Functionalization of Diamond and Its Application in High Performance Liquid Chromatography and Solid Phase Extraction
2010
Functionalization of Diamond and its Application in High Performance Liquid Chromatography and Solid Phase Extraction Gaurav Saini Department of Chemistry and Biochemistry Doctor of Philosophy The primary focus of my work was to chemically functionalize diamond as normal and reversed phases for solid phase extraction (SPE) and high performance liquid chromatography (HPLC). Diamond was functionalized with -NH2 groups via self-limiting adsorption of an amine-containing polymer, polyallylamine (PAAm), onto oxidized diamond particles. The chemical stability of these particles was improved by thermal curing or chemical crosslinking with 1,2,5,6-diepoxycyclooctane. The reversed phase material for SPE was synthesized by reacting amine-functionalized diamond particles with long chain alkyl and a perfluorinated isocyanate. Unlike commercially available silica, functionalized diamond particles were stable under extreme pH conditions (pH 0-14). Functionalized diamond particles were used for SPE, although their lack of porosity resulted in poor analyte capacity. To create materials with greater surface area, core-shell diamond particles were synthesized via layer-by-layer deposition of PAAm and nanodiamond onto solid microdiamond. These particles had higher surface areas than solid diamond particles, and their application in SPE and HPLC was demonstrated. As a related project, I demonstrated microlens array patterning (MAP) for selective adsorption of PAAm during microarray fabrication. Initially, alkyl monolayer terminated silicon surfaces were photopatterned with thousands of wells using a microlens array. PAAm was then deposited in the presence of a cationic surfactant to limit nonspecific adsorption of PAAm. Finally, reactions of selectively adsorbed PAAm were shown with glutaric anhydride, phenylenediisothiocyanate, biotin NHS-ester and an oligonucleotide (DNA). My third project concerned the synthesis of an abrasion resistant hydrophobic coating on the surface of nylon and silicon oxide substrates using chemical vapor deposition (CVD) of two silanes. The synthesis consists of four steps: 1) plasma oxidation of the substrate, 2) treatment with 3-isocyanatopropyltrimethoxysilane, 3) exposure of the treated surfaces to water vapors, and 4) treatment with a perfluorinated silane to make the surfaces hydrophobic. The coating is not visible to the eye and does not change the feel of the surface. Time-of-flight secondary ion mass spectrometry (ToF-SIMS), X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry, contact angle goniometry, scanning electron microscopy (SEM), environmental scanning electron microscopy (ESEM), Rutherford backscattering spectroscopy (RBS) and nuclear reaction analysis (NRA) were used to characterize the resulting materials.
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