JOURNAL OF MATERIALS SCIENCE 29 (1994) 2445-2458

Thermal stability of advanced Ni-base

superalloys
H. M. T A W A N C Y , N. M. A B B A S , A. I. A L - M A N A
Metrology, Standards and Materials Division, Research Institute, King Fahd University of
Petroleum and Minerals, PO Box 1639, Dhahran 31261, Saudi Arabia
T. N. R H Y S - J O N E S
Turbine Aerofoils Research and Development and Surface Technology, Rolls-Royce plc,
PO Box 31, Derby DE24 8B J, UK

Exposures consisting of 1 to 900 h at 1000 and 1100 ~ after an ageing treatment of 1 6 h at

870 ~ were used to study the thermal stability of selected y'-strengthened Ni-based
superalloys representing conventional, directional solidification, and single-crystal castings.
Various techniques of microscopy, spectroscopy and diffraction were used to characterize the
microstructure. Primary MC carbides in the alloys studied were found to be stable toward
decomposition into lower carbides. In the aged condition, the strengthening y' phase assumed
a cuboidal morphology; however, all alloys also contained varying proportions of coarse
lamellar y' and hyperfine cooling y'. On an atomic scale, the nature of the cuboidal y'-matrix
interface was found to vary from coherent to partially coherent. However, the overall lattice
mismatch varied from one alloy to another depending upon its composition and the
distribution of various elements in carbide phases and lamellar y' phase. Directional growth of
the cuboidal y' phase upon exposure to higher temperatures was found to be accelerated by a
large initial lattice mismatch leading to a considerable loss of coherency, as indicated by the
observation of dislocation networks around the y' particles. Although the composition of the
y' phase remained essentially unchanged, there was a marked change in matrix composition.
Sigma phase was found to precipitate in all alloys, but its thermal stability was a function of
alloy composition. The initial decrease in hardness followed by a hardening effect during
exposure could be explained in terms of the partial dissolution of the y' phase and
precipitation of sigma phase.

1, I n t r o d u c t i o n Extensive reviews have dealt with the mechanical

Although structural applications of ceramics, com- properties of the y' phase based upon the Ni3A1
posites and intermetallics in gas turbine engines may composition as well as y'-containing alloys [11, 12].
have potential for extending their temperature cap- Typically, the mechanical properties of y'-strength-
abilities [1], it is unlikely that these materials could ened alloys are evaluated after solution annealing, and
replace the superalloys at least in the foreseeable a standard ageing treatment designed to precipitate
future [2]. Improvements in engine thrust, fuel the strengthening y' phase. Subsequent prolonged ex-
consumption and durability continue to be largely posure to higher temperatures, however, ean cause
dependent upo n advances in superalloy technology as significant changes in the volume fraction and mor-
well as cooling systems. Advances in casting-alloy phology of the y' phase [13-19]. Misfit dislocations
development as well as the improvement in melting between the y' and y phases can form readily either
practices have significantly contributed to increasing during prolonged exposure to elevated temperatures
the temperature capabilities of Ni-base superalloys [13] or during plastic deformation [20, 21], resulting
strengthened by the Y' phase [3-6]. Directional solidi- in loss of coherency between the two phases. Other
fication [7, 8] and single-crystal castings [8] are important microstructural changes include precipit-
among the most important techniques developed to ation of topologically close-packed phases such as the
control the microstructure. In most advanced super- sigma phase [20, 21] and decomposition of primary
alloys, the strength of the Y' phase is optimized by ad- carbides [19, 22, 23].
ditions of Ti and Ta, and additional strengthening It was the objective of this investigation to study
of the matrix solid solution (Y phase) is provided by the thermal stability of selected Ni-base superalloys
additions of Mo, W and Re [9, 10]. representing three classes of castings: (i) conventional
0022-2461 9 1994 Chapman & Hall 2445
(Inconel alloy IN 100), (ii) directional solidification Specimens for light optical metallography were
(alloy MAR M 002 DS), and (iii) single crystal (alloys etched in Marble's reagent (10g copper sulphate,
RR 2000 and SRR 99)*. 50 ml HC1 and 50 ml H 2 0 ). As-polished specimens
were used for structural analysis by X-ray diffraction.
Thin-foil specimens for AEM experiments were pre-
2. Experimental procedure pared by the jet polishing technique in a solution
Table I summarizes the nominal chemical composi- consisting of 30% nitric acid in methanol at about
tions of the alloys investigated. As can be seen, alloy - 20 ~ All specimens were examined at 200 kV.
RR 2000 is essentially the single-crystal version of the
cast alloy IN 100 where grain-boundary strengthening
elements such as C, B and Zr are eliminated. Similarly, 3. Results and discussion
alloy SRR 99 is the single-crystal version of alloy 3.1. Microstructure in the aged condition
MAR M 002 DS. Fig. 1 illustrates light optical micrographs and X-ray
Specimens examined were in the form of rods about diffraction patterns derived from the alloys studied
20 mm in length and 8 mm in diameter. All specimens in the aged condition. Occasionally, voids typical of
were heat-treated for 1 h at 1100 ~ in argon atmo- cast metal products were observed, particularly in the
Sphere, air-cooled, aged for 16 h at 870~ in argon single-crystal alloys. All alloys contained MC carbides
and finally cooled in argon. Henceforth, this will be assuming script, cubic and/or semi-rounded morpho-
referred to as the aged condition. The mean blade logies. However, the cubic morphology was parti-
temperature during engine operation is usually about cularly pronounced in alloy MAR M 002 which could
900-1000 ~ but the temperature may locally rise to be related to the presence of Hf [24]; As expected, the
l l00~ due to hot-spot conditions. To cover this polycrystalline alloys (IN 100 and MAR M 002) con-
range, aged specimens were exposed for 1, 8, 24, 100, tained greater densities of MC carbides in compar-
500 and 900h at 1000 and l l00~ to study the ison with their single-crystal versions (RR 2000 and
thermal stability of each alloy. SRR 99).
Light optical metallography, scanning electron In addition to reflections of the matrix (y phase,
microscopy (SEM) and the transmission electron face-centred cubic solid solution), all diffraction pat-
microscopy (TEM) mode of an analytical electron terns contained characteristic superlattice reflections
microscope (AEM) were used to characterize the of the y' phase (L12 supeflattice, face-centred cubic)
microstructure. Structural analysis was conducted by such as the (1 00) and (1 1 0) as shown in Fig. 1. Since
X-ray diffraction using CuK~ radiation. Energy- and the volume fraction of carbide phases in each alloy
wavelength-dispersive X-ray spectroscopy (EDXS was less than about 10%, no carbide reflections were
and WDXS, respectively) were used to determine the observed. As shown in Fig. la, alloy IN 100 had
microchemical composition of bulk specimens in the a random grain orientation; however, because of
SEM. Also, EDXS employing an ultra-thin window the relatively small diameter of the X-ray beam in
detector was used to determine the microchemical comparison with grain size, the intensities of some
composition of thin-foil specimens in the scanning reflections were unusually high. For the directionally
transmission electron microscopy (STEM) mode of an solidified alloy MAR M 002 and the single-crystal
AEM. alloys RR 2000 and SRR 99, the (2 0 0) reflections were
the most intense, reflecting the normal ( 1 0 0 ) growth
T A B L E I Nominal chemical compositions of the alloys studied direction [25].
For all alloys studied, the y' phase assumed three
Element Composition (wt %) distinct morphologies: (i) lamellar, (ii) cuboidal and
(iii) spherical, but the cuboidal morphology was
IN 100 RR 2000 MAR M SRR 99
002 DS
predominant. Coarse lamellar y' was particularly ob-
served near the surface as shown in Fig. 2. Evidently,
Cr 9.5 10 9 8.5 this form of y' had formed during solidification and
A1 5.5 5.5 5.5 5.5 could not be completely redissolved during solution
Ti 4.75 4 1.5 2.2
annealing [25]. Because of the 75-100~ higher
Co 15 15 10 5
Mo 3 3 0.5" 0.5"
melting range of the single-crystal alloys in compar-
W 0.2" 0.5 a 10 9.5 ison with the polycrystalline versions, they contained
Ta - 0.05" 2.5 2.8 greater proportions of lamellar y'.
Hf - 0.05 a 1.25 0.05" Fig. 3 illustrates the cuboidal y' phase providing the
V 0.95 1 - -
main source of mechanical strength and which had
Zr 0.95 0.0P 0.055 0.0P
Fe 1~ 0.1a 0.5 a 0.1 a
formed during thermal ageing. All alloys studied con-
B 0.015 - 0.015 - tained about the same volume fraction of cuboidal
C 0.175 0.015 0.15 0.015 y' (68-70%), estimated metallographically using the
Ni Bal. Bal. Bal. Bal. point counting method [26]. The average particle size
ranged from about 0.32 gm in alloy SRR 99 to 0.63 ~tm
a Maximum. in alloy IN 100. Such a range of particle size is

* Inconel is a registered trademark of the Inco family of companies, MA R M is a registered trademark of Martin Marietta Corporation, while
SRR and RR are registered trademarks of Rolls-Royce plc.

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