Graduate Thesis Or Dissertation
 

Synthesis and Characterization of Alkylammonium Salts of Butyltin-Polyoxotungstates for Thin Film Functionalization

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https://ir.library.oregonstate.edu/concern/graduate_thesis_or_dissertations/x059cf628

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  • Metal-oxo clusters are discrete, soluble pieces of bulk metal oxide. Cluster size, monodispersity, and chemical properties allow for potential use as solution-based precursors for functional metal oxide films. Classical monoalkyltin-oxo clusters are either charge neutral or stabilized by anions. The structure of Cs₄.₅H₂.₅[(BuSn)₃(α-SiW₉O₃₇)]*2H₂O enables its use in established ion exchange mechanisms. Three new alkylammonium isolated butyltin-polyoxotungstate species were synthesized and two new alkylammonium isolated phosphotungstate species to compare properties to: TMA₄H₃[(BuSn)₃(α-SiW₉O₃₇)], denoted TMA-BuSn₃W₉ THA₄H₃[(BuSn)₃(α-SiW₉O₃₇)], denoted THA-BuSn₃W₉ THTDA₆H[(BuSn)₃(α-SiW₉O₃₇)], denoted THTDA-BuSn₃W₉ THA₅H2[α-PW₁₁O₃₉], denoted THA-W₁₁ THTDA₆H[α-PW₁₁O₃₉], denoted THTDA-W₁₁ All three structures were characterized in solution by small-angle X-ray scattering (SAXS), electrospray ionization mass spectrometry (ESI-MS), and multinuclear NMR. Thermogravimetric analysis (TGA) was utilized to understand thermal chemistry and to help provide insight into cluster stoichiometry. In addition, all species were spun-cast onto Si(110) and characterized by atomic force microscopy (AFM) and ellipsometry. All other characterization techniques performed were application dependent. Thin film deposition from water-based precursors allows for sustainable fabrication of microelectronic devices. TMA⁺ counterions are ideal candidates for metal-oxo, solution-based precursors due to their size and volatility. Solution characterization of TMA-BuSn₃W₉ suggests that monodispersed, Keggin ion species primarily exist in solution. This work presents deposition of smooth, amorphous films with lithographic potential. The solubility and biocidal nature of polyoxometalate-ionic liquids (POM-ILs) have pioneered the fabrication of antimicrobial, water resistant coatings. Butyltin functionalization presents a unique hybrid POM-IL system for the deposition of smooth, water resistant thin films. Solution deposition of THA-BuSn₃W₉ and THTDA-BuSn₃W₉ allow for durable, conformal coatings displaying the most hydrophobic POM-IL functionalized surfaces to date. In addition, both derivatives exhibit antimicrobial activity towards Gram-negative bacteria, Escherichia coli.
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  • Pending Publication
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  • 2020-05-29 to 2021-06-30

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