Scripta Materialia 45 (2001) 503508

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Formation of MC-c=cH eutectic bers and their eect on stress rupture behavior in D/S Mar-M247LC superalloy
J.S. Baea, J.H. Leea*, S.S. Kimb, and C.Y. Joc
Department of Metallurgy and Materials Science, Changwon National University, Sarim-dong, Changwon 641-773, South Korea b Division of Materials Science and Engineering, Advanced Materials Research Center, Gyeongsang National University, Chinju 660-701, South Korea c High Temperature Materials Laboratory, KIMM, Changwon 641-010, South Korea
a

Received 21 November 2000; received in revised form 2 April 2001; accepted 13 April 2001

Keywords: Solidication; Nickel; Liquids; Interface; Fibers

Introduction Nickel-based superalloys are extensively used in turbine blades and other engine parts on account of their creep strength and resistance to oxidation at elevated temperatures [1]. Mar-M247LC is a modied version of superalloy Mar-M247 with enhanced carbide stability, castability and ductility, achieved by lowering the carbon content. The carbides precipitated at grain boundaries play an important role in the strengthening of grain boundaries at elevated temperatures. Uniformly distributed ne carbides inhibit grain boundary sliding and enhance elevated temperature strength; however, coarse or continuous script-like carbides are detrimental because they serve as crack initiation sites and crack propagation paths [28]. Much attention has been given to the production of aligned brous dispersions of carbides. If the rod phase is strong enough and the matrix phase is suciently ductile, a composite material with high strength and ductility could be obtained [9]. There has been considerable interest in developing in situ composite superalloys, such as TaC or NbC eutectic composites in c matrix, for use at high temperatures [10]. At a relatively low solidication rate of 0.5 lm/s, MC-c=cH eutectic composed of continuous MC bers in the c=cH matrix was found to form in the directional solidication of the Mar-M247LC. The MC-c eutectic could be grown such that it comprised
*

Corresponding author. E-mail address: ljh@sarim.changwon.ac.kr (J.H. Lee).

1359-6462/01/$ - see front matter 2001 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved. PII: S 1 3 5 9 - 6 4 6 2 ( 0 1 ) 0 1 0 4 9 - 1

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more than 60% of the steady state structure of the directionally solidied rod between solid fractions of 0.2 and 0.8. The creep-rupture time of these composite structures proved to be as long as that found for the Mar-M247LC single crystal superalloy in a 196 MPa/982C creep-rupture test.

Experimental A master ingot of Mar-M247LC superalloy was obtained from CannonMuskegon Co. (MI, USA); its nominal composition is shown in Table 1. Mar-M247LC superalloy rods were directionally solidied at a low withdrawal rate of 0:5 lm/s in a modied Bridgeman type furnace at 1630C. Eutectic solidication with a planar solid/liquid interface could be obtained at this solidication rate. An 8 mm OD 5 mm ID alumina tube was used and the growing solid/liquid interface was quenched during directional solidication. Longitudinal and transverse sections of the directionally solidied specimen were polished and etched using Kalling's reagent. The microstructure of the specimen was observed by OM and SEM (JEOL JSM5800). In addition, a 17 mm OD 12 mm ID tube was used to obtain a directionally grown MC-c=cH eutectic sample for high temperature creep-rupture test. In order to evaluate the high temperature creep properties of the MC-c=cH composite, a directionally solidied rod with a diameter of 12 mm was prepared to sucient length such that the composite microstructure was at least 50 mm. The directionally solidied composite was aged at 871C, and the creep-rupture test was carried out according to ASTM E139 (gauge length 23 mm, gauge diameter 4.5 mm) at 196 MPa/982C. The microstructure after creep failure was observed by OM and SEM.

Results and discussion MC-c=cH rod eutectic growth At the low solidication rate of 0.5 lm/s, a planar interface was observed, but the directionally solidied microstructure changed along the rod, where the sample length for the directional solidication was 80 mm. As the directional solidication progressed, the composition of liquid increased due to the segregation of elements (except c phase forming elements). When the solidication fraction reached a certain value, the composition of solid/liquid interface front came to a eutectic composition. The experimental results showed that the c planar interface was formed at low solidication fractions
Table 1 Chemical composition of Mar-M247LC (wt.%) Element Composition C 0.07 Co 9.5 Cr 8 Al 5.5 Ti 0.7 Ta 3.3 Mo 0.5 W 9.4 Zr 0.02 B 0.016 Hf 1.4 Ni Balance

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Fig. 1. Quenched solid/liquid interface morphologies with solidication fractions at 0:5 lm/s. (a) c planar at fs 0:2, (b) MC-c=cH eutectic at fs 0:4, (c) c=cH eutectic at fs 0:95.

fs 0:2, where the MC-c eutectic composite was formed at higher solidication fractions ranging from 0.4 to 0.8. The c=cH eutectic was observed near the end of the rod fs 0:95, as shown in Fig. 1. Table 2 shows the relationship between solidication fraction and solid/liquid interface structure. These results indicate that solidication starts with a c planar structure. As solidication proceeds, the structure changes to MC-c eutectic planar before becoming c=cH eutectic. The sequence of solidication in the sample at fs 0:95 is shown schematically in Fig. 2. This result clearly demonstrates that the nal freezing microstructure in the interdendritic region during Ni-base superalloy solidication is c=cH eutectic. The c phase with a planar solid/liquid interface was formed as an initial transient of the directionally solidied rod, where the c=cH eutectic was formed as a nal transient.
Table 2 Microstructure of the solid/liquid interface at a solidication rate of 0:5 lm/s Solidication fraction fs in 80 mm D/S rod 0.2 0.4 0.8 0.95 Interface structure c planar MC/c eutectic MC/c eutectic c=cH eutectic Carbide shape Octahedral blocky Continuous rod Continuous rod Elongated blocky

Fig. 2. Schematic of the directionally solidied rod quenched at fs 0:95.

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Fig. 3. Micrographs of the MC-c=cH eutectic at fs 0:4 of Fig. 1(b). (a, b) Transverse section, (c, d) longitudinal section.

The MC-c eutectic could form more than 60% of the steady state structure of the directionally solidied rod. Fig. 3 presents a transverse section of the eutectic composite microstructure, where the MC rods are uniformly distributed in the c matrix. It appears that carbides of 23 lm diameter are dispersed at the grain boundaries and throughout the matrix. To observe the accurate morphology of the MC ber, the sample was deeply etched with modied Kalling's reagent. Creep-rupture properties To understand the mechanical properties of the MC-c composite in the directionally solidied Mar-M247LC superalloy, specimens were prepared from a directionally solidied 12 mm diameter rod for creep-rupture testing. The creep-rupture specimens were aged at 872C for 20 h for the cH precipitation in the c phase, which resulted in the MC-c=cH composite. The creep-rupture time for equiaxed, single crystal and MC-c=cH composite structure Mar-M247LC, respectively, is presented in Table 3. The average creep-rupture time for
Table 3 Comparison of creep-rupture times between equiaxed, MC-c=cH composite and single crystal Mar-M247LC alloys Equiaxed [11] Rupture time (h) 74.4 MC/c eutectic composite 116 Single crystal [11] 119.4

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Fig. 4. Micrographs after creep failure. (a, b) OM, (c, d) SEM micrographs. The loading direction was bottom to top. (a) Shows homogeneous crack initiation, (b, c) show that the MC carbides initiate and block cracks, and (d) shows MC carbides free from reaction with the c=cH matrix.

MC-c=cH composite was 116 h at 196 MPa/982C. This value, which was the average of two test results, was comparable to that of the single crystal Mar-M247LC alloy. Longitudinal views after the creep-rupture test are shown in Fig. 4. The creep deformation in the MC-c=cH composite structured Mar-M247LC was found to be very uniform throughout the matrix, as demonstrated in Fig. 4(a). In addition, the grain boundary area of the MC-c=cH composite was largely intact. Such behavior in the MC-c=cH composite structured Mar-M247LC does not resemble that of the typical directionally solidied microstructure, which cracked along the grain boundary ledges that were perpendicular to the direction of load, or the single-crystalline microstructure, which underwent interdendritic fracture during creep deformation. Interestingly, Fig. 4(b) and (c) suggests that the MC carbide bers would eectively block crack growth, as well as acting as crack-nucleating sites. As shown in Fig. 4(c), the coalescence of cracks, as initiated at the interface between ber and matrix, was often stopped by the presence of another ber. Although the rupture life of the composite structure of the alloy was either comparable to, or slightly lower than, that of the single crystal in the present study, the high-temperature mechanical properties of the MC-c=cH composite including creep strain, tensile ductility and fracture toughness may overall exceed those of the single-crystalline counterpart. Moreover, high-magnication SEM observation demonstrated that the carbides in the present alloy were free from any reactions with the matrix even after the creep test, as shown in

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Fig. 4(d). In conclusion, the presence of ne, continuous and in situ carbide bers in the c matrix during solidication could be benecial for the Mar-M247LC alloy by homogenizing the deformation, and blocking crack growth during creep deformation. Further studies are, however, required to quantify the eect of bers on the mechanical properties of Mar-M247LC alloys. Conclusions A MC-c composite structure in Mar-M247LC was obtained by directional solidication at a relatively low growth rate of 0:5 lm/s. As solidication proceeded, the structure changed from c planar to the MC-c eutectic planar before ending up with the c=cH eutectic structure. The MC-c eutectic could be induced to form more than 60% of the directionally solidied rod. The bers of MC carbides were continuous and ne, with diameters of 23 lm. The carbide, as composed of refractory elements in MarM247LC displayed an excellent stability at high temperatures. In the present study, the rupture life of the composite structure of the alloy was observed to be slightly lower than that of single crystal. The creep deformation was, however, extremely uniform in the composite structure. It is therefore possible that the high-temperature mechanical properties (including creep strain, tensile ductility and fracture toughness) of MarM247LC could be improved by use of the MC-c=cH composite structure that provides homogenization of creep deformation and blocking of crack growth during creep deformation. References
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