Additive Manufacturing 81 (2024) 104021

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Additive Manufacturing
journal homepage: www.elsevier.com/locate/addma

Dissolution of the Laves phase and δ-precipitate formation mechanism in

additively manufactured Inconel 718 during post printing heat treatments
Vivek Kumar Singh a, Debaraj Sahoo a, Murugaiyan Amirthalingam b, Shyamprasad Karagadde a,
Sushil K. Mishra a, *
a
Department of Mechanical Engineering, Indian Institute of Technology Bombay, Mumbai 400076, India
b
Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036, India

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

Keywords: The microstructures of additively manufactured Inconel 718 consist of the primary phase (dendritic) and the
Additive Manufacturing secondary phases (Laves and carbides). Among the secondary phases, the Laves phase, in particular, adversely
Inconel 718 affects the mechanical performance of the material. A post-processing heat treatment is necessary to eliminate
In situ TEM
undesirable secondary phases. The objective of the present study is to eliminate long-chain Laves using heat
Laves phase
treatment below the δ – solvus temperature and thereby establish the real-time dissolution mechanism of Laves
δ – phase
phase. The specimens are produced using the laser powder bed fusion (LPBF) process, followed by two different
heat treatment procedures based on the temperatures determined using Scheil calculation, and those below the δ
– solvus temperature. While the Laves phase is invariably found in the as-printed stage, this study demonstrates
the successful elimination of a long singular chain of Laves phase when heat treated below the δ – solvus
temperature. Additionally, the real-time transformation and growth mechanisms of δ – phase during annealing,
are effectively captured through in situ heat treatment in a Transmission Electron Microscope (TEM). A re-
distribution of the solute from the Laves phase to the γ – matrix is observed, with the δ – phase in the form of
a needle on either side of the Laves at 900 ◦ C. The in situ observations have shed important insights on the
transformation mechanism of Laves phase to δ – phase in additively manufactured Inconel 718 samples.

1. Introduction structure, equilibrium δ (Ni3Nb) with orthorhombic D0a structure and

Nickel-based superalloy covers a wide spectrum of applications in
the aerospace domain, with about 50% of the jet engine parts being
manufactured using them, owing to their excellent elevated temperature
strength, creep performance and corrosion/oxidation resistance [1,2].
In recent years nickel-based superalloy produced via additive
manufacturing has drawn significant interest from the aerospace in­
dustry [3]. Among several nickel-based superalloys manufactured by
Laser Powder Bed Fusion (LPBF) process, precipitation hardenable
Inconel 718 alloy is the most widely used [4] due to its good weldability
as compared to other nickel-based superalloys [5]. Inconel 718 alloy is
used in the hottest section of the jet engine, such as turbine blades,
turbocharger rotors and combustors [6,7]. The major phases that are
present in the as-printed (ASP) and heat-treated conditions in Inconel
718 are the cubic γ-matrix, cubic γ′ (Ni3[Al, Ti, Nb]) having L12 struk­
turbericht designation, metastable γ′′ (Ni3Nb) with tetragonal D022
the topology closed packed Laves phase ([Ni, Cr, Fe]2[Nb, Mo, Ti]) with
hexagonal closed packed C14 structure [8–10].
During the solidification stage of the LPBF of Inconel 718, alloying
elements such as Nb, Mo, and Ti segregate from the dendritic core to
inter-dendritic liquid resulting in the formation of Laves phases and
carbides [11,12]. Continuous and semicontinuous networks of Laves
phase at the inter-dendritic region are often detrimental to tensile
properties [13,14], high-cycle fatigue life [15], corrosion behavior [16],
and hot cracking [17]. Nb is the major contributing element in the
formation of Laves which leads to the depletion in Nb for the formation
of precipitation hardenable phase γ″. Hence, decomposing the Laves
phase is essential. Various efforts have been made in the context of
controlling Laves phase formation by using a pulsed laser in place of a
continuous beam [18,19], flat head laser profile instead of Gaussian
profile [20] and reducing the content of Nb in the alloy [16]. However,
the heat treatment route is established to be the most appropriate in

* Corresponding author.
E-mail address: sushil.mishra@iitb.ac.in (S.K. Mishra).

https://doi.org/10.1016/j.addma.2024.104021
Received 24 August 2023; Received in revised form 26 December 2023; Accepted 1 February 2024
Available online 5 February 2024
2214-8604/© 2024 Elsevier B.V. All rights reserved.
V.K. Singh et al.
decomposing the Laves phase and producing the
precipitation-hardenable phases [21–26].
The heat treatment procedure typically involves homogenizing
above the eutectic temperature, where all secondary phases are dis­
solved, followed by ageing treatment. Sui et al. [24] studied the disso­
lution kinetics after homogenization using Avrami and Singh-Flemings
model. At the start of homogenization, the dissolution mechanism is
dictated by long-range diffusion of Nb and γ to Laves solid-solid inter­
facial reaction; however, with time, the interfacial reaction becomes the
dominant controlling mechanism. Tucho et al. [25] showed immense
grain coarsening for the heat treatment carried out at 1250 ◦ C for 7 h. Ge
et al. [27] carried out in situ heat treatment in TEM for as-cast Inconel
718 and reported a new pseudo-orthogonal Ni7Nb2 phase with a similar
composition as the δ – phase formed near the γ/Laves eutectic region.
Koul et al. [28] characterize the elevated temperature mechanical
properties in LPBF Inconel 718 through in situ TEM technique. The
formation of γ′ and γ″ precipitates at 700 ◦ C and δ – phase from γ″ have
been reported. However, the evidence on Laves phase and δ precipita­
tion Laves phase has not been addressed.
The homogenization above the eutectic temperature can lead to
dimensional changes and distortion in shape, especially in thin sections
[29] and further results in compromised mechanical properties due to
coarsening of the metal carbides [23,30]. This affects the employability
of AM in producing thin and complex structures. However, the possi­
bility of annealing at lower temperatures, below the δ – solvus tem­
perature, for reducing the long chain of Laves is not explored. While the
dissolution of the Laves from a long chain into discrete chunks upon heat
treatment (above δ – solvus temperature) is well understood, an un­
derstanding of the real-time mechanism of phase transformation at
annealing temperatures does not exist in the reported literature. In the
present work, a detailed microstructural study on the effect of heat
treatment on Laves phase and the transformation mechanism of the δ -
precipitation is carried out. The heat treatment cycles are adopted based
on CALPHAD calculation and industry-standard AMS5662. The indus­
try–standard heat treatment (below δ – solvus temperature) resulted in
the elimination of the long chain Laves phase. Apart from the external
heat treatment studies, the mechanism of the real-time dissolution of
Laves phase and the evolution of δ and γ″ precipitates are studied using
in situ heat treatment in TEM. Precipitation of δ – phase at the site of
Laves phase has occurred at 900 ◦ C. The effect of heat treatment on
Laves phase has been estimated through XRD phase fraction quantifi­
cation and micro-hardness measurement.
2. Materials and methods
2.1. Material processing
Laser powder bed fusion (LPBF) process of additive manufacturing
was employed to fabricate a cuboidal shape Inconel 718 specimen of 10
mm × 10 mm × 120 mm from pre-alloyed spherical-shaped powder
procured from Indo-MIM, India. The deposition was performed on the
Intech iFusion SF1 powder-bed fusion printer, with a circular build plate
of 150 mm diameter and a built height of 180 mm. The setup is equipped
with a 500 W solid-state Yb fibre laser to provide the energy required to
cause the fusion of powder particles. The build chamber was completely
shielded, and continuous purging of nitrogen gas at a rate of 8 l/min was
supplied to maintain an inert environment. The process parameter used
for the current study is provided by the original equipment manufac­
turer. The process parameters used are as laser power: 285 W, scanning
speed: 960 mm/s, laser spot size: 80 µm, layer thickness: 40 µm, hatch
spacing: 110 µm, substrate temperature: 70 ◦ C and scanning strategy: bi-
directional with 67◦ inter-layer rotation. The chemical composition of
the deposited sample measured through the inductive coupled atomic
emission spectroscopy (ICP-AES) is provided in Table 1.
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Additive Manufacturing 81 (2024) 104021
Table 1
Chemical Composition of Inconel 718 sample.
Element Ni Cr Fe Nb Mo Ti Al
wt% Bal. 18.48 19.4 4.56 2.87 1 0.35
2.2. Heat Treatment
Heat treatment was carried out on Inconel 718 samples in the Muffle
Furnace, with a maximum temperature range of 1200 ◦ C. Two heat
treatment cycles were considered for this study as shown in Fig. 1. A
Thermo-Calc simulation was performed to determine the homogeniza­
tion (HOM) temperature above which all the secondary phases are dis­
solved in the matrix (see supplementary Fig. S1 (a)). For the solution
treatment and ageing (STA) treatment, SAE AMS5662 [26,30,31] heat
treatment cycle was adopted.
2.3. Material characterization
The as-printed (ASP) and heat-treated samples were sectioned to
10 mm × 10 mm × 5 mm using a wire Electric Discharge Machine
(EDM) for metallography, hardness, and X-ray diffraction (XRD) ex­
amination. The sample surfaces were mirror polished using 300 –
2500 µm grade SiC paper, followed by final polishing using colloidal
silica (MetSil40) of 0.04 µm. To reveal the microstructural features,
samples were electro-etched using 10% oxalic acid at 3 – 5 V for 5 – 20 s.
The Electron Backscatter Diffraction (EBSD) was performed after the
samples were electro-polished using a chemical solution containing
70 vol% methanol, 20 vol% perchloric acid and 10 vol% butanol at 15 V
for 20 s and − 10 ◦ C. The Gemini 300 Scanning Zeiss Electron Micro­
scope (SEM) attached with the EBSD detector (Make: Oxford In­
struments) was used to carry out the EBSD measurements. The EBSD was
carried out for a scan area of 1000 µm × 1000 µm with a step size of
1 µm at an accelerating voltage of 20 kV. Aztech HKL software was used
for the post-processing of EBSD data. The composition profile was
mapped using an Energy Dispersive X-ray spectroscopy (EDS) detector
(Make: Oxford Instruments) attached with SEM. The EDS mapping was
conducted on etched sample in secondary electron (SE) mode, employ­
ing a voltage of 20 kV.
The samples for TEM analysis were prepared by first sectioning a
0.5 mm thickness foil from the bulk sample using wire-EDM, followed
by mechanically polishing down to 70 µm and then punching a 3 mm
diameter disk. The final TEM lamella is obtained by subjecting the disk
Fig. 1. Heat-treatment cycle for homogenization (HOM) and solution treat­
ment & ageing (STA) conditions.
V.K. Singh et al. Additive Manufacturing 81 (2024) 104021

to twin jet polishing using a solution of 80 vol% methanol and 20 vol%
perchloric acids keeping the parameter as 15 V and − 25 ◦ C. The TEM
analysis was carried out at 300 kV on Thermo Scientific, Themis 300 G3
setup. The EDS scan in TEM was carried out using Super-X detection
system featuring four silicon drift detectors (SDD) having enhanced
sensitivity. The EDS scan performed on ASP, HOM and STA condition
samples at a dwell time of 10 μs capturing 480 frames for duration of
100 min. The in situ heat treatment was carried out inside the TEM on
GATAN 628 heating holders. The heating rate considered for the current
analysis is 12 ◦ C /min to reach a temperature of 900 ◦ C. After every 100
◦
C, the image position is adjusted to account for the thermal drift. The
sample was kept at 900 ◦ C for 190 min to capture the dissolution of
Laves phase and the evolution of δ – precipitates. The same sample was
then held at 700 ◦ C for 7 h to analyze the γ" precipitation.
Atom probe tomography (APT) was carried out for the as-printed
(ASP) and heat-treated sample (STA condition) on CAMECA LEAP

Fig. 2. (a) SEM micrograph of ASP sample in BD, (b) & (c) EDS elemental map of Nb & Mo, respectively. (d) & (e) microstructure of a particular melt pool, (f) & (g)
higher magnification image of HAZ and solidified zone, respectively, (h) & (i) columnar microstructure of the solidified & HAZ, respectively and (j) & (k) columnar
microstructure perpendicular to plane of observation in as solidified and & HAZ respectively.

3
V.K. Singh et al.
5000XR in laser acquisition mode. The parameters for the APT analysis
are temperature: − 223.15 ◦ C, pulse energy: 30 pJ for ASP and 60 pJ for
STA, pulse rate: 200 kHz for ASP and 125 kHz for STA and detection
rate: 0.3%. The needle-shaped APT lift-out was prepared using Focused
Ion Beam FEI Helios G4UX. The post-processing of the raw data was
accomplished using the Integrated Visualization and Acquisition Soft­
ware (IVAS) 3.8.14 version of CAMECA. The mass spectrum peaks were
carefully indexed and calibrated. The dataset contained 13396715 ions
for the ASP sample and 6081750 ions for the STA sample.
XRD 2θ analysis was carried out on Malvern Panalytical Empyrean
equipment over an area of 3 mm × 3 mm. The XRD data were post-
processed on high score plus software to quantify the phase fraction
by carrying out the Rietveld analysis. Hardness measurements were
done on a polished sample using HMV SHIMADZU Vickers’ hardness
tester. For each sample, 50 indentations were taken at a load of 9.807 N
with a dwell time of 10 s on each indent.
3. Results and discussion
3.1. Microstructure of as-printed samples
SEM method was used for microstructure characterization and
shown in Fig. 2. The SEM image in Fig. 2(a) shows the columnar den­
dritic microstructure in the as-printed condition. The bright and dark
contrast observed at the inter-dendritic site are due to topographic
contrast arising due to presence of irregular morphology Laves phase.
The EDS map results in Fig. 2(b) and (c) show that the inter-dendritic
segregates are rich in Nb and Mo acquired using Lα1 X-ray character­
istic spectrum. Secondary phases such as Laves and carbides form in this
solute-rich region, which will be later ascertained from the TEM and
APT analysis. The dark contrast phase of the inter-dendritic site repre­
sents the precipitate-free γ matrix. As elements like Nb and Mo are
getting rejected during the solidification, they first combine with the
carbon atom to form metal carbides. After the carbon atom gets
exhausted, further rejection of this heavier element results in the for­
mation of the Laves phase at the eutectic. The solidification process
responsible for forming Laves phase is L(liquid)→L +
γ→(L +NbC/γ)→L + Laves/γ[18]. The as-printed microstructure can be
divided into three zones: solidified region, fusion boundary (FB) and
heat-affected zone (HAZ), as depicted in Fig. 2(e) and (f). The solidified
region, also known as the melt pool, is the hemispherical contours in
which columnar dendrites have grown epitaxially in the direction of a
negative thermal gradient. The magnified image of the HAZ and solid­
ified region in Fig. 2(g) and (h) clearly denotes coarsening in the
microstructure compared to the solidified region. The as-printed parts
depict two orientations of the columnar dendritic first parallel to the BD,
Fig. 2(i and j) and another perpendicular to BD Fig. 2(k and l), which is
due to the inter-layer rotation of 67◦ during the printing. The primary
dendritic arm spacing (PDAS) for the columnar dendrite in the BD has
increased almost 3 – 4 times from 0.4 – 0.7 µm of the solidified region to
1.8 – 2.75 µm of the HAZ. Similarly, the mean PDAS for the dendrite
perpendicular to the build direction (Fig. 2(k) and (l)) calculated based
on the area-method [32] has increased from 0.5 µm to 1.44 µm. The
same trend follows for the secondary dendritic arm spacing (SDAS),
which increases 6 – 7 times from solidified region (60 – 80 nm) to the
HAZ (280 – 575 nm). The size of the secondary dendrite also increases
from 200 – 360 nm to 520 – 600 nm. The increase in SDAS can be
explained by Kattamis and Flemings [33] model. There is variation in
composition between the larger secondary arm and smaller arm,
creating a gradient of solute flux from the larger arm to the smaller arm.
In order to maintain equilibrium composition, this incoming solute flux
dissolves and remelts the smaller arm, thereby increasing the SDAS,
which leads to coarsening in the microstructure.
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Additive Manufacturing 81 (2024) 104021
3.2. Heat-treatment response on the microstructure
Microstructure analysis was performed on heat treated samples using
SEM and EBSD technique. Fig. 3 depicts the microstructure of the ASP,
HOM, and STA conditions in the build direction (BD), transverse di­
rection (TD), and scanning direction (SD). The SEM image in Fig. 3(a)
shows the columnar dendritic microstructure in BD, and the top view
shows the cross-section of the dendritic structure. The inter-dendritic
decorated with segregated solutes forming Laves phase and carbides
as marked in the Fig. 3(a). The Inverse Pole Figure (IPF) map obtained
by EBSD analysis (Fig. 3(b)) represents the ASP samples having
columnar microstructure with their preferred growth direction in
< 001 > , i.e. build direction, which is the direction of least resistance
for FCC crystal growth during solidification [33].
ASP samples were homogenized at 1150̊ C for 1 h based on Thermo-
Calc calculations, which resulted in the elimination of the dendritic
structure and long-chain Laves phase (Fig. 3(c)). In contrast to the re­
sults obtained under the ASP condition, the microstructure is homoge­
neous in all three directions. There are discrete spherical shape
precipitates present in the homogenized condition, which could be the
carbides and oxides. The IPF in Fig. 3(d) shows a recrystallized equiaxed
structure with annealing twins rather than the columnar grains with a
loss of texture when compared to ASP. The grain size is almost homo­
geneous in all three directions with grain size distribution ranging from
31 to 33 µm. The average grain size is 32 µm. The recrystallization
process under ASP conditions is primarily driven by the thermal stress
resulting from the rapid heating and cooling cycles. In addition to the
thermal stress conditions that occur during printing, the nucleation
mechanism of recrystallization involves grain boundary migration, sub-
grain coalescence, and twinning-related nucleation [34,35]. During
homogenization, the dissolution of the Laves phase follows a three-step
process. Initially, the long chain Laves phase decomposes at the
inter-dendritic site, followed by the transfer of solute into the matrix and
subsequent diffusion of solute within the matrix. [36].
Fig. 3(e) and (f) provide the microstructure results of the STA con­
dition. SEM micrograph shows needle shape δ precipitates primarily at
the inter-dendritic regions and γ″ and γ′ precipitate uniformly distributed
inside the matrix. Disc shape γ″ with a length of ~ 220 nm and a width of
~ 44 nm and spherical shape γ′ with a diameter of ~ 60 nm are present
in the STA condition as seen in Fig. 3(g). STA conditions also led to the
dissolution of the dendritic solidification structure and the long-chain
Laves phases in the sample. The IPF map in Fig. 3(f) depicts a
columnar-type grain structure similar to the ASP condition having a
preferred growth affinity in < 001 > direction.
The {100} Pole figure in the BD-TD plane corresponding to ASP,
HOM and STA condition are shown in Fig. 4. The ASP condition has a
strong texture in {100} along BD and TD. After homogenization, the
sample is completely recrystallized and has a very weak texture. STA
condition pole figure shows similar texture as ASP, with a lower texture
intensity. This signify that most of the grains are not recrystallized for
the STA condition.
3.3. Morphology and composition of phases
In order to confirm the phases observed in SEM micrographs (Figs. 2
and 3), TEM and APT were performed. Fig. 5(a) & (c) shows the TEM
bright field image in BD for matrix and Laves phase along with the
corresponding SAED pattern in Fig. 5. (b) & (d), respectively. The
diffraction pattern for the γ matrix is indexed along the [001] zone axis,
and for the Laves phase, it is indexed along [1341] zone axis. The SAED
pattern confirms that Laves phase present in the inter-dendritic channel
of the as-printed specimen has an HCP crystal structure. The EDS maps
obtained under TEM in Fig. 5(e) show the inter-dendritic region is rich in
Nb, which indicates the presence of Laves phase. The spherical shape
precipitate as observed in the TEM micrograph is rich in Ti, Al, Nb, C and
V.K. Singh et al. Additive Manufacturing 81 (2024) 104021

Fig. 3. Microstructure of the BD-SD, BD-TD & TD-SD plane: (a), (c) & (e) SEM micrograph of ASP, HOM & STA condition respectively, (b), (d) & (f) IPF of ASP, HOM
& STA condition respectively and (g) SEM micrograph of STA condition for the red rectangular box in (e).

O as shown in EDS maps. In order to analyze the concentration gradient
within the spherical precipitate a line scan is taken along it, as shown in
inset Fig. 5(f). The concentration profile reveals that center of the pre­
cipitate is rich in Al and O and the periphery is rich in Nb, Ti and C. APT
was carried on an as-printed sample extracted from the Laves phase
region. Fig. 5(g) shows the reconstruction map for the ASP sample in
which a cuboid is passed through to measure the composition profile
over the length of the cuboid. An interface is formed due to variation in
composition where an Nb-rich region is clearly distinguished. The
composition profile in Fig. 5(i) shows a high concentration of Nb marked
as Nb-rich region in Fig. 5(g), where Nb composition shows a sudden
jump in concentration, reaching 20 at% Nb. The 20 at% Nb composition
is close to the eutectic composition of Ni-Nb phase diagram, where a
eutectic solidification proceeds as L→γ +Laves [37], indicating that the
Nb-rich region in Fig. 5(g) is the Laves phase. Fig. 5(h) shows an
iso-surface plot for Nb, Ti and C superimposed with a Co ion map. The

5
V.K. Singh et al.
Fig. 4. {100} Pole figure in the BD-TD plane corresponding to ASP, HOM, and STA condition.
proxigram shown in Fig. 5(j) for the marked iso-surface in Fig. 5(h)
reveals that a near-spherical shape carbide phase rich in Nb, Ti, and C is
formed. Carbides of the form (Nb, Ti) C are formed in the ASP condition,
which were also revealed from the TEM EDS map.
The composition map for the homogenization condition is shown in
Fig. 6(a). The line scan along the precipitate in Fig. 6(c) and (d) shows a
similar trend as the ASP condition, which confirms the presence of Al2O3
and (Nb, Ti) C. Annealing twins can be seen in the homogenized con­
dition (Fig. 3(d) and Fig. 6(b)) as also confirmed by its SAED pattern.
These annealing twins are formed during recrystallization of as printed
γ-matrix.
Fig. 7(a) and (c) shows the TEM micrograph of the STA condition
containing the δ – phase and γ″- phase, respectively and their corre­
sponding SAED pattern are shown in Fig. 7(b) and (d). SAED pattern
shows δ and γ″ precipitate is present in superposition with γ – matrix
phase. Orthorhombic δ – phase is indexed along the [001] zone axis, and
the tetragonal γ″- phase is indexed along the [111] zone axis. The STEM
elemental map in Fig. 7(e) shows that the needle shape δ – phase is rich
in Nb and Ni, justifying their composition. Spherical morphology pre­
cipitates rich in Ti and Al are found here, indicating this being γ′ pre­
cipitate. APT sample for the STA condition was extracted from γ″, γ′ rich
region, and APT results are shown in Fig. 7(f) and (g). The iso-surface
plot for Nb, Al, and Ti is superimposed with the Al ion map and repre­
sented in Fig. 7(f). The γ′ and γ″ precipitates appear as duplets and
triplets in conjunction with each other. This co-precipitation process is
governed by the solute’s availability and the potential for enriching Al
+ Ti to form γ′, as well as enriching Nb to form γ″ [2,38]. γ′ (shown in
blue) and γ″ (shown in purple) are formed with iso-concentration of Al
+ Ti) as 8.9% and Nb as 16%. The cuboid along the γ′ and γ″ precipitate
provides the concentration profile in Fig. 7(g), which shows an increase
in the concentration of Nb for γ″ precipitate and Al + Ti) for γ′
precipitate.
3.4. Microstructural evolution during in situ heat treatment
In situ TEM study was performed to understand the different pre­
cipitate formation with the temperature. The microstructure evolution
was captured throughout the temperature range, from room tempera­
ture to 900 ◦ C, as shown in Fig. 8. High dislocation density and long
chain Laves phase can be seen in the as-printed samples (Fig. 8(a)). With
an increase in temperature to 500 ◦ C, there is a significant reduction in
dislocation density (Fig. 8(b)), which gets completely dissolves with
increase in temperature at 850 ◦ C and above (Fig. 8(c-f)). At 850 ◦ C and
above (Fig. 8(c-f)), the Laves phase thickness is decreased with low
contrast compared to lower temperature conditions. The observed
phenomenon can be attributed to the rejection of solute atoms from the
Laves phase towards the matrix phase. As the temperature and holding
time increase, this rejection of solute atoms from the Laves phase to the
dendrite intensifies. At 900 ◦ C with a holding time of 20 min (Fig. 8(e)),
the δ – phase precipitates observed at the Laves phase site, which is
absent in the 2 min of holding time. The δ – phase further grow into the
6
Additive Manufacturing 81 (2024) 104021
matrix as needle-like shape with time, as observed after a holding time
of 150 min (Fig. 8(f)).
There are two different mechanisms through which δ – phase pre­
cipitates in Inconel 718. The first method is when metastable γ″ is sub­
jected to favorable thermodynamics and kinetics conditions, and it gets
transformed to orthorhombic δ – phase with the same stoichiometry
composition (Ni3Nb) [10]. The other method of δ – phase nucleation is
from γ matrix by changing the stacking sequence from abcabc type to
abab type [39,40]. The δ – phase can also precipitate from the
inter-dendritic site rich in Nb. Fig. 9(a) provides the schematic of δ phase
precipitation based on the experimental evidence obtained in Fig. 8. The
ASP sample at the inter-dendritic site has the long-chain Laves phase.
There is a chemical potential (calculated from Thermo-Calc) difference
between the Nb component of Laves phase and matrix, as seen in Fig. 9
(b). This chemical potential gradient results in the re-distribution of
solute (Nb) from the Laves phase to the γ-matrix on heating. When
appropriate thermodynamic and kinetic conditions are achieved (at
900 ◦ C with a 20-minute holding period), δ –phase begins to precipitate
and grows over time in the form of a needle shape on either side of Laves
phase into the dendrites. Thus, the formation of δ – phase at the Laves
site could be understood as the diffusion of Nb solute into the matrix,
which has segregated to the inter-dendritic site during solidification and
led to the formation of Laves phase. Laves site, which has a large amount
of Nb solute, has become a preferable location for δ – phase formation
under the favorable condition of temperature and time. The formation of
δ – phase at Laves site can be considered as the intermediate stage of
decomposition of Laves phase and back diffusion of solute to the matrix
[41]. The as – printed sample heat-treated at around 900 ◦ C shows the
precipitation of δ – phase near Laves phase site [42–45]. Kumara et al.
[42] showed through phase-field simulation that precipitation of δ –
phase close to Laves phase with the driving force being local composi­
tion enriched with Nb. A similar phenomenon has been seen after STA
heat treatment [43]. Liu et al. [44] reported that the formation of delta
phase at Laves sites after ageing treatment at 890 ◦ C resulted in the
dissolution of Laves phase. The long chain Laves phase is dissolved into
discrete chunks as the Laves are separated into pieces by the δ – phase. It
could be deduced that the Laves phase gets dissolved to facilitate the
formation of δ – phase [45].
Further investigation was conducted to interpret the growth of δ over
time, which depicted a sigmoidal growth of δ - phase as shown in Fig. 9.
(c). The growth is initially slow up to 700 ◦ C because it takes time for the
suitable thermodynamic conditions to be met and enough δ -phase
nuclei to form. The initial size of the delta phase is equivalent to the size
of the Laves phase with a small increment in size up to 700 ◦ C. Beyond
700 ◦ C, significant growth can be seen, wherein the growth is due to the
localization of solute, which eventually transforms to δ – precipitate at
900 ◦ C. At 900 ◦ C, the δ growth rate is rapid: consuming the Nb solute at
the Laves phase and hence the Laves phase. Since the Laves phase site
becomes the nucleation site for δ – precipitate, it can be ascertained that
the Laves has transformed to δ or the δ precipitated from the Laves
phase. Towards the end of the process, δ growth reaches saturation
V.K. Singh et al. Additive Manufacturing 81 (2024) 104021

Fig. 5. (a) & (c) TEM micrograph of ASP in BD for matrix and Laves phase respectively, (b) & (d) are corresponding SAED pattern, (e) STEM elemental map for Ni,
Nb, Cr, Fe, Ti, Al, Mo, C & O, (f) concentration profile for line map taken along the spherical phase. (g) APT reconstruction map for ASP condition, (h) iso plots for Ti,
C & Nb superimposed with Co ion map, (i) atomic concentration profile along a cube in (g), and (j) proxigram for the precipitate in the red rectangular box of (h).

7
V.K. Singh et al.
Fig. 6. Microstructure after homogenization: (a) STEM elemental map for Ni, Nb, Cr, Fe, Ti, Al, Mo, C & O, (b) TEM micrograph showing annealing twin (inset
showing the SAED pattern), (c) discrete precipitates in the homogenized condition and (d) corresponding concentration profile for line map taken along the
precipitate.
resulting in a sigmoidal growth curve, as seen in Fig. 9(c). There is a drop
in Nb wt% from the Laves phase site to the dendritic core, due to which δ
size becomes stable after a particular holding time. It is being reported
that the formation of δ – phase only occurs if the amount of Nb is suf­
ficient, i.e., beyond 6.8 wt% [46].
The samples used for in situ analysis at 900 ◦ C (Fig. 8) were further
subjected to ageing treatment at 700 ◦ C. Fig. 10 shows the microstruc­
tural evolution during in situ heat treatment at 700 ◦ C. Fig. 10 (a) and
(b) show TEM micrograph aged at 700 ◦ C for 2 mins and 3 h, respec­
tively, with needle shape δ – phase nucleated at the inter-dendritic Laves
phase. The γ″ phase precipitation starts at 700 ◦ C after a holding time of
7 h, as seen in Fig. 10 (c) and (d). At the same temperature and similar
time, another region was also captured (Region 2) and shown in Fig. 10
(e) and (f), showing uniform precipitation γ″ in the matrix. The γ″ pre­
cipitate is largely nucleated at grain interiors as opposed to δ – phase,
which mainly precipitates at the inter-dendritic site having Laves phase.
The formation of γ″ phase is due to the ordered transformation of the
FCC γ lattice to BCT D022 structure wherein Nb occupies the corner and
center site. The activation energy for the formation of γ″ phase
(203.2 kJ/mol) is equivalent to the diffusion of Nb in γ matrix
(202.59 kJ/mol) [47]. Thus, the formation mechanism of γ″ phase could
be understood as the diffusion of Nb solute in the matrix. Mantri et al.
[29] showed a large amount of ellipsoidal γ″ phase precipitated at the
dendritic core in line with current findings, and γ″ occurs in a region
which is rich in Nb and Mo.
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Additive Manufacturing 81 (2024) 104021
3.5. Effect of different regimes of heat treatment on Laves phase
Fig. 11 (a) shows the intensity vs 2θ plot obtained from the XRD
scans for ASP, HOM, and STA conditions. The phase fractions from XRD
data were calculated by a Rietveld refinement technique with a good­
ness of fit of less than 1.6, which confirms the reliability of the calcu­
lation. The as-printed sample consists of a higher fraction of Laves phase,
amounting to 11.5%, while the Laves phase is almost negligible in the
HOM and STA conditions. The accuracy of obtaining a phase fraction
through XRD is ± 1% [48], resulting in a little deviation from the exact
phase fraction. Microhardness values for the ASP, HOM and STA con­
ditions are displayed in Fig. 11 (b). After homogenization, there is a
32.3% decrease in hardness compared to the ASP condition. STA con­
dition provides the highest hardness with an increase of almost 27%
with respect to the ASP condition. This increase in hardness is attributed
to the precipitation of γ′ and γ″ as duplet and triplet morphology on
ageing [38]. Sui et al. [21] showed that the small granular Laves phase
remaining after heat treatment provides better strength and ductility
compared to the long chain Laves phase. Annealing at 980 ◦ C for 1 h is
sufficient in homogenizing the segregated Nb and Ti into the matrix and
hence dissolving the Laves phase [49].
4. Conclusions
A comprehensive study on the effect of heat treatment on the Laves
phase and the real-time transformation kinetics of Laves phase at
elevated temperatures was studied on the additively manufactured
IN718 samples. The mechanism of precipitation of δ – phase and γ″ phase
V.K. Singh et al.
Fig. 7. (a) & (c) TEM micrograph for STA taken in BD for δ and γ″ phase respectively, (b) & (d) corresponding SAED pattern, (e) STEM elemental map for Ni, Nb, Cr,
Fe, Ti, Al, Mo, C & O, (f) APT iso-surface plots for Nb, Al & Ti superimposed on Al ion map and (g) atomic concentration profile along a cube in (f).
through in situ heat treatment in TEM was carried out. Based on the
experimental evidence, the following summary can be deduced:
• The inter-dendritic site in the ASP sample has a long-chain Laves
phase. APT result showed a sharp jump in Nb composition along a
Laves phase reaching the eutectic composition of stoichiometric
Laves formation.
• Upon heat treatment, there is a decomposition of the dendritic
structure and solute-rich region and, subsequently, the continuous
network of Laves phase. Homogenization condition results in an
equiaxed structure with the formation of annealing twins due to
recrystallization. While the STA condition results in the formation of
δ, γ″ and γ′ precipitates.
• The in situ TEM study reveals the real-time dissolution behavior of
Laves phase at an elevated temperature with the precipitation of δ –
phase, which grew in the form of a needle on either side of the Laves
phase. The δ growth shows a sigmoidal profile, with the initial and
9
Additive Manufacturing 81 (2024) 104021
end growth being slower. As the Laves phase site becomes the
nucleation site for δ – precipitate, it can be ascertained that the Laves
has transformed to δ or the δ precipitated from the Laves phase.
• The XRD and SEM micrography analysis depict that the STA heat-
treatment condition is sufficient for the LPBF parts to decompose
undesirable long-chain Laves phase. Due to the dissolution of the
long chain Laves phase, there is a diffusion of Nb atoms in the matrix,
leading to the formation of γ′′ in the STA condition which results in an
increase in hardness of the sample.
CRediT authorship contribution statement
Singh Vivek Kumar: Writing – review & editing, Writing – original
draft, Methodology, Data curation, Conceptualization. Sahoo Debaraj:
Writing – review & editing, Visualization, Investigation. Mishra Sushil
K.: Writing – review & editing, Supervision, Resources, Project admin­
istration. Amirthalingam Murugaiyan: Writing – review & editing,
V.K. Singh et al. Additive Manufacturing 81 (2024) 104021

Fig. 8. In situ heat treatment in TEM at (a) 20 ◦ C, (b) 500 ◦ C, (c) 850 ◦ C, (d) 900 ◦ C, holding time of 2 min, (e) 900 ◦ C, holding time of 20 min & (f) 900 ◦ C, holding
time of 150 min.

Fig. 9. (a) Mechanism of δ – precipitation at the site of Laves phase, which is rich in Nb, (b) chemical potential calculated from TCNi10 database of Thermo-calc for
Nb component of Laves phase & γ – matrix and (c) sigmoidal growth of δ-precipitates.

10
V.K. Singh et al. Additive Manufacturing 81 (2024) 104021

Fig. 10. In situ heat treatment in TEM at 700 ◦ C: (a) Holding time of 2 min, (b) Holding time of 3 h, (c), (d) (e) and (f) Holding time of 7 h. (d) magnified image of the
marked area in (c). (e) and (f) are at a different location, showing a higher amount of γ″ precipitate, (f) being the higher magnification image of (e).

Fig. 11. (a) XRD plot and (b) micro-hardness plot for as-printed and heat-treated conditions.

Supervision, Resources, Conceptualization. Karagadde Shyamprasad: Data availability

Writing – review & editing, Supervision, Funding acquisition,
Conceptualization. Data will be made available on request.

Declaration of Competing Interest Acknowledgements

The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
The authors extend their gratitude to the MMMF Lab, Solidification
Lab and TEM Facility, MEMS Department at IIT Bombay for granting
access to microscopy facilities. The authors are also grateful to Joining
and Additive Manufacturing Lab, IIT Madras, India, for helping in car­
rying out the sample fabrication on the Intech iFusion SF-1 PBF ma­
chine. The authors acknowledge the National Facility for Atom Probe

11
V.K. Singh et al.
Tomography, IIT Madras and Sophisticated Analytical and Instrumen­
tation Facility, IIT Bombay, for conducting the APT experiments. The
authors are thankful to Dr Bhagyaraj J for his help in TEM indexing. This
research did not receive any specific grant from funding agencies in the
public, commercial, or not-for-profit sectors.
Appendix A. Supporting information
Supplementary data associated with this article can be found in the
online version at doi:10.1016/j.addma.2024.104021.
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