Mössbauer studies of iron stabilised polymethacrylates

Polymethyl methacrylate (PMMA), polyethyl methacrylate (PEMA) and polybutyl methacrylate (PBuMA) containing ferric chloride and ferrous sulphate as stabilisers, were prepared by free radical polymerization. Mössbauer spactra of ferrous sulphate stabilised polymers don't show any change in the value of isomer shift (1.30 mm/s) while quadrupole splitting values are quite different from those for pure ferrous sulphate. This indicates that environment of Fe²⁺ moiety changes in polymers and thus stabilises the polymers. In case of ferric chloride stabilised polymers the isomer shift values don't differ significantly for different polymethacrylates but quadrupole splitting values increase from polymethyl methacrylate to polybutyl methacrylate. The TGA analysis shows that the inclusion of iron salts stabilises the polymers by 40°C (approx.) and at higher temperatures α-Fe₂O₃ is formed.     

Laser initiation of PETN–iron nanoparticle composites

The dependences of the probability of explosion initiation in pentaerythritol tetranitrate samples with different contents of iron nanoparticles on the fluence of the first- (λ = 1064 nm) and second-harmonic (λ = 532 nm) pulses of a neodymium laser are measured. The laser initiation threshold for PETN–iron nanoparticle composites nonmonotonically depends on the mass fraction of nanoparticles. The optimal values of the mass fraction of iron nanoparticles at which the sensitivity to laser irradiation is maximal (0.4 wt % for the first harmonic and 0.15 wt % for the second) are determined. It is demonstrated that the amplitude of the optoacoustic signal under non-explosion conditions reaches its maximum for composites with the optimal values of the mass fraction of nanoparticles.     

A Mössbauer study of iron and iron–cobalt nanotubes in polymer ion-track membranes

Iron and iron–cobalt nanostructures that were synthesized in polymer ion-track membranes have been studied via Mössbauer spectroscopy combined with raster electron microscopy, energy-dispersion analysis, and X-ray diffraction data. The obtained nanostructures are single-phase bcc Fe_1–xCo_x nanotubes with a high degree of polycrystallinity, whose length is 12 μm; their diameter is 110 ± 3 nm and the wall thickness is 21 ± 2 nm. Fe²⁺ and Fe³⁺ cations were detected in the nanotubes, which belong to iron salts that were used and formed in the electrochemical deposition. The Fe nanotubes exhibit eventual magnetic moment direction distributions of Fe atoms, whereas Fe/Co nanotubes have a partial magnetic structure along the nanotube axis with a mean value of the angle between the magnetic moment and nanotube axis of 34° ± 2°. Substituting the Fe atom with Co in the nearest environment of the Fe atom within the Fe/Co structure of nanotubes leads to a noticeable increase in the hyperfine magnetic field at the ⁵⁷Fe nuclei (by 8.7 ± 0.4 kOe) and to a slight decrease in the shift of the Mössbauer line (by 0.005 ± 0.004 mm/s).     

Preparation and characterization of iron–molybdate thin films

Mixed Fe–Mo oxides are used in industrial catalytic processes of selective oxidation of methanol to formaldehyde. For better understanding of the structure-reactivity relationships of these catalysts we aim to prepare well-ordered iron–molybdate thin films as model catalysts. Here we have studied Mo deposition onto Fe₃O₄ (111) thin films produced on Pt(111) as a function of Mo coverage and annealing temperature using LEED, AES, STM and IRAS. At low temperatures, the iron oxide film is covered by Mo = O terminated molybdena nanoparticles. Upon oxidation at elevated temperatures (T > 900 K), Mo species migrate into the film and form new bonds with oxygen in the film. The resulting films maintain the crystal structure of Fe₃O₄, and the surface undergoes a (√3 × √3)R30° reconstruction. The structure is rationalized in terms of Fe substitution by Mo in the surface layers.     

Processing of gadolinium–iron garnet under non-equilibrium conditions

We have investigated the mechanosynthesis of gadolinium iron garnet (GdIG) by high-energy ball-milling of 3.(Gd₂O₃)?+?10.(α-Fe) followed by thermal annealing conducted at moderate temperatures (1100 °C). The samples were characterized by X-ray diffraction and Mössbauer spectroscopy in order to determine the influence of the milling time on the final products. For as-milled samples the results revealed the enlargement of the magnetic component belonging to iron and a discrete paramagnetic component. The formation of a garnet phase was observed in all as-annealed samples treated at 1100 °C for 6 h in quantities proportional to the time of grinding the precursors. Evidently, high-energy ball milling of Gd₂O₃?+?α-Fe powders is an important step in GdIG synthesis by a ceramic method. Single-phase garnet is observed for the samples milled for 12 and 24 h treated at 1100 °C for 6 h.     

Mössbauer spectroscopic properties of tin-doped iron oxides

The ⁵⁷Fe Mössbauer spectra recorded in situ from tin-doped Fe₃O₄ at elevated temperature in vacuo shows the Curie temperature to decrease with increasing concentrations of the dopant. Thermal treatment under oxidising conditions results in the initial formation of tin-doped γ-Fe₂O₃ which subsequently undergoes a phase transformation to tin-doped α-Fe₂O₃. ⁵⁷Fe Mössbauer spectroscopy at elevated temperatures shows the Néel temperature for tin-doped γ-Fe₂O₃ to be lower than that of pure γ-Fe₂O₃. The ¹¹⁹Sn Mössbauer spectra recorded from all the tin-doped iron oxides show the presence of a hyperfine magnetic field at the Sn⁴⁺ site which is more complex in the spectra recorded from tin-doped γ-Fe₂O₃ and α-Fe₂O₃.     

Mössbauer study of CO-precipitated Fischer-Tropsch iron catalysts

Mössbauer spectroscopy studies of precipitated Fischer-Tropsch (FT) iron catalysts, viz. 100 Fe/5 Cu/4.2 K/x SiO₂, wherex=0,8, 16, 24, 25, 40, or 100, have shown that reduction of the oxide precursor in CO gives rise to -carbide Fe₅C₂ whose amount decreases with an increase of SiO₂ content. The -carbide is converted into magnetite Fe₃O₄ while catalyzing the FT synthesis reaction. A correlation between FT activity and the content of -carbide in the catalysts was found, which indicated that -carbide is active for FT synthesis reaction.     

Thermal transition behaviour of iron oxide–polypyrrole nanocomposites

Distinct thermal transitions have been observed in nanocomposites based on iron oxide–polypyrrole prepared by simultaneous gelation and polymerization process. The transition behaviour for various iron oxide–polypyrrole compositions was investigated with the help of differential scanning calorimetery. It has been observed that the samples show a magnetic to nonmagnetic transition at 410 °C. The presence of exothermic peak at 410 °C is a strong indication of magnetic transition corresponding to γ-Fe₂O₃ phase of iron oxide to a nonmagnetic α-Fe₂O₃ phase in these nanocomposites. However such a transition was not observed in nanocomposites containing lesser concentration of conducting polymer.     

Distribution of iron atoms in Fe-Mn alloys with the structure of β-Mn

X-ray analysis and Mössbauer spectroscopy were used to study the distribution of iron atoms in Fe-Mn alloys isostructural to -Mn and to determine the iron concentrations in the positions 8(c) and 12(d) of the -Mn structure in alloys of different compositions.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 3, pp. 86–89, March, 1981.     

Comparative study of core–shell iron/iron oxide gold covered magnetic nanoparticles obtained in different conditions

In this study, we report the synthesis and characterization of the core–shell Fe covered with Au shells nanoparticles with mean diameters between 5 and 8 nm. The inverse micelles method was utilized to produce the samples. X-ray diffraction studies show that both core–shell systems have the expected crystalline structure. High resolution transmission electron microscopy and atomic emission spectroscopy techniques give additional information concerning the structure and composition of nanoparticles. An intermediate shell of amorphous oxidized iron was found between the magnetic Fe core and the external gold shell. The magnetic behavior of different core–shell samples shows no hysteresis loop indicating the superparamagnetic behavior of Fe@Au systems. The superparamagnetic behavior is also evidenced from FC and ZFC dependences of the magnetization versus temperature. By using the temperature dependence of the thermoremanent magnetization combined with magnetization versus applied magnetic field, the effective anisotropy constant was determined. The Fe/Au interface contribution to the effective anisotropy constant was calculated and discussed in relation with the combined shape and stress anisotropies.     

Mössbauer study of iron removal in a montmorillonite

⁵⁷Fe Mössbauer spectroscopy in conjunction with atomic absorption spectrometry and X-ray powder differaction analyses have been used to study the iron present in a montmorillonite prior to and after different successive stages of two deferration processes. Fe³⁺ ions occupy mainly octahedrical M(2) sites in the mineral structure; no impurities of iron oxides were detected. The quite efficient deferration by HCl refluxing produced a substantial alteration of lamellar structure of montmorillonite, whilst dithionite/citrate treatment did not induce severe structural changes but had low iron removal efficiency.     

Magnetic properties of substitutional solid solutions of nickel and iron hexacyanoferrate–hexacyanochromate

In order to evaluate the influence of substitution at the central metal ion position in transition hexacyanometallates in some detail, the magnetic studies were carried out on a series of solid solutions of metal hexacyanometallates of the composition M[Fe^II(CN)₆]_{1? x} [Cr^III(CN)₆] _x , where M?=?Ni^II and Fe^III. The temperature and field dependences of magnetization were studied using a superconducting quantum interference device magnetometer. The field dependence of the samples at 5?K shows a hysteresis behaviour. For M?=?Ni^II, the transition temperature increases with increase in the substitution of low-spin Fe(III) by Cr(III) in the hexacyanometallate unit. The saturation magnetization was found to decrease with increase in the iron concentration. The observed variation in the magnetic properties, such as the value of T _C and the nature of magnetic ordering, is attributed to the variation in the composition of the transition-metal ion in the coordination sphere of carbon. On the other hand, for M?=?Fe^III, the transition temperature and saturation magnetization remained almost unchanged, indicating that substitution at the carbon coordination site did not produce any change in the magnetic interaction among the transition-metal ions through the cyanide ions.     

Effect of vanadium neighbors on the hyperfine properties of iron–vanadium alloys

The electronic and magnetic structures of Fe–V alloys are calculated using the discrete-variational and full-potential linearized-augmented-plane wave methods. The derived hyperfine properties at Fe sites are studied against the number of Fe atoms in the neighbouring shells. As expected the magnetic hyperfine field depends strongly on the number of Fe atoms in the first and second shells of neighbours while its dependence on the variation of atoms in the third shell is weak. The calculated distribution of the magnetic hyperfine fields at the Fe sites, are compared to the experimental data of Krause et al. (Phys Rev B 61:6196–6204, 2000). The contact charge densities and the magnetic moments are also calculated. It was found that the contact charge density increases with increasing V contents and this leads to negative isomer shift on addition of V.     

Mössbauer and magnetization studies of iron oxide nanocrystals

Monodisperse iron oxide nanocrystals have been produced following non-hydrolytic, thermal decomposition routes. Spherically shaped particles with diameter of 4 and 12 nm and cubic shaped particles with an edge length of 9 nm have been studied. The particles have been shown to consist of mainly maghemite. A reduction of the saturation magnetic hyperfine field is observed for the 4 nm particles as compared to the corresponding bulk value. The anisotropy energy determined from the temperature variation of the magnetic hyperfine field was strongly enhanced for the 4 nm particles.     

Mössbauer spectroscopic study of iron fluoride surface layers

The reaction products formed during exposure of iron foils to hydrogen fluoride in the presence of atmospheric oxygen and water have been examined with conversion electron Mössbauer spectroscopy (CEMS) [1]. After exposure for several hours the product in the corrosion layer was found to consist mainly of the mixed-valence iron fluoride, Fe₂F₅·7H₂O. Although the products formed during the initial steps of the reaction could not be completely characterized, a model for the reaction process is suggested.     

Chemical Synthesis of Highly Magnetic, Air-Stable Silica-Coated iron Particles

Highly magnetic and air-stable silica-coated Fe particles have been prepared by a rapid and simple method. The specific magnetization of the sample can be as high as 201 Am^2 /kg even including silica, which is a non-magnetic material. The iron particle coated with silica is passivated and protected from oxidation. The influences of H2 reduction temperature on structure and magnetic properties are also studied.     

Mössbauer study of the dynamics of iron ions in bipyramidal positions of strontium hexaferrite

The dynamics of Fe³⁺ ions in bipyramidal 2b positions of a type M hexaferrite are studied on single-crystal and polycrystalline SrFe₆Ga₆O₁₉ samples in the paramagnetic temperature range. We show that when the angle between the c axis of the crystal and the direction of -ray emission varies from 0 to 32 the area under the resonance lines corresponding to Fe³⁺ ions in 2b positions increases by a factor of roughly 1.5. The effect is more pronounced upon passing from a single-crystal sample (=0) to a polycrystalline sample. A comparison of the line intensities under different experimental conditions served as a basis for an evaluation of the difference between the mean-square displacements of the Fe³⁺ ions in 2b positions along the c axis in the perpendicular plane.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 1, pp. 5–8, January, 1991.     

Measurements of Rayleigh–Taylor instability growth of laser-shocked iron–silicon alloy

The Rayleigh–Taylor (RT) instability of liquid iron alloys is important for understanding the core formation mechanism in the Earth. Here we first report the measurement of RT instability growth for a liquid iron–silicon (Fe–Si) alloy, which is one of the major candidate for the material of the Earth’s core, using a high power laser. We optimized the measurement setup and analytical technique to observe the growth of perturbation on an Fe–Si sample surface. The growth of perturbation amplitude on the Fe–Si alloy under high pressure and temperature was successfully observed using in situ X-ray radiography. The growth rate of the RT instability for the Fe–Si alloy on about 1000?GPa was estimated to be 0.3 ns^?1.     

Uses and perspectives of Mössbauer spectroscopic studies of iron minerals in coal

The processes involved in the utilization of coal are affected by the minerals contained in it. Due to the presence of iron as a major constituent of coal mineral matter, and to the fact that the iron minerals, especially pyrite, and their transformation products play an important role in coal uses, ⁵⁷Fe-Mössbauer spectroscopy appears as an attractive tool in coal research. Mössbauer studies related to the characterization of iron phases, coal oxidation and quantitative determination of pyritic sulphur are discussed in this work.     

Effect of magnetic pulse treatment on the magnetic characteristics of yttrium–iron garnets

The effect weak (10–100 kA m^–1) low-frequency (10–20 Hz) pulsed magnetic fields have on the surface structure and magnetic characteristics of yttrium–iron garnet Y₃Fe₅O₁₂ is studied by means of electron and Mössbauer spectroscopy. A mechanism is proposed for the variation of saturation magnetization in Y₃Fe₅O₁₂ after magnetic pulse treatment. The mechanism is associated with the change in the spin state of iron ions localized in the tetrahedral sublattice.