Optimum conditions for intercalation of lacunary tungstophosphate(V) anions into layered Ni(II)-Zn(II) hydroxyacetate
- Departamento de Quimica Inorganica e Ingenieria Quimica, Universidad de Cordoba, Campus Universitario Rabanales, Edificio Marie Curie 1a Planta, 14071 Cordoba (Spain)
- GIR-QUESCAT, Departamento de Quimica Inorganica, Universidad de Salamanca, Salamanca (Spain)
Acetate containing nickel-zinc hydroxysalts (LHS-Ni-Zn) have been synthesized by coprecipitation and hydrothermal treatment. The acetate anions were exchanged with PW{sub 12}O{sub 40}{sup 3-} anions, and optimum conditions to attain the maximum level of W in the compound have been identified. The W intercalated compound was characterized by powder X-ray diffraction, FT-IR spectroscopy, thermogravimetric and differential thermal analyses, scanning electron microscopy and transmission electron microscopy. The exchange of LHS-Ni-Zn with PW{sub 12}O{sub 40}{sup 3-} at pH=3 for 72 h leads to a solid with a basal spacing of 9.62 A and a W content (weight) of 37%. The hydrothermal treatment at 90 deg. C for 24 h increases this value to 48% with a W/Zn molar ratio of 1.38, which corresponds to a layered compound with lacunary tungstophosphate anions in the interlayer space. The intercalated solid is stable up to 250 deg. C, the layer structure collapses on dehydroxylation and amorphous compounds were identified at 500 deg. C. Two crystalline phases, NiO (rock salt) and a solid solution (Zn{sub 1-x}Ni{sub x})WO{sub 4}, were identified by powder X-ray diffraction at high temperature (ca. 1000 deg. C). - Graphical abstract: Optimum conditions for intercalation of Keggin-type anions in Ni, Zn hydroxysalts have been identified. Lacunary species are formed via partial depolymerization of the starting anion. The thermal decomposition of the intercalated phases has been also studied.
- OSTI ID:
- 21212107
- Journal Information:
- Journal of Solid State Chemistry, Vol. 181, Issue 11; Other Information: DOI: 10.1016/j.jssc.2008.07.037; PII: S0022-4596(08)00400-3; Copyright (c) 2008 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ACETATES
ANIONS
COPRECIPITATION
DEPOLYMERIZATION
DIFFERENTIAL THERMAL ANALYSIS
INFRARED SPECTRA
NICKEL COMPOUNDS
NICKEL OXIDES
PYROLYSIS
SCANNING ELECTRON MICROSCOPY
SOLID SOLUTIONS
TEMPERATURE RANGE 1000-4000 K
THERMAL GRAVIMETRIC ANALYSIS
TRANSMISSION ELECTRON MICROSCOPY
TUNGSTATES
X-RAY DIFFRACTION
ZINC COMPOUNDS