Loading channels of SiO 2 mesoporous matrices with Fe oxides

After embedding hematite nanowires (15 wt.% Fe) into a MCM-41 hard template, we have explored alternative routes to induce the structural transformations that lead from hematite to maghemite and magnetite embedded nanowires. The impregnation media (ethanol or water) and the calcination atmosphere (air and NO/He) on the hematite nanowires production play a significant role at the time of reducing and re-oxidizing the embedded hematite nanoparticles. The solids were characterized by X-ray diffraction, nitrogen adsorption, and Mössbauer spectroscopy. The results indicate that the effect of the solvent on the structural properties of the iron species is more important than the calcination atmosphere. The best conditions for iron magnetic nanowires not to get outside of the MCM-41 channels over the treatments are reached using water as the solvent and air as the calcination atmosphere. When ethanol is the solvent used over the preparation step, the end iron oxides are in the form of nanotubes spread out on the amorphous silica walls of the matrix.     

A Comparative Study of Iron Concentrates by Mössbauer Spectroscopy and Optical Microscopy

Five samples of iron-ore concentrates used for the production of pellets were heated at different temperatures under air atmosphere and characterised by chemical analysis, optical microscopy and Mössbauer spectroscopy. In all samples it was observed the presence of specular hematite, martite, and goethite in different proportions, whereas one sample also contains 15% (w/w) of magnetite. The presence of residual goethite was observed in the samples heated at 300°C, whereas the magnetite was only converted to hematite after heating at 900°C. However, the results of the optical microscopy pointed to the existence of large amounts of goethite even in the samples heated at 900°C, which is obviously incorrect. Therefore, it can be concluded that the reflectance of hematite derived from goethite is similar to that of the original goethite, limiting the use of optical microscopy for these types of samples.     

Evidence from Mössbauer spectroscopy of neo-formation of magnetite/maghemite in the soils of loess/paleosol sequences in China

Samples of four different loess/paleosol couplets of a loess sequence in Huangling (China) have been studied with ⁵⁷Fe Mössbauer spectroscopy. Each sample was separated into strongly, weakly and very weakly magnetic fractions. The iron mineralogy of the strongly magnetic fractions of both loess and soils consists of magnetite/maghemite and hematite together with some silicates. The soils contain some additional small-particle maghemite. From the spectral behaviour a similarity in terms of morphology and crystal chemistry for hematite throughout the whole section could be inferred. The ratio of iron in magnetite and maghemite to that in hematite differentiates well between the loess and soil samples. These results strongly suggest the neo-formation of magnetite/maghemite in the soils.     

CEMS study of stainless steel films deposited by pulsed laser ablation of AISI316

Thin stainless steel films deposited on SiO₂/Si wafer were prepared by a pulsed laser ablation of austenite stainless steel (AISI316), and characterized by conversion electron Mössbauer spectrometry (CEMS) using a He gas proportional counter. As-deposited films were composed of a magnetic phase. When deposited films were heated in air at various temperatures, the hyperfine field of the magnetic phase increased. Hematite was produced on the surface, and the magnetic orientation changed from parallel to in-plane at random with the increase of heating temperatures. The metallic iron and magnetite were produced at 400°C in dry Ar + 5%H₂ atmosphere. When the film was heated in wet Ar + 5%H₂ atmosphere at 600°C, maghemite was produced on the surface, and austenite phase was produced in the inner film.     

Synthesis of hematite nanowires using a mesoporous hard template

The influence of the impregnation media (ethanol or water) and the calcination atmosphere (air and NO/He) on the hematite nanowires production embedded on a hard template (MCM-41) was studied. The solids were characterized by X-ray diffraction, Mössbauer spectroscopy and magnetic measurements. The results obtained indicate that the more appropriate conditions for the iron oxide nanowires to get inside the MCM-41 hard template seem to be reached using water as a solvent and air as calcination atmosphere.     

Synthesis and characterization of hollow ��-Fe2O3 sub-micron spheres prepared by sol�Cgel

In this work we report the preparation of magnetic hematite hollow sub-micron spheres (??-Fe₂O₃) by colloidal suspensions of ferric nitrate nine-hydrate (Fe(NO₃)₃·9H₂O) particles in citric acid solution by following the sol?Cgel method. After the gel formation, the samples were annealed at different temperatures in an oxidizing atmosphere. Annealing at 180°C resulted in an amorphous phase, without iron oxide formation. Annealing at 250°C resulted in coexisting phases of hematite, maghemite and magnetite, whereas at 400°C, only hematite and maghemite were found. Pure hematite hollow sub-micron spheres with porous shells were formed after annealing at 600°C. The characterization was performed by X-ray diffraction (XRD), Mössbauer spectroscopy (MS) and scanning electron microscopy (SEM).     

Specific Features of the Structural State of Iron Ions in Iron-Containing Composites Irradiated by Fast Electrons

The present paper analyzes the valence-coordination state of iron atoms in polymer composite materials fabricated from polystyrene and iron-ore concentrates – magnetite and hematite – upon exposure to fast electrons with energy of 6.2 MeV and fluence of 10¹⁸ electrons/cm². Changes in the phase content and valence-coordination and magnetic states of iron atoms are established. After irradiation, the hematite phase is transformed into the magnetite phase with a predominance of Fe³⁺ ions with [FeO₄] coordination, and the magnetite phase forms the wüstite-type (FeO) phase in which Fe²⁺ ions are arranged in [FeO₆] coordination.     

Mössbauer and mineral magnetic studies on archaeological potteries from Adhichanallur, Tamilnadu, India

Megalithic potteries collected from Adhichanallur, Tamilnadu, India (Lat. 8°44′ N; Long. 77°42′ E) have been subjected to various spectroscopic and rock magnetic studies. The type of clay, their origin, level of structural deformation due to firing, firing temperature and atmospheric condition followed during making the potteries are analyzed. The potteries were subjected to Mössbauer and X-ray diffraction studies to analyze the iron phases in them. It is found that the samples were made of local clay (red clay), fired above 600°C under open atmospheric and/or reduced atmospheric conditions and air has been allowed during cooling. The Mössbauer spectra reveal the presence of Fe^3?+?, Fe^2?+? and iron oxides of hematite and magnetite. The firing temperature and firing conditions established from Mössbauer studies are similar to the observation made from FT-IR studies. The magnetic mineral types, the mass fractions and the domain states of the constituent magnetic grains were elucidated from a range of rock magnetic measurements including variation of susceptibility with low field, frequency and temperature, hysteresis parameters and isothermal remanence acquisition data. The magnetic mineralogy of most pottery samples was dominated by magnetite/(titano) magnetite, while magnetic grain size spectrum varies from very fine (super paramagnetic) to fine (stable single domain, pseudo single domain). The reversible thermo magnetic behavior reflects no mineralogical transformations during reheating and all the samples show same Curie temperature 580°C due to magnetite. From the above information it is demonstrated that these samples are suitable for determining the reliable ancient geomagnetic field intensity values existed during that period.     

减压氩气环境下激光显微光谱分析再现性和灵敏度的研究

以金属合金光谱分析标样为样品，采用激光显微发射光谱分析系统在减压氩气环境下，实验研究了光谱分析再现性和灵敏度。以原子线作为分析线的RSD减压氩气环境好于常压空气环境，以离子线作为分析线的RSD基本相同，样品的组成和元素的浓度对分析线的RSD有较大的影响。测定的铝合金样品Cu,Zn,Mg浓度曲线斜率是空气环境下的1．5－2倍，表明分析灵敏度得到明显改善，有利于激光显微光谱分析范围的扩展。     

Industrial Responsibility in the Emission of Particulate Matter in the Atmosphere

The present investigation consists of the application of several techniques such as Mössbauer spectroscopy, X-ray diffraction, atomic absorption, electron probe micro analysis (EPMA), and thermo-gravimetric analysis, to the identification of the particulate matter in atmospheric aerosols in the metropolitan region of Vitória (MRV), ES, Brazil. The main sources of particulate matter and its emission characteristics within the steel industry have been studied to identify its contribution to air particles in Vitória region. The analysis reveals the total amount of industrial emission of the iron containing components in the atmosphere. The presence of goethite, hematite, magnetite, pyrite, silicates, marine chloride and total absence of heavy metals could be confirmed.     

Reduction of hematite with ethanol to produce magnetic nanoparticles of Fe3O4, Fe1 − x O or Fe0 coated with carbon

The production of magnetic nanoparticles of Fe₃O₄ or Fe⁰ coated with carbon and carbon nanotubes was investigated by the reduction of hematite with ethanol in a Temperature Programmed Reaction up to 950°C. XRD and Mössbauer measurements showed after reaction at 350°C the partial reduction of hematite to magnetite. At 600°C the hematite is completely reduced to magnetite (59%), wüstite (39%) and metallic iron (7%). At higher temperatures, carbide and metallic iron are the only phases present. TG weight losses suggested the formation of 3–56 wt.% carbon deposits after reaction with ethanol. It was observed by SEM images a high concentration of nanometric carbon filaments on the material surface. BET analyses showed a slight increase in the surface area after reaction. These materials have potential application as catalyst support and removal of spilled oil contaminants.     

Synthesis of magnetic nanoparticles: effects of polyelectrolyte concentration and pH

This study refers to the effect of sodium polyacrylate concentration (1 to 5 mass %) and pH (10 to 12) on the synthesis of magnetic nanoparticles (magnetite?Cmaghemite) and their characterization by Mössbauer spectroscopy. The magnetic particles were obtained by coprecipitation method using iron chloride (II) and iron chloride (III) as precursor reagents and sodium polyacrylate as stabilizing agent. All samples showed Mössbauer broad resonance lines in typical doublet and sextets patterns of magnetite or maghemite with corresponding wide particle size distributions. The stability of magnetic particles was carried out by measuring particle sizes with dynamic light scattering (DLS). The z-average values for magnetic particles were in the range 24 to 590 nm and no significant change in size was observed on aging by leaving this material in air for 20 days. X-ray diffraction patterns showed characteristic peaks of the spinel structure and have an increase in their broadening as the pH decreases, effect that is dominated by the decrease in crystallite sizes. The nanoparticles showed to be magnetic at pH 12 and at room temperature.     

The physical theory of rock magnetism

Magnetite and hematite are representative of the ferrimagnetic and weakly ferromagnetic minerals which are responsible for the magnetic properties of rocks reviewed in this paper. Magnetite grains are multi-domains in the size range of interest (0.1 μ–1000 μ), whereas hematite grains in the same size range are almost certainly single domains. Properties discussed are coercivity, susceptibility, magnetic viscosity, thermo- and isothermal remanence, alternating field demagnetization, anhysteretic, chemical and detrital magnetization, anisotropy, piezomagnetic effects and self-reversals. Problems requiring more experimental data are emphasized, especially the basal plane anisotropy of hematite, the Barkhausen discreteness of domains in magnetite and the possibility that grains of cubic minerals may have some uniaxial character arising from grain shape or internal strains.     

A Fourier transform infrared (FTIR) and thermogravimetric analysis (TGA) study of oleate adsorbed on magnetite nano-particle surface

Magnetite nano-particles were coated with sodium oleate and the spectral behaviour of the coating layer was studied by FTIR spectroscopy after the particles had been heated in air and argon. Magnetite was synthesized by controlled co-precipitation and subsequently coated with sodium oleate. Thermal analysis in combination with mass spectroscopy was carried out to support the FTIR spectroscopic interpretations, but also to monitor the decomposition and surface reaction of oleate adsorbed on the magnetite surface. It was deduced from FTIR and TGA results that the oleate molecules are bonded to iron atoms by a bidentate mononuclear complex and form essentially a single layer with a distance between oleate molecules of ∼36 Å². It was shown by IR as well as Raman spectroscopy that oleic acid, when heated in air, undergoes decomposition implying that new carbon-oxygen bonds are formed. Heating the iron oxide-oleate system in air also implies oxidation of the double bond at the C:9 position of the alkyl chain and formation of intermediate oxygen-rich molecules. An enthalpy change of ΔH = 49.86 J/g was obtained for oleate desorption/decomposition at ∼350 °C under argon atmosphere and a carbonaceous graphitic species resulted from this decomposition.     

颗粒度对鞍山式铁矿反射光谱特征的影响研究

岩矿反射光谱的决定因素是其成分及含量,变异因素主要为颗粒度、粗糙度、观测角度、表面形态等。为明确颗粒度与鞍山式铁矿反射光谱之间的关系,采用SVC HR-1024便携式地物光谱仪对鞍山式铁矿的两种主要铁矿石(赤铁矿、磁铁矿)进行不同颗粒度下的可见光-近红外光谱测试,分析颗粒度对赤铁矿、磁铁矿反射光谱的影响规律,并明确颗粒度的敏感波段与稳定波段,为以后的定量反演工作提供参考。结果表明,颗粒度对赤铁矿、磁铁矿反射光谱的影响规律具有显著差异。当赤铁矿试样粒径由0.03 mm增加到1 mm时,光谱反射率随颗粒度增加而逐渐减小,二者呈现显著负相关关系。但是在不同的波段处,赤铁矿反射光谱受颗粒度的影响程度不同,在350~550 nm波段,反射光谱受颗粒度影响非常微弱,为赤铁矿反射光谱对颗粒度的稳定波段;在550~950 nm波段,反射光谱受颗粒度影响较微弱;在950~1 250 nm波段,反射光谱受颗粒度影响较显著;在1 250~2 500 nm波段,反射光谱受颗粒度影响非常显著,为赤铁矿反射光谱对颗粒度的敏感波段。当赤铁矿试样粒径大于1 mm之后,赤铁矿反射光谱多重叠,受颗粒度影响显著减弱,且二者无明显相关性。当磁铁矿试样粒径由0.03 mm增加到4 mm时,磁铁矿反射光谱对颗粒度的响应非常微弱,颗粒度引起的光谱反射率变化不超过3%,且颗粒度与磁铁矿反射光谱间无相关性,二者间联系微弱。该研究揭示了颗粒度对鞍山式铁矿反射光谱的影响规律,定量分析了颗粒度对赤铁矿、磁铁矿反射光谱的影响程度,并确定了颗粒度与试样反射率符合的函数分布关系,为提高鞍山式铁矿的品位反演精度奠定了良好基础。     

Mössbauer spectroscopy studies of the magnetic properties of ferrite nanoparticles

Studies of the ferrite nanoparticles prepared by the chemical decomposition of iron chlorides with a various ratio ξ = Fe³⁺/Fe²⁺ are herein presented. The microstructure and the magnetic properties have been studied by transmission electron microscopy (TEM), X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). The TEM studies show that the nanoparticles have almost a spherical shape with the diameter of (12 ± 2) nm for all samples. The measured XRD pattern was mainly composed of lines which were indexed with a cubic spinel structure. The analysis of the Mössbauer data shows that the microstructure of the nanoparticles consists of the core formed by nonstoichiometric magnetite and maghemite shell. A small amount of hematite, probably on the surface of the nanoparticles with ξ = 1.75, 2.0, was detected. At temperatures T ≤ 150 K the spin canting of surface maghemite with ξ = 2.25 was observed while for the samples with ξ = 1.75, 2.0 such effect was suppressed by the presence of hematite on the surface of the nanoparticles. Infield Mössbauer spectra with ξ = 1.75, 2.0 show that magnetic moments of the magnetite/maghemite core are parallel while magnetic moments of the surface hematite are perpendicular to the direction of the external magnetic field.     

Mechanochemical and magnetomechanical synthesis of hematite nanoparticles

Samples of hematite were exposed to mechanochemical activation by high energy ball milling for 0–27 h. The milling-induced changes to the structural and magnetic properties of hematite were characterized by X-ray diffraction (XRD) and Mössbauer spectroscopy. The particle size was found to decrease from 80 to 16.5 nm after 8 h of ball milling time, followed by a small increase to 19.8 nm at the end of the milling period. An overall expansion of the crystalline lattice parameters a and c with the milling time was deduced. The magnetic hyperfine field decreased with the ball milling time, from 51.46 down to 50.68 T after 27 h of grinding. Magnetite and traces of iron were observed at the longest milling time employed. The recoilless fraction (f ) was measured simultaneously using a dual Mössbauer absorber consisting of hematite and a stainless steel etalon. The f factor first decreased with the milling time due to occurrence of nanoparticles in the system, had a maximum at 12 h due to agglomerations of nanoparticles and exhibited a second maximum at 27 h, due to the appearance of magnetite in the system. More samples of hematite were subjected to magnetomechanical activation by magnetic ball milling for 52 and 134 h. A phase mixture of hematite and magnetite was observed.     

Iron oxide nanoparticles modified with oleic acid: Vibrational and phase determination

A simple path methodology to detect the phase composition of iron oxide nanoparticles modified with oleic acid based on vibrational spectroscopy is present here and applied on three different nanoparticles prepared by co-precipitation method. Firstly, the phase composition, magnetite, maghemite, and hematite, is determined using a reference intensity ratio methodology on X-ray diffraction pattern. Also, the size of each sample was calculated by Scherrer equation. Scanning, transmission electron microscopy, microanalysis and electron diffraction show a core magnetite particles size of around 10 nm for all particles. Based on lattice vibrations, we find a concentration of around 80% of magnetite and a hematite phase lower than 5%. Whereas, the magnetite composition from X-ray diffraction shows 76%. We also investigate the metal-organic interaction and disorder degree of organic molecule conformation by infrared and Raman spectroscopy analysis. Hematite lattice vibrations show more alterations as it interacts with the organic acid. Finally, magnetic measurements at room temperature of the modified particles, suggest a superparamagnetic behavior and high saturation magnetization.     

Magnetite microcrystals for magneto-rheological fluids

We report a new synthetic method for the preparation of micrometric prismatic crystals of magnetite by means of a coprecipitation reaction of aqueous solutions of iron salts and ammonium oxalate, followed by thermal decomposition of the precipitate in an inert atmosphere. Magnetite prismatic crystals grown by this procedure are homogeneous in size and morphology. We also study the structure and orientation of the magnetic domains.     

Effects of sputtering atmospheres on magnetic properties of amorphous films of BiFeO3-ZnFe2O4

Amorphous films of rf sputtered (1–2_x)BiFeO₃-xZnFe₂O₄ show a ferromagnetic character when annealed in air at high temperatures due to the formation of ordered clusters. The effects of sputtering parameters on the magnetic properties of such annealed films with x = 0.4 have been studied through static magnetization and ferromagnetic resonance measurements. For samples sputtered in a mixed oxygen—argon atmosphere, the magnetization and the uniaxial anisotropy field are smaller than for films deposited in a pure oxygen atmosphere. One also observes a relatively large ferromagnetic resonance line-width and gyromagnetic ratio for oxygen—argon sputtered samples. The possible presence of magnetically ordered clusters consisting of divalent iron ions in samples deposited in oxygen—argon atmospheres may account for the above observations.