Synthesis and characterization of some reduced zirconium halides
High temperature equilibrium experiments have revealed several new zirconium subhalides as well as nonstoichiometry among the better-known trihalides. Product characterization by standard gravimetric and electron microprobe analyses was allied with x-ray powder and single crystal work. Accurate lattice parameters for phases of known cell type were determined from high precision x-ray powder data obtained by Guinier methods with Si powder as an internal standard. Up to 50 g batches of ZrCl and the hitherto unreported ZrBr have been prepared stoichiometrically from ZrX/sub 4/ and thin (3 to 4 mils) Zr turnings. Virtually 100% yields of >99.5% pure ZrCl/sub 3/ and ZrBr/sub 3/ were subsequently made by reacting well-ground mixtures of ZrX/sub 4/ with the very soft graphitic monohalides. Since ZrI does not exist, ZrI/sub 3/ was prepared from ZrI/sub 4/ and ZrI/sub 1/./sub 8/, the most reduced iodide phase. New compounds in the Zr--Cl and Zr--Br systems were prepared either by isopiestic equilibration of ZrX and ZrX/sub 3/ and/or via transport in a thermal gradient. A single crystal structure determination has shown the ZrCl/sub 2/./sub 5/ phase to be the first Group IVB M/sub 6/ cluster compound. It crystallizes in space group Ia3d with Z = 16 and is isostructural with Ta/sub 6/Cl/sub 15/.
- Research Organization:
- Ames Lab., IA (USA)
- DOE Contract Number:
- W-7405-ENG-82
- OSTI ID:
- 7305522
- Report Number(s):
- IS-T-736
- Country of Publication:
- United States
- Language:
- English
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360601* -- Other Materials-- Preparation & Manufacture
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400100 -- Analytical & Separations Chemistry
BROMIDES
BROMINE COMPOUNDS
CHEMICAL ANALYSIS
CHEMICAL COMPOSITION
CHEMICAL PREPARATION
CHLORIDES
CHLORINE COMPOUNDS
COHERENT SCATTERING
CRYSTAL STRUCTURE
DIFFRACTION
ELECTRON MICROPROBE ANALYSIS
GRAVIMETRIC ANALYSIS
HALIDES
HALOGEN COMPOUNDS
IODIDES
IODINE COMPOUNDS
MICROANALYSIS
MOLECULAR STRUCTURE
QUANTITATIVE CHEMICAL ANALYSIS
SCATTERING
STOICHIOMETRY
SYNTHESIS
TEMPERATURE GRADIENTS
TRANSITION ELEMENT COMPOUNDS
X-RAY DIFFRACTION
ZIRCONIUM BROMIDES
ZIRCONIUM CHLORIDES
ZIRCONIUM COMPOUNDS
ZIRCONIUM IODIDES