Preparation and structural studies of the hydrolysis products of titanium, niobium and zirconium alkoxides

Technical Report · Fri Jul 01 04:00:00 EDT 1977

OSTI ID:7295171

Peercy, P S; Dosch, R G; Morosin, B

Raman scattering, analytical and x-ray techniques were used to investigate the structural units in amorphous hydrolysis products of the alkoxides of Nb, Ti and Zr and in the corresponding sintered materials. These materials are used for ion exchange in the proposed radioactive waste disposal process. The starting solution for the Nb system yielded crystals containing (Nb/sub 10/O/sub 28/)/sup 6 -/ ions as the basic structural unit; however, this form for the polyniobate ion was not observed in any other stages of the synthesis or in any phase of the ion exchange material after sintering. The two crystalline phases of the Nb ion exchange material which occur on sintering were determined to be Na/sub 2/Nb/sub 4/O/sub 11/ and Na/sub 13/Nb/sub 35/O/sub 94/. No stable crystals have been obtained for the initial Ti and Zr compounds so the initial ionic configurations could not be determined. Upon sintering, the Ti ion exchange material exhibits four crystalline phases. The structure and ionic configuration of the two higher temperature phases were determined to be Na/sub 2/Ti/sub 3/O/sub 7/ and Na/sub 2/Ti/sub 6/O/sub 13/. In contrast, the Zr ion exchange material initially crystallizes in a cubic stabilized zirconia phase and at higher sintering temperature the structure converts to the monoclinic baddeleyite phase of ZrO/sub 2/. For each of the systems the only truly amorphous phase encountered was the final ion exchange material. 2 figures.

• Research Organization: Sandia Labs., Albuquerque, N.Mex. (USA)
• DOE Contract Number: EY-76-C-04-0789
• OSTI ID: 7295171
• Report Number(s): SAND-76-0556
• Country of Publication: United States
• Language: English

Related Subjects

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AMORPHOUS STATE
CHEMICAL PREPARATION
CHEMICAL REACTIONS
CRYSTAL STRUCTURE
DECOMPOSITION
FABRICATION
HYDROLYSIS
ION EXCHANGE MATERIALS
LYSIS
MANAGEMENT
NIOBATES
NIOBIUM COMPOUNDS
OXYGEN COMPOUNDS
RADIOACTIVE WASTE DISPOSAL
RAMAN SPECTRA
SINTERING
SOLVOLYSIS
SPECTRA
STRUCTURAL CHEMICAL ANALYSIS
SYNTHESIS
TITANATES
TITANIUM COMPOUNDS
TRANSITION ELEMENT COMPOUNDS
WASTE DISPOSAL
WASTE MANAGEMENT
ZIRCONIUM COMPOUNDS