57Fe Mössbauer spectra of a cleaned Weipa, Australia, kaolin showed that a considerable fraction of the structural iron exhibits paramagnetic relaxation between 4°K and 300°K, the first time that this has been observed for ferric ions in a mineral. The sample also contained a very fine particle ferric oxide/oxyhydroxide phase, probably of secondary origin.

57Fe Mössbauer spectra have been used to interpret the effects of different cleaning processes on the iron mineralogy of a Weipa, Australia, kaolin. A magnetically separated fraction contained 28% of its iron as hematite likely of secondary origin. An initial centrifugal size separation was shown to give an improved final product, and oxalic acid was found to be more efficient at removing Fe from the kaolinite surface than dithionite bleach. The Mössbauer spectra clearly show that beneficiation steps which give a substantial increase in kaolin brightness result in only minor changes in the clay iron mineralogy. Similar results were also obtained for two commercially available kaolins.

Several samples of large- and small-particle magnetite (Fe3O4), as well as its thermal decomposition products formed at different temperatures and atmospheres, have been studied extensively by Mössbauer spectroscopy (MS), both with and without an applied field of 6T. Synthetic mixtures of magnetite and poorly- or well-crystallized maghemite have also been studied. Large-particle magnetite (MCD > 200 nm), when heated in air for 12 hours at T < 400°C, transforms to a mixture of well-crystallized hematite and magnetite, the latter one remaining stoichiometric, according to the relative area-ratios obtained from MS. Thermal treatment at 1300°C in a controlled O2 partial pressure, produced a mixture of stoichiometric and nonstoichiometric magnetite, but the latter component seems to be composed of particles with different degrees of nonstoichiometry. The Mössbauer spectra of the decomposition products at T < 200°C in air of small-particle magnetite (MCD ~ 80 nm) could be successfully interpreted as a mixture of magnetite and maghemite, rather than nonstoichiometric magnetite. This suggestion is further supported by the experiments with the synthetic mixtures. It is clearly demonstrated that is not possible, even by applying a strong external field, to separate the contribution of the A-site of magnetite from that of maghemite.

Synthetic, relatively well-crystallized aluminum-substituted maghemite samples, γ-(Aly·Fe1−y)2O3, with y = 0, 0.032, 0.058, 0.084, 0.106 and 0.151 have been studied by X-ray diffraction and zero-field Mössbauer spectroscopy in the range 8 K to 475 K, and also with an external field of 60 kOe at 4.2 K and 275 K. It was found that there are two different converging models for fitting the zero-field spectra of the maghemites with a superposition of two Lorentzian-shaped sextets, both resulting in inconsistent values for the hyperfine fields (Hhf) and/or the center shifts (δ) of the tetrahedral (A) and octahedral (B) ferric ions. From the applied-field measurements it is concluded that there is a constant difference of 0.12 ± 0.01 mm/s between δB and δA, regardless of the Al content. For the Al-free sample the center shifts are found as: δA = 0.370 mm/s and δB = 0.491 mm/s at 4.2 K and δA = 0.233 mm/s and δB = 0.357 mm/s at 275 K (relative to metallic iron), with an estimated error of 0.005 mm/s. Both δA and δB are observed to decrease with increasing Al concentration. The effective hyperfine fields for the non-substituted maghemite sample are: Heff,A = 575 kOe and Heff,B = 471 kOe at 4.2 K and Heff,A = 562 kOe and Heff,B = 449 kOe at 275 K, with an error of 1 kOe. The B-site hyperfine field remains approximately constant with Al substitution, while for the A site a slight decrease with increasing Al content was observed.

Synthetic aluminum-substituted maghemite samples, γ-(Fe1-xAlx)2O3, have been prepared by thermal decomposition of Al-lepidocrocite (γ-Fe1-xAlxOOH), with × = 0, 0.04, 0.06, 0.14 and 0.18. The particles are needle-shaped and the mean crystallite diameter along the [311] crystallographic direction was found to be between 2.0 and 5.0 nm. Mössbauer spectra were collected at 6 K and from 80 K up to 475 K at steps of 25 K. In a wide range of temperatures the spectra of the non-substituted sample consist of a superposition of a broad sextet and a superparamagnetic doublet, whereas for the Al-maghemites this range is much smaller. From the temperature variation of the fractional doublet area two different parameters were defined: the temperature corresponding to a 50/50 doublet-sextet spectrum (T1/2), and the temperature below which the doublet ceases to exist (T0). These two parameters (T1/2 and T0) decrease from 390 K and 92 K (Al-free sample), to 118 K and 64 K (4 mole % Al) and to 100 K and 48 K (18 mole % Al), respectively. The average hyperfine fields at 6 K undergo a steep drop in going from the Al-free sample (Hhf = 506 kOe) to the sample with 4 mole % Al (Hhf = 498 kOe), but for higher substitutions the effect is much smaller. The A- and B-site quadrupole splittings, obtained from the data between 220 K and 475 K, were found as: ΔEQ,A = 0.86 ± 0.04 mm/s and ΔEQ,B = 0.65 ± 0.04 mm/s for the 4 mole % Al sample. The characteristic Mössbauer temperature, determined from the temperature dependence of the average isomer shift, was found to be in the range of 500–600 K.

Nanocomposites of polyvinylidene fluoride loaded with various amounts of γ-Fe2O nanoparticles, with an average size ranging between 20 and 40 nm, have been obtained by melt mixing and investigated using various experimental techniques [Superconducting Quantum Interference Device, Mössbauer, and Thermogravimetric Analysis]. Magnetic and Mössbauer measurements confirmed the presence of maghemite and a trace of a paramagnetic iron compound. Magnetic data are consistent with a blocking temperature close to room temperature (RT), showing a decrease in the coercive field as the temperature is increased. A weak exchange bias was noticed in all nanocomposites investigated at all temperatures and tentatively ascribed to surface spin disorder. The temperature dependence of the coercive field obeys the Kneller law. The nanocomposites exhibit superparamagnetic behavior near RT. Most magnetic measurements have been performed below the blocking temperature, revealing thus a complex behavior. The dependence of the mass loss derivative versus temperature, as obtained by thermogravimetric analysis, exhibits a single peak due to the thermal degradation of the polymeric matrix. A weak increase in the thermal stability of the polymeric matrix upon loading with maghemite is reported.

Equimolar mixtures of zero-dimensional graphene (SkySpring Nanomaterials, 1-5 nm particle size) and zinc ferrite nanoparticles (Alfa Aesar, 50 nm particle size) were exposed to mechanochemical activation by high-energy ball milling for time intervals of 0-12 hours. Their structural and magnetic properties were analyzed by Mӧssbauer spectroscopy and magnetic measurements. The spectra of zinc ferrite milled without graphene were fitted with one quadrupole-split doublet (quadrupole splitting 0.5 mm/s, isomer shift 0.23 mm/s) and indicated that zinc ferrite was superparamagnetic. The line width of the doublet increased from 0.41 to 0.64 mm/s, which correlates with a reduction in particle size as effect of the ball milling processing performed. When graphene was added to the milling powders, the Mӧssbauer spectra showed the appearance of another quadrupole doublet, with a quadrupole splitting of 0.84 mm/s and an isomer shift of -0.38 mm/s. Its abundance to the spectrum remained constant to 4.48% while the milling time was increased. This second doublet could be related to carbon atoms occupying neighborhoods in the proximity of iron atoms. Hysteresis loops were recorded in an applied magnetic field of 5 T at a temperature of 5 K. A change in the approach to saturation of the loop was observed, with saturation being achieved for the sample milled for 12 hours with graphene. Zero-field-cooling-field-cooling (ZFC-FC) was performed on all samples between 5-300 K with an applied magnetic field of 200 Oe. Graphene was found to stabilize the magnetic properties of the milled system of powders to a blocking temperature of about 90 K.

Mössbauer spectra of iron-bearing tourmaline, obtained at different temperatures, show the existence of thermally-activated charge delocalization among clusters of iron atoms situated in the Y and Z octahedra of the tourmaline structure. The temperature dependence indicates an unusually high activation energy for the delocalization process which suggests that the process takes place between crystallographically non-equivalent sites. Annealing of the tourmaline in hydrogen is observed to inhibit the delocalization process, thus localizing the electron into the Z-site.

X-ray diffraction (XRD), transmission Mössbauer spectroscopy, and vibrating sample magnetometry were used to study the influence of precipitates on the magnetic properties of aged Fe–Cr–Mo alloys. XRD patterns and Mössbauer spectra showed that the alloys have body-centered cubic structure similar to that of α-Fe. Small amounts of precipitates were also identified with relative fraction found to be related to Mo content, aging times, and temperatures. Magnetic measurements showed that the increase in the density of precipitates contributes significantly to the increase in the magnetic hardness of the material. This mechanism is related to a process of pinning of magnetic domain walls. It was also found that saturation magnetization is affected by the Mo content in the alloy. The techniques used in this work were shown to be very useful to understand the mechanisms through which the formation of precipitates affects the magnetic properties of the alloys and may be used as complement to the usual microscopy-based techniques for this purpose.

Samples of Ni57-xNdxFe18Ga25 with x=2 and 4 were prepared in ribbon form by rapid quenching via melt spinning route. The samples were analyzed by X-ray diffraction (XRD), magnetic measurements and Mössbauer spectroscopy, both in the as-quenched form and after thermal annealing at 900 oC for 2 min and 400 °C for 2 hours. For x=2 the Nd atoms are completely dissolved in the Ni-Fe-Ga matrix, while for x=4 the additional occurrence of the secondary 2:17 phase could be resolved. These findings were supported by the analysis of hyperfine magnetic field distributions obtained from the non-linear least-squares fitting of the Mössbauer spectra.

Amorphous ferromagnetic alloy with the composition Fe56Co24Nb4B13Si2Cu1 was obtained by rapid quenching from the melt. Samples cut from the ribbons were annealed at 450, 550, 650 and 750 °C in a vacuum furnace. 57Fe Mössbauer spectroscopy was used to identify the phases formed based on the refined values of the hyperfine parameters. The as-quenched specimen was analyzed with a hyperfine magnetic field distribution and corresponded to an in-plane orientation of the magnetic moment directions. The sample annealed at 450 °C was found to be in a nanocrystalline state due to observation of the (FeCo)-Si alloy with the DO3 structure. The balance of the composition was represented by a metalloid-enriched amorphous grain boundary phase. In contradistinction to this, the samples annealed at 550-750 °C were totally crystallized and the new phases formed were α-(FeCo), (FeCo)2(BSi) and (FeCo)3(BSi). These findings suggest that nanocrystallization is obtained only at select processing temperatures. A new set of Mössbauer spectra was obtained by recording simultaneously the intensity transmitted by a sandwich of the sample with the stainless steel etalon, based on the dual absorber method recently introduced by us. The values of the recoilless fraction can be derived from the relative spectral areas. The f factor value dropped from 0.6 to 0.37 for the sample annealed at 450 °C, consistent with the onset of nanocrystallization in the system. For the completely crystallized specimens, the f factor maintained values close to 0.5. This indicates that the presence of quenched-in stresses may play a role in the ability of samples to undergo recoilless emission and absorption of gamma rays.

Synthesis, structural, magnetic properties and heating efficiency of γ-Fe2O3 nanoparticles have been investigated. X-ray diffraction (XRD) and Mössbauer spectroscopy show that the obtained nanoparticles are mainly composed of maghemite phase (γ-Fe2O3). Williamson-Hall method shows that the crystallite is around 14nm.The specific absorption rate (SAR) under an alternating magnetic field is investigated as a function of frequency. A highest SAR value of 12W/g for frequency 523 kHz was obtained.

Most recently, magnetic ceramic nanoparticles have attracted considerable scientific interest from the basic research point of view and for their prospective use in chemical sensing, catalysis and electrochemical applications. In this paper we report the successful synthesis of xSnO2-(1-x)α-Fe2O3 system by hydrothermal synthesis and that of xZrO2-(1-x)α-Fe2O3 system by mechanochemical activation. The two nanoparticle systems were analyzed side-by-side using X-ray diffraction (XRD) and Mössbauer spectroscopy. The latter technique was used in its complexity, including the determination of the recoilless fraction using our dual absorber method. This was correlated with the onset of new phases in the systems of interest.

Single phase, a FeVO4 triclinic crystalline structure was successfully synthesized by annealing the mechanochemically milled xV2O5·(1-x)α-Fe2O3 composites (x = 0.5) at 550 °C for 1 h. X-ray powder diffraction (XRD) and Mössbauer spectroscopy were combined for a detailed study of the assisting role of the mechanochemical milling process. Mechanochemical milling homogeneously mixed the starting materials of α-Fe2O3 and V2O5 and substantially decreased their average grain sizes. The partially V5+-substituted α-Fe2O3 phase and Fe3+-substituted V2O5 could be the important intermediate phases in the production of FeVO4 single phase. In addition, xV2O3·(1-x)α-Fe2O3 (x = 0.1, 0.3, 0.5, and 0.7) solid solutions were successfully synthesized by mechanochemical activation of V2O3 and α-Fe2O3 mixtures. Complete solid solutions exist after 12 h ball-milling time for all studied x values. The synthesized xV2O3·(1-x)α-Fe2O3 solid solutions with x = 0.5 and 0.7 were mainly paramagnetic at room temperature. The study demonstrates that the transformation pathway is related to the valence state of the metallic specie of the oxide used in connection with hematite.

In this study, we use THz spectroscopy in the energy range between 45 GHz to 3000 GHz (1.5 cm-1 and 100 cm-1) as a non-destructive diagnostic tool to characterize the corrosion by-products (rust) on aged steel structural components that are usually embedded in concrete. The THz radiation has been shown to penetrate concrete with extinction coefficients between (1.0 to 2.3) x 10-2 GHz-1 cm-1, depending on the composition and the moisture content of the concrete. The previously reported antiferromagnetic resonance (AFR) near 140 GHz in iron oxide composites was found to be less than our current detection sensitivity (fractional absorbance sensitivity of >10%). However, a strong transition centered near 725 GHz (24 cm-1) has been observed for the first time. This feature has appeared in reflection from several different samples of mildly corroded steel plates and has been tentatively attributed to a broad phonon density of states commonly referred to as the “Boson peak” found in disordered materials. By taking advantage of this strong transition and a powerful excitation sources in the AFR region, we expect THz spectroscopy and imaging to be an effective diagnostic tool with broad applications in corrosion diagnostics and inspection.

Pressure induced magnetic phase transition of iron hydride was investigated with an in-situ Mössbauer spectrometer using synchrotron radiation (SR). The spectrometer is composed of a high resolution monochromator, an X-ray focusing device, a variable frequency nuclear monochromator and a diamond anvil cell. The optical system, advantages of the spectrometer and the observed high pressure magnetic phases of iron hydride are described.

X-ray detection on hydrogen related events is difficult due to its extremely small scattering factor. In this report, we have used nuclear resonance vibrational spectroscopy (NRVS) to examine the nature of the Fe–H vibrational modes in several FeH model complexes, which shines light on the possible measurements on the Fe-H vibrations inside real biological systems in the future.

Here we report on the synthesis of multiferroic BiFeO3 ceramics by mechanical activation and detailed investigation into its magnetic behavior. The mechanically milled ceramic was calcined at temperatures up to 800°C. X-ray diffraction studies show only the pure BiFeO3 phase forms at 700°C. Vibrating sample magnetometer (VSM) measurements were carried out up to 1.5 Tesla and the results show a weak magnetic ordering in the ceramics. The magnetic measurements were also done on the samples heat treated under various cooling conditions. VSM measurements showed pronounced effect of cooling on the Magnetization vs Field curves. Mössbauer measurements show that short range Fe2O3 ordering is still present in the sample that goes undetected by XRD. This component decreases as the calcination temperature is increased. The nature of magnetic ordering improves upon heating from 600 to 700°C, also suggested by pure BiFeO3 phase formation at 700°C. Magnetization vs Temperature measurements conducted on the sample heat treated at 700°C for 1hr followed by cooling in air show an antiferromagnetic transition at ∼370°C.

Magnetic nanophases nucleated within horse spleen apoferritin nanotemplates under in vivo physiological conditions and in vitro reconstitution were characterized by Mössbauer spectroscopy in lyophilized form. Mössbauer spectra recorded at 80 K indicate that for the in vivo produced ferritin the presence of phosphates within the ferritin biomineral core results in larger quadrupole splittings, both at interior and surface sites, 0.62 mm/s and 1.06 mm/s, respectively, as compared to 0.56 mm/s and 0.75 mm/s for the reconstituted ferritin. Data collected at lower temperatures give blocking temperatures of 55 and 40 K for in vitro and in vivo samples. At 4.2 K, both samples give similar saturation hyperfine field values for the interior (495 kOe) and surface (450 kOe) iron sites. The temperature dependence of the reduced hyperfine magnetic fields at the interior iron sites is consistent with the collective magnetic excitations model, due to the particle's magnetization precession about the anisotropy axis. In contrast, a marked decrease in the reduced hyperfine field at surface sites with increasing temperature indicates a more complex spin excitation energy landscape at the surface.

We identified both crystalline and amorphous phase of human spleen particles. The silicon particles in the spleen were 10-30 μm large. Silicon, silicon-aluminium and silicon-calcium particles by EDX were found. We assume that the silicon must enter the organism from the external environment and the presence of silicon in the human spleen is consequence of the cleaning function of human spleen.

Mössbauer spectroscopy of studied tissues revealed different phase of iron oxide in the human spleen. On the ground of this consideration we can claim all samples of investigated tissues exhibit presence of two different paramagnetic iron phases, both based on three-valent (Fe3+) atoms. Consequently only 4 different iron-oxides correspond with experimental results. Multielemental composition of iron particles was found by EDX analysis. We suppose that pH and time are significant factors influence biomineralization of iron in the human spleen.