oxide/carbide (indicated with the white
arrows), dislocation cell network and dislocations inside the cells retained from as-printed condition. (b) High magnification BF micrograph and corresponding SAED pattern of γ′ and γ′′
precipitates along the [011]γ zone axis. The solid circles correspond to superlattice reflections that belong to both γ′ and γ′′ phases. (c) High-resolution TEM micrograph taken along [011]γ
showing distribution of γ′′ nanoprecipitates throughout the γ matrix.
8
Materials and Design 198 (2021) 109228
dynamic regimes. However, a statistically significant difference in the
yield strength was noted (in both regimes) between the BD-center
and the other orientations (SD, TD, and BD-edge). In the quasi-static re-
gime, post-hoc Tukey tests indicated a significant difference between
BD-center and TD (p=0.003), and BD-center and SD (p=0.018). In
the dynamic regime, however, post-hoc Tukey tests indicated only a
statistically significant difference between BD-center and BD-edge
(p=0.028), but no significant difference was found between the BD-
center and SD (p=0.146), and BD-center and TD (p=0.065) speci-
mens. It is important to note that the large AM volume was subjected
to a 1250 °C for 1 h, which may have led to a non-uniform temperature
distribution throughout the volume. Combined with the slow precipita-
tion kinetics of IN718, the non-uniform temperature of the AM volume
resulted in a lower density of nanoprecipitates in BD-center compared
to the other specimen orientations, which in turn resulted in lower
yield strength compared to the rest of the samples.
A comprehensive study of response of specimens in the AB and DA
conditions can be found in Ref. [20], and the corresponding supporting
material and a summary of the findings in the stress-strain response
of the AB and DA conditions are presented next. The AB condition
yield strength was measured to be around 771 MPa in the quasi-static
regime and 800 MPa in the dynamic regime on average, with no statis-
tically significant difference between the loading directions. The DA
heat treatment resulted in a doubling of the yield strength of the mate-
rial in both regimes to yield strength values around 1433 MPa (with a
standard deviation of 85 MPa) in the quasi-static regime and
1600 MPa in the dynamic regime. The increase in the values of the
yield strength in the DA condition compared to the AB condition are at-
tributed to the precipitation of the hardening phases (i.e., γ′ and γ′′)
while maintaining the dislocation cells in the DA material [11]. In the
DA condition, material behavior is loading-direction dependent; speci-
mens loaded along the BD exhibit a lower yield strength than the TD
or SD regardless of strain rate. This difference in mechanical behavior
is attributed to the assumption of random distribution of the precipi-
tates combined with the remaining fiber texture after the DA heat treat-
ment. DA specimens then have fewer favorably oriented slip systems in
the TD and SD directions (compared to the BD direction), which blocks
dislocation motion resulting in the need of a higher stress to cause mi-
croscopic yielding in the TD and SD specimens compared to the BD.
The anisotropy observed serves as one of the motivations of the current
study to determine a heat treatment that can improve the compressive
yield strength of the material relative to the AB condition while decreas-
ing its deformation anisotropy.
In comparison to the available mechanical response of AM IN718 in
the literature, the results in both regimes show certain similarities and
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al. Materials and Design 198 (2021) 109228

Fig. 10. (a) Conventional BF micrograph and corresponding SAED of AM IN718 after being recrystallized at 1250 °C for 1 h showing formation of nano precipitates throughout the matrix.
(b) High-resolution TEM micrograph taken along [011]γ showing formation of γ′ and γ′′ nanoprecipitates.

stress-strain curves from all preparation conditions from [50] were dig-
itized and overlaid on the plots in Figs. 11 and 12. Even though the pro-
cessing parameters used to additively manufacture the specimens in
Ref. [50] are different from the parameters used in this study, the mi-
crostructures reported exhibit comparable grain sizes and features
(e.g., particles pinning the grain boundary and annealing twins in the
SR and HIP conditions, respectively). In the quasi-static regime, the
yield strength in the AB condition from [50] exhibited lower value
(618 MPa)) than the AB condition from [20] (771 MPa), followed by
the SR condition which is slightly higher yield strength (892 MPa)
than the AB condition presented herein and comparable to the lower
limit of the RC condition presented herein (830 MPa). The hardening
in the SR condition was attributed to the formation of the γ′ and γ′′ pre-
cipitates. The HIP condition exhibited a yield strength value (930 MPa)
comparable to the upper limit of the RC condition (950 MPa), and the
STA condition a stress strain curve that fits in between the higher

Fig. 11. Engineering stress-strain curves under uniaxial compressive loading in the quasi-
static regime. Curves of tested RC condition from all three principal directions (including
the BD cylinders extracted from the edge and the center of the AM IN718 volume, refer
to Fig. 2) and curves serving for the basis of comparison. The other curves are for the AB
condition (nominal average stress-strain curve from all curves from the three principal
directions), DA condition (nominal average stress-strain curve from all curves from the
three principal directions) in Ref. [20], and other heat-treatments from literature Ref.
[49] as discussed in Section 3.3.

differences. Studies that focus on the dynamic response of IN718 are

limited, therefore it is expected that the processing parameters would
differ. However, the comparison with available literature help contextu-
alize the mechanical behavior of the suggested RC heat treatment.
Babamiri et al. [50] studied the mechanical response of AM IN718 in
the quasi-static and dynamic regimes under compression and tension
in four different preparation conditions. The material was tested in the
as-built condition, and three heat treatments (i.e., SR, HIP, and STA). In
the SR condition, the AB material was subjected to 1065 °C ± 25 °C
for 1.5 h in a vacuum atmosphere, in the hot isostatic pressing condition
the material was subjected SR and then to 1163 °C ± 25 °C for 4 h at Fig. 12. Engineering stress-strain curves under uniaxial compressive loading in the high-
102 MPa ± 1.72 MP, and in the STA condition the material was sub- strain rate regime regime. Curves of tested RC condition from all three principal
jected to the SR and HIP followed by 1065.5 °C ± 2 °C for a time com- directions (including the BD cylinders extracted from the edge and the center of the AM
mensurate with cross-sectional thickness, argon purge cool at a rate IN718 volume, refer to Fig. 2) and curves serving for the basis of comparison. The other
curves are for the AB condition (nominal average stress-strain curve from all curves
equivalent to air cool then heated up to 760 °C ± 15 °C for 10 h ±
from the three principal directions), DA condition (nominal average stress-strain curve
30 min, then furnace cooling to 650 °C ± 15 °C and held at 650 °C ± from all curves from the three principal directions) in Ref. [20], and other heat-
15 °C for 20 h followed by quenching in an argon purge. The compressive treatments from the literature Ref. [49] as discussed in Section 3.3.

9
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al.
limit of the RC condition and comparable to the DA condition at a yield
strength value of 1220 MPa.
3.4. Deformation anisotropy
Quasi-statically and dynamically tested specimens have shown a dif-
ference in the deformation in the AB and DA conditions depending on
the loading direction [20]. The specimens that were extracted and
loaded in the build direction expanded isotropically; whereas, those
loaded in the transverse and sweep directions expanded elliptically
with the major axis extending along the build direction. Measurements
of the aspect ratio of the post-mortem specimens in all three prepara-
tion conditions for each of the principal directions are shown in Fig. 13.
The AB and DA specimens show an aspect ratio around 1.00 for spec-
imens loaded in the build direction and between 1.10 and 1.20 for the
specimens loaded in the sweep and transverse directions. In contrast,
specimens in the RC condition show mean aspect ratios below 1.05, re-
gardless of the principal direction from which the specimens were ex-
tracted and loaded.
To assess the statistical significance of the heat-treatments on the
post-mortem aspect ratios, an ANOVA was performed on the values
grouped in preparation condition under each processing direction
(n = 3). No statistically significant difference has been found between
the specimens in the build direction in all three preparation conditions
(p=0.433), as can be concluded from Fig. 13. However, values of the
aspect ratios in the SD and TD were respectively tested in all three
preparation conditions and were found to be statistically different.
Post-hoc Tukey tests reveal a lower statistically significant difference
between specimens in the AB and DA conditions extracted from the
TD (p=0.006) and SD (p=0.049), compared to their respective
principal-direction specimens in the RC condition. Hence, it has been
statistically proven that the RC heat-treatment has successfully re-
sulted in the reduction of the anisotropy in the plastic deformation
of the L-PBF IN718 samples.
The values of the aspect ratios suggest that the recrystallization of
the grains resulted in a decrease in the anisotropy of the deformed spec-
imens. In fact, looking at Fig. 7(b), the ellipticity of the grains is indepen-
dent of the principal direction compared to the AB and DA case shown in
Fig. 7(a). That is also evident in the IPF map of the RC condition that
shows equiaxed grains compared the columnar grains that grow along
the build direction in the AB and DA conditions, Fig. 3(g) vs. Fig. 3(b).
The nominally equiaxed grains in the RC condition exhibit nominally
Fig. 13. Post-mortem aspect ratio (major axis/minor axis) of the samples in the AB, DA,
and RC conditions. The aspect ratio is defined as the ratio of the major axis over the
minor axis as defined in the inset of the figure. An aspect ratio of 1.0 is representative of
a circular cross-section sample and a ratio larger than 1.0 suggests an elliptical cross-
section.
10
Materials and Design 198 (2021) 109228
uniform in-plane grain dimensions in all directions, resulting in no in-
plane preferred deformation direction. Therefore, independent of the
loading direction, the samples in the RC condition exhibit reduced
anisotropy.
4. Conclusions
In this study, the effects of the recrystallization of a L-PBF IN718 vol-
ume on the mechanical response in quasi-static and dynamic regimes
were presented, along with a discussion of the underlying microstruc-
ture. As highlighted previously, there have been few studies examining
the dynamic behavior of AM IN718. Such data is needed in order to con-
tinue to move AM from the laboratory setting to industry, as IN718 is an
important aerospace alloy whose in-use environments can include
high-strain rate loading.
The recrystallization heat treatment has successfully achieved the
following objectives:
• Increase in the yield strength of the material compared to the as-built
condition studied previously in the literature. Such a result was unex-
pected given the threefold grain size increase and a cooling rate which
provides limited time for precipitation. However, the γ′ and γ′′ nano-
precipitation network observed via TEM provides adequate material
strengthening to achieve a stress-strain behavior matching that of
much more time intensive and costly post-build heat treatments
(e.g., HIP AM IN718).
• Decrease the anisotropy in the deformation of the IN718 specimens
compared to the as-built and age-hardened conditions reported pre-
viously in the literature. The decrease in the anisotropic deformation
is attributed to the recrystallization which caused grains to transition
from columnar to equiaxed, hence a reduction of the [100] fiber
texture.
The aforementioned results provide a path for the design of L-PBF
IN718 parts with tailored properties. The type of heat-treatment to be
applied to AB L-PBF IN718 should be tailored to the desired mechanical
properties for a given application. For example, properties such as in-
crease in the yield strength and decrease of the deformation anisotropy
are of interest for applications in extreme pressure and temperature
conditions relevant to the defense and aerospace industries. Therefore,
depending on the application that requires IN718 with given properties
the authors recommend the following:
• In the case where deformation anisotropy is not a limitation, we
suggest using the DA for almost doubling the yield strength under
quasi-static and dynamic compression regimes. However, the printing
orientation of the part should be taken into account in the context of
deformation anisotropy.
• In the case where deformation anisotropy is not desirable and a trade-
off of less improvement of the yield strength (compared to the DA
condition) is acceptable, the RC heat treatment is recommended.
In the future, further investigations of novel post-processing heat-
treatments for L-PBF IN718 should be explored. With respect to the cur-
rent work the solutionizing heat treatment represents an underaged
condition. Thus, future heat treatments could be designed to apply
prolonged aging to improve yield strength while maintaining the
more isotropic deformation behavior presented herein. The authors rec-
ommend that the metal additive manufacturing community focuses on
IN718 with tailored microstructures to support certification and qualifi-
cation of L-PBF IN718.
Data availability
The raw/processed data required to reproduce these findings cannot
be shared at this time as the data also forms part of an ongoing study.
N. Kouraytem, J. Varga, B. Amin-Ahmadi et al.
CRediT authorship contribution statement
Nadia Kouraytem: Conceptualization, Investigation, Data curation,
Formal analysis, Writing - original draft, Visualization. John Varga: Re-
sources, Investigation. Behnam Amin-Ahmadi: Investigation, Formal
analysis, Writing - review & editing. Hadi Mirmohammad: Investiga-
tion. Raphaël A. Chanut: Investigation, Formal analysis, Writing - re-
view & editing. Ashley D. Spear: Writing - review & editing, Funding
acquisition. Owen T. Kingstedt: Conceptualization, Writing - original
draft, Project administration.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgments
The research described herein was supported by the Department of
Defense Office of Economic Adjustment under award no. ST1605-19-03.
This work made use of University of Utah shared facilities of the Micron
Technology Foundation Inc. Microscopy Suite sponsored by the College
of Engineering, Health Sciences Center, Office of the Vice President for
Research, and the Utah Science Technology and Research (USTAR) ini-
tiative of the State of Utah. The authors would like to thank the ADAPT
Center and Drs. Branden Kappes and Aaron Stebner at Colorado School
of Mines for providing AM material. The authors would also like to
thank Dr. Paulo Perez for his training and assistance when using equip-
ment at the University of Utah Nanofab, Dr. Taylor Sparks and Marcus
Parry and Drs. Steven Naleway and Isaac Nelson for access and help to
use the furnace for heat treatment, Jeff Kessler for support while
performing quasi-static compression experiments at the Kay and Larry
DeVries Strength of Materials Laboratory, and Prof. Daniel O. Adams
and Dr. Sungwon Kim for access and training on the Sonix ultrasonic
scanner.
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