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Abstract
Neutron, 
and Mössbauer spectroscopy were used to study the possibility of cold nuclear fusion in Fe90Zr10 amorphous ribbon having high hydrogen absorbing ability. No significant changes in the neutron and in the spectra were found at deuterization performed electrochemically at different cathodic potentials. The observed differences between the Mössbauer spectra of samples deuterized in air and in nitrogen atmosphere can be explained by decrease of deuterium uptake as well as by a small heat effect due to reaction of hydrogen with oxygen dissolved in water in the case of electrolysis carried out in air.
Abstract
A number of dibutyltin(IV) complexes of polyhydroxyalkyl carboxylic acids (O donor atoms) and amino acids (O,N donor atoms) were prepared in the solid state. The binding sites of the ligands were determined by means of FT-IR, Raman and 13C NMR spectroscopy. Partial quadrupole splitting calculations were utilized to determine the coordination geometry around the Sn(IV) centre by means of Mössbauer measurements. The results showed that in the solid state oligomeric complexes are formed, with the -COO- groups as bridges between the organometallic cations. The {Sn} atoms are mostly in trigonal bipyramidal surroundings. The Sn-O and Sn-C bond distances were determined by EXAFS measurements to be 207-234 and 295 pm, respectively. Evaluation of the pH-metric and NMR titration curves in Me2Sn(IV)-D-gluconic acid system revealed that the equilibria in aqueous solution are fairly complicated. In acidic solution, the formation of 1 : 1 and 1 : 2 -COO- coordinated species predominate, but deprotonation of the alcoholic -OH groups also starts at very low pH. In the pH range 5-9, NMR provides experimental evidence of ligand-exchange reactions without pH-metrically detectable proton release. In alkaline solution, further deprotonation processes occur, resulting in either alkoxo or mixed hydroxo complexes. The carboxylate coordination is expected for the amino acid ligands but the shift of the νN-H stretching vibrations in the FT-IR spectra demonstrated that the ammine group also binds to the metal ion in the solid Bu2Sn(IV)complexes.
Summary
The double perovskites, AFe0.5Mo0.5O3with A=(Ba,Sr) or (Sr,Ca), were prepared by a sol-gel method, and the substitution effect at site A was studied by Mössbauer spectrometry. In the Mössbauer spectra of the double perovskite (Ba, Sr)Fe0.5Mo0.5O3, the isomer shifts decreased fromδ=0.72 mm/s to δ=0.4 mm/s and the internal magnetic fields increased with the increase of the Sr content. The Ba-rich samples were shown to contain superparamagnetic components under the same preparation conditions. Better crystallinity and larger hyperfine fields were obtained when 5% of the Sr-content of SrFe0.5Mo0.5O3was substituted by Ca as compared with substitution by Ba. Phonon density of states (DOS) of SrFe0.5Mo0.5O3substituted with Ca or Ba were obtained by nuclear inelastic scattering. The peaks of phonon DOS were shifted, depending on chemical compression/expansion of the lattice. The chemical pressure effect could be observed in the Mössbauer spectra and the phonon DOS spectra.
Summary
This paper describes the Mössbauer investigations of iron(III) salts in aqueous solutions in the presence of indole-3-alkanoic acid ligands. The measurements showed two parallel reactions between the ligands and ferric ions: a complex formation and a redox process. The oxidation process takes place in the ligands, and a part of Fe3+is reduced to Fe2+.
Abstract
The paper offers three applications of nuclear methods in the research of chemical structure. First, progress in positron annihilation spectroscopy is illustrated by a positron beamline study, which obtained results that are not available through conventional experiments. The positron beam was used for the study of Langmuir-Blodgett (LB) films containing 4-58 layers of arachidic acid and its salts. These measurements have shown that this emerging technique is capable of characterizing even such elusive systems. Second, the potential of Mössbauer spectroscopy to answer current challenges of solid state chemistry are shown in a study on perovskites of recent interest. 151Eu Mössbauer spectroscopy was used to study the effect of Pr substitution in EuBa2Cu3O7-
. It was shown that the introduction of Pr into the rare earth site as well as into the Ba site results in the appearance of extra electrons both in the copper oxide planes and at the 4f shell of Eu cations. The observed effects were explained by the hole filling effect of Pr. Finally, a survey is presented on the recently developed techniques for nuclear resonant scattering of synchrotron radiation, an exciting and very rapidly developing extension to conventional Mössbauer spectroscopy. An interesting new result is that nuclear inelastic scattering experiments performed on solutions of 57Fe complexes show contribution from vibrations rather than from diffusion to the inelastic spectra.
Abstract
We studied the long-term (190 hours) behaviour of [Zn(propyltetrazole)6](BF4)2 single crystal under high-vacuum (HV) conditions (10–8 torr) with a depth-sensitive technique of positron annihilation spectroscopy (PAS). The obtained data indicate the slow formation of a new near-surface structure which is formed by the decomposition of the [Zn(propyltetrazole)6]2+ ions. The assumption of such a decomposition process was confirmed by additional mass spectroscopic measurements.
Abstract
Samples of TiN hard coatings prepared by physical vapour deposition (PVD) were investigated by means of depth-sensitive positron annihilation spectroscopy. The results indicate that the samples are at the limits of the applicability of this method presumably due to the high defect concentration. Our findings also show that, though the samples are thoroughly characterized by other independent methods, they might not be sufficient to explain all aspects of positron-solid interactions in these cases.
Abstract
Introduction of the Mössbauer nuclei 57Fe into Hg-1223 phase and that of 57Fe and 151Eu into Tl-1212 and Tl-1223 superconductors were investigated. Samples of high phase purity were obtained. Scanning electron microscopy and optical microscopy in normal and polarized light were employed to study the microstructure of the specimens. Energy dispersive X-ray analysis showed that 57Fe in the Hg-based samples and 57Fe as well as 151Eu in the Tl-based compounds, entered superconducting phases. Incorporation of Eu3+ into the superconducting phase favored the formation of the Tl-1212 phase. Mössbauer spectroscopy showed that Eu3+ entered the Ca-site. Two doublets found in the 57Fe Mössbauer spectra in both the Hg-1223 and the Tl-1223 phase referred to two different micro-environments of Fe3+. The assignment of the 57Fe Mössbauer spectra was made under the assumption that Fe favored the 1223 phase. Fe3+ may replace Cu in both the square pyramidal, five-fold oxygen coordinated Cu sites between the Ca and Ba-(Sr)-O layers, and in the square planar, four-fold oxygen coordinated Cu sites the Ca layers in the superconducting phases in both the Hg- and the Tl-based materials. From the relative areas of the two doublets, we concluded that the Fe3+ preferred the square planar Cu site.
Abstract
A real specimen originating from the primary circuit of a VVER-440 type pressurized water cooled nuclear reactor has been studied by Conversion Electron Mössbauer Spectroscopy (CEMS) in order to find out how the AP-CITROX decontamination procedure modifies the structure and composition of the surface oxide layer of stainless steel which is used in the steam generator. Other methods like voltammetry, gravimetry, and SEM-EDAX were also applied to characterize the samples and to help the interpretation of CEMS results. It was found that, in contradiction with expectations, the presence of the surface magnetite layer could not be convincingly identified even on the non-decontaminated sample. This finding together with the relatively weak Mössbauer signals indicated that the surface oxide layer is strongly Fe-depleted. It was also concluded that the upper layer of the bulk steel (under the oxide layer) has an altered composition probably due to irradiation-enhanced diffusion of the metallic constituents. It was established that the AP-CITROX decontamination procedure does not exert detrimental effects on the thickness and composition of the surface oxide layer.
Abstract
Sr0.95Ca0.05Fe0.5Co0.5O3-
and Sr0.5Ca0.5Fe0.5Co0.5O3-
perovskites were studied by 57Fe emission Mössbauer spectroscopy. It was found that Co prefers lower valence and lower coordination number than Fe in both compounds. The comparison of the emission and transmission Mössbauer spectra of the CO2 treated materials revealed a preferred formation of Fe-containing products in reaction with CO2 in Sr0.5Ca0.5Fe0.5Co0.5O3-
, and it is proposed that such a reaction can be responsible for phase separation in Sr0.95Ca0.05Fe0.5Co0.5O3–
after absorption and partial desorption of CO2 at 950 °C.
