Materials Science and Engineering A355 (2003) 114
/125

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Effect of standard heat treatment on the microstructure and

mechanical properties of hot isostatically pressed superalloy inconel
718
G. Appa Rao a,*, Mahendra Kumar a, M. Srinivas a, D.S. Sarma b
a
Defence Metallurgical Research Laboratory, Defence Research and Development Organisation, Ministry of Defence, Government of India, PO
Kanchanbagh, Hyderabad-500058, India
b
Department of Metallurgical Engineering, Institute of Technology, Banaras Hindu University, Varanasi 221 005, India

Received 28 May 2002; received in revised form 2 January 2003

Abstract

Ni
/Fe base superalloy, Inconel 718, was processed through powder metallurgy (P/M) hot isostatic pressing (HIP) route. In order
to balance the strength and ductility, the HIPed material was given the standard heat treatment, viz. solution treatment at 980 8C
for 1 h/water quenched (WQ) to room temperature and a two-step ageing treatment consisting of 720 8C for 8 h/furnace cooling
(FC) at 55 8C h1 to 620 8C and holding at 620 8C for 8 h before air cooling (AC) to room temperature. Optical microscopy and
scanning electron microscopy (SEM) studies on the heat treated alloy have shown a homogeneous microstructure with fine grain size
(25 mm) along with the presence of prior particle boundary (PPB) networks. Transmission electron microscopy (TEM) on the heat
treated material has revealed the presence of oxides, MC carbides and d-precipitates at the grain boundaries and a uniform
precipitation of fine gƒ and g? strengthening phases in the matrix. Tensile and stress rupture tests were performed on the heat treated
material. While the yield strength (YS) and ultimate tensile strength (UTS) of the HIPed and heat treated alloy at room temperature
and 650 8C were comparable to those of conventionally processed wrought IN 718, its ductility was lower. The stress rupture life of
the HIPed alloy improved marginally due to heat treatment and met the minimum specification requirement of life hours but the
rupture ductility was found to be inferior to that of the wrought material. The fractography of the failed samples has revealed the
transgranular ductile mode of fracture in the as-solution treated alloy, while intergranular mode of failure with the decohesion of
PPBs occurred more predominantly in the aged condition. This change of fracture mode with ageing treatment shows the ductility
dependence on the relative strength of the matrix and PPBs. The TEM studies on the deformed alloy have revealed that the brittle
oxides and carbides at the prior particle boundaries coupled with the fine gƒ and g?-precipitates in the matrix are responsible for low
ductility at 650 8C. The investigations of the present study have led to better understanding of the structure
/property relationships
in HIP/heat treated alloy 718 and suggest that the standard heat treatment recommended for wrought IN 718 is not suitable for
HIPed alloy and has to be modified to realise optimum properties.
# 2003 Elsevier Science B.V. All rights reserved.

Keywords: Inconel 718; Isostatically pressed; Standard heat treatment

1. Introduction elevated temperatures, alloy 718 is most widely used in

Inconel 718 is a nickel
/iron base superalloy strength-
ened primarily by ordered body centred tetragonal
(BCT) gƒ-Ni3Nb and ordered face centred cubic (FCC)
g?-Ni3(Al,Ti)-precipitates [1]. Based on its good strength
combined with an excellent resistance to oxidation at
* Corresponding author. Fax: /91-40-4340-683/4341-439.
E-mail address: gouduapparao@rediffmail.com (G.A. Rao).
0921-5093/03/$ - see front matter # 2003 Elsevier Science B.V. All rights reserved.
doi:10.1016/S0921-5093(03)00079-0
aerospace, nuclear and petrochemical industries [2,3]. It
is generally processed through conventional ingot me-
tallurgy route and is available in the bar and sheet
forms. Several advanced melting and casting techniques
have been developed for this alloy, but the melt related
problems such as macro-segregation, formation of
freckles, laves phase and white spots leading to large
scatter in the mechanical properties could not comple-
tely be avoided in wrought products made from big
 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
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ingots [4]. Elimination of such segregation is a time
consuming and expensive process [5]. For an improved
alloy homogeneity and finer microstructure, processing
of alloy 718 via powder metallurgy (P/M) route is
preferred [6]. Hot isostatic pressing (HIP) is one of the
most powerful P/M techniques specially used for con-
solidation of spherical shaped prealloyed powders of
high temperature materials such as nickel base super-
alloys and alloy steels to near net shaped components
with near theoretical density and isotropic properties [7].
It has been well established that a direct HIP approach
for manufacture of intricate shaped components offers
an attractive cost savings since excess material (for
machining) and forging is not needed [8].
By use of P/M(HIP) route a near net shaped integral
turbine rotor from AISI 304 stainless steel has success-
fully been developed in our laboratory. The steel in the
as-HIPed condition has shown the strength and ductility
values much better than that of wrought material.
Therefore, the as-HIPed components could be used in
the impulse type turbine of liquid propulsion engines of
aerospace vehicles. The HIP technology developed for
the steel components was found to be ideally suited for
producing the integral turbine rotors with the desired
properties and substantial cost savings. In view of the
above advantages the development of a very similar
component from a nickel base superalloy Inconel 718
via HIP route has been undertaken. The integral turbine
rotors of alloy 718 are proposed for use in reactive type
turbine of space vehicles with short service life but
subjected to high temperature and high stresses. There-
fore, the material specified for this component is a nickel
base superalloy instead of austenitic stainless steel.
Before making the full size component the prealloyed
powder of IN 718 was consolidated to its near theore-
tical density by HIPing at 1200 8C under 120 Mpa
pressure for 3h. The microstructure and the room
temperature tensile properties of the as-HIPed alloy
were studied in detail and have been reported recently
elsewhere [9]. The ultimate tensile strength (UTS) and
the ductility of HIPed material were comparable to
those of the wrought (forged and heat treated) IN 718,
however, its YS was found to be lower as per the
aerospace materials specification (AMS) 5662G stan-
dard [10]. The lower YS of the material was attributed to
the low volume fraction of gƒ and g? strengthening
precipitates due to the lack of post HIP heat treatment.
In order to improve the mechanical properties, the
HIPed alloy was solution treated at 980 8C for 1 h/
water quenched (WQ). This was followed by a two-step
ageing treatment consisting of 720 8C for 8 h/furnace
cooling (FC) at 55 8C h 1 to 620 8C and holding at
620 8C for 8 h before air cooling (AC) to room
temperature [11]. The microstructure and mechanical
properties of HIP/heat treated material are discussed
in this paper.
115
2. Experimental procedure
The chemical composition and physical properties of
argon atomised alloy 718 powder used in this study are
given in Tables 1 and 2, respectively. The particle
morphology of powder is shown in Fig. 1. The powder
was consolidated by HIPing at 1200 8C under 120 Mpa
pressure for 3h. The details of HIP capsules and the
powder degassing parameters have been reported else-
where [9]. The HIPed material was solution treated at
980 8C for 1 h and then cooled to room temperature by
quenching in water. Subsequently this material was
given a two-step ageing treatment at 720 8C for 8 h
followed by FC at 55 8C h 1 to 620 8C and holding at
620 8C for 8 h before AC to room temperature. For
optical microscopy and scanning electron microscopy
(SEM) examination, the specimens from the heat treated
samples were mechanically polished and etched with a
chemical solution consisting of 50% HCl, 10% HNO3,
2% HF and 38% of distilled water. Thin foils for
transmission electron microscopy (TEM) studies were
prepared from the heat treated and deformed alloys.
Polishing of thin foils was carried out in a Fischionne
twin-jet electro polishing machine using an electrolyte
consisting of 78% methanol, 10% lactic acid, 7% sulfuric
acid and 2% hydrofluoric acid at a temperature of /
30 8C. The foils were examined in a JEOL-200CX
electron microscope operating at 120/160 kV. To
evaluate the tensile and stress rupture properties the
test specimens were prepared from the heat treated
material as per the ASTM-E8 and ASTM-E139 stan-
dards, respectively. The tensile tests were conducted at
room temperature and at 650 8C using an Instron
universal tensile testing machine at a strain rate of
6.56 /10 4 s 1. The stress rupture tests were carried
out at 650 8C under a stress of 690 MPa. The surfaces of
the failed specimens were examined in SEM to study the
fracture characteristics.
Table 1
Chemical composition of IN 718 alloy (wt.%)
Element Gas atomised powder Specification for wrought alloy
samplea (AMS: 5663)
Cr 19.6 17
/21
Fe 18.9 16
/20
Nb 4.7 4.75
/5.5
Mo 3.1 2.8
/3.3
Al 0.5 0.2
/0.8
Ti 0.8 0.65
/1.15
C 0.03 0.08 max
O 275 ppm
/
Ni Balance Balance
a
The powder was manufactured and supplied by M/s. Osprey
Metals Ltd., UK.
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Table 2
Physical properties of gas atomised IN 718 alloy powder

Particle shape Spherical

Size distribution Mesh size (mm) (/106/75) (/75/63) (/63/53) (/53/37) (B/37)
Weight (%) 10.2 8.5 17.7 27.7 35.9
Mean particle size 50 mm (by sieve analysis)
Apparent density 4.18 g cm 3 (51% of theoretical value)
Tap density 5.17 g cm 3 (63% of theoretical value)
Flow rate 20 s per 50 g

and TiO2 particles whereas the carbides were found to

Fig. 1. Particle morphology of gas atomised Inconel 718 superalloy
powder.
3. Results
3.1. Microstructure
The microstructure of the as-HIPed alloy 718 is
shown in Fig. 2. It consists of fine grain structure with
annealing twins and prior particle boundary (PPB)
networks decorated with the oxides and MC carbides.
The oxides at the PPBs have been identified as Al2O3
be enriched with Nb and Ti [9]. The microstructure of
the alloy solution treated at 980 8C per 1 h presented in
Fig. 3 reveals the precipitation of d-Ni3Nb-phase with
acicular morphology at the prior particle boundaries
and at the grain boundaries, however, the d-phase has
globular morphology when present in the matrix. The
thin foils from the solution treated alloy were examined
by TEM. The bright field image in Fig. 4(a) coupled
with the selected area electron diffraction pattern
(SADP) in Fig. 4(b) showed that the austinite matrix
of the solution treated alloy is free from gƒ and g?
coherent precipitates but contained intergranularly pre-
cipitated d-plates. In addition, the presence of very fine
oxides of diameter about 0.1 mm and some randomly
distributed blocky type carbide particles with a diameter
of 0.3 mm at the grain boundaries is visible in the bright
field micrograph presented in Fig. 4(d).
The HIP/solution treated alloy was given the two-
step ageing treatment as per the standard schedule. Fig.
5 shows the typical microstructure of the aged alloy
consisting of prior particle boundaries of shape similar
to that of prealloyed powder particles. The presence of
subgrains within the bigger powder particles is also
evident from the above micrograph. The dark particles
seen at the grain boundary triple points are found to be
the oxides and MC carbides. The grain size measure-
ment of the fully heat treated alloy showed an average

Fig. 3. Microstructure of HIPed Inconel 718 superalloy solution

Fig. 2. Microstructure of as-HIPed Inconel 718 superalloy. treated at 980 8C for 1 h.
 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
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Fig. 5. Optical micrographs of HIPed Inconel 718 superalloy heat

treated as per the standard schedule.

grain size of 25 mm and has been found to similar to

that of the as-HIPed material. The SEM micrograph of
the aged alloy is shown in Fig. 6 to illustrate the
precipitation of d-phase with plate-like morphology at
the PPBs and has created the waviness in the boundaries
of coarser particles. The presence of annealing twins is
also visible in the above micrograph. The TEM study
was carried out on the thin foils prepared from the aged
alloy to better understand its phase structure. The bright
filed image presented in Fig. 7(a) shows the preferential
precipitation of d-phase with plate-like morphology at
the particle boundaries and its tendency to grow
towards grain interior/matrix is also evident from the
above figure. The TEM micrograph presented in Fig.
7(b) reveals the decoration of prior particle boundaries
with MC carbides as well as the precipitation of d-phase
at these boundaries. When compared with as-HIPed
alloy, the carbide population at the PPBs appeared to
increase after heat treatment. Such increase in the
carbide precipitation at the PPBs has also been reported

Fig. 4. TEM micrographs of HIPed Inconel 718 superalloy solution

treated at 980 8C for 1 h. (a) Bright field image shows the grain
boundary d-phase. (b) SAD pattern corresponding to (a). (c) Key to
the SAD pattern in (b). (d) Bright field image shows d-phase, oxides Fig. 6. SEM micrographs of HIPed Inconel 718 superalloy heat
and MC carbides at the grain boundaries. treated as per the standard schedule.
118 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
/125

Fig. 7. TEM micrographs of HIPed Inconel 718 superalloy heat

treated as per the standard schedule. (a) Shows the presence of d-phase
at the prior particle boundaries. (b) Shows the presence of MC
carbides and d-phase at the PPBs.

in HIP/heat treated LC astroloy, which comes under

the g?-strengthened class of Ni-base superalloys [12].
In order to illustrate the morphological characteristics
of the strengthening phases in the fully heat treated
alloy, thin foil micrographs were obtained from the
matrix. Fig. 8(a) and (b) show the typical bright field
image and selected area diffraction pattern of thin film
structure with (001) orientation, respectively. The sec-
ondary diffraction spots in the SADP are due to the
presence of ordered gƒ and g?-precipitates in the matrix.
The (100), (010) and (110) reflections in the SADP are
both due to the gƒ and g?-precipitates whereas, (1/2 1 0) Fig. 8. TEM micrographs of HIPed Inconel 718 superalloy heat
and (1 1/2 0) type reflections are only due to gƒ-phase. treated as per the standard schedule showing the presence of gƒ and g?
The TEM images from the (1 1/2 0) and (110) super- in the matrix. (a) Bright field image. (b) SAD pattern with [001]
orientation corresponding to (a). (c) Key to the SAD pattern in (b).
lattice reflections presented in Fig. 9(a) and (b), respec-
tively, to show the two variants of gƒ-phase. It can be
seen from the Fig. 9(a) that the gƒ-precipitates are disc seen in the above micrograph are found to be the gƒ-
shaped particles with 5 nm thick and 15 nm in diameter precipitates. The round particles with approximately 4.0
and distributed uniformly. Fig. 9(b) consists of both gƒ nm in diameter and faintly visible in the above micro-
and g?-precipitates. The particles with bigger diameter graph are presumably the gƒ-precipitates.
 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
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Fig. 9. TEM micrographs of HIPed Inconel 718 superalloy heat
treated as per the standard schedule. (a) Dark field image with [100]
orientation with 1 1/2 0 reflection showing gƒ precipitates. (b) Bright
field image with [001] orientation with 110 reflection showing gƒ and g?
precipitates.
3.2. Tensile properties
The tensile properties of alloy 718 in the as-HIPed,
solution treated and aged conditions at room tempera-
ture are given Table 3. For the purpose of comparison,
the AMS specification values for wrought (forged and
heat treated) material have also been included in this
Table. These results indicate that after solution treat-
Table 3
Tensile properties of alloy 718 evaluated at room temperature
Material condition Test temperature (8C)
As-HIPed 25
HIP/solution treated 25
HIP/solution treated and aged 25
AMS 5662G specification for wrought material 25
119
ment, there has been a drastic decrease in YS and UTS
of the HIPed material while substantial improvement
( /100%) has taken place in both the % elongation and
% reduction in area. As opposed to this the ageing
treatment has resulted in a considerable improvement of
yield strength (YS) (about 26% over the YS of as-HIPed
material) with a marginal increase in the UTS (about
6%). However, considerable drop occurred in % elonga-
tion (55%) and in % reduction in area (35%). The YS,
UTS and % reduction in area obtained in the present
investigation agree well with those of the specification
for the wrought alloy but the % elongation value is
slightly less for the present investigation.
The tensile properties of the aged material evaluated
at 650 8C, given in Table 4, indicate that the strength
values (YS and UTS) of HIPed alloy 718 are compar-
able to those of conventionally processed wrought
material as per the AMS 5596 standard [10], but the
ductility was extremely poor. There has been about a
12% increase in YS and UTS at 650 8C due to heat
treatment but the % elongation and % reduction in area
have not changed. Surprisingly the ductility values at
650 8C are far less than those obtained at room
temperature.
3.3. Stress rupture properties
The stress rupture properties of the as-HIPed and
HIP/heat treated materials were evaluated at 650 8C/
690 MPa and the data are given in Table 5. These results
indicate that the rupture life of the as-HIPed material
improved considerably due to heat treatment, i.e. from
17 h in the as-HIPed condition to 27 h after heat
treatment and has got the minimum expected life for the
wrought heat treated material. The rupture ductility has,
however, been found to be much less than the specified
value for the wrought material.
3.4. Fractography
The fracture surfaces of the solution treated as well as
the aged materials were examined in SEM. The solution
treated material showed fully dimpled rupture (Fig. 10),
suggestive of a transgranular ductile mode of failure
resulting in the high value of elongation of about 38%
(Table 3). In contrast to this the fracture surface of the
0.2%YS (MPa) UTS (MPa) %EL %RA
993 1334 19.4 22.0
480 975 38 48.6
1260 1413 8.6 16.0
1035
/1167 1275
/1400 12
/21 15
120 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
/125

Table 4
Tensile properties of heat treated alloy 718 evaluated at 650 8C

Material condition Test temperature (8C) 0.2%YS (MPa) UTS (MPa) %EL %RA

As-HIPed 650 907 1028 3.0 6.0

HIP/solution treated and aged 650 1018 1140 3.0 7.7
AMS 5596 specification for wrought material 650 860
/1000 1000
/1200 12
/19 15

aged material showed PPB facets with a few areas of fine

dimples suggesting that failure has taken place due to
the decohesion of PPBs which correspond to a reduced
%EL and %RA (Fig. 11). The fractograph of the aged
sample tested at 650 8C also reveals the presence of PPB
facets and fine dimples in the interior of the grains (Fig.
12). It may be noted that majority of PPB facets seen in
the above figure are of the boundaries of fine size
powder particles and appear to be smooth when
compared with those of coarser particles. This suggests
that the boundaries pertaining to fine powder particles
become more brittle at 650 8C than those of coarser
ones. The presence of fine dimples in the interior of
coarser grains indicates the formation of micro voids at
the matrix
/precipitate interface.
Fig. 10. Fractograph of HIPed and solution treated Inconel 718
3.5. TEM of deformed alloy
superalloy specimen tensile tested at room temperature.

To understand the low ductility of the heat treated

Fig. 11. Fractograph of HIPed and standard heat treated Inconel 718
superalloy tensile specimen tested at room temperature.
alloy as compared with the as-HIPed alloy, TEM studies
have been carried out on the gauge portion of the tensile
samples. Fig. 13(a) and (b) are TEM micrographs from
the as-HIPed alloy deformed at room temperature. The
slip traces as well as the high dislocation density with
extremely fine precipitation of gƒ and g? strengthening
phases are clearly visible in Fig. 13(a). Fine precipitates
are seen along the PPB at which the slip has been
obstructed is seen in Fig. 13(b). This alloy has a high
ductility of 19.4% (Table 3).
Fig. 14(a) and (b) are TEM micrographs from the
HIPed and heat treated alloy deformed at room
temperature. Fig. 14(a) shows slip traces as in Fig.
13(a) but the difference is that in addition to fine
spherical carbides, there has been some grain boundary
d-precipitation. Precipitation of gƒ and g? also occurs in
the matrix as shown in Fig. 14(b). The TEM micro-
graphs of the HIPed and heat treated alloy deformed at
650 8C are shown in Fig. 15(a) and (b). Coarse PPB

Table 5
Stress rupture properties of superalloy 718

Material condition Test conditions Rupture life %EL

As-HIPed 650 8C/690 MPa 17 h 1.0

HIP/solution treated and aged 650 8C/690 MPa 27 h 2.1
AMS 5596 specification for wrought material 650 8C/690 MPa 23 min 4.0 min
 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
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Fig. 12. Fractograph of HIPed and standard heat treated Inconel 718
superalloy tensile specimen tested at 650 8C.
Fig. 13. TEM micrographs of as-HIPed Inconel 718 superalloy tensile
specimen tested at room temperature. (a) Bright field image from the
gauge portion of the deformed specimen shows the slip traces and high
dislocation density with fine precipitation of strengthening phases. (b)
Bright field image from the gauge portion of the deformed specimen
shows the obstruction of slip at the PPBs.
121
Fig. 14. TEM micrographs of HIPed and standard heat treated
Inconel 718 superalloy tensile specimens tested at room temperature.
(a) Bright field image from the gauge portion of the deformed specimen
shows slip traces and d-phase at the PPBs. (b) Bright field image from
the gauge portion of the deformed specimen shows extensive pre-
cipitation of strengthening phases in the matrix.
precipitates are seen in Fig. 15(a) while much coarser
plates of d are seen prominently in Fig. 15(b). It appears
that the brittle oxide and carbide particles at the PPBs
coupled with the extremely fine gƒ and g? precipitates in
the matrix that result in high strength (HS) are
responsible for low ductility of the alloy at 650 8C.
4. Discussion
The structure and properties of the HIPed alloy have
been reported recently by us elsewhere [9]. The alloy
consists of a highly homogeneous microstructure (Fig.
2) with an average grain size (25 mm) much finer than
that of conventionally processed wrought alloys (100
mm). In the as-HIPed condition, the UTS and ductility
values of the alloy were comparable to that of wrought
heat treated material but the YS is lower due to the lack
of extensive precipitation in the present as-HIPed alloy
(Table 3). In order to improve the mechanical proper-
122 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
/125
Fig. 15. TEM micrographs of HIPed and heat treated Inconel 718
superalloy tensile specimen tested at 650 8C. (a) Bright field image
from the gauge portion of the deformed specimen shows the presence
of coarse precipitates at the PPBs. (b) Bright field image from the
gauge portion of the deformed specimen shows the coarse d-
precipitates at the PPBs.
ties, a standard heat treatment was given to the HIPed
material. It was observed that the initial grain size of the
HIPed alloy was not altered due to the standard heat
treatment. The similar grain sizes observed in the HIPed
alloy before and after heat treatment are attributed to
the presence of prior particle boundaries decorated with
Al2O3 and TiO2 particles as well as the MC carbides,
which will impede grain growth. In addition, the
precipitation of grain boundary d-phase during solution
treatment at 980 8C also contributes to the retardation
of grain growth. It may be noted that the grain size of
the HIPed material is dictated by the initial powder
particle size as the fine powder will have smaller grains
than those of coarser ones. As a result, the HIPed
products produced from fine powder result in finer grain
size than that obtained from the coarser ones.
Wrought products of alloy 718 intended for HS
applications at intermediate temperatures /650 8C
are need to have grain sizes of ASTM 10 or even better
[13]. However, due to the initial coarser grain size of
ingots (ASTM-4 or coarser), achieving such a fine grain
structure in the wrought products is found to be difficult
by standard processing (SP) and HS processing routes.
In SP, the alloy is forged at 1100 8C and the forge
reduction will be about 30%. Subsequently the forged
components are heat treated as per the standard
schedule consisting of solution treatment at 980 8C
per 1 h followed by two-step ageing at 720 8C per 8 h
per furnace cooled to 620 8C and holding at 620 8C per
8 h and air cooling to room temperature. Since forging
operation is carried out well above the d-Ni3Nb solvus
temperature of 1010 8C the grain growth is unimpaired
by the d-precipitates in this process. The average grain
size of the standard processed components would be
about ASTM 5. This process is found to be used for
making the components with complex geometry. To
improve the alloy strength by grain size refinement, the
HS processing is adopted. In this route the forging is
carried out at 1050 8C and the forge reduction will be
about 50%. The forged components are heat treated as
per the standard schedule as mentioned earlier. Due to
the reduced forging temperature, the grain size of the
HS processed components is usually finer than that
realised by SP and conforms to ASTM 8.
In order to produce still finer grain size, a direct age
(DA) processing technique has, therefore, been estab-
lished for alloy 718 [14], in which forging of components
is performed at d sub solvus temperature /950 8C with
an increased forge reduction usually more than 50%.
The forged products are given the standard two-step
ageing treatment with out going in for solutioning of
grain boundary delta. As a result, DA processed
components exhibit fine grain size of ASTM 10 and
higher fatigue strength. However, this technique is
limited to geometrically simple shapes due to low
forging temperatures and the initial coarse grain struc-
ture. This limitation can be overcome by use of HIPed
billets, which are more amenable to deformation at
lower temperatures due to their initial fine grain size
(ASTM 8 or better). Very recently Habel et al. [15]
reported that the P/M (HIPed) superalloys with a
significantly reduced tendency for grain growth can
allow higher forging temperatures and, therefore, re-
quires lower forging loads. Watwe et al. [16] demon-
strated the grain growth insensitivity of large P/M 718
billets to preheating and the slow cooling conditions of
forging. This shows the potential of fine grain size
HIPed alloy 718 billets or preforms for making the
critical components with complex geometry by super-
plastic forming which results in improved fatigue
properties. It has been also been reported [17], that the
fine grain size of the HIPed material is an added
advantage for improved ultrasonic inspectability of
near net shaped components due to substantially
reduced noise level.
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The precipitates found in the matrix and at the grain
boundaries of HIP/heat treated alloy 718 are very
similar to those of conventionally processed wrought
material; except that that the presence of PPB networks
in this alloy. These networks are an undesirable micro-
structural feature of the HIPed nickel base superalloys
and their presence has been attributed to the high
oxygen content of the prealloyed powder [18]. But it
may be noted that the PPBs do not form in the HIPed
alloys like AISI-304 stainless steel though the oxygen
content of the powder is as high as 400 ppm [19]. The
reason for this is that the formation of stable oxides does
not occur on the powder particle surface since the steel is
free from the elements such as Al, Ti, and Zr which have
a strong affinity for oxygen. The microstructure of the
as-HIPed steel has, therefore, been found to be as good
as that of the wrought (forged and annealed) steel and
its mechanical properties were much better than their
wrought counterparts. Apart from the composition and
oxygen content, the HIP processing parameters also
govern the PPB precipitation in nickel base superalloys.
The higher HIPing temperature results in lower con-
centration of PPB networks than that could be achieved
with lower temperature [20]. However, high HIPing
temperature followed by slow cooling rates to room
temperature tend to show an increased PPB precipita-
tion because more time is available for the diffusion of
Al, Ti and C from the grain interior to the boundaries.
Secondly, the carbides dissolved at high temperature
tend to reprecipitate in more continuous form during the
slow cooling stage [21]. Therefore, a HIP system
provided with a fast cooling arrangement would be
ideal for exploiting the advantages of high HIPing
temperature.
Solution treatment at 980 8C for 1 h has shown
intergranular precipitation of d-phase with acicular
morphology, while it has a globular morphology when
present within the matrix (Fig. 3). The d is an incoherent
precipitate and does not contribute to alloy strengthen-
ing. But it is found to be desirable for grain size control
during processing and heat treatment of the wrought
alloy. The presence of d-phase at the grain boundaries
has been reported to be beneficial for enhanced ductility
and toughness [22]. Very recently Valencia et al. [23],
reported that the stress rupture ductility of powder
injection moulded and sintered alloy 718 increased as
the volume fraction of grain boundary d increased with
some compromise on rupture life. This is in conformity
with the earlier observations of Merrick et al. [6], that
small quantities of acicular d-phase at the grain bound-
aries of P/M extruded alloy has conferred an irregular
morphology to the grain boundaries and thereby
restricted grain boundary sliding and improved rupture
ductility. In the absence of d-phase at the grain
boundaries, only fine gƒ and g? precipitates form and
hence the grain boundaries more or less remain straight
123
which provides an easy path for crack propagation and
notch brittleness. Chen et al. [24], have investigated the
effect of the density of grain boundary d-precipitates r
on the creep deformation behaviour of wrought alloy
718. Their investigations have revealed that the rupture
time and total creep strain decrease with increase in the
value of r when its value is below about 45%. However,
when the value of r is above 45% both rupture time and
creep strain tend to increase with increase in r and
attain a much higher values for r of 70% than that of
the material free of grain boundary d-precipitates.
Thin foils from the HIP/heat treated alloy were
examined by TEM, however, the strengthening precipi-
tates could not easily be resolved in bright field
image(Fig. 8(a)). This has been attributed to the high
density of precipitates causing excessive coherency strain
field contrast around the individual particles. However,
by use of selected area electron diffraction and dark field
imaging methods the morphology, size and distribution
of gƒ and g? strengthening phases in this alloy could be
established. A typical [001] diffraction pattern in Fig.
8(b) revealed the presence of both gƒ and g?. The
superlattice reflection of (1 1/2 0) clearly showed the
disc shaped gƒ-precipitates with fine size(Fig. 9(a)), while
the superlattice reflection of 110 could illustrate the
spherical morphology of the g? with relatively smaller
diameter than that of gƒ-precipitates(Fig. 9(b)). The
morphological characteristics of gƒ and g?-precipitates
are very similar to those of wrought IN718 reported by
Paulonis et al. [25]. However, the size of these particles
are finer than that of wrought IN 718 and the
precipitates have been found to be well distributed.
This shows the enhanced degree of alloy homogeneity
due to the use of fine powders that normally encounters
faster cooling kinetics during atomisation when com-
pared with that for a large size ingot [26]. The disc
shaped gƒ (Ni3Nb) is the principal strengthening phase
in alloy 718. The presence of round shaped g?-Ni3(Al,Ti)
precipitates also contribute to the alloy strengthening.
Due to the presence of small particles with different
morphology, there is no need of bimodal distribution of
precipitates in alloy 718 where as such distribution is
mandatory for g? strengthened Ni-base superalloys for
better creep performance. The gƒ usually forms at a
higher temperature of ageing (720 8C) while the pre-
cipitation of g? takes place at the lower temperature of
ageing (620 8C) [27]. Both the phases are metastable and
at higher temperature usually more than 650 8C the gƒ
coarsens very fast and transforms into either g? or
orthorhombic d [28]. As a result, the alloy loses its
strength and thus the applications of alloy 718 is limited
to 650 8C.
The tensile properties of the alloy in the as-HIPed,
solution treated and aged conditions were compared to
correlate the strength and ductility values with micro-
structure. The strength values (YS and UTS) of HIPed
124 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
/125
alloy decreased drastically after solution treatment while
there has been a substantial improvement in its ductility
(Table 3). The lower strength values associated with
higher ductility are obviously due to the dissolution of
gƒ and g?-phases during solution treatment. It can be
seen from the above Table that the YS of the alloy has
substantially been increased on ageing and is even
higher than that of the heat treated wrought IN 718,
while the UTS values are comparable. The improvement
in the YS is due to the extensive precipitation of gƒ and
g?. The YS and UTS of the HIPed material at 650 8C
are comparable to those of the wrought alloy (Table 4).
The high YS of the HIPed material can be attributed to
its fine grain size coupled with more uniform precipita-
tion of strengthening phases [29]. Comparison of the
tensile properties of the alloy in the three different
conditions clearly indicates that the ductility of the
material is closely related to the relative strength of the
prior particle boundaries and the matrix. The dissolu-
tion of gƒ and g? matrix strengthening precipitates
during solution treatment led to the substantial increase
in the %EL and %RA values while their precipitation on
ageing resulted in lower %EL and %RA. In either case
the PPB precipitates remained the same. Deterioration
of ductility at elevated temperature can be attributed to
the presence of PPBs decorated with oxides and MC
type carbide particles resulting in the premature failure
[30
/32].
The drop observed in the ductility of aged material
clearly correlates with the fracture mode associated with
the failed specimens, which showed the predominance of
fracture along the prior particle boundaries (Figs. 11
and 12). The PPBs are decorated with the brittle oxides
and MC type carbides [9,33]. As a result, the deforma-
tion is localised at the PPBs due to the difficulty in
transfer of slip across them. This leads to the break
down of slip compatibility at the incoherent particle
matrix interfaces, which becomes a favourable site for
void nucleation [34]. Since the oxides and the carbide
particles are closely spaced all along the prior particle
boundaries (Fig. 15), they provide a continuous path for
crack propagation and ultimately lead to intergranular
fracture with reduced ductility. On the other hand, the
solution treated material (Fig. 10) has shown the
predominance of a ductile transgranular mode of
fracture coupled with substantial improvement in the
ductility. It may be noted that solution treatment at
980 8C for 1 h, hardly has any effect on the PPB
networks as they have been decorated with the stable
oxides (Al2O3 and TiO2) and MC type (Nb, Ti) C
carbides. Although the PPBs were present in the
solution treated alloy, fracture did not occur along
these boundaries. This is because the matrix has become
much softer than the PPBs due to the dissolution of gƒ
and g? strengthening phases during solution treatment.
The softer matrix could relax the stress concentration at
the PPBs during deformation. This has delayed the
fracture and allowed the material to deform well and
finally led to a transgranular mode of failure. Based on
these observations it could be inferred that the low
ductility of the HIP/heat treated alloy 718 is closely
related to the relative strengths of the matrix and PPB
networks.
The stress rupture properties of the alloy showed a
marginal improvement in rupture life due to the heat
treatment as per the standard schedule (Table 5). While
this improvement is attributed to the alloy strengthening
due to the precipitation of gƒ and g? during ageing, the
grain boundary d-precipitation that resulted from the
solution treatment is considered to be responsible a
moderate improvement in the rupture ductility. Several
investigators have reported earlier a considerable im-
provement in the ductility when the volume fraction of
grain boundary d-phase was increased [6,23], by giving a
high temperature ageing treatment ( /870 8C for 4 h).
However, ageing at the above temperature for a longer
period would cause gƒ coarsening and formation of
precipitate free zones, which will affect the alloy
strength. Since the HIPed alloy consisted of PPBs
decorated with the stable oxides and brittle carbides,
variation in size and volume fraction of grain boundary
d- may not show a significant effect on rupture ductility.
However, the dissolution of PPB precipitates and
disruption of the networks would result in overall
improvement of properties. Therefore, the recom-
mended heat treatment for wrought alloy is not
adequate for HIP processed alloy 718 and has to be
modified to realise optimum properties.
5. Conclusions
Hot isostatically pressed Inconel 718 superalloy heat
treated as per the AMS 5662 standard schedule for
wrought material has shown a homogeneous phase
structure with a fine grain size coupled with the PPB
networks.
The uniform precipitation of gƒ and g?-phases during
heat treatment has resulted in substantial improvement
of YS and slight improvement in UTS in HIPed alloy
and were found to be better than those of wrought IN
718. However, the presence of brittle oxides and
carbides at the PPBs coupled with fine gƒ/g? precipi-
tates in the matrix have led to a lower ductility.
The stress rupture life and ductility of the alloy have
also improved marginally after heat treatment and has
got the minimum expected life for wrought heat treated
IN 718, however, the rupture ductility was found to be
much less than the specified value. This suggest that the
recommended heat treatment for wrought alloy is not
suitable for HIP processed alloy and has to be modified
to realise optimum properties.
 G.A. Rao et al. / Materials Science and Engineering A355 (2003) 114
/125
Acknowledgements
The authors gratefully acknowledge the Defence
Research and Development Organisation (DRDO) for
providing the financial support for this study. The
authors would like to thank Dr D. Banerjee, Director
DMRL for his constant encouragement for this study.
Thanks are also due to Y.N. Chary, P. Ravinder Rao, P.
Raja Rao, John David, Dr K. Satya Parasd and D.G.
Deshpande for their technical support in the experi-
mental work.
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