Silica-containing -zirconium phosphate (-ZrSiP) was prepared by the precipitation method. X-ray diffractometry was used to characterize -ZrSiP and to compare it with other -zirconium phosphates (ZrP). A monoclinic cell with parameters of a=0.9038 nm, b=0.529 nm, c=1.4183 nm and =91.76° was identified for -ZrSiP, i.e. silica modifies the original -ZrP structure. The specific surface area of -ZrSiP was found to be two orders of magnitude higher then that of -ZrP.
Anomalous temperature dependent changes were found in 2-1-2-2 Type Tl-containing high temperature superconductor around the TC1. The anomaly can be interpreted as relaxation changes due to Cooper pairing with energy predicted by the BCS theory.
57Fe transmission Mössbauer spectroscopy and X-ray diffractometry were used to study clay mineral samples originated from two different regions (Um-arrazm and Alkawasim) of Libya in order to get information about their mineralogical composition to assess their potential for use in the Libyan oil industry. In the samples originated from Um-arrazm calcite, akaganeite and nontronite while in the samples originated from Alkawasim quartz, akaganeite, montmorillonite, kaolinite, illite, mica and hematite were identified with different ratios by using diffraction method. The differences in the phase composition of iron-containing phases of samples from different localities have reflected in the complex Mössbauer spectra at both 300 K and 80 K. For the samples originated from Um-arrazm the Mössbauer parameters of subspectra were identified as nontronite and akaganeite.
57Fe and151Eu Mössbauer spectroscopy and X-ray diffractometry measurements were performed with europium and iron containing Tl2(Ca0.8Eu0.2)Ba2(Cu0.98Fe0.02)2O8 and EuBa2Cu3O7-d high temperature superconductor samples in order to study the effect of europium incorporated in a Tl-containing high temperature superconductor. Significant differences have been found between the57Fe Mössbauer spectra of Tl-containing samples with and without Eu or between the151Eu Mössbauer spectra of Tl-containing and 1-2-3 type superconductors. The results can be interpreted by assuming that Eu can be localized at the Ca site in the Tl-containing superconductor.
The mixed zirconium, titanium, hafnium and first-row transition metal oxides (containing phosphorous oxide) were prepared
using ion exchange method followed by calcinations at 1020 K during 12 h. The resulted mixed oxides were identified by XRPD
method and studied their thermal behaviour by TG-DTA analysis. As a result of thermal analysis there were found one exothermic
(with a peak at about 950 K), and one endothermic (with a peak at about 1300 K) processes, both without mass loss. The observation
was valid for all investigated samples.
The analysis of XRPD patterns of the investigated samples showed well-defined crystal phases characteristic of each oxide.
The XRPD analysis also verified the phase transition of tetravalent metal oxides from orthorhombic to tetragonal, observed
by DTA analysis.
The prepared amorphous
γ-ZrP\SiO2 composite had a complicated composition,
since a part of γ-ZrP is converted to α-form during the exfoliation
of it. The γ-ZrP\SiO2 composite have specific surface
area of 421 m2g–1.
The acidic P–OH groups of the lamellae species placed on the surface
(it is ≈1.0 meq g–1), do not destroy until
the temperature of 1030 K. During the thermal treatment the total mass loss
of 7.79% was found. This value corresponds to 0.42 mole of H2O
per molecule unit. The water loss process was found very slow, because of
the placing of bilamellar species in the composite.
A new terminology of Mössbauer pattern analysis is introduced. In this approach Mössbauer parameters are considered as functions of a number of externally adjusted physical parameters at which the spectrum has been recorded. Our approach can also help to systematize Mössbauer data for the identification of individual physical or chemical species from the corresponding patterns present in the spectrum.
The thermal behavior of tin containing oxalate, EDTA, and inositol-hexaphosphate were investigated. The end products of synthesis were identified by Mössbauer-, XRD analyses, and FTIR studies. The thermal decompose of the samples was studied by DTA-TG analysis. The simultaneously obtained DTA and TG data makes it possible to follow the thermal decomposition of the investigated samples. The tin oxalate decomposed in the temperature range of 520–625 K through tin carbonate formation and finally yielded CO2 and SnO. The tin EDTA complex first lost its hydrate bound water till 520 K. The followed thermal events related to the pyrolysis of anhydrous salt. The intense exothermic process that exists in the temperature range of 820–915 K is due to the formation of SnO2. The tin sodium inositol-hexaposphate lost its hydrate bound water (∼10%), up to 460 K. The following sharp exothermic process, in the temperature range of 680–750 K is due to the decomposition and parallel oxidation of organic part of the molecule. At the end of this process, a mixture of phosphorous pentaoxide, sodium carbonate, and tin dioxide is obtained.
Tin(II/IV) phosphate was prepared by various synthetic methods. The different methods resulted in tin phosphate with different properties, i.e., different crystalline form and behaviour during thermal treatment. The prepared materials have 3 mol water of crystallisation, which they lose in different ways. Total mass loss was between 20 and 30%. This could be connected with water loss, going generally in two steps in parallel with endothermic processes. At the end of thermal treatment, tin pyrophosphate is obtained, irrespective of the method of preparation used.
A new user-friendly software for analysis of Mössbauer-spectra has been developed. The program makes use of the advantages provided by the current generation of fast personal computers. An Evolution Algorithm1,2 is used for global search of Mössbauer parameters in order to enhance the reliability of the obtained results. Fitting of Lorentzians, Pseudo-Voigt line profiles, and deriving hyperfine-field distributions including correlations and combinations and Mössbauer Line Sharpening by Fourier transformation provide a wide range of applicability.