Synthesis and characterization of oxide interstitial derivatives of zirconium monochloride and monobromide
The reactions of ZrO/sub 2/ (zirconium oxide) with double-metal-layered ZrCl (zironium chloride) and ZrBr (zirconium bromide) at approx. 980/sup 0/C and with Zr metal at 930/sup 0/C have been studied with the aid of high-resolution (Guinier) powder pattern data. The products of the first reaction are ZrX(O/sub y/) (XO/sub y/oxychloride or oxyobromide), an expanded ZrX structure, and Zr(O/sub x/) from solution of ZrO/sub 2/ in the metal, viz., ZrX + nZrO/sub 2/ = ZrX(O/sub y/) + nZr(O/sub x/). The oxygen composition of both products (y,x).varies continuously up to the point of ZrO/sub 2/ saturation where n, y, and x are respectively 0.27 (1), 0.43 (2), and 0.42 for chloride and 0.22 (2), approx. 0.35, and approx. 0.42 for bromide. Single-crystal x-ray results for ZrBrO/sub approx. 0.23/, ZrClO/sub 0.29/, and ZrClO/sub 0/ /sub 43/ establish the retention of the basic ZrX structure (R anti 3 m) and the concentration of oxygen, which is distributed randomly in the distorted tetrahedral interstices between the zirconium layers. The last named composition (a = 3.4984 (2) A, c = 27.065 (4) A) is in equilibrium with ZrO/sub 2/ and gave a refined structure with R = 0.046 and R/sub w/ = 0.056 for 141 independent reflections with 2theta less than or equal to 59.9/sup 0/. UPS (Photoelectron spectroscopy) measurements show that the chloride oxide is still metallic.
- Research Organization:
- Case Western Reserve Univ., Cleveland, OH
- DOE Contract Number:
- W-7405-ENG-82
- OSTI ID:
- 5596895
- Journal Information:
- Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 22:22; ISSN INOCA
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
400201* -- Chemical & Physicochemical Properties
BROMIDES
BROMINE COMPOUNDS
CARBIDES
CARBON COMPOUNDS
CHALCOGENIDES
CHEMICAL REACTIONS
CHLORIDES
CHLORINE COMPOUNDS
COHERENT SCATTERING
CRYSTAL DEFECTS
CRYSTAL LATTICES
CRYSTAL STRUCTURE
CRYSTALLOGRAPHY
CRYSTALS
DATA
DIFFRACTION
ELECTRON SPECTROSCOPY
ELEMENTS
EXPERIMENTAL DATA
FLUORIDES
FLUORINE COMPOUNDS
HALIDES
HALOGEN COMPOUNDS
HIGH TEMPERATURE
INFORMATION
INTERSTITIALS
LATTICE PARAMETERS
MEDIUM TEMPERATURE
METALS
MOLECULAR STRUCTURE
MONOCLINIC LATTICES
MONOCRYSTALS
NITRIDES
NITROGEN COMPOUNDS
NUMERICAL DATA
OXIDES
OXYBROMIDES
OXYCHLORIDES
OXYGEN COMPOUNDS
PHOTOELECTRON SPECTROSCOPY
PNICTIDES
POINT DEFECTS
POWDERS
SCATTERING
SPECTROSCOPY
SULFIDES
SULFUR COMPOUNDS
TEMPERATURE DEPENDENCE
TETRAGONAL LATTICES
TIME DEPENDENCE
TRANSITION ELEMENT COMPOUNDS
TRANSITION ELEMENTS
VERY HIGH TEMPERATURE
X-RAY DIFFRACTION
ZIRCONIUM
ZIRCONIUM BROMIDES
ZIRCONIUM CARBIDES
ZIRCONIUM CHLORIDES
ZIRCONIUM COMPOUNDS
ZIRCONIUM FLUORIDES
ZIRCONIUM NITRIDES
ZIRCONIUM OXIDES
ZIRCONIUM SULFIDES