A study on the formation of solid state nanoscale materials using polyhedral borane compounds

Date of Award


Degree Type


Degree Name

Doctor of Philosophy (PhD)




James T. Spencer


Titanium boride, Thin films, Aerosol pyrolysis, Carborane dicarboxylic acid, Boron-dopped carbon nanotubes, Carborane metal organic frameworks, Metal borides

Subject Categories



The formation of boron containing materials using a variety of methods was explored. The pyrolysis of a metal boride precursor solution can be accomplished using a one-source method by combining TiCl 4 , B 10 H 14 and CH 3 CN in one reaction vessel and pyrolyzing it at temperatures above 900 °C. Amorphous dark blue colored films were obtained after the pyrolysis reactions. Well-defined spherical shaped grains or particles were observed by SEM. The amorphous films generated contained titanium, however, the determination of the boron content of the films was inconclusive. This one pot method making metal boride thin films has the advantage of being able to dictate the stoichiometry of the reactants.

Another part of this work represents the first report of both the use of metal boride materials and the use of a titanium-based compound for the formation of nanotubes. This method provides a facile method for generating well-formed boron-containing carbon nanotubes in a "one-pot" process through an efficient aerosol process.

The formation of metal boride corrosion resistant layers was also explored. It was shown that metallic substrates can be effectively boronized using paste mixtures containing boron carbide and borax. The formation of a Fe 4 B 2 iron boride phase was achieved, however, this iron boride phase does not give enough corrosion protection. The formation of a corrosion resistant metal boride coating with strong adhesion was accomplished by boronization of a thermal sprayed nickel layer on the surface of steel.

Surfactants were explored as possible nanoreactors in which metal boride nanoparticles could be formed to use as nanotube growth catalyst via room temperature reaction. Different surfactants were used, but none of them successfully generated very well dispersed metal boride nanoparticles. Nanoparticles with varying shapes and sizes were generated which were highly amorphous.

The carboxylic acid derivative of closo -C 2 B 10 cages was explored as a ligand in the hydrothermal preparation of coordination polymers with zinc salts. It was found that the stability of the cage is apparently insufficient under these conditions and cage degradation was observed. Consequently, a preliminary investigation of the preparation of dipyridyl derivatives of both the closo -C 2 B 10 and the closo -B 12 cages was performed.


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