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.     

Mössbauer study of Fe-Re alloys prepared by mechanical alloying

The room temperature Mössbauer spectra of ⁵⁷Fe were measured for nanocrystalline iron-based solid solutions Fe _1?x Re _x , prepared by mechanical alloying with x in the range 0.01 ≤ x ≤ 0.04. The obtained data were analysed in terms of the binding energy E _b between two rhenium atoms in the Fe-Re system. The extrapolated value of E _b for x = 0 was used for computation of enthalpy of solution of rhenium in iron. The result was compared with that resulting from the cellular atomic model of alloys by Miedema as well as with value, derived from proper data for Fe-Re solid solutions obtained by melting in an arc furnace. From the comparison it follows that our findings are in agreement with the Miedema’s model predictions and previous Mössbauer studies.     

Mössbauer study of the mechanical alloying of highly concentrated Fe–Cr alloys

Mössbauer spectroscopy and X-ray diffraction are used to investigate the kinetics of the mechanical alloying (MA) of Fe and Cr powdered mixtures with Cr contents of 20 to 48 at % in the initial mixtures. Variations during mechanical alloying in specimens with Cr contents of ≤30% and >30% in the initial mixtures are observed for the first time. After MA, specimens are characterized by heterogeneous concentration distributions of Cr and Fe atoms in particles, especially at Cr concentrations of >30% in the initial mixture.     

Mössbauer and XRD study of hot dip galvanized alloy

Mössbauer spectroscopy has been used to investigate the nature of the Zinc-Iron alloys present within the Hot Dip Galvanized (HDG) layers of steel with a silicon content of 0.35 %. The investigation also studied the impact of the powder coating pretreatment on the nature of the alloy layers. The acid etching process within the pretreatment process in particular would be expected to have a significant impact on the HDG layer. This study utilized ⁵⁷Fe Mössbauer spectroscopy to examine identically processed samples prior to and post pre treatment. XRD and ⁵⁷Fe CEMS measurements were performed on hot galvanized S355J2 + N samples, forming sandwiched structure. Both XRD and CEMS reveal the presence of dominant steel phase in accordance with its estimated occurrence on the surface of the sandwiched samples. Minor Γ-Fe3Zn10, ζ-FeZn15 and solid solution Fe-Zn as well as minor Fe-Si phases could also be identified.     

Probe Mössbauer spectroscopy of the grain boundaries of a Mo-O nanocrystalline system obtained by mechanical alloying

The localization of Fe atoms in the process of mechanical alloying of a Mo powder composite with 8 at % O at boundaries of the bcc Mo grains has been investigated by Mössbauer spectroscopy on impurity ⁵⁷Fe isotope atoms (1 at %), X-ray diffraction, and Auger spectrometry. The process begins with the formation of a nanostructure (～10 nm) in bcc Mo and ends with the formation of a bcc supersaturated solid solution with O atoms at interstitial positions and Fe atoms at substitutional positions. The presence of oxygen in the boundaries of bcc Mo grains leads to an extraordinarily large isomer shift (2 mm/s with respect to α-Fe) for the grainboundary component in the Mössbauer spectrum. This circumstance makes it possible to consider ⁵⁷Fe-O complexes as new probes for studying grain boundaries of powder nanocrystalline materials. As a result, the following three structural components have been identified in the mechanically activated system: a grain boundary and distorted near-boundary regions with the common name interface and a grain with the perfect (defect-free) structure. For powder nanocrystalline (～10 nm) materials subjected to intense mechanical treatment in a planetary ball mill, the widths of the unrelaxed grain boundary and interface average over the entire volume of particles have been experimentally estimated as 0.2 and 1 nm, respectively.     

Mössbauer and XRD study of Al-Sn linished steel bimetal alloy

Aluminium alloy free CS1 type steel (0.06 wt% C, 0.45 wt% Mn) and samples of cold roll bonded steel bimetal alloys (MAS15 and MAS16) were fabricated and investigated by X-ray diffraction (XRD), ⁵⁷Fe conversion electron Mössbauer spectroscopy (CEMS) at room temperature. XRD has revealed only the existence of the alpha iron solid solution (steel) phase in the steel only sample, while identified steel and metallic Al and Sn constituent phases in the bimetallic alloys. ⁵⁷Fe Mössbauer spectroscopy revealed the presence of 4 % secondary iron-bearing phase attributed mainly to iron oxide/ oxyhydroxides (ferrihydrite) besides the steel matrix on the surface of the steel sample. A significant difference between the occurrences of the secondary phase of differently prepared bimetal alloys found in their ⁵⁷Fe CEM spectra allowed to identify the main phase of debris as different iron oxide/ oxyhydroxides.     

Mössbauer and XRD study of novel quaternary Sn-Fe-Co-Ni electroplated alloy

Constant current electrochemical deposition technique was used to obtain quaternary alloys of Sn-Fe-Co-Ni from a gluconate electrolyte, which to date have not been reported in the literature. For the characterization of electroplated alloys, ⁵⁷Fe and ¹¹⁹Sn Conversion Electron Mössbauer Spectroscopy (CEMS), XRD and SEM/EDAX were used. XRD revealed the amorphous character of the novel Sn-Fe-Co-Ni electrodeposited alloys. ⁵⁷Fe Mössbauer spectrum of quaternary deposit with composition of 37.0 at% Sn, 38.8 at% Fe, 16.8 at% Co and 7.4 at% Ni displayed a magnetically split sextet (B = 28.9T) with broad lines typical of iron bearing ferromagnetic amorphous alloys. Magnetically split ¹¹⁹Sn spectra reflecting a transferred hyperfine field (B = 2.3T) were also observed. New quaternary Sn-Fe-Co-Ni alloys were successfully prepared.     

A pre-Columbian copper alloy smelting furnace: Mössbauer and XRD study of the firing conditions

Samples from a pre-Columbian furnace used for copper alloy smelting on the Pampa de Chaparrí in northern Peru during the Middle to Late Sicán Period (AD 900–1375) were studied by Mössbauer spectroscopy, X-ray diffraction and X-ray fluorescence. The data thus obtained allow conclusions as to the temperatures and oxidation-reduction conditions prevaling at different positions inside the furnace during the smelting process.     

Mössbauer study of the Cu-Zn alloy system

Using the 93.3keV transition in⁶⁷Zn, the Lamb-Mössbauer factor, the electron density and the electric field gradient at the Zn nucleus have been determined for pure Zn metal, the ^–, ^–, ^–, and -phases as well as pure Cu metal.     

Mössbauer and XRD study of intercalated CaFe-layered double hydroxides

N-containing fully saturated (L-prolinate) or aromatic (indole-2-carboxylate) heterocyclic anions were immobilised in CaFe-layered double hydroxide with the dehydration-rehydration method from aqueous ethanol or acetone. The structure of the resulting organic-inorganic hybrids was characterised mainly with powder X-ray diffraction and ⁵⁷Fe Mössbauer spectroscopy, and as supplementary analysis scanning electron microscopy, energy dispersive X-ray spectroscopy with elemental mapping and molecular modelling were also applied. It was found that the solvent mixture used for the synthesis caused enormous difference in the interlayer spacings of the obtained inorganic-organic hybrids.     

Mössbauer spectroscopy study of iron oxide nanoparticles obtained by spray pyrolysis

Mössbauer spectroscopy was used in this study to investigate magnetite nanoparticles, obtained by spray pyrolysis and thermal treatment under H₂ reduction atmosphere. Room temperature XRD data indicate the formation of magnetite phase and a second phase (metallic iron) which amount increases as the time of reduction under H₂ is increased. While room temperature Mössbauer data confirm the formation of the cubic phase of magnetite and the occurrence of metallic iron phase, the more complex features of 77 K-Mössbauer spectra suggest the occurrence of electronic localization favored by the different crystalline phase of magnetite at low temperatures which transition to the lower symmetry structure should occur at T ～120 K (Verwey transition).     

Mechanism and kinetics of solid-state amorphization by mechanical alloying of Al65Cu 35−x Nb x

In the present study, we have synthesized a number of Al-based Al₆₅Cu_35???x Nb_x ternary alloys by mechanical alloying and undertaken a detailed characterization of their microstructural evolution by X-ray diffraction, high-resolution transmission electron microscopy and positron annihilation spectroscopy. To predict the phase-equilibrium in a given ternary powder blend subjected to mechanical alloying, we have modified the Miedema model to incorporate the influence of interfacial energy contribution in solid-state amorphization and analytically calculate the enthalpy and Gibbs energy of ternary amorphous and nanocrystalline solid solutions. The predicted trend compares well with the experimental data. Finally, an attempt has been made to determine the mechanism of solid-state amorphization in Al₆₅Cu_35?xNb_x alloys utilizing both experimental results and model-based thermodynamic calculations.     

Complementary 57Fe and 119Sn M?ssbauer study of mechanochemical redox reaction

A non-thermal route to oxide nanocomposites by mechanochemical redox reactions in the ??-Fe₂O₃ + SnO system is presented. The important impact of the work, from the methodology point of view, is the combined application of ⁵⁷Fe and ¹¹⁹Sn Mössbauer spectroscopies to the study of the mechanically induced redox processes, resulting in the reduction of ??-Fe₂O₃ and the oxidation of SnO. In addition, the obtained product was characterized by X-ray diffraction and transmission electron microscopy.     

Properties of Fe–Ga based powders prepared by mechanical alloying

Alloys of Fe–Ga with starting compositions of 17, 19, 21, 23, and 25 at% Ga and Fe₈₁Ga₁₇Z₂ (Z=Si, Sn) have been prepared by mechanical alloying. Samples were milled in a SPEX Model 8000 mill with a ball to sample weight ratio of about 4:1. Phase formation as a function of milling time has been investigated for the 19 at% Ga sample and suggests that milling times of 12 h produce fully alloyed samples. Alloys have been studied by electron microprobe, X-ray diffraction, vibrating sample magnetometery and ⁵⁷Fe Mössbauer effect spectroscopy. Fully milled powders have measured compositions of Fe_100−xGa_x with x=15.7, 17.0, 19.0, 22.4, and 24.0 and Fe_83.1Ga_15.2Z_1.7 (for both Z=Si and Sn). X-ray diffraction showed the presence of a disordered bcc phase with no indication of an ordered D0₃ phase. However, the latter is difficult to observe with X-ray diffraction because of the low intensity of the fcc superlattice peaks. A bimodal Fe hyperfine field distribution as obtained from Mössbauer effect spectra indicated the presence of two discrete Fe environments. The results suggested a lower degree of Ga clustering than has been previously observed in Fe–Ga alloys, of similar composition, prepared by melt spinning. The microstructure is similar to that of Fe–Ga thin films prepared by combinatorial sputtering. Some samples have also been studied after annealing at 800 °C for 8 h. No changes were observed in X-ray diffraction patterns after annealing. However, Mössbauer effect studies show the formation of D0₃ and L1₂ order in annealed samples analogous to the phases observed in melt spun ribbons of similar composition.     

57Fe Mössbauer study of Lu2Fe3Si5 iron silicide superconductor

With the advent of Fe–As based superconductivity it has become important to study how superconductivity manifests itself in details of ⁵⁷Fe Mössbauer spectroscopy of conventional, Fe-bearing superconductors. To this end, the iron-based superconductor Lu₂Fe₃Si₅ has been studied by ⁵⁷Fe Mössbauer spectroscopy over the temperature range from 4.4 K to room temperature with particular attention to the region close to the superconducting transition temperature (T_c=6.1 K). Consistent with the two crystallographic sites for Fe in this structure, the observed spectra appear to have a pattern consisting of two doublets over the whole temperature range. The value of Debye temperature was estimated from temperature dependence of the isomer shift and the total spectral area and compared with the specific heat capacity data. Neither abnormal behavior of the hyperfine parameters at or near T_c, nor phonon softening were observed.     

Mössbauer spectroscopy study of the EuO:Fe spintronic material

The states of iron and europium in the EuO:Fe composite spintronic material have been studied by means of room-temperature Mössbauer spectroscopy. In both cases, two sets of lines indicating the ferromagnetism and superparamagnetism of metallic iron nanoparticles in the composite and the appearance of a fraction of europium ions in the Eu³⁺ oxidation state in the matrix in addition to the main Eu²⁺ state have been observed in the respective spectra. In the europium case, the observation implies the possibility of a partial spin polarization of paramagnetic europium ions in Eu-Fe-O clusters and an increased specific magnetization of the composite.     

Mössbauer study of the ageing effects on the structure of CuZnSn shape memory alloy

Using the¹¹⁹Sn Mössbauer spectroscopy the study of ageing effects on the structure of a CuZnSn shape memory alloy was performed.Two stages of ageing at 200 C were observed.The first stage is connected with formation of DO₃ structure and the second stage with precipitation of and phases.     

Mössbauer spectra obtained by modulation of a scattering crystal

We have carried out numerous experiments with supersources having intensities in the 100 Curie range. These sources usually require massive shielding, and are not easily moved to carry out Mössbauer spectroscopy. Several of these sources can be used with microfoil conversion electron (MICE) detectors, but they cannot be moved easily either because of the delicate microfoils used, which ideally have thicknesses less than the range of the internally converted electrons. Here, we describe a technique for doing Mössbauer spectroscopy by oscillating a monochromating crystal parallel to the reciprocal lattice vector of the Bragg reflection, this being used to filter out extraneous photons from the beam. Specifically, an LiF crystal is used in diffraction experiments as a filter to scatter the 46.5-keV Mössbauer gamma rays from¹⁸³Ta by setting it at the (200) Bragg reflection. In the present measurements, the LiF crystal was mounted in the transmission mode and oscillated with a crank along the scattering vectorQ to produce the velocity modulation, with the source, sample and absorber all at rest. The velocity components of the filtering crystal along the incident and scattered beams cause the measured linewidth to be equal to the usual Mössbauer width divided by 2 sin, where is the Bragg angle. Measured widths for the (200), (400), (600) and (800) Bragg reflections agreed with the calculated values of 12.08, 6.04, 4.03 and 3.02 cm/s, within our experimental uncertainties. The technique could have applications not only to MICE detectors, but also to very narrow resonances such as⁶⁷Zn, where the increased velocities required for small Bragg angles could be an advantage and lead to enhanced resolution.