Exploration of synthetic methods to crystallize transition metal compounds containing the hydrotris(3,5-dimethyl-1,2,4-triazolyl)borate ligand
The hydrotris(3,5-dimethyl-1,2,4-triazolyl)borate anion ([BH(dmtrz)3]-) was studied to see if it can be used to produce coordination compounds. Single crystals of four coordination compounds, M[BH(dmtrz)3]2 (M = Mn, Fe, Ni, Zn) were grown. M[BH(dmtrz)3]2 crystallized in a triclinic cell. They are 0-D coordination complexes with two ligands octahedrally coordinated to the metal center. The synthesis of compounds containing Co2+ and Cu2+ have not produced single crystals. In an effort to produce single crystals for analysis with single crystal X-ray diffraction, fabrication of a microfluidic device for synthesis using slow diffusion was attempted. Microfluidic device structuring using Liquid Glass, poly(methyl methacrylate) (PMMA), and Teflon/glass tubing was studied. While a microfluidic device was not successfully constructed due problems with solvent flow in the PMMA and Teflon/glass tube systems, and difficulties in the fabrication of the Liquid Glass, the Liquid Glass system shows potential. Differences in size and surface area to mass ratios of the silica nanopowder used (12 nm and 50 mm) may have contributed to the sintering problems that occurred when making the glass structures. SEM analysis revealed that the 12 nm silica used partially sintered at 1300 °C. Further experimentation is required to determine the optimum sintering temperature and temperature program for nanoparticles of that size.