Synthesis and characterization of some reduced zirconium halides

Technical Report · Tue Feb 01 00:00:00 EST 1977

DOI:https://doi.org/10.2172/7305522· OSTI ID:7305522

Daake, R. L.

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., Ames, IA (United States)
• DOE Contract Number: W-7405-ENG-82
• OSTI ID: 7305522
• Report Number(s): IS-T-736
• Resource Relation: Other Information: Thesis
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ZIRCONIUM BROMIDES
CHEMICAL COMPOSITION
CHEMICAL PREPARATION
MOLECULAR STRUCTURE
ZIRCONIUM CHLORIDES
ZIRCONIUM IODIDES
CRYSTAL STRUCTURE
ELECTRON MICROPROBE ANALYSIS
GRAVIMETRIC ANALYSIS
STOICHIOMETRY
TEMPERATURE GRADIENTS
X-RAY DIFFRACTION
BROMIDES
BROMINE COMPOUNDS
CHEMICAL ANALYSIS
CHLORIDES
CHLORINE COMPOUNDS
COHERENT SCATTERING
DIFFRACTION
HALIDES
HALOGEN COMPOUNDS
IODIDES
IODINE COMPOUNDS
MICROANALYSIS
QUANTITATIVE CHEMICAL ANALYSIS
SCATTERING
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
ZIRCONIUM COMPOUNDS
360601* - Other Materials- Preparation & Manufacture
400100 - Analytical & Separations Chemistry