Investigation of Fe-Mg-Alloys Produced by Ion Implantation

Iron and magnesium are insoluble elements with each other and there is no phase diagram. However, it is possible to produce artificial alloys by ion implantation, in this study by iron implantation into magnesium. Samples are investigated by conversion electron Moessbauer spectroscopy, Auger electron spectroscopy and x-ray diffraction. While at low doses gaussian shaped iron profiles and paramagnetic doublets as Mössbauer spectra are obtained, the iron concentration reaches at the highest dose 90 at.-% in maximum and the Mössbauer spectrum shows a dominant ferromagnetic fraction. The x-ray diffraction pattern let conclude that a dilated α-iron lattice is formed. Microhardness of all samples is clearly increased due to the implantation.     

Effect of particle size and alloying with different metals on 57Fe Mössbauer spectra

Iron nanoparticles of various sizes have been synthesized using the chemical route which involves the preparation of iron bipyridine complexes in presence of different capping agents followed by thermal decomposition at 450°C in inert atmosphere. The bimetallic nanoalloys of Fe with Mg and Pd have also been prepared by following the same route. The resulting nanoparticles have been characterized by EDX-RF, XRD, AFM and ⁵⁷Fe Mössbauer spectroscopy. The appearance of quadrupole doublets in the Mössbauer spectra of Fe nanoparticles indicates the absence of magnetic interaction and variation in parameters is due to the varying particle size. The Mössbauer spectrum of Fe–Mg₂ bimetallic nanoalloy shows two doublets indicating the presence of superparamagnetism. The two doublets can be attributed to change in s-electron density of iron resulting from its two neighboring magnesium atoms. Fe–Pd nanoalloy Mössbauer spectrum is characterized by having a superparamagnetic doublet and a ferromagnetic sextet.     

Sol-gel synthesis and dilute magnetism of nano MgO powder doped with Fe

Mg oxides doped with 1 % ⁵⁷Fe were prepared by a sol-gel method, and annealed at various temperatures. Nano-size Mg oxides were characterized by Mössbauer spectrometry, magnetization and XRD measurements. The crystalline size of MgO increases with increase of annealing temperature. Samples annealed at 600 °C and 800 °C gave only doublet peaks of paramagnetic Fe³⁺ in Mössbauer spectra although Fe³⁺ doping into MgO induced a distorted structure and showed weak ferromagnetism. It is considered that the magnetic property is due to defect induced magnetism by doping Fe³⁺ into MgO. For a sample heated at 1000 °C, it is found from low temperature Mössbauer spectra that Fe³⁺ species are located at the core and shell of fine MgFe₂O₄ grains and diluted in MgO matrix.     

Valence and magnetic states of impurity iron ions in the La<Subscript>0.75</Subscript>Sr<Subscript>0.25</Subscript>Co<Subscript>0.98</Subscript>Fe<Subscript>0.02</Subscript>O<Subscript>3</Subscript> perovskite

The local magnetic and valence states of impurity iron ions in the rhombohedral La_0.75Sr_0.25Co_0.98 ⁵⁷Fe_0.02O₃ perovskite were studied using Mössbauer spectroscopy in the temperature range 87–293 K. The Mössbauer spectra are described by a single doublet at 215–293 K. The spectra contained a paramagnetic and a ferromagnetic component at 180–212 K and only a broad ferromagnetic sextet at T < 180 K. The results of the studies showed that, over the temperature range 87–295 K, the iron ions are in a single (tetrahedral) state with a valence of +3. In the temperature range 180–212 K, two magnetic states of Fe³⁺ ions were observed, one of which is in magnetically ordered microregions and the other, in paramagnetic microregions; these states are due to atomic heterogeneity. In the magnetically ordered microregions in the temperature range 87–212 K, the magnetic state of the iron ions is described well by a single state with an average spin S = 1.4 ± 0.2 and a magnetic moment μ(Fe) = 2.6 ± 0.4μ _B .     

Atomic jump processes in metallic systems: In-beam Mössbauer studies

An in-beam Mössbauer spectrometer was set up at the VICKSI heavyion accelerator in Berlin. Coulomb excited Mössbauer nuclei can be implanted into arbitrary sample materials. Measuring temperatures may be varied from 5 K to 650 K. A typical scpectrum shown in this work can be measured within a few hours.⁵⁷Fe was implanted into metals having large atomic volumes: Al, α-Zr, β-Sn. In these matrices the strongly undersized iron atom tends to occupy interstitial sites and may undergo dynamic processes.     

Hyperfine interactions in solid state reaction of hematite with aluminium

The solid state reaction of hematite with aluminium has been induced by mechanical alloying. Mössbauer spectroscopy and X‐ray diffraction have been used to investigate the reaction products. The reaction was completed in a time longer than 15 min but shorter than 30 min. During the reaction a Fe(Al) bcc solid solution was obtained as a matrix, with Al₂O₃ as reinforcement. After prolonged milling both components were in a nanocrystalline paramagnetic state.     

Mössbauer spectroscopy study of mechanically alloyed Fe2O3–(Al, Co and WC) systems

Mössbauer spectroscopy revealed that a central hyperfine interaction doublet and an additional sextet characterized the appearance of new phases in the mechanically alloyed Fe₂O₃–Al and Fe₂O₃–Co systems. In the Fe₂O₃–Al system, the intensity of the central super paramagnetic doublet which represents small particles of iron, increased with increasing milling time from 5 to 30 h of mechanical alloying. The magnetic sextet characterizing hematite vanished in the room temperature Mössbauer spectra of samples produced after 25 h of mechanically alloying the 50% Fe₂O₃ and 50% Al system. In general XRD peak broadening was observed as a result of extensive material structural distortion and formation of small particles. Fe, Al₂O₃ and mixed iron–aluminium oxide phases were identified in the XRD patterns with a small persistence of the iron oxide up to 20 h of mechanically alloying the 1:1 system Al–Fe₂O₃. In the 50% Co–50% Fe₂O₃ system, a 55% abundant new phase CoFe₂O₄ was observed, from the Mössbauer spectra of the system. The presence of this new phase was confirmed by the XRD analysis. The high energy ball milling of WC–Fe₂O₃ revealed a more effective grinding compared to hematite alone. The hematite particles were reduced to nanosized particles.     

Change in the Form of Cementite in High Carbon Steel Wires

The change of carbides in 0.97 wt% carbon steel wires induced by cold drawing has been investigated by using Mössbauer spectroscopy and X-ray diffraction. The specimen wires have been drawn from 5mm down to 0.2mm in diameter. The carbide is confirmed to be cementite by the X-ray diffraction. Typical ⁵⁷Fe Mössbauer spectra obtained from the particles extracted from the wires show the superposition of a typical ferromagnetic cementite pattern and a rather broad paramagnetic doublet The relative intensity of the paramagnetic doublets increases as an increase in the degree of drawing. The cementite particles extracted from the outer parts of the wire behave as paramagnetic at 300K while the particles from the interior parts of the wire behave as an ordinary ferromagnetic cementite. The amount of the ferromagnetic cementite in the wire decreases with an increase in the degree of drawing. This means that the cementite has decomposed and dissolved into the matrix during the heavy deformation.     

Mössbauer effect and X-ray diffraction investigation of Si–Fe thin films

An X-ray diffraction and ⁵⁷Fe Mössbauer spectroscopy investigation of Si_{100– x} Fe _x (0?<?x?<?80) thin films prepared by combinatorial sputtering methods is reported. Resulting Mössbauer spectra were fit to Voigt-based distributions of quadrupole doublets for paramagnetic spectral components and Zeeman split sextets for ferromagnetic spectral components. In conjunction with the X-ray measurements, these results show that the Si-rich films are a mixture of dilute Fe in amorphous Si and an approximately equiatomic amorphous SiFe phase. Fe-rich films show the presence of a ferromagnetically ordered phase. For x?<?73, this ferromagnetic phase is amorphous or nanostructured and for x?≥?73, the phase is shown to be a crystalline bcc phase. Results are discussed in terms of short-range structural ordering in these alloys.     

Magnetic properties of fcc (Co95Fe5)1-xAlx ribbons

Rapidly quenched (Co₉₅Fe₅)_1-xAl_x ribbons are investigated by X‐ray diffraction, magnetization, and Mössbauer effect measurements. A single fcc phase is obtained for all ribbons x ? 10 at.%. The lattice constant increases linearly with x and is discussed in connection with magnetic moment. The influence of Al substitution on both magnetization and Fe‐atom hyperfine field (H) is studied. At 296 K, the magnetization decreases linearly while H drops nonlinearly as x increases. Al substitution leads to substantial differences in iron hyperfine fields in bcc and fcc systems. Fe moment is perturbed differently by Al substitution in fcc (Co₉₅Fe₅)_1-xAl_x and bcc Fe–Al systems.     

CEMS characterisation of Fe/high-κ oxide interfaces

The interfaces between Fe and different high-κ oxides are investigated by means of conversion electron Mössbauer spectroscopy (CEMS). Information on the magnetic ordering at the interface is obtained from the magnetic hyperfine splitting of the Mössbauer spectra. The reactivity of the Fe atoms at the interface (intermixing) is also estimated by CEMS. X-ray diffraction (XRD) and X-ray reflectivity (XRR) provide additional information on the intermixing and different phases present at the interface. CEM-spectra show the presence of both ferromagnetic and paramagnetic phases. CEMS and XRD results show that the Fe/HfO₂ and Fe/Al₂O₃ interfaces are the least reactive. The degree of intermixing between Fe and the high-κ oxide is determined by the oxide surface roughness.     

Mössbauer Spectroscopic Study on Vertical Distribution of Iron Species in Sediments from Qinghai Lake,China

In this study, ⁵⁷Fe Mössbauer spectroscopy has been applied to sediments collected from Qinghai Lake in Qinghai Province, China, to investigate the vertical distribution of iron species. Their Mössbauer spectra consisted of four doublets ascribable to one paramagnetic high-spin Fe³⁺, two paramagnetic high-spin Fe²⁺ with different quadrupole splittings, and one diamagnetic low-spin Fe²⁺ that corresponds to pyrite (FeS₂). The distribution of pyrite suggested climatic changes during the past nine thousand years. It was demonstrated that the iron speciation in the salt lake sediments by Mössbauer spectroscopy can be used to reconstruct the past environment.

     

Magnetic structure of ion-implanted bubble garnets

The surface magnetic structure of bubble garnet films implanted with 80 keV Ne⁺ ions has been investigated by conversion-electron Mössbauer spectroscopy in conjunction with backscattered X-ray Mössbauer spectroscopy. For lower doses (～1–3 × 10¹⁴Ne⁺cm^-2) a ferrimagnetic component with in-plane magnetization coexists with a smaller paramagnetic phase in the implanted layer; for a dose of 5 × 10¹⁴Ne⁺cm^-2 only a paramagnetic phase is observed.     

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.     

Mössbauer spectroscopy and X-ray diffraction study of FexMn0:70−xAl0:30 (0:40 < x < 0:70) alloys prepared by mechanical alloying

In order to study the structural and magnetic behaviour of Fe_xMn_0.70?xAl_0.30 (0.40≤x≤0.70) alloys prepared by mechanical alloying, Mössbauer spectroscopy and X‐ray diffraction techniques have been employed. All the alloys were prepared in 24 h and, in addition, for x=0.45 milling times of 4, 8, 12, 16 and 24 h were considered. X‐ray diffraction showed that all samples exhibit bcc‐type reflections. A slight decrease in grain size and a slight increase in lattice parameter with increasing Mn content were observed. For x=0.45, an increase in grain size with milling time has been evidenced. For this composition and 4 h of milling, the more intensive peak (1?1?0) was fitted with three peaks corresponding to that of Mn, Fe and the alloy, respectively. For 12 h milling only bcc peaks of the alloy were obtained. As the Fe concentration was increased beyond x=0.50, a phase change from paramagnetic to ferromagnetic, as well as an increment in the mean hyperfine field with x, was detected. For x=0.45 and 4 h of milling we registered the presence of both a single line, corresponding to the alloy, and a hyperfine field distribution with peaks in 27.5 and 23 T, as well as peaks at lesser fields. These peaks are associated to Fe sites with two or more Al and/or Mn atoms as next neighbours. These results are in agreement with those obtained by X‐ray diffraction.     

Structural and Mössbauer studies of aerosol FeCu nanoparticles in a wide composition range

Structure and magnetic state of aerosol FeCu nanoparticles of 10–30 nm size with Cu content of 0.6–92.1 at.% have been examined by X-ray diffraction and Mössbauer spectroscopy. The FeCu particles have been shown to consist of an iron core surrounded by a copper and Fe oxide shell. With increasing Cu content the iron core having a bcc structure is reduced down to its complete disappearance followed by vanishing ferromagnetism of the particles. Within the copper content from 4.9 to 74.3 at.% the bcc and fcc phases coexist, with the fcc phase having a lattice constant close to that of pure copper and the bcc lattice constant being slightly higher than that for pure Fe due to embedding Cu atoms into the Fe lattice. At Fe-rich FeCu samples a presence of two-spin (ferromagnetic and paramagnetic) components of the fcc Fe is also observed. In the case of a thin copper shell there is only the ferromagnetic fcc Fe, whereas with further thickening of the shell both spin states of the fcc Fe appear existing up to a 20% Cu content. For FeCu samples with a higher Cu content they disappear due to oxidation of the copper grains. The Cu-rich samples with Cu content higher 80 at.% have a fcc structure, with the lattice constant being slightly higher than that of copper and they are paramagnetic. A slight increase of the lattice constant is due to the penetration of small iron aggregations into the Cu grains. In contact with air, the FeCu particles become covered with Fe₃O₄ and Cu₂O. Their long-term exposure to ambient conditions leads to further oxidation process of Cu₂O to CuO.     

Identification of Green Rust Compounds in the Aqueous Corrosion Processes of Steels; the Case of Microbially Induced Corrosion and Use of 78 K CEMS

Fe(II)-Fe(III) hydroxy-sulphate Green Rust 2, GR2(SO₄ ^–), is obtained by microbially induced corrosion of steel. Transmission Mössbauer spectroscopy (TMS) was used to characterise the corrosion products of steel sheet piles under the biofilm at low sea-water level in a harbour. To understand the process, iron coupons maintained in aqueous solutions of 4 M NaCl and 0.1 M NaHCO₃ of pH 7.4 were studied by X ray diffraction and conversion electron Mössbauer spectroscopy (CEMS) at 78 K. The Fe(II)-Fe(III) hydroxy-carbonate, GR1(CO₃ ^–), covers the surface, as predicted by the E_h-pH diagram.     

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.     

Mössbauer study of Fe in 3C-SiC following 57Mn implantation

Our investigations on substitutional and interstitial Fe in the group IV semiconductors, from ⁵⁷Fe Mössbauer measurements following ⁵⁷Mn implantation, have been continued with investigations in 3C-SiC. Mössbauer spectra were collected after implantation and measurement at temperatures from 300 to 905 K. Following comparison with Mössbauer parameters for Fe in Si, diamond and Ge, four Fe species are identified: two due to Fe in tetrahedral interstitial sites surrounded, respectively, by four C atoms (Fe_i.C) or four Si atoms (Fe_i,Si) and two to Fe in (or close to) defect free or implantation damaged substitutional sites. An annealing stage at 300–500 K is evident. Above 600 K the Fe_i,Si fraction decreases markedly, reaching close to zero intensity at 905 K. This is accompanied by a corresponding increase in the Fe_i,C fraction.     

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.