Low-temperature solution synthesis of alloys and intermetallic compounds as nanocrystals
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The synthesis of solid state materials has traditionally been accomplished using rigorous heating treatments at high temperatures (1,000°C) to overcome the slow rate of diffusion between two reactants. Re-grinding and re-heating treatments improve the rate of reaction between two solids; however, the high temperatures required to overcome the diffusion barrier limit the products accessible to the most thermodynamically stable phases. In this work, nano-scale solids such as alloys and intermetallics were synthesized via solution techniques where metal compounds are reduced by NaBH4 or n-butyllithium at temperatures below 300°C. To form hollow particles, metal nanoparticles of Co, Ni, Pb were synthesized via reduction by NaBH4 in water and reacted with K2PtCl6, which resulted in the formation of alloys in the case of Co-Pt and Ni-Pt. PbPt intermetallic hollow particles were synthesized by heating a composite of PbO and hollow Pt nanoparticles in tetraethylene glycol (TEG) at 140 °C. With n-butyllithium as a reducing agent, Au3M (M= Fe, Co, Ni) nanoparticles could be synthesized as isolatable solids in the L12 structure. PtSn and AuCu3 intermetallics were synthesized using NaBH4 and TEG. The PtSn and AuCu3 nanoparticles were characterized by transmission electron microscopy in attempts to learn about the phase diagrams of nanoscale solids. The purpose of this work was to synthesize nanoparticles via solution-mediated routes at low temperatures in compositions and morphologies not observed in the bulk, and learn about the phase diagrams of nanoparticles to understand why it is possible to access solids at temperatures significantly below those used in traditional solid state chemistry.
Vasquez, Yolanda (2008). Low-temperature solution synthesis of alloys and intermetallic compounds as nanocrystals. Doctoral dissertation, Texas A&M University. Available electronically from