Graduate Thesis Or Dissertation
 

Syntheses and structures of new inorganic borates

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  • Several new solid-state inorganic borates have been prepared and characterized. Single crystals of the simple orthoborate ScB0₃ were grown and its structure was determined by single-crystal X-ray methods. The new borates Li₃Sc(B0₃)₂, LaSc₃(B0₃)₄, NdSc₃(B0₃)₄, SrNaB0₃, and Li4Ln4MB90₂₃ (Ln = Y, Er, and Gd; M = Al and Ga) were identified from phase analyses in the systems Li₂0-Sc₂0₃-B₂0₃, La₂0₃-Sc₂0₃-B₂0₃, Nd₂0₃-Sc₂0₃-B₂0₃, SrO-Na₂0-B₂0₃, and Li₂0-Ln₂0₃- M₂0₃-B₂0₃. Structural characteristics of these compounds have been established by single-crystal X-ray methods. The orthoborate Li₃Sc(B03)₂ exhibits strings of alternating Sc-centered octahedra and Li-centered rectangular planes. The compounds LaSc₃(B0₃)₄ and NdSc₃(B0₃)₄ are isostructural to other examples of the mineral Huntite. The La derivative crystallizes in a monoclinic space group with no evidence obtained for a phase transition to a higher symmetry variant. The Nd derivative crystallizes in a high symmetry, rhombohedral structure. The structure of SrNaB0₃ is similar to that of the compound K₂CO₃, exhibiting a small distortion of the packing of the Sr²⁺ and 0²⁻ ions from that observed for the Ba²⁺ and 0²⁻ ions in the oxide BaNi0₃. The structure of the compound Li4Ln4MB80₂₃ contains the unique, isolated borate ring [B8₈0₂₀ ]16-. These rings stack over fused rings of Ln-centered square antiprisms to afford one-dimensional channels filled with Li atoms and an orthoborate B0₃ group. Optical properties including fluorescence, infrared absorption, and second harmonic generation have been measured for the compounds Li3Sc(B0₃)₂, LaSc₃(B0₃)₄, and NdSc₃(B0₃)₄. When doped with the ion Cr³⁺, the compounds Li₃Sc(B0₃)₂ and LaSc₃(B0₃)₄ exhibit broad emission bands in the near infrared, indicating the presence of weak crystal fields at the SO⁺ (Cr³⁺) sites. Energy transfer is observed in the doped compound Cr³⁺:NdSc₃(B03)₄; excitation into the Cr ³⁺ absorption band affords strong luminescence only from the Nd3⁺ ion. The low conversion efficiency of the compound LaSc₃(B0₃)₄ for second harmonic generation of the 1064 nm line of a Nd ³⁺ :YAG laser is rationalized from the symmetry characteristics of the calculated components of the hyperpolarizability tensor.
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