Radio-frequency induced effects in amorphous and nanocrystalline Fe73.5Cu1Nb3Si13.5B9

The rf collapse and sideband effects are used to study the microstructure of the Fe_73.5Cu₁Nb₃Si_13.5B₉ alloy in the amorphous and nanocrystalline state. Nanocrystalline grains of -Fe(Si) are formed as a result of annealing of the amorphous alloy at 520–570 °C. The results show that the complete rf collapse of magnetic hfs in the Mössbauer spectra occurs only in the amorphous phase. The rf collapse is strongly affected by the onset of the nanocrystalline phase and is suppressed when the Fe₃B and Fe₂B phases are formed. Partial collapse allows us to follow the remaining crystalline fractions during the crystalline process. The rf sidebands disappear due to the formation of nanocrystals because of the vanishing magnetostriction.     

Mössbauer Study of the Fe3B/Nd2Fe14B Nanocomposite Magnet by the Addition of Co

The addition of Co to Nd₄Fe_77.5–x Co _x Hf_0.5Ga_0.5B_18.5 (0x5) was found to enhance the magnetic properties of Fe₃B/Nd₂Fe₁₄B nanocomposite magnets. The enhancement resulted from the fact that Co tends to retard the formation of Fe₃B from the amorphous matrix but to accelerate that of Nd₂Fe₁₄B. The decreased interval between the crystallization temperature of Fe₃B and Nd₂Fe₁₄B led to a uniform grain size distribution of both phases during the annealing treatment. The additive Co was confirmed to partition mainly to Nd₂Fe₁₄B crystals rather than to Fe₃B which was traced by XRD and Mössbauer spectroscopy as well. About 72 vol.% of Fe₃B, 27 vol.% of Nd₂Fe₁₄B, and a small amount of Fe around 1 vol.%, respectively, were found to form. However, the volume fraction of each phase did not vary by the addition of Co up to 5 at.%.     

Mössbauer spectroscopy applied to the study of Nd-Fe-B permanent magnets corrosion

Powdered Nd-Fe-B-type permanent magnets were heated at 200 C for times up to 32 days. The evolution of the Nd₂Fe₁₄B magnetic phase, followed by⁵⁷Fe Mössbauer spectroscopy, evidenced the positive influence of both the hydrogen decrepitation process and Co, Nb and V additives on the corrosion resistance.     

The temperature dependence of the Mössbauer hyperfine parameters in Nd2Fe14B

We have determined the temperature dependence of the internal hyperfine field, isomer shift, and quadrupole shift at each of the six iron sites in Nd₂Fe₁₄B. The hyperfine parameters are consistent with the local iron site environments. The quadrupole and isomer shifts and their temperature dependences support our assignments of the relative ordering of the internal hyperfine fields as j₂>k₂>ck₁>j₁>c. We obtain a Mössbauer temperature of 390 K for Nd₂Fe₁₄B, which compares well with the Debye temperature of 420K for pure iron.     

Phase monitoring during Nd15Fe77B8 preparation by the calciothermic reduction-diffusion process

We have examined the effect of various parameters involved in the preparation of the Nd₁₅Fe₇₇B₈ alloy by the calciothermic reduction-diffusion process. Both Nd₂O₃ and NdCl₃ were utilized as starting raw materials. Shorter reaction times and lower heating temperatures are required for the chloride than for the oxide. Among the characterization techniques used to evaluate the final product, Mössbauer spectroscopy was invaluable for the determination of the (Nd_1.1Fe₄B₄)/(Nd₂Fe₁₄B) ratio, which should be as low as possible.     

A Mössbauer effect study of the interstitial hydrides and nitride of Nd2Fe17

The Mössbauer effect spectra of Nd₂Fe₁₇H₃, Nd₂Fe₁₇H₅, and Nd₂Fe₁₇N₃ have been measured at several temperatures between 85 and 295 K and fitted with a model which is similar to that used for the analysis of the Mössbauer effect spectra of Nd₂Fe₁₇ and Nd₂Fe₁₇N_2.6. The weighted average isomer shift increases in going from Nd₂Fe₁₇ to its hydrides and nitride, an increase which results mainly from the lattice expansion. The changes in the individual isomer shifts upon hydrogenation may be understood in terms of the expansion of the Wigner-Seitz cell volume and the presence of hydrogen or nitrogen near neighbors at a specific site. The 295 K weighted average hyperfine field increases from 157 kOe in Nd₂Fe₁₇ to 243 kOe in Nd₂Fe₁₇H₃, 280 kOe in Nd₂Fe₁₇H₅, and 318 kOe in Nd₂Fe₁₇N₃, a sequence determined by the Curie temperatures. In contrast, the weighted average hyperfine field at 85 K and the saturation magnetization at 5 K for Nd₂Fe₁₇H₃ are lower than those of Nd₂Fe₁₇, presumably because of thec-axis lattice contraction which occurs upon hydrogenation of this compound. The main difference between the effect of hydrogenation and nitrogenation resides in the substantial increase observed for the 9d and 18h hyperfine fields upon nitrogenation.     

Mössbauer study of the structure of amorphous invar and a two-level model of the expansion anomaly

The methods of Mössbauer spectroscopy and dilatometry are used to study the local atomic structure and thermal expansion of amorphous invar alloy Fe₈₃B₁₇. It is assumed that the alloy contains regions in which the local order corresponds to metastable orthorhombic and tetragonal phases of the composition Fe₃B. The quantitative ratio of these regions is determined from Mössbauer spectra and is found to be 1:3. A quantitative two-level model of volumetric striction is presented. It is proposed in the model that heating is accompanied by reversible relaxation of orthorhombic configurations of the Fe₃B type to tetragonal configurations, which in turn shortens the distance between iron atoms.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 12, pp. 43–46, December, 1989.     

Temperature dependence of the Mössbauer spectra of amorphous and nanocrystallized Fe86Zr7Cu1B6

Mössbauer measurements have been performed on amorphous and nanocrystalline alloy ribbons of nominal composition Fe₈₆Zr₇Cu₁B₆. The nanocrystalline samples were obtained by annealing the as-quenched alloy at different temperatures in the range between 650 and 870 K. Mössbauer spectra of the as-quenched amorphous sample have been recorded at 77 K, room temperature and above the Curie temperature (330 K) at 360 K. We have also performed Mössbauer measurements at room temperature in the nanocrystalline alloys to characterize the phases that appear after the annealing and their relative concentration. The as-quenched sample spectra reveal the existence of two inequivalent sites for Fe. Such a feature is also observed in the remaining amorphous phase of the annealed samples. In the first steps of crystallization, -Fe precipitates and its concentration increases with the annealing temperature. The experimental results suggest that the composition of the whole amorphous phase does not suffer large changes during crystallization.     

Mössbauer spectroscopy studies of spin reorientations in amorphous and crystalline (Co0.2Fe0.8)72.5Si12.5B15 glass coated micro-wires

Thermo-gravimetric, differential scanning calorimetry and comprehensive ⁵⁷Fe Mössbauer spectroscopy studies of amorphous and crystalline ferromagnetic glass coated (Co_0.2Fe_0.8)_72.5Si_12.5B₁₅ micro-wires have been recorded. The Curie temperature of the amorphous phase is T_C(amorp) ∼730 K. The analysis of the Mössbauer spectra reveals that below 623 K the easy axis of the magnetization is axial-along the wires, and that a tangential or/and radial orientation occurs at higher temperatures. At 770 K, in the first 4 hours the Mössbauer spectrum exhibits a pure paramagnetic doublet. Crystallization and decomposition to predominantly α-Fe(Si) and Fe₂B occurs either by raising the temperature above 835 K or isothermally in time at lower temperatures. Annealing for a day at 770 K, leads to crystallization. In the crystalline material the magnetic moments have a complete random orientation. After cooling back to ambient temperature, both α-Fe(Si) and Fe₂B in the glass coated wire show pure axial magnetic orientation like in the original amorphous state. The observed spin reorientations are associated with changes in the stress induced by the glass coating.     

Approximation of Mössbauer spectra of metallic glasses

Mössbauer spectra of iron-rich metallic glasses are approximated by means of six broadened lines which have line position relations similar to those of -Fe. It was shown via the results of the DISPA lineshape analysis that each spectral peak is broadened owing to a sum of Lorentzian lines weighted by a Gaussian distribution in the peak position. This paper presents the Mössbauer parameters of amorphous metallic Fe₈₃B₁₇ and Fe₄₀Ni₄₀B₂₀ alloys derived from the fitted spectra.We would like to thank Dr. P. Duhaj for the preparation of amorphous samples.     

Magnetic and structural features of amorphous FeMo-based alloys

NANOPERM-type FeMoCuB alloys are studied using magnetic and Mössbauer measurements in the as-prepared amorphous state. It is shown that the Fe₇₆Mo₈Cu₁B₁₅ (A) and Fe₇₄Mo₈Cu₁B₁₇ (B) alloys exhibit the magnetic dipole and electrical quadrupole interactions well detected in the room-temperature Mössbauer spectra. The thermomagnetic measurements above the room temperature indicate a vanishing of the magnetic interactions at approximately 310 K (A) and at 340 K (B), respectively. The low-temperature DC magnetic measurements show an anomaly around 200 K which is also a boundary at which zero-field Mössbauer measurements of both samples reflect the gradual “vanishing” of the electrical quadrupole interactions and appearance of another magnetically ordered component. The Mössbauer measurements in the field of 4 MA/m yield a survival of quadrupole and an enhancement of magnetic dipole interactions.     

High pressure Mössbauer spectroscopy using a diamond anvil cell

Recent applications of high pressure Mössbauer spectroscopy using a diamond anvil cell are presented. High pressure Mössbauer studies of two perovskite-related iron oxides SrFeO_2.97 and CaFeO₃, magnetite Fe₃O₄, and wüstite Fe_1– O have been carried out at 300 K at pressures of up to 74 GPa. A preliminary result by the resonant forward scattering of synchrotron radiation for high pressure Mössbauer spectroscopy using a diamond anvil cell is also presented.     

Microstructure of supersaturated fcc Al–Fe alloys: A comparison of rapidly quenched and mechanically alloyed Al98Fe2

Alloys of the composition Al₉₈Fe₂ have been prepared by rapid quenching from the melt and mechanical alloying methods and have been studied by Xray diffraction techniques and room temperature ⁵⁷Fe Mössbauer effect methods. Results may be summarized as follows: The rapidly quenched sample is a single phase supersaturated fcc Al–Fe alloy. Mössbauer effect spectra indicate the presence of a substantially greater degree of Fe clustering than is expected for a random distribution of atoms on the lattice sites. Mechanically alloyed samples have been studied as a function of milling time and show the initial formation of a supersaturated fcc phase with microstructural properties which are quite similar to those of the rapidly quenched sample. Further milling results in the reduction of the average grain size and the formation of an amorphous phase. Mössbauer studies and previously reported phase diagrams suggest that a substantial fraction of the Fe resides in this phase.     

Structural and magnetic properties of rapidly solidified (Ce0.2Fe0.8)1-x Al x ribbons determined by X-ray diffraction and Mössbauer spectrometry

(Ce_0.2Fe_0.8)_1-x Al _x (0 x 0.9) ribbons have been prepared by planar flow casting under an He atmosphere with a linear velocity of 29 m s^-1. Analyses of the ribbons by X-ray diffraction and⁵⁷Fe Mössbauer spectrometry in the temperature range 4–300 K show that all the ribbons are crystalline. With increasingx, the observed phases are Ce(Fe, Al)₂, Ce₂(Fe, Al)₁₇, CeFe_4+y,Al_8-y and the single fcc aluminium phase. For the different phases, the line intensities of the Mössbauer spectra agree with previous results on the preferential substitution sites for aluminium. A coherent hyperfine parameters set was deduced from fitting spectra in the temperature range 4–300 K.     

Comparison of ball milling of Fe/Cr powders and Fe-Cr crystalline alloy

Using the mechanical attrition technique (MA), we have prepared a Fe-Cr alloy starting with a mixture of elemental iron and chromium powders with a nominal composition of 28 at% of Fe and 72 at% of Cr. MA was also performed on solid solutions of Fe₂₈Cr₇₂ crystalline alloy. The Mössbauer effect of the mechanically alloyed powder from Cr and Fe metals has been compared with that from crystalline alloy.     

The influence of Cu and Nb on the crystallization products of annealed FeCuNbSiB

Depending on different Nb and Cu concentration, we studied the formation of nano- and microcrystalline phases in differently annealed samples of FeCuNbSiB. First, the kinetics of crystallization was explored by measuring the temperature-dependent electrical resistivity and magnetization. After this, we collected Mössbauer spectra and did an X-ray diffraction analysis of annealed samples at chosen temperatures to discover the different crystalline phases. It was found how the onset of crystallization had been shifted towards other temperatures. The analysis of Mössbauer spectra shows that building up the well-known DO₃ structure of Fe₃Si is disturbed in the alloy without Cu. At higher Nb content, we resolve two different crystallization steps in the formation of Fe₃Si and a new crystalline phase, probably being a structure like Fe₂₃B₆.     

Criteria for stabilizing a high spin d4 electronic configuration: Application to the synthesis and the mössbauer characterization of high spin iron (IV) in oxides

A Mössbauer study has been carried out on different oxides with the general formula (A, A)₂M_0.50Fe_0.50O₄ (A=Ca, Sr, Ba: A=La; M=Li, Mg, Zn, Ga, Ni). In all these phases with K₂NiF₄-type-derived structure the distortion of the (FeO₆) octahedra is sufficient to stabilize a high spin state for iron (IV) . An interpretation of the evolution of Mössbauer parameters is proposed, based on bond competition considerations.     

Mössbauer spectra of Nd2Fe14B and related compounds

Mössbauer spectra and ac susceptibility data on Nd₂Fe_{1 4} B with substitution of Pr or Sm for Nd indicate that the spinreorientation temperature is depressed by Pr substitution but increased in alloys containing Sm so that it occurs at roomtemperature for Nd_{1 2}Sm₅Fe_{7 6}B₇. In the Nd end-member, the onset of the transition appears about 210 K although the main reorientation is at 134 K. Nickel shows no marked site preference: its effects are to increase slightly the Curie temperature and reduce the iron moment.