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Rapid synthetic routes to refractory intermetallics, transition metal carbides, solid solutions, and hybrid materials

Posted on:1998-06-25Degree:Ph.DType:Thesis
University:University of California, Los AngelesCandidate:Holm, Steven RichardFull Text:PDF
GTID:2461390014474091Subject:Chemistry
Abstract/Summary:
Quite often solid state chemistry is hampered by very long reaction times and high temperatures. This is necessary to overcome the inherently slow mobility and diffusion rates that are present in solids. The bulk of this dissertation describes experiments and reactions schemes to overcome these difficulties.; The second chapter of this dissertation involves the use of sol-gel chemistry which makes it stand out from the rest of the dissertation. This sol-gel route to was used to create a solid lithium electrolyte with an ionic conductivity as high as a liquid. This is can be accomplished through the sol-gel technique because it is very easy to generate a porous silica network whose pores act as a sponge and can be filled with an ionic liquid to achieve a high ionic conductivity. The material was characterized extensively by traditional impedance techniques as well as techniques such as fourier transform infra-red (FTIR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, thermogravimetric analysis (TGA), Mass Spectrometry (MS) and differential scanning calorimetry (DSC) to evaluate the thermal and physical properties of the material.; The remainder of the dissertation is concerned with two high temperature rapid routes to materials which are referred to as solid state metathesis and single displacement reactions. They are most easily described as a mixture of solids which upon local heating react very exothermically to produce highly crystalline products and an easily removable by-product salt. This salt by-product is the main driving force behind these reactions and propels the reactions to temperatures of 1300{dollar}spcirc{dollar}C and higher. The majority of the work is directed towards producing refractory intermetallic phases of transition metal aluminides and transition metal carbides. The materials were characterized mainly through the use of powder X-ray diffraction and SQUID magnetometry when applicable. The dissertation also discusses the flexibility of these reactions towards producing solid solutions of carbides as well as between carbides and nitrides and the benefits gained by conducting these reactions under extreme conditions of confinement with zero free volume allowed for the reactants or products to expand.
Keywords/Search Tags:Solid, Transition metal, Reactions, Carbides
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