J. Megyeri

Thermoanalytical investigation of layered titanium salts

The investigated materials have similar routes of thermal decomposition; i.e. they lose their crystal water first, then at a higher temperature their structural one. At least the result TiP2O7 goes through a phase change at about 1000 K. The amorphous titanium phosphate lost its crystal and structural water at higher temperature than those of crystalline forms. Both α- and γ-titanium phosphates and also their transition metal containing forms have layered structure. In case of α- and γ-forms after the loss of crystal water a phase change occurs which is followed by the decomposition of the molecule. Various transition metals containing γ-titanium phosphates lose their crystal water at the same temperature, with the exception of Ni containing ones. The process is finished in this case at temperature 90 K higher than that of the others.

Comparative study of layered tetravalent metal phosphates containing various first-row divalent metals. Synthesis, crystalline structure

The transition metal forms of α-zirconium-. titanium-, and hafnium phosphates were prepared by ion exchange method. Their structure was investigated by X-ray powder diffraction (XRPD) method. It was found that the transition metal containing phosphates have the same layered structure as the pristine tetravalent metal phosphates, except for the increase of interlayer distance from 7.6 Å to ∼9.5 Å. As a result of the incorporation of transition metals in the layers, the c-axis is increased from ∼15 Å to ∼20 Å (in the case of titanium phosphate to ∼25 Å). All other parameters (a, b and β °) are practically unchanged.

X-ray powder diffraction study of chromium-vanadium oxide compounds prepared by “soft chemistry” methods

A novel aqueous method was used to synthesise mixed chromium-vanadium oxide hydrates with various chromium content, via the reaction of peroxo-polyacids of chromium and vanadium. The resulting materials are gelatinous. The dehydration of the gels result in a brown coloured amorphous powder. Depending on the chromium content, the compounds have a different characteristic crystallisation temperature upon the further heating. The crystalline compounds, except for the low chromium ones, go on a phase transition and decompose with increasing temperature.By refining the XRPD measurement data of the compounds, the type and parameters of the unit cells were determined. The experimental data were in concordance with the calculated values, using the PWC code. The lattice parameters and the crystalline structure were changed with the variation of chromium content.

Thermal Decomposition of Hafnium Phosphate and Related Materials

The thermal decomposition of hafnium phosphate (both in amorphous and crystalline forms), molybdate and tungstate was investigated. Hafnium phosphate has a layered structure, that of molybdate and of tungstate are tetragonal one. On investigating these materials two main endothermic processes with mass loss were observed in the temperature range of 298–1023 K. These processes were identified as crystal and structural water loss of the materials. The total mass loss of hafnium phosphate, molybdate and tungstate was 11,35 and 6.0%, respectively. In the case of mixed hafnium-titanium salts various crystal water quantities were found, depending on the titanium content of the sample.

Thermal Decomposition of Several Layered Zirconium Salts

The thermal decomposition of zirconium molybdate, tungstate and arsenate were investigated. The total mass losses of the investigated materials were 12.5, 11 and 8.5%, respectively. Despite having different crystal dimensions and structure the thermal decomposition of the samples takes place in a similar way. During heating two main endothermic processes with mass loss were observed. At the end of the thermal decomposition, oxides of the original materials were observed. The mentioned mass losses originate partly from the crystal water loss of the materials. The calculated crystal water content in the original molecule was 1.3 and 1 mole/molecule unit, respectively. Furthermore, for zirconium arsenate, a sublimation process was recorded above 960 K.