Browsing by Subject "Inorganic"
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Item A thermogravimetric study of some gas-solid reactions(Texas Tech University, 1964-08) Nesbitt, Lyle EdwinNot availableItem An investigation of the system PbO-Cr2O3(Texas Tech University, 1961-05) Schaefer, Weldon ErnestNot availableItem Non-aqueous potentiometric titrations of weak acids(Texas Tech University, 1969-08) Sparks, Roy LynnNot availableItem Photocurable Inorganic-Organic Hydrogels for Biomedical Applications(2011-02-22) Hou, YapingThere are two primary objectives of this dissertation research. The first objective was to prepare a library of inorganic-organic hydrogels from methacrylated star polydimethylsiloxane (PDMSstar-MA) and diacrylated poly(ethylene oxide) (PEO-DA) with tunable chemical and physical properties for use as tissue engineering scaffolds. These inorganic-organic hydrogels provide a useful platform to study the effect of scaffold properties on cell behavior in tissue culture. Twenty compositionally unique hydrogels were prepared by photo-crosslinking varing molecular weights (Mn) of PEO-DA (Mn = 3.4k and 6k g/mol) and PDMSstar-MA (Mn = 1.8k, 5k and 7k g/mol) at varying weight ratios (up to 20 wt% PDMSstar-MA). Introduction of PDMSstar-MA caused formation of discrete PDMS-enriched "microparticles" dispersed within the PEO hydrogel matrix. The swelling ratio, mechanical properties in tension and compression, non-specific protein adhesion and cytotoxicity of hydrogels were studied. The second objective was to prepare thermoresponsive nanocomposite hydrogels, which are mechanically robust and can remove adhered cells via thermal modulation. Such hydrogels may be useful as "self-cleaning" membranes for implanted biosensors to extend their lifetime and efficiency. These hydrogels are comprised of a poly(Nisopropylacrylamide) (PNIPAAm) hydrogel matrix and polysiloxane colloidal nanoparticles (~220 nm and 50 nm ave. diameter). Due to the low preparation temperature, the nanocomposite hydrogels exhibited a homogeneous morphology by SEM analysis. The volume phase transition temperature (VPTT, ~33 degrees C) of the nanocomposite hydrogels was not altered versus the pure PNIPAAm hydrogel, which is near body temperature. Generally, nanoparticles led to improve mechanical properties versus pure PNIPAAm hydrogels. When these nanocomposite hydrogels are heated above the VPTT, they become more hydrophobic. When they are reversibly switched from a water-swollen to a deswollen state, the change in surface properties, as well as swelling-deswelling, was effective upon the removal of adhered cells.Item Ring size interconversions of cyclopolyphosphines(Texas Tech University, 1982-05) Pirakitigoon, SukonNot availableItem Synthesis and characterization of n-heterocyclic phosphenium and arsenium salts(2011-05) Hoberg, Clint R.; Cowley, Alan H.; Holliday, Bradley JTwo ligand types were employed for the one-step preparations of heavy group 15 cations, namely, diazabutadiene (DAB) and bis(imino)acenaphthene (BIAN). By exploiting the redox properties of these ligands, in conjunction with two different synthetic strategies, it was possible to synthesize a variety of phosphenium and arsenium salts in relatively high yields. The first synthetic method took advantage of the known equilibrium between PI/PI3 in solution. The second synthetic route employed SnCl2 as the reducing agent for converting the reactive trihalides ECl3 into the corresponding “ECl” moieties (E = P, As).Item Synthesis and characterization of patterned surfaces and catalytically relevant binary nanocrystalline intermetallic compounds(2009-05-15) Cable, Robert E.As devices and new technologies continue to shrink, nanocrystalline multi-metal compounds are becoming increasingly important for high efficiency and multifunctionality. However, synthetic methods to make desirable nanocrystalline multi-metallics are not yet matured. In response to this deficiency, we have developed several solution-based methods to synthesize nanocrystalline binary alloy and intermetallic compounds. This dissertation describes the processes we have developed, as well as our investigations into the use of lithographically patterned surfaces for template-directed self-assembly of solution dispersible colloids. We used a modified polyol process to synthesize nanocrystalline intermetallics of late transition and main-group metals in the M-Sn, Pt-M?, and Co-Sb systems. These compounds are known to have interesting physical properties and as nanocrystalline materials they may be useful for magnetic, thermoelectric, and catalytic applications. While the polyol method is quite general, it is limited to metals that are somewhat easy to reduce. Accordingly, we focused our synthetic efforts on intermetallics comprised of highly electropositive metals. We find that we can react single-metal nanoparticles with zero-valent organometallic Zinc reagents in hot, coordinating amine solvents via a thermal decomposition process to form several intermetallics in the M??-Zn system. Characterization of the single-metal intermediates and final intermetallic products shows a general retention of morphology throughout the reaction, and changes in optical properties are also observed. Following this principle of conversion chemistry, we can employ the high reactivity of nanocrystals to reversibly convert between intermetallic phases within the Pt-Sn system, where PtSn2 ? PtSn ? Pt3Sn. Our conversion chemistry occurs in solution at temperatures below 300 ?C and within 1 hour, highlighting the high reactivity of our nanocrystalline materials compared to the bulk. Some evidence of the generality for this process is also presented. Our nanocrystalline powders are dispersible in solution, and as such are amenable to solution-based processing techniques developed for colloidal dispersions. Accordingly, we have investigated the use of lithographically patterned surfaces to control the self-assembly of colloidal particles. We find that we can rapidly crystallize 2-dimensional building blocks, as well as use epitaxial templates to direct the formation of interesting superlattice structures comprised of a bidisperse population of particles.Item Synthesis and material properties of supramolecules containing fluorinated organomercurials(2009-05-15) Taylor, Thomas JacksonThis dissertation details the synthesis and analysis of novel supramolecular species that feature simple fluorinated organomercurials, such as trimeric perfluoroortho- phenylene mercury ([o-C6F4Hg]3). These organomercurials can complex a variety of unsaturated substrates including arenes and alkynes. The major emphasis was on developing molecular architectures that are held together in part by secondary Hg-Calkyne interactions. Diphenylpolyynes, hydrocarbons featuring extended regions of unsaturation, were found to complex with [o-C6F4Hg]3 in a series of adducts. While the internal structures of the hydrocarbons themselves were found to be basically unaltered, within the crystals the polyynes were physically separated from one another by intervening molecules of [o-C6F4Hg]3, preventing them from cross-linking. This leads to a substantial stabilizing effect, for example [o-C6F4Hg]3 and Ph(CC)4Ph form a 2:1 adduct that is stable at temperatures up to 120 ?C above the pure hydrocarbon. Adducts of [o-C6F4Hg]3 and molecules containing a 1,3,5-triethynyl benzene core display a variety of novel properties. 1,3,5-tris(trimethylsilylethynyl) benzene forms binary supramolecular stacks with [o-C6F4Hg]3. The structure also displays large cylindrical 1-dimensional cavities. These cavities are lined with non-polar groups, have an internal diameter of 6.2 ?, and remain stable in the absence of guests. The compound readily interacts with and reversibly adsorbs simple alkanes. 1,3,5-tris(phenylethynyl) benzene forms similar stacks with [o-C6F4Hg]3, albeit without the cavities. Upon irradiation with visible and ultraviolet light, this adduct emits a long-lived emission that was hitherto unreported. From computer calculations and lifetime measurements, it appears this radiation is the phosphorescence of the pure hydrocarbon. Intensive structural studies have also been performed on adducts containing polyaromatic compounds, including phenanthrene, and the organomercurials [o- C6F4Hg]3, pentafluorophenyl mercury chloride and bromide. These experiments were performed to determine if Lewis acid-p complexes could be made with monofunctional mercury compounds. Polyaromatic hydrocarbons, such as phenanthrene and diphenylacetylene, were used as the substrates for these investigations. While all the mercurials formed adducts with the substrates, the photophysical measurements were not uniform and indicate that [o-C6F4Hg]3 has a stronger heavy-atom effect because of the cooperativity of the three mercury atoms.