Development of Combinatorial Methods for Alloy Design and Optimization

Abstract

The primary goal of this research was to develop a comprehensive methodology for designing and optimizing metallic alloys by combinatorial principles. Because conventional techniques for alloy preparation are unavoidably restrictive in the range of alloy composition that can be examined, combinatorial methods promise to significantly reduce the time, energy, and expense needed for alloy design. Combinatorial methods can be developed not only to optimize existing alloys, but to explore and develop new ones as well. The scientific approach involved fabricating an alloy specimen with a continuous distribution of binary and ternary alloy compositions across its surface--an ''alloy library''--and then using spatially resolved probing techniques to characterize its structure, composition, and relevant properties. The three specific objectives of the project were: (1) to devise means by which simple test specimens with a library of alloy compositions spanning the range interest can be produced; (2) to assess how well the properties of the combinatorial specimen reproduce those of the conventionally processed alloys; and (3) to devise screening tools which can be used to rapidly assess the important properties of the alloys. As proof of principle, the methodology was applied to the Fe-Ni-Cr ternary alloy system that constitutes many commercially important materials such as stainless steels and the H-series and C-series heat and corrosion resistant casting alloys. Three different techniques were developed for making alloy libraries: (1) vapor deposition of discrete thin films on an appropriate substrate and then alloying them together by solid-state diffusion; (2) co-deposition of the alloying elements from three separate magnetron sputtering sources onto an inert substrate; and (3) localized melting of thin films with a focused electron-beam welding system. Each of the techniques was found to have its own advantages and disadvantages. A new and very powerful technique for rapid structural and chemical characterization of alloy libraries was developed based on high intensity x-radiation available at synchrotron sources such as the Advanced Photon Source (APS) at Argonne National Laboratory (ANL). With the technique, structural and chemical characterization of up to 2500 discrete positions on a library can made in a period of less than 4 hours. Among the parameters that can be measured are the chemical composition, crystal structure, lattice parameters, texture, and grain size. From these, one can also deduce isothermal sections of ternary phase diagrams. The equipment and techniques needed to do this are now in place for use in future combinatorial studies at the ORNL beam line at the APS. In conjunction with the chemical and structural investigations, nanoindentation techniques were developed to investigate the mechanical properties of the combinatorial libraries. The two primary mechanical properties of interest were the elastic modulus, E, and hardness, H, both of which were measured on alloy library surfaces with spatial resolutions of better than 1 m. A nanoindentation testing system at ORNL was programmed to make a series of indentations at specified locations on the library surface and automatically collect and store all the data needed to obtain hardness and modulus as a function of position. Approximately 200 indentations can be made during an overnight run, which allows for mechanical property measurement over a wide range of chemical composition in a relatively short time. Since the materials based on the Fe-Ni-Cr system often find application in highly carburizing and harsh chemical environments, simple techniques were developed to assess the resistance of Fe-Ni-Cr alloy libraries to carburization and corrosion. Alloy libraries were carburized by standard techniques, and the effectiveness of the carburization at various points along the sample surface was assessed by nanoindentation hardness measurement. Corrosion tests were conducted by placing library specimens in highly corrosive aqueous environments, with the corrosion resistance assessed using surface profilometry to measure the local surface recession relative to inert markers. Collectively, the suite of newly developed tools and techniques paves the way for combinatorial design, discovery, and optimization of a wide variety of alloys, thus leading to improved materials in manner that crosscuts the needs of a large number of energy intensive industries. Among those that would be directly impacted are: aluminum, chemicals, forest products, glass, metal casting, petroleum, steel, forging, heat treating, and welding.