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Materials Today: Proceedings 5 (2018) 7716–7724 www.materialstoday.com/proceedings

IMME17

Effect of Heat Treatment on the Microstructure and Mechanical

Properties of Inconel 718
Anbarasan Na*,Bikash Kumar Guptaa,Prakash Sa,Muthukumar Pa,
Oyyaravelu Rb ,John Felix Kumar Ra,Jerome Sa
a
Department of Metallurgical and Materials Engineering,National Institute of Technology,Tiruchirappalli-620015,India
b
School of Mechanical Engineering,VIT University,Vellore-632014,India.

Abstract

The welding of Inconel 718 is considerably difficult due to the formation of heat affected zone (HAZ) microfissuring and there
are many factors such as elemental segregation, grain size and secondary phase distribution influence microfissuring. The effect
of the above-mentioned factors can be controlled by the suitable heat treatment. In this study, an attempt has been made to
understand the effect of heat treatment on the microfissuring. Inconel 718 sheets were solutionized at 980 °C and 1066 °C for the
period of 1 hour soaking used were subsequently cooled by furnace cooling (FC) and iced brine quenching (ICE). The
microstructural observation revealed the grain size increase in sample subjected to 1066°C heat treatment. SEM & EDS results
showed more segregation of Nb around grain boundaries in 1066°C heat treated samples. Nevertheless, there is an increase in
hardness of FC samples due to evolution of γʹ and γʹʹ precipitates which were confirmed from X-Ray diffraction results.
© 2017 Elsevier Ltd. All rights reserved.
Selection and/or Peer-review under responsibility of International Conference on Emerging Trends in Materials and
Manufacturing Engineering (IMME17).

Keywords: Microfissuring; Inconel 718; Precipitation strengthening

* Corresponding author. Tel.: +91-9487588129.

E-mail address: naanbarasan@gmail.com

2214-7853 © 2017 Elsevier Ltd. All rights reserved.

Selection and/or Peer-review under responsibility of International Conference on Emerging Trends in Materials and Manufacturing Engineering
(IMME17).
 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724 7717

1. Introduction

Heat treatment is one of the primary material processing technique used to enhance the microstructural and
mechanical properties of nickel based super alloys in wrought and cast conditions. The heat treatment processes
determine the producibility of the alloy in operations such as welding and machining. Inconel 718 is a versatile super
alloy with superior creep, fatigue resistance and widely used in aerospace, thermal and nuclear power generation
components. This alloy is characterized by austenite matrix with many secondary phases. The standard heat
treatment process for this alloy includes homogenisation, solution annealing and precipitation hardening [1]. This
alloy gains its superior strength primarily through the double aging process which is mainly due to the formation of
sluggish Nb based γʹʹ(Ni3Nb) intermetallic precipitates along with γʹ(Ni3(Al,Ti)) precipitates due to the presence of
small amount of Al and Ti content in the alloy. Along with the precipitates other secondary phases such as
orthorhombic δ(Ni3Nb), topographical closed-packed structure like hexagonal laves and rhombohedral μ evolved
during heat treatment cycles. These phases lead to both beneficial and adverse effects on the mechanical properties
of the alloy and increase the creep, tensile and hardness but ductility of the alloy is reduced due the presence of
phases such as NbC, δ and laves phase [2].
All the above-mentioned phases in alloy can be controlled by the proper choice of heat treatment cycles which the
alloy could undergo and their volume fraction and distribution determine its microstructure and mechanical
properties. Defects such as microfissuring can arise due to the presence of a continuous laminate of NbC phases
around the grain boundaries which act as prerequisite for it during welding and this gets aggravated by the selection
of inappropriate heat treatment process [3]. Several reports have addressed this issue and been concluded that the
extent of microfissuring is dependent on the pre-weld heat treatment process and suggested that age hardening is not
advisable prior to the welding process [1,3,4]. Heat treatment also affects metallurgical features like grain growth
and elemental segregation at grain boundaries and this is prominent in both cast and wrought alloys. During this
process, there is an increase in internal energy of the grain in a polycrystalline material and causes increased
mobility of alloying elements. The magnitude of diffusion of alloying elements is greatly dependent on duration of
the heat treatment. Inconel 718 is being a heavily alloyed material and prone to segregation of the alloying elements
at the grain boundaries which are the sites of high energies and possibility of formation of undesirable phases is also
high. Xiao et al. [8] used a homogenization heat treatment for cast Inconel 718 at 1066°C to reduce the boron (B)
segregation at the grain boundaries on cast components and this treatment has provided a better resistance to HAZ
microfissuring while the of the volume fraction of NbC, δ and laves was also greatly reduced. Nader et al. [9]
reported that in cast products the volume fraction of NbC and Ni2Nb are not affected by solution anneal heat
treatment process. Benhadad et.al [10] observed that minor elements have greater influence on the weldability and
concluded that the effect of B was severe, which supports the claims of Xiao et al. [8] and other authors. The cooling
rate also affects the segregation of phases and elements, altering their mechanical properties Hongyu et al. [11] used
iced brine quenching, oil quenching and air quenching for obtaining desired size of γʹ precipitates.
Most of the heat treatment studies on Inconel 718 have focused on cast alloys [8,9,12] and they found that the
homogenisation treatment greatly helps in the reduction of the topographical closed packed phased such as laves
phase in the cast products. But in Inconel 718, almost 45% of products are wrought products and sufficient data are
not available on how wrought alloy would react to various heart treatment process [13]. Earlier research by Decker
[14] on nickel based super alloys in wrought form showed that the type of heat treatment and cooling rates have
affected the stress rupture properties of these alloys. Michael Pereira et al. [15] studied the ballistic impact properties
of Inconel 718 sheets and his studies revealed that the solution annealed condition leads to better properties than age
hardening process. While researchers have focused on the effect of temperature and time on the mechanical and
microstructural properties such as elemental segregation and grain growth, very less work have been done on the
effect of cooling rates. In the present study, iced brine quenching and furnace cooling methods were employed and
such extreme ends of the cooling rates were considered. The Nb segregation has been analysed in this study since it
has a susceptibility to segregate around the grain boundaries and favour the formation of precipitates and secondary
phases like NbC around it and also by controlling their formation through heat treatment process could reduce
microfissuring.
7718 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724

2. Experimental Procedure

Inconel 718 in wrought form was manufactured by VIM/VAR and then thermomechanical processed. Inconel
718 was used for the present research work and the chemical composition of the alloy is shown in Table 1. Samples
of size 10x10x3mm were used for the heat treatment studies and the details of the heat treatment conditions are
given below. The graphical representation of heat treatment cycle is shown in Fig.1a. Heat treatment was carried out
in a furnace at a heating rate of 10°C/min.

 As received condition (VIM/VAR).

 Soaking at 980°C for 1hour and instantly quenched in Iced brine (980°C/1hr+ICE).
 Soaking at 980°C for 1hour and furnace cooling (980°C/1hr+FC).
 Soaking at 1066°C for 1hour and instantly quenched in Iced brine (1066°C/1hr+ICE).
 Soaking at 1066°C for 1hour and furnace cooling (1066°C/1hr+FC).

Table 1. Elemental wt % composition of wrought Inconel 718.

Fe Ni Cr Nb Mo Ti Al Co C Mn Si P S B Cu
19.62 51.98 18.5 4.84 3.14 1.03 .552 .076 .057 .084 .076 .006 .010 .003 0.021

The iced brine quenching (ICE) and furnace cooling (FC) have a cooling rate of 13600°C/min and 5°C/min
respectively and the iced brine solution has a composition of 10%NaCl in water at 0°C. Following the heat
treatment, standard metallographic sample preparation was performed and the polished samples were electrolytically
etched by 10% oxalic acid in water. The microstructural (OM) studies were conducted by using Leica DM2700M
optical microscope (OM) and Carl Zeiss Scanning electron microscope (SEM) with oxford energy dispersive
spectroscopy X-ray analysis capability(SEM/EDS). Elemental analysis around the grain boundary was performed
using EDS. The variations in hardness due to the heat treatment process was analyzed using a Matsuzawa Vickers
microhardness tester with an indentation load of 500g at a dwell time of 10s.Average of five random readings on the
etched surface for each sample were used for measuring the microhardness values. The polished samples were used
for X-ray diffraction study and the diffraction patterns of various phases were obtained using Rigaku, Ultimate IV
diffractometer with Cu Kα radiation(1.54056A) and with a step size of 0. 05°.The scan speed of 5°/min was fixed
over a 2θ range of 30° to 100°.

Fig. 1. (a) Heat treatment cycles to be performed; (b) TTT diagram for Inconel 718.

3. Results

Fig.2 a-e show the micrographs of as received and heat treated samples. It is observed that fine grain structure is
seen in as received and samples solutionized at 980°C whereas coarser grains are seen in the samples soaked at
1066°C. Table 2 shows the grain sizes of various samples. The as received and 980°C/1hr solutionized samples
 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724 7719

have similar ASTM grain size number #8 which corresponds to an average grain diameter of 20µmm while the
samples at 1066°C exhibited a considerable increase in the average grain diameter to 125µmm which corresponds to
a ASTM grain size of #3[16]. The cooling rate due to iced brine and furnace cooling did not affect the grain size
during the heat treatment cycles.
From the SEM/EDS analysis showed in Fig.3 and Table.3 that weight percentage and distribution of the Nb around
the grain boundaries varied due to various heat treatment cycles as, the weight percentage of Nb decreased at 980°C
compared to the as received sample and then increased at 1066oC as shown in elemental mapping Fig .3c. Nb
segregated around the grain boundaries, while there was an equilibrium distribution of Nb in matrix and the grain
boundaries at 980°C Fig.3b. The cooling rates had little effect on the segregation of Nb.
Microhardness values of various heat treated samples are shown in Table 2 and graphical representation is shown
in Fig.4. The data show that the hardness of the furnace cooled sample is relatively comparable to iced brine
quenched sample at both soaking temperatures. The 1066°C/1hr Iced brine quenching achieved the least hardness
value with respect to the baseline value of the as received condition. The X-Ray diffraction results showed well
defined diffraction peaks for the various phases which evolve during the heat treatment process as shown in Fig.5.
The γ, δ and NbC phases were indexed in the XRD pattern. The X-Ray profiles of 980°C/1hr+FC and
1066°C/1hr+FC samples showed side band profiles (marked by an arrow in Fig.5) which is attributed to evolution of
various strengthening phases and these phased greatly influenced the increase in hardness values.

Table 2. Grain Size and Microhardness values.

Heat treatment cycle ASTM grain size Average grain Microhardness(HV)
Number diameter(µmm)
As received 8 20 259.1
980°C/1hr+ICE 8 20 237.8
980°C/1hr+FC 8 20 395.3
1066°C/1hr+ICE 3 125 196.2
1066°C/1hr+FC 3 125 398.2

Table 3. SEM/EDS analysis of grain boundary Nb wt%.

Heat treatment cycle As Received 980°C/1hr+ICE 980°C/1hr+FC 1066°C/1hr+ICE 1066°C/1hr+FC
Niobium-wt% 5.71 3.29 4.16 4.65 4.32

4. Discussion

4.1. Grain growth during Heat treatment

As mentioned above in the result section the grain growth was significant at the soaking temperature of
1066°C/1hr as compared to 980°C/1hr irrespective of the cooling rate. Since 1066oC is high enough temperature
(but less than NbC liquation temperature 1176°C) for grain growth process [17]. This grain growth is associated
with a decrease in strain at the center of the grain which results in low hardness as shown in Table 2. This decrease
in the strain is caused due to the decrease in the dislocation density as the dislocation tend to migrate towards the
grain boundaries and this can be confirmed by the presence of row of etch pits in Fig.3d. and these pits represent the
site of edge dislocation [18]. As the Hall-Petch relation states, the grain coarsening effect also causes loss in
mechanical strength of the alloy. It also promotes grain boundary sliding stress which can initiate triple point crack
and if an intergranular layer of NbC is present after the heat treatment process it would result in propagation of HAZ
microfissuring in welding [3].
7720 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724

Fig. 2. (a) As Received; (b) 980°C/1hr+ICE;(c) 980°C/1hr+FC;(d) 1066°C/1hr+ICE;(e) 1066°C/1hr+FC.

4.2. Analysis of sample from as received condition

The as received material with an average grain size of 25µm (ASTM#8) and possessed a hardness value of
258Hv. This is primarily due to the thermomechanical heat treatment process used for grain refinement after the
VIM/VAR process. The X-Ray diffraction pattern established this fact since only γ phase was detected in the
absence of other strengthening phases. With a high Nb content of 5.71wt % (Table 3) around the grain boundaries
and the lack of Nb in matrix. It suggests the possibility of finely dispersed discontinuous NbC formed around the
grain boundaries. But the absence of NbC peaks in wrought alloy indicated that their volume fraction and in the
form of a discontinuous layer around the grain boundaries [14, 19].
 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724 7721

Fig. 3. SEM/EDS mapping of Nb in heat treated samples a) (a) As Received; (b) 980°C/1hr+ICE;(c) 980°C/1hr+FC;(d) 1066°C/1hr+ICE;(e)
1066°C/1hr+FC;
7722 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724

4.3. Analysis of sample solutionized at 980°C

The nominal heating rate of 10°C/min made sure that no stresses were induced during the heat treatment and this
heating rate results in precipitation of low volume fraction γʹ, γʹʹ and δ phases as shown in the (TTT diagram) Fig.1.b
and also rate of precipitation of γʹʹ, δ phases are sluggish than γʹ [6]. At a soaking temperature of 980°C /1hr, stress
relaxation took place with the γʹ, γʹʹ phases being overage and γʹʹ transformed to stable δ phase having a solvus
temperature above 1000°C and its volume fraction is increases [6]. During furnace cooling at 5°C/min the γʹ, γʹʹ
phases are precipitated but the XRD pattern in Fig.5 is not showing the presence of γʹ, γʹʹ peaks due to their low
intensities [6]. The presence of γʹʹ in the diffraction pattern can be confirmed by deconvoluting the broadened γ (1 1
1) peak of furnace cooled sample and the distribution of sideband profiles (arrowed region in Fig.3) indicate the
presence of a microaustenite region (γʹ-fcc) within the γ matrix [20, 13]. The presence of these precipitates is also
supported by the microhardness results showed in Fig.6 where the furnace cooled samples exhibited higher hardness
compared to iced brine quenched samples, since sufficient time was prevailed for the precipitates to evolve on the
account of its slow cooling rate (5°C/min) than iced brine quenching (13600°C/min)[13].But the iced brine
quenched samples had not shown any side band profiles in the diffraction patterns to identify the presence of γʹ, γʹʹ
phases in the γ matrix and this indicates the failure of these phases to precipitate at a faster cooling rate resulting in
low hardness Fig.6.The element mapping of Nb (Fig.3) showed good distribution of Nb in γ matrix region of
samples resulting from both cooling rates. It is also observed that there is a loss in Nb content at the grain
boundaries in comparison to the as received material [Table.3] this indicates that grain boundary cleaning [23]
action has occurred at this temperature. The slight increase in the Nb content in furnace cooling condition indicate
the evolution of precipitates [20,22].

Fig. 4. Microhardness for the Heat Treatment cycles

 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724 7723

Fig. 5. X-Ray diffraction pattern for the Heat-treated samples.

4.4. Analysis of sample solutionized at 1066°C

The soaking temperature of 1066 °C/1hr resulted in dissolution of most of the secondary phases in the γ matrix
except NbC (dissolution temperature is 1176°C). The diffraction pattern of 1066 °C/1hr furnace cooled samples are
comparable to that of 980°C /1hr furnace cooled one indicating the presence of all the secondary phases and the
similarity is also extended to the high hardness values shown in Table.1. But the diffraction pattern of the iced brine
quenched sample did not show peak broadening and sideband profiles which indicate that there could have been
very less γʹ and γʹʹ phases but the NbC peaks are seen. The hardness value of the iced brine quenched sample is the
7724 Anbarasan et al,. / Materials Today: Proceedings 5 (2018) 7716–7724

lowest among all conditions because of the larger grain size, lower stress in the grains and the dissolution of the
primary strengthening phases.
Nb segregation was prominent around the grain boundaries of iced brine quenched and furnace cooled samples
while the segregation allows the formation of Nb based precipitates [22,11] in furnace cooled cycle in the iced brine
quenched samples it results in the formation of NbC as detected by the diffraction peaks.

5. Conclusions

The effect of heat treatment on the Inconel 718 alloy has been studied and following conclusion were arrived
through the results obtained by various material characterization techniques used. The heat treatment cycles which
include a soaking temperature of 1066°C /1hr resulted in larger grain size of average grain diameter 125µm while
980°C /1hr soaking temperate did not induce any grain growth and the cooling techniques used also had no
influence on the grain size. The furnace cooling condition enhanced the hardness of the material in both soaking
temperatures due to the precipitation strengthening γʹ and γʹʹ phases while there has been no precipitation during
iced brine quenching owning to their high cooling rates resulted in less hardness. Nb segregation was profound in
the high soaking temperature of 1066°C /1hr resulting in precipitation of secondary phases around grain boundaries
while 980°C /1hr treatment resulting in even distribution of Nb in the matrix and grain boundary regions. Samples at
1066°C soaking temperature caused formation of NbC, reduction in hardness due to iced brine quenching and a
large grain size and they can be detrimental to mechanical strength of the alloy and this cycle will make Inconel 718
more prone to microfissuring.

Acknowledgements

The authors would like to acknowledge the support provided by the Department of Metallurgical and Materials
Engineering- National Institute of Technology Tiruchirappalli, School of Mechanical Engineering-VIT University
and Government of India.

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