Chemically induced reduction: A viable process for synthesizing γ-TiAl based intermetallic matrix composite powders containing nanocrystalline TiC

Abstract

A chemically induced reduction process has been developed for synthesizing intermetallic matrix composites (IMCs) consisting of titanium aluminide and titanium carbide. The process involves the reduction of metal chlorides (TiCl4 and AlCl3) with metallic lithium in polar organic solvents such as acetonitrile (MeCN) and tetrahydrofuran (THF) to form a colloidal precursor. The as-prepared precursors have been either directly heat treated in ultra-high-purity argon (UHP-Ar) or pretreated in hydrogen (H2) followed by further heat treatment in UHP-Ar. The powders have been characterized primarily using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Results of the structural analyses conducted on the heat-treated precursors derived using MeCN as a solvent indicate the formation of either single-phase titanium carbide (TiC) or a composite mixture of γ-TiAl and nanocrystalline TiC, depending on the heat-treatment conditions. The formation of TiC is related to the strong interaction between TiCl4 and the polar organic solvents, resulting in the formation of adducts which contain primary Ti-C linkages. Pretreatment of the precursors derived using MeCN as a solvent in H2 promotes the removal of carbon and results in the formation of the composite mixture of γ-TiAl and TiC after subsequent Ar treatment at 1200 °C. At this stage, washing the pretreated powders in water helps to minimize and even eliminate any impurity phases to a large extent, leaving behind phase-pure composites containing γ-TiAl and TiC after the final Ar treatment. However, extended pretreatment in H2 appears to be ineffective toward removal of additional carbon and leads to formation of hydride-phase impurities. On the other hand, the reductive reaction conducted using THF as a solvent results in minimizing the amount of carbon while inducing the formation of γ-TiAl during direct Ar treatment of the precursors. This is because of the weaker interaction between TiCl4 and THF. Transmission electron microscopy was used to characterize the size distribution of the constituent phases. The analysis shows that the composite synthesized using these chemical approaches consist of discrete nanocrystalline TiC particles (<20 nm) that are uniformly distributed intermixed with submicron sized γ-TiAl (0.1 to 0.2 µm). Thus, the new chemical process proposed in this study demonstrates the potential for synthesizing in situ composites containing fine distribution of γ-TiAl and nanocrystalline TiC. Such composites could potentially exhibit unique mechanical properties and deformation behavior useful for high-temperature structural applications.