Mössbauer and X-ray study of the Fe 65 Ni 35 invar alloy obtained by mechanical alloying

Fe₆₅Ni₃₅ samples were prepared by mechanical alloying (MA) with milling times of 5, 6, 7, 10 and 11 h, using a ball mass to powder mass ratio of 20:1 and at 280 rpm. The samples were characterized by X-ray diffraction (XRD) and transmission ⁵⁷Fe Mössbauer spectrometry. The X-ray diffraction pattern showed the coexistence of one body centered cubic (BCC) and two face centered cubic (FCC1 and FCC2) structural phases. The lattice parameters of these phases did not change significantly with the milling time (2.866 Å, 3.597 Å and 3.538 Å, respectively). After 10 h of milling, the X-ray diffraction pattern showed clearly the coexistence of these three phases. Hence, Mössbauer spectrometry measurements at low temperatures from 20 to 300 K of this sample were also carried out. The Mössbauer spectra were fitted using a model with three components: the first one is a hyperfine magnetic field distributions at high fields, related to the BCC phase; the second one is a hyperfine magnetic field distribution involving low hyperfine fields related to a FCC phase rich in Ni, and the third one is a singlet related to a FCC phase rich in Fe, with paramagnetic behavior. As proposed by some authors, the last phase is related with the antitaenite phase.     

Low temperature 151Eu and 57Fe Mössbauer study of mechanically alloyed EuFeO3

Low temperature ⁵⁷Fe Mössbauer spectra of mechanically alloyed EuFeO₃ prepared by mechanical alloying depicts an interesting transformation in its hyperfine magnetic state, from a triple phase magnetic system at room temperature to a single phase ferromagnetic state at 20 K. The hyperfine magnetic field increased by 12% at 20 K from its room temperature. The isomer shift and quadrupole splitting values exhibit a peak around 200 K. Low temperature ¹⁵¹Eu Mössbauer measurements show that the line-width increased to its maximum value at 80 K which is 45% compared to its room temperature value not enough to suggest splitting.     

Production of spin polarized 12N through heavy ion reactions

The structural and magnetic properties of Ho substituted BiFeO₃ (BHFO) have been investigated using ⁵⁷Fe Mössbauer spectroscopy and X-Ray diffraction (XRD) as a function of temperature. The Mössbauer spectrum obtained at room temperature for the as-synthesized BHFO sample exhibits broadened features due to the hyperfine field distributions related to the local variation of the neighbourhood of Fe and the magnetic hyperfine splitting patterns are indicative of magnetic ordering, mostly probably screwed or slightly antiferromagnetic. The spectrum was fitted with two superimposed asymmetric sextets, with similar hyperfine magnetic fields of B_hf1 = 48.0(1) T and B_hf2 = 49.0(1) T, corresponding to rhombohedral BFO. The hyperfine fields of the magnetic components decreased systematically with increasing temperature to a ‘field distribution’ just below the Néel temperature, T_N ~ 600 K. At temperatures above 600 K, the spectral line associated with the Bi₂₅FeO₄₀ impurity phase dominates the spectra. This phase is confirmed by XRD measurements. From the temperature dependence of the site populations of the spectral components an average Debye temperature of θ _D = 240(80) K has been estimated.     

Structural and magnetic properties of Fe–Ni mecanosynthesized alloys

Fe_100???x Ni _x samples with x?=?22.5, 30.0 and 40.0 at.% Ni were prepared by mechanical alloying (MA) with milling times of 10, 24, 48 and 72 h, a ball mass to powder mass (BM/PM) ratio of 20:1 and rotation velocity of 280 rev/min. Then the samples were sintered at 1,000°C and characterized by X-ray diffraction (XRD) and transmission Mössbauer spectrometry (TMS). From the refinement of the X ray patterns we found in this composition range two crystalline phases, one body centered cubic (BCC), one face centered cubic (FCC) and some samples show FeO and Fe₃O₄ phases. The obtained grain size of the samples shows their nanostructured character. Mössbauer spectra were fitted using a model with two hyperfine magnetic field distributions (HMFDs), and a narrow singlet. One hyperfine field distribution corresponds to the ferromagnetic BCC grains, the other to the ferromagnetic FCC grains (Taenite), and the narrow singlet to the paramagnetic FCC grains (antitaenite). Some samples shows a paramagnetic doublet which corresponds to FeO and two sextets corresponding to the ferrimagnetic Fe₃O₄ phase. In this fit model we used a texture correction in order to take into account the interaction between the particles with flake shape and the Mössbauer $\upgamma$ -rays.     

Mössbauer effect in natural strunzite, ferristrunzite and ferrostrunzite

The temperature dependence of the ferric and ferrous hyperfine fields in natural samples of strunzite, ferristrunzite and ferrostrunzite is determined by Mössbauer spectroscopy between 4.2 K and their magnetic transition temperatures (T _N), i.e. 50.5±0.5 K, 43.0±0.5 K and 44.0±0.5 K respectively, which are determined by Mössbauer thermoscanning. Two dominating magnetically split ferric subspectra were consistently present in all of the samples and are related to the Fe(1) and Fe(2) sites in the crystallographic structure, but an unambiguously assignment to a specific site is not possible. The difference between the corresponding hyperfine fields is very small. In the strunzite sample these fields are well defined and rather weakly dependent of temperature. In the other samples the corresponding hyperfine fields are more distributed especially at higher temperatures (below T _N). The relative contribution in the spectra of the third magnetic ferric component differs strongly between the samples and is assigned to ferric ions at the Mn site. At the lowest temperatures applied, its hyperfine field exceeds all other field values, but it decreases rather rapidly with increasing temperature, in so far that the corresponding spectral lines make a crossover with the lines of the other ferric subspectra. The magnetically split spectra of ferrostrunzite consist additionally of a ferrous magnetic component, which could be successfully analysed by introducing two magnetically split ferrous subspectra, which strongly overlap with each other but also with the ferric components. At higher temperatures in the magnetic region all subspectra overlap more and in the case of ferri- and ferrostrunzite the ferric hyperfine fields were distributed over a wider range.     

237Np and 57Fe Mössbauer study of NpFeGa5

⁵⁷Fe and ²³⁷Np Mössbauer ōmeasurements have been performed for NpFeGa₅, which is one of the so-called neptunium 1-1-5 compounds. The ⁵⁷Fe Mössbauer spectra below T _N = 118 K show the magnetically ordered state. The magnitude of the hyperfine magnetic field at the ⁵⁷Fe nucleus is determined to be 1.98 ± 0.05 T at 10 K. From the ²³⁷Np Mössbauer spectrum at 10 K, the hyperfine magnetic field at the ²³⁷Np nucleus is 203 T and the hyperfine coupling constant is determined to be 237 T/μ_B using the Np atomic magnetic moment of 0.86 μ_B determined by the neutron diffraction study.     

Mössbauer studies of impactites from Huamalies province in Huanuco Region

This report is about the X-ray diffraction and Mössbauer studies of three impactite samples denominated PMe-8, PMe-9 and PMe-11 from Huamalies Province in Huánuco Region, Peru. When terrestrial rocks are submitted to pressures higher than 60 GP, the majority is completely melted, forming a kind of glass called impactites. X-ray diffraction indicates the presence of quartz as the principal mineralogical phase in all samples. The ⁵⁷Fe Mössbauer spectra at room temperature of samples PMe-8 and PMe-9 show broadened spectra that were fitted using a distribution model. The most probable field of the magnetic component is 34 T, corresponding to the presence of small particles of goethite, confirmed by the 4.2 K spectrum. For the sample PMe-11, the MS showed the presence of well crystallized hematite.     

A Mössbauer spectroscopic study of the effect of molybdenum during preparation of Nd-Fe-B magnets

Elements in atomic ratios Nd₂(Fe_0.9Mo_0.1)₁₄B were melted in an induction furnace and annealed in order to examine the effect of molybdenum during the preparation of Nd-Fe-B magnets. A phase analysis has been made from ⁵⁷ Fe Mössbauer spectroscopic measurements in the temperature range of 100 to 700 K. It is found that two iron containing phases are formed, one Mo rich Fe alloy and the other Nd-Fe(Mo)-B isostructural to Nd₂Fe₁₄B. The Nd_1.1Fe₄B₄ phase usually found in Nd-Fe-B magnets is not observed in these samples. The Curie temperature, T_c, is found to be 605(5) K from the Mössbauer as well as vibrational sample magnetometer measurements on the same sample. At low temperatures, the average hyperfine field at Fe nuclei is found to show a decrease with respect to the value for Nd₂Fe₁₄B.     

Evidence of magnetic broadening in Mössbauer spectra of superconducting FeTe 0.8 S 0.2

Magnetic properties of the FeTe_0.8S_0.2 superconductor were studied by Mössbauer spectroscopy. Low-velocity Mössbauer spectra that were recorded in the temperature range from 5.7 K up to 300 K show a paramagnetic doublet with a broadening at temperatures below 77 K. The broadening can be explained by the appearance of a distribution of hyperfine magnetic fields due to the magnetic ordering of a part of the sample. The magnetically ordered fraction starts to decrease at temperatures below 20 K indicating a possible competition with the onsetting superconductive state.     

Tin-doped spinel-related oxides of composition M3O4 (M = Mn, Fe, Co)

Tin-doped compounds of spinel-related M₃O₄ (M = Fe, Mn, Co) have been studied by ¹¹⁹Sn and ⁵⁷Fe Mössbauer spectroscopy in the temperature range of 20–600 K. The ¹¹⁹Sn Mössbauer spectra recorded down to 20 K from the non-iron-containing compounds of Co₃O₄ and Mn₃O₄ contained only doublets showing no transfer of magnetic properties from cobalt or manganese to the dopant tin ions. In contrast, the tin-doped-(FeCo)₃O₄ and (FeMn)₃O₄ gave ¹¹⁹Sn and ⁵⁷Fe Mössbauer spectra, which showed magnetic hyperfine interactions. The Curie temperature has been estimated for the former sample.     

57Fe hyperfine interactions in M1 and M2 sites of olivine from Omolon meteorite: study using Mössbauer spectroscopy

Study of olivine (Fe, Mg)₂SiO₄ from Omolon meteorite was performed using Mössbauer spectroscopy with a high velocity resolution at 295 and 90 K. Components related to ⁵⁷Fe in crystallographically non-equivalent M1 and M2 sites in olivine were determined and its Mössbauer hyperfine parameters were evaluated at both temperatures. A Fe^2?+?–Mg^2?+? distribution coefficient and a temperature of cation equilibrium distribution for olivine from Omolon were evaluated on the basis of Mössbauer parameters.     

Structural study of spheroidal graphite cast iron with 4% Si and Mo additions; effects of thermal treatment

The Mössbauer spectrum of the as-cast sample is in agreement with a statistical distribution of Si. The carbides of (Fe?Mo?Si)₃C and (Fe?Mo?Si)₆C type are paramagnetic down to 77 K. The Mössbauer spectrum of the as-quenched sample is mainly influenced by Si. For the tempered samples, a gradual disappearence of austenite is observed while the transformation of martensite into ferrite detected from the hyperfine field distribution occurs between 773 K and 873 K.     

Mössbauer studies of GdFe2 − x Hf x alloys

GdFe_2???x Hf _x alloys, where x?=?0, 0.10, 0.15, 0.20, and 0.30, are produced by arc-melting of pure elements. The samples are investigated by x-ray diffraction and Fe⁵⁷ Mössbauer spectroscopy at 78 K and 300 K. We find that the alloy system GdFe_2???x Hf _x have the single phase cubic Cu₂Mg type structure in the whole concentration range. Mössbauer spectroscopic results show that all the samples studied are magnetically ordered at 78 K, and at room temperature. The room temperature spectra are fitted with two magnetic components where the direction of magnetization is along the [111] while the spectra at 78 K are fitted with four magnetic subspectra indicating a complex direction of magnetization for all samples under investigation. The average magnetic hyperfine field and the average isomer shift are found to decrease almost linearly with increasing the Hf concentration at 78 K and 300 K due to the replacement of Fe by nonmagnetic Hf.     

Magnetic phase diagram of the FexMn0.7-xAl0.3 alloys series obtained by Mössbauer spectroscopy

By Mössbauer spectroscopy the magnetic phase diagram of the Fe_xMn_0.7-xAl_0.3 spin glass alloy has been obtained. X-ray diffraction (XRD) has shown that all the alloys are in the BCC phase. The broad spectral lines observed in the Mössbauer spectra are indicative of the disordered character of these alloys. Depending on the composition and the temperature the alloys behave as paramagnetic (P), ferromagnetic (F) and reentrant spin glass (RSG). For the alloys rich in iron the only detected magnetic transition is from F to P. For medium iron content two transitions were observed, namely from RSG to F and from F to P. The RSG phase is obtained as a consequence of the disordered character of the alloys and the competitive exchanges due to iron and manganese atoms.     

Thermal equilibrium defects in iron-based alloys

The Mössbauer spectra of ⁵⁷Fe were measured for the thermal equilibrium b.c.c. Fe_0.947V_0.053 and Fe_0.956Co_0.044 solid solutions being at temperature ranging from 300 to 1,000 K. The obtained data were analysed in terms of concentration of unoccupied sites in the 14-site surroundings of an ⁵⁷Fe Mössbauer probe in a b.c.c. sample. It turned out that the probe detects unoccupied sites in its neighbourhood when the temperature of the material studied does not exceed about 900 K. This result suggests that the Mössbauer spectroscopy “sees” the pre-vacancy effect revealed by the positron annihilation spectroscopy in the early 1960s.     

Magnetic and Mössbauer spectroscopic studies of NiZn ferrite nanoparticles synthesized by a combustion method

The properties of nanocrystalline Ni_0.5Zn_0.5Fe₂O₄ synthesized by an auto-combustion method have been investigated by magnetic measurements and Mössbauer spectroscopy. The as-synthesized single phase nanosized ferrite powder is annealed at different temperatures in the range 673–1,273 K to obtain nanoparticles of different sizes. The powders are characterized by powder X-ray diffraction, vibrating sample magnetometer, transmission electron microscopy and Mössbauer spectroscopy. The as-synthesized powder with average particle size of ~9 nm is superparamagnetic. Magnetic transition temperature increases up to 665 K for the nanosized powder as compared to the transition temperature of 548 K for the bulk ferrite. This has been confirmed as due to the abnormal cation distribution, as evidenced from room temperature Mössbauer spectroscopic studies.     

Mössbauer study of spin structure transformation from an incommensurate to a commensurate state

We present crystallographic and magnetic properties of NiCr_1.98 ⁵⁷Fe_0.02O₄ by using X-ray diffractometry (XRD), vibrating sample magnetometry (VSM), and Mössbauer spectroscopy. The lattice constants a₀ were determined to be 8.318 Å. The ferrimagnetic Neel temperature (T _N) for NiCr_1.98 ⁵⁷Fe_0.02O₄ is determined to be 90 K. The Mössbauer absorption spectra for all chromites at 4.2 K show two well developed sextets superposed with small difference of hyperfine fields (H _hf) caused by Cr^3?+? ions in two different magnetic sites. The values of the isomer shifts show that the charge states of Fe are Fe^3?+? for all temperature range. Ni-chromites Mössbauer spectra below T _N present aline broadening due to a Jahn–Teller distortion and show that spin structure behavior of Cr ions change from an incommensurate to a commensurate state.     

Effect of Ni on the lattice parameter and the magnetic hyperfine field in (Fe70Al30)100 − x Ni x alloys

Samples of the (Fe₇₀Al₃₀)_100???x Ni _x system, with x?=?5, 10, 15, and 20, were prepared by mechanical alloying using milling times of 12, 24, 36, 48, and 72 h and characterized by X-ray diffraction (XRD) and Mössbauer spectrometry (MS). XRD of all the samples allowed us to identify the BCC structure as the main component. A decreasing lattice parameter, as the milling time and Ni content increase, was obtained. The MS experiments were carried out at room temperature. The spectra were fitted with a hyperfine magnetic field distribution (HMFD). The Mean Hyperfine Fields (MHF) are ranged between 27 and 29 T with a small dependence with the milling time and was not strongly influenced by Ni content. An additional paramagnetic single line in the spectra of samples with x?=?20 and that of sample with x?=?15 and milled during 72 h must be included. The Mössbauer spectral area of this phase increases when the milling time increases and it was associated to an FCC phase.     

Mössbauer study of nano-TiO2 doped with Fe

A Mössbauer study of nano-TiO₂ doped with Fe is presented. The samples are prepared by sol-gel method, doping Fe by 5, 10 and 15 wt.%, respectively, which are measured with XRD, TEM and Raman spectra. Especially, Mössbauer spectra are emphasized in this study. The anatase phase is major in both doped and no-doped sample. The α-Fe₂O₃ phase is also in the doped samples. The grain size of doped sample is in 5–20 nm range, the major grains are about 13 nm. And the grain size of no-doped sample is about 8 nm. Studying Mössbauer spectra and Raman spectra, we concluded that in the doping process the Fe³⁺ ions entered anatase lattice and substituted Ti⁴⁺ ions. However, the amount of Fe ions in the site is limited to about 1.5 wt.%. It does not increase as the doping Fe increase. The more Fe doped, the more α-Fe₂O₃ formed. For comparing conveniently, it also can be described as (Ti_0.98Fe_0.02)O₂ by atomic percent.     

Systematic study of mechanical deformation on Fe3Al x Si1−x powders by Mössbauer spectroscopy

The Mössbauer technique has been used to measure hyperfine magnetic fields, isomer shifts and relative areas of ⁵⁷Fe atoms located at various sites in Fe₃Al _x Si_1?x series with x?=?0, 0.3, 0.5, 0.7. Four samples were crushed; then they were annealed for 10 h at 1,023 K and cooled down at 3°/min in order to recover the DO₃ stable phase. Mössbauer studies revealed that annealed samples have a DO₃ structure, whereas deformed samples are partially disordered, with both ordered DO₃ and disordered A2 structures, even though X-rays measurements do not show superstructure peaks. The amount of disordered structure decreases with Si content.