Solid Freeform Fabrication 2021: Proceedings of the 32nd Annual International
Solid Freeform Fabrication Symposium – An Additive Manufacturing Conference
Reviewed Paper
Effects of Heat Treatment and Fast Neutron Irradiation on the Microstructure and
Microhardness of Inconel 625 Fabricated via Laser-Powder Bed Fusion
T. Keya1, V. O'Donnell2, J. Lieben1, A. Romans1, G. Harvill1,
M. Andurkar3, J. Gahl2, S.M. Thompson3, and B. C. Prorok1
1Department of Materials Engineering, Auburn University, Auburn, AL 36849
²University of Missouri Research Reactor (MURR), University of Missouri, Columbia, MO
65211
3Alan Levin Department of Mechanical & Nuclear Engineering, Kansas State University,
Manhattan, KS 66506
Abstract
The microstructure of Inconel 625 fabricated via Laser-Powder Bed Fusion (L-PBF) was
investigated in as-printed and heat-treated conditions. The very high cooling rates inherent to the
L-PBF process generally result in fine microstructures and complex residual stress fields which
requires annealing to reduce stress and tailor the microstructure to obtain the desired mechanical
properties. Inconel 625 alloy, a nickel-based superalloy, continues to be a common material
employed with the L-PBF process. The unique microstructure produced by the L-PBF process and
different phases introduced by different heat treatment processes require investigation to facilitate
the material’s wide range of applications. This paper investigates the influence of heat treatments
at 700°C, 900°C and 1050°C for one hour on the microstructure and microhardness of the L-PBF
parts. The parts were irradiated using ‘fast’ neutrons in University of Missouri Research Reactor
Center (MURR). The microhardness before and after radiation are also compared.
1. Introduction
Laser Powder Bed Fusion (L-PBF) offers the ability to fabricate metal parts with highly-
customized geometries, tailored structures and consolidated assemblies. This additive
manufacturing (AM) method has several advantages of traditional manufacturing methods,
including, fabrication-friendly environments promoting lean production by reducing material
waste, fabrication of parts made from a broad range of materials including superalloys, and
reduction of fabrication time and cost [1-2]. During the L-PBF process, a focused high-energy
laser beam selectively melts a powder layer accompanied with rapid cooling/solidification for a
predetermined shape defined via computer aided drawing (CAD) data. This process is followed by
the coating of a new powder layer that is melted selectively to the previous layer. This cycle goes
on until the final product is completely manufactured. During L-PBF, very high heat fluxes are
imposed for creation of a melt pool which results in very high thermal gradients within the heat
affected zone [3]. These thermal gradients manifest into significant residual stress distributions.
During solidification, cooling rates can be as high as 103 K/s to 106 K/s, whereas for traditional
methods, e.g. casting, has a cooling rate on the order of 1 to 103 K/s [4]. These complex thermo-
mechanical phenomena lead to fine dendritic inhomogeneous microstructures that require
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investigation; often to determine how an L-PBF material performs relative to its wrought
counterparts.
Inconel 625 (Alloy 625, IN625) is a nickel superalloy with exceptionally superior
mechanical properties that derives its strength from solid solution strengthening by chromium (Cr),
molybdenum (Mo) and niobium (Nb) atoms [4, 5]. In addition to solid solution strengthening,
IN625 exhibits precipitation hardening primarily from the precipitation of the fine metastable γ″
phase. It is suitable for high temperature applications and is corrosion resistant making it an ideal
candidate for aerospace, medical or energy sectors.
Researchers have reported formation of γ″, δ, Pt2Mo-type phase, Laves phase and carbides
in the typical FCC γ matrix of IN625 [6]. Floreen et al. reported formation of γ″ precipitates at
593℃-760℃ and formation of Laves and δ precipitates at 704℃-982℃ in wrought IN625 [6].
The stable δ phase, which can be needle or plate shaped, is formed upon dissolution of metastable
γʺ precipitate due to local rises in Nb content [7,8]. Dinda et al. studied the microstructure of IN625
fabricated via Laser aided Directed Energy Deposition (L-DED) and reported a stable dendritic
structure, even at 1000℃ [9]. Hu et al. found reduced ductility with increasing temperature in L-
PBF IN625 [10]. This decrease in ductility is caused by intergranular cracking due to
inhomogeneous microstructure introduced by the L-PBF process. Stoudt et al. reported faster
precipitation in L-PBF IN625 compared to wrought material [11]. The nature of the L-PBF process
causes localized concentration of Nb and Mo atoms that acts as the driving force to form δ
precipitates at 870℃ in as quickly as 15 minutes. δ phase formation can be controlled by a stress
relieving heat treatment and modifying Nb and Mo content. Another study on forged, L-PBF and
Laser Melting Deposition (LMD) IN625 revealed heterogeneous microstructure with columnar
dendrites in the latter two [12]. The microstructure in L-PBF IN625 is finer and more textured than
that found in the forged and LMD microstructures. The L-PBF microstructure can contribute to a
material’s superior hardness and strength, as well as its poor ductility relative to wrought material.
Heat treatment of IN625 parts at 1100℃ makes the mechanical properties more comparable to that
of wrought parts. The superior mechanical properties found in L-PBF IN625 may also be attributed
to high dislocation density along with the fine dendritic microstructure [13]. Marchese et al.
reported formation of γʺ precipitates and Cr-rich carbides after heat treating L-PBF IN625 at 700℃
for 24 hours which caused high strength with poor ductility. Recrystallization occurred after
annealing the material at 1150℃ for 2h resulting in dissolution of precipitates and a mixture of
large as well as fine grains. Li et al. also reported high dislocation density as well as high residual
stress in L-PBF IN625 [14]. In addition, the precipitation of the δ phase at 800℃ and 900℃ was
found to result in higher hardness [14]. Precipitates or carbides usually are not found in as-built L-
PBF IN625 [15]. Decrease in lattice constant after heat treatment was also found which is attributed
to significant carbide precipitation.
A detailed investigation of effects of nuclear radiation on microstructure and mechanical
properties of AM IN625 can facilitate use of this alloy in nuclear reactors. Related studies found
embrittlement and increase in hardness due to irradiation induced defects and precipitation.
Hashimoto et al. conducted a study on ion irradiated Inconel 718 that was traditionally
manufactured, solution annealed (SA) and precipitation hardened (PH) [16]. Samples were
irradiated using Fe+, He+ and H+ beams of different strength at 200℃. Nanoindentation on
irradiated samples revealed an increase in hardness for both SA and PH conditions. Higher dose
and He injection on SA samples induced larger concentration of Frank loops and cavities resulting
in irradiation-induced hardening. In Fe irradiated PH IN718, softening occurred due to incoherent
γʹ and γʺ precipitates. In He irradiated PH samples, hardening was observed with increasing He
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concentration for up to 14 at%, then softening occurred at 20 at% He concentration due to
dissolution of precipitates. Another study on Nimonic PE-16 (another nickel-based superalloy)
alloy also emphasizes on He embrittlement over γʹ precipitation hardening [17]. Angeliu et al.
suggested reduction in helium concentration and solute segregation to control radiation hardening
[18]. Song et al. presented a comprehensive study on proton irradiated stainless steel, Ni based
alloys and ferritic alloys [19]. Most samples showed formation of voids, dislocation loops and
precipitates upon irradiation at 360℃ and 2.5 dpa. IN625 experienced enrichment of Cr and Mo
on grain boundaries and precipitation of Pt2Mo-type phase induced by the irradiation. Ni-based
alloys found to be more prone to radiation damage compared to ferritic alloys. Cieslik et al.
reported traditionally manufactured IN625 to be more resistant to ion irradiation compared to its
L-PBF counterpart [20]. Softening occurred for wrought alloy with increase in fluence whereas L-
PBF IN625 experienced softening at 1.0 dpa and hardening at 3.0 dpa. The nano-hardness of the
as-built L-PBF IN625 was found to be about 8% higher than that of wrought IN625 before
irradiation. Increase in hardness for wrought IN625 was about 3%, but there was 6% increase in
hardness for L-PBF IN625 after irradiation at 0.1 dpa. Softening at 1.0 dpa can possibly be
attributed to grain growth and migration of defects such as voids, loops, and dislocations. Fincher
et al. suggested post-radiation annealing to alleviate some radiation damage in solution annealed
IN718 [21]. In-situ annealing at 300℃-500℃ for short period of time can relieve embrittlement
induced by H+ and Ni2+ ions to some extent.
The objective of this research work is to investigate the effects of different heat treatment
schedules comprising of 700oC, 900oC, 1050oC for 1 hour on the microstructure and micro-
hardness of IN625 fabricated by L-PBF. Metallurgical characterization is carried out on as-printed
and heat-treated samples to analyze formation of precipitates. Fast neutron irradiation was
conducted on another similarly processed set of samples and micro-hardness was measured
afterwards. Finally, sample hardness data were compared before and after irradiation. There is lack
of studies that focus on microstructure and mechanical properties of additively manufactured
IN625 irradiated by fast neutrons. This study will provide a better understanding of microstructural
evolution of L-PBF IN625 before and after heat treatment and open doors to further investigate
the effects of fast neutron irradiation on as-printed and heat-treated L-PBF IN625 for facilitating
their use in low nuclear attenuation applications.
2. Experimental Methods
2.1 Material and L-PBF Process Parameters
A Concept Laser MLab Cusing 100R L-PBF AM systems was used to produce all IN625
specimens. The AM machine was equipped with a 100 W fiber laser that has a wavelength of
1070 nm. The build volume of the machine measures 90 x 90 x 80 mm. Cubes with dimensions of
10x10x10 mm3 were additively manufactured. The laser power was set to 90 W with a scan speed
of 800 mm/s. The laser diameter was 80 µm and the layer thickness is set to 25 µm with a hatch
spacing of 60 μm. A density of 99.79% was achieved with these parameters. The compositions of
the Inconel 625 powder used for L-PBF and the wrought Inconel 625 are indicated in Table 1.
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Table 1: Elemental composition of Inconel 625 powder (% in weight)
Element Ni Cr Mo Fe Nb+Ta Co C P S Al Ti Mn
% wt Bal 21 9 <5.0 3.5 <1.0 < 0.1 <0.015 <0.015 <0.4 <0.4 <0.5
2.2 Heat Treatment
After separating the specimens from the built plate, each of them was exposed to a different
heat treatment except one that was kept in the as-printed condition. Heat treatments were
performed at 700℃, 900℃ and 1050℃ for 1h each. Temperature inside the furnace was measured
using a K-type thermocouple and all samples were air cooled.
Heat treatment parameters were chosen for precipitation of the metastable γʺ and stable δ
phase. Fig. 1(a) shows the complete TTT diagram for wrought IN625 [22] and Fig. 1(b) shows the
thermal exposure conditions for δ formation in additively manufactured IN625 compared to
wrought IN625 [11]. It may be seen from Fig. 1(b) that the time for δ phase formation for the same
temperature is drastically reduced for the AM-LPBF samples compared to wrought. This behavior
can be explained by the segregation of solute elements during solidification, which increases the
probability for secondary phase formation. During L-PBF, the cooling rates are much higher than
those experienced during conventional processes. This is known to lead to a finer dendritic
structure with smaller dendrite spacing. Zhang et al. showed that L-PBF produces a finer
microstructure for IN625 than other AM processes (Electron Beam Melting and L-DED) and that
the cellular/columnar substructures are enriched in Mo and Nb, while Ni and Cr are deficient [23].
(a) (b)
Figure 1: (a) Time-Temperature-Transformation (TTT) diagram of IN625, adapted from [22], (b) TTT
diagram comparing the presence of δ-phase in additively manufactured IN625 to the wrought material.
The dashed lines estimate approximately 1 %-volume fraction of δ-phase, adapted from [11]
2.3 Metallographic Sample Preparation
Specimens were sectioned parallel to the build direction and hot mounted on
CONDUCTOMOUNTTM mounting resin. Grinding and polishing were carried out on each sample
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down to 0.25 μm colloidal silica suspension. To reveal microstructure, samples were electro-
etched with 70% phosphoric acid at 3-5 volts for 5-40 seconds.
2.4 Characterization Techniques
Scanning Electron Microscopy (SEM) was used to characterize microstructure before and
after heat treatment on L-PBF specimens. A JEOL 7000F SEM unit was used to take high
magnification images of the microstructure of the samples. Vickers hardness was also measured
using a Phase-II Micro Vickers Hardness Tester before and after heat treatment and fast neutron
irradiation.
2.5 Irradiation
A 25-week irradiation study was conducted on polished L-PBF samples in the as-printed
and heat-treated conditions. ‘Fast’ neutrons produced from a cyclotron (GE PETtrace) at
University of Missouri Research Reactor Center (MURR). This experiment looked at hardness
value changes in the samples as the irradiations progressed. Samples were periodically removed
for hardness testing over the course of the experiment to track variations. Samples were placed in
a cyclotron vault, next to a fluorine-18 production target. The neutron flux inside the cyclotron
vault had been modeled, showing that the neutrons resulting from the 18O(p, n)18F reaction have
energies of 0.4 MeV to 16.5 MeV, and that the neutron flux in the vault is, conservatively, between
1.8 ×109 and 3.0 ×109 n cm-2 s-1 [24]. To standardize the results, the neutron flux was converted to
1 MeV equivalent neutrons, resulting in an equivalent flux between 2.4×109 and 4.0×109 n cm-2 s-
1
of mono-energetic neutrons.
3. Results and Discussion
3.1 Microstructure: As-printed condition
Microstructures of the as-printed L-PBF IN625 specimens are shown in Fig. 2. Typical ‘U’
or ‘C’ shaped melt pools related to the laser scanning process are visible on the surface parallel to
build direction. Although it is difficult to measure the exact width due to overlapping, the width
of the melt pool is about 100-120 μm. The overlapping is also a result of the employed hatch
spacing, thus resulting in relatively high density with no gaps between melt pools. This
morphology is formed when the material rapidly solidify after melting by the laser source as soon
as the laser moves. Li et al. also reported similar morphology that is more ‘V’ shaped resembling
welding tracks [15]. The angle of the ‘V’ is a function of laser scanning speed and any increase in
scanning speed decreases the angle and the melt pool becomes narrower.
At higher magnification, cellular and columnar grains can be observed as shown in Fig.
2(b). This may indicate growth of dendrites in different directions. An overall columnar growth
along build direction is found as indicated by arrows on Fig. 2(b). The growth of the dendritic
structure through melt pools is shown in Fig. 2(c). The dendrites are about 500 nm wide with Nb
and Mo segregation on an interdentritic region and a Ni- and Cr-rich dendritic core as reported by
other studies [14, 23].
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(a) (b) (c)
Figure 2: SEM micrographs of as-printed L-PBF IN625 after electro-etching, (a) Melt pools on the plane
parallel to build direction, (b) Cellular and dendritic microstructure at higher magnification, (c) Dendritic
growth through melt pool boundaries at higher magnification.
3.2 Microstructure: Heat Treated at 700℃
Microstructure of the L-PBF specimens after 1 hour heat treatment at 700⁰C are shown in
Fig. 3. At lower magnification, melt pools are noticeable after 1h (Fig. 3a) and it looks very similar
to the as-printed microstructure (Fig. 2a). Dendritic microstructure and elemental segregation at
the interdendritic region are more evident at higher magnification (Fig. 3b-c). These observations
agree with other studies performed L-PBF IN625 [11, 13, 15]. Several research groups reported
formation of metastable γʺ precipitate in the range of 550-750℃ [6-7, 25-28]. γʺ precipitate has a
tetragonal structure with composition of Ni3(Nb, Ti, Al). These precipitates can be plate, disc, lens,
spherical or elliptical shaped. It can take a long time to form γʺ phase in traditionally manufactured
IN625, but precipitation may occur as soon as in 1h in AM materials [15]. Some areas observed in
fig. 3(a, b) appear to be deficient of precipitation which may be attributed to elemental
inhomogeneity throughout the sample. Areas with Nb depletion may not be able to form γʺ
precipitates as carbides like NbC forms [6]. Precipitation is also affected by Ti content in the
material.
Build Direction
Figure 3: SEM micrographs of L-PBF IN625 after heat treating at 700℃ for 1 hour; (a) Melt pools on the
surface parallel to build direction, (b) Melt pools with cellular and columnar growth at higher
magnification, (c) Precipitation at interdendritic region.
3.3 Microstructure: Heat Treated at 900℃
Fig. 4 presents the microstructure after heat treatment at 900⁰C for 1h. Remnants of the
melt pools can still be observed after 1h of heat treatment (Fig. 4a, b). While some precipitation is
evident in certain areas, some areas have been recrystallized due to the dissolution of elemental
segregation/precipitation that exist in the as-printed and 700℃ heat treated conditions. Plate and
needle shaped particles are formed along sub-grain boundaries after 1h that resemble δ phase as
shown in Fig. 4c [6, 29]. δ precipitates have orthorhombic structure with composition of Ni3Nb or
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Ni3(Nb, Mo) [6, 25]. It can be acicular, plate or globular shaped, although acicular, thin rod or
needle shaped particles are most common. It is easier to detect and separate δ particles from its
unique morphology. Laves phase forms at around the same temperature range in IN625, but it has
a “blocky” irregular shape and its formation in IN625 is limited due to lower Fe content compared
to IN718 [6]. Stable δ phase forms from metastable γʺ precipitates when it dissolves into the matrix
leaving high local concentration of Nb atoms [15, 29]. It usually starts forming at grain boundaries,
then spreads out throughout the grain. Researchers have reported formation of δ phase formation
at 650-982℃ [6, 25, 28, 29]. As can be seen from the TTT diagrams in Fig. 1, longer time might
be required if the temperature is relatively low to form the precipitates. Baldan et al. reported
evident formation of δ phase at 725℃ after 500h for traditionally manufactured IN625 [29]. Also
shown in fig. 1, δ precipitates form much faster in AM materials compared to wrought IN625. Due
to the nature of the L-PBF process, there is Nb enrichment along interdendritic regions that triggers
formation of precipitates that are Cr deficient, but enriched with larger Nb and Mo atoms [4].
Stoudt et al. reported formation of δ particles in L-PBF IN625 at 870℃ after 15 minutes [11]. Lass
et al. reported formation of plate shaped δ precipitates at 870℃ for 1h in L-PBF IN625 [4].
Figure 4: SEM micrographs of L-PBF IN625 after heat treating at 900℃ for 1 hour; (a) Melt pools on the
plane parallel to build direction, (b) Columnar microstructure at higher magnification, (c) Precipitation in
columnar regions.
3.4 Microstructure: Heat Treated at 1050℃
Microstructure of heat-treated sample at 1050℃ for 1h is presented in Fig. 5. Melt pool
boundaries, dendrites, elemental segregation, and most precipitates disappear at this heat treatment
temperature causing complete recrystallization. Equiaxed grains with some annealing twins are
visible. Presence of annealing twins indicates release of some residual stress that formed due to
rapid cooling during the L-PBF process [12, 14]. Although not investigated in this study, some
irregular block shaped MC, M6C or other carbides might be present after this heat treatment
temperature [13, 15, 25, 26]. These carbides are often randomly distributed and have no specific
orientation relative to the γ matrix [7]. Melt pools, precipitates and dendrites disappear usually at
temperatures above 1000℃ [6, 12, 15]. Sufficient recrystallization with some primary carbides is
reported to occur at 1150℃ in L-PBF IN625 [13,14, 15, 23].
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Figure 5: SEM micrographs of L-PBF IN625 after heat treatment at 1050℃ for 1h.
3.5 Hardness: Before and After Irradiation
Vickers hardness data for the as-printed and heat treated samples before and after
irradiation are shown in Fig. 6. It may be seen that the pre-irradiation hardness of the as-printed L-
PBF sample is about 340.50±6.06 HV which is close to literature values [12, 15]. It is much higher
than wrought IN625 which is about 260±5 HV [12]. The high cooling rates during the L-PBF
process cause “trapping” of Nb and Mo atoms and this phenomenon builds up residual stress in
the material resulting in higher hardness compared to wrought or forged IN625 [12, 14, 15].
Heat treating at 700℃ for 1h increases pre-irradiation hardness by about 5% which
indirectly indicates γʺ precipitation [12]. Hardness before irradiation keeps decreasing with
increases in temperature. Although δ precipitate causes hardening of material [15], the hardness
decreases at 900℃. The effect of γʺ dissolution, release of residual stress and increase of grain size
may dominate over that of δ phase formation [12, 14]. The hardness decreases at 1050℃ and
becomes 266.6±5.02 HV which is close to wrought IN625 values found in the literature [12]. This
phenomenon is caused by dissolution of precipitates and increase in grain size [12, 14, 15].
As-printed and heat-treated L-PBF samples were irradiated using fast neutrons produced
at MURR. Over the course of the experiment, hardness values of the samples were measured
intermittently, as summarized in Fig. 6. The post-irradiation hardness of all samples display both
softening and hardening, but they are relatively consistent after a fluence of 2.05×1015 n/cm2. All
samples saw notable changes between the initial pre-irradiation measurements and the
measurement taken after 8.57×1014 n/cm2 fluence. After that, hardness values did not show much
change. Relevant studies are not available that investigate effect of fast neutron irradiation on the
microstructure and mechanical properties of L-PBF IN625, but some have reported irradiation
hardening due to formation and rearrangement of defects and precipitates in the material [19, 20,
30, 31]. The presence of both hardening and softening effects is not uncommon [31]. Irradiation
can give rise to local strain causing formation of loops that promote hardening [30]. It can also
promote formation and growth of precipitates [19]. Defects like voids, loops or interstitials can
form and accumulate resulting in increased hardness. On the other hand, dissolution of precipitates,
increase in grain size, or resettling of the defects can cause softening [20].
The 1-MeV-equivalent neutron fluence at the end of the 25 weeks was 9×1015 n/cm2. This
fluence would be considered low for a typical material damage study but was enough to get
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preliminary results that show this method of fast neutron irradiation is viable for future
experiments.
Figure 6: Vickers hardness as function of accumulated neutron fluence for L-PBF specimens.
4. Conclusions
The microstructure and microhardness of L-PBF IN625 before and after heat treatment
have been investigated in this study. The microhardness after fast neutron irradiation is also
presented and compared. Some important observations from this study are outlined below:
1. L-PBF produces fine dendritic microstructure in IN625 that grows along the build direction
due to rapid cooling.
2. Melt pool boundaries and interdendritic segregation are retained through heat treatment at
700℃. At 900℃, melt pools start to dissolve and intergranular precipitation can be observed.
3. Melt pools, elemental segregation and precipitates are dissolved at 1050℃ and equiaxed grains
with annealing twins are formed.
4. As-printed L-PBF IN625 has higher hardness compared to wrought IN625.
5. L-PBF samples heat treated at 700℃ for 1h displayed the highest hardness among all samples
before irradiation, whereas 1050℃ sample showed the lowest hardness among L-PBF samples
and most comparable to wrought IN625.
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6. Both hardening and softening occur in L-PBF IN625 during continuous exposure to fast
neutrons up to 9×1015 n/cm² normalized fluence.
L-PBF technology can be a very powerful tool for modern nuclear reactor applications, but
extensive research is required to investigate the performance of materials like IN625 with a
complex microstructure produced using the technology. This study sheds light on evolution of
microstructure of L-PBF produced IN625 superalloy in as-printed and heat-treated conditions at
various temperatures which can be very useful to explain its mechanical properties like
microhardness. Hardness after irradiation is also investigated after different levels of fluence which
is a step forward towards understanding the performance of L-PBF IN625 in low nuclear
attenuation applications.
Acknowledgement
This material is based upon work supported by the U.S. Department of Energy’s Office of Nuclear
Energy under Award Number DE-NE0008865.
Disclaimer
This report was prepared as an account of work sponsored by an agency of the United States
Government. Neither the United States Government nor any agency thereof, nor any of their
employees, makes any warranty, express or implied, or assumes any legal liability or responsibility
for the accuracy, completeness, or usefulness of any information, apparatus, product, or process
disclosed, or represents that its use would not infringe privately owned rights. Reference herein to
any specific commercial product, process, or service by trade name, trademark, manufacturer, or
otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring
by the United States Government or any agency thereof. The views and opinions of authors
expressed herein do not necessarily state or reflect those of the United States Government or any
agency thereof.
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