Studies of iron and iron oxide layers by electron spectroscopes

Thin iron oxide layers prepared “in situ” in the ultra high vacuum on polycrystalline iron substrate were investigated by electron spectroscopy methods—X-ray photoelectron spectroscopy (XPS) and elastic peak electron spectroscopy (EPES), using spectrometer ADES-400. The texture and the average grain size of the iron substrate foil have been examined by glancing angle X-ray diffraction (XRD). Qualitative and quantitative estimation of investigated oxide layers was made using (i) the relative sensitivity factor XPS method, (ii) comparison of binding energy shifts of Fe 2p photoelectron line and (iii) non-linear fitting procedure of Fe 2p photoelectron lines.Both, sputter-clean polycrystalline iron substrate and finally grown Fe_2.2O₃ layer, were investigated by the EPES method to measure the electron transport parameters used for quantitative electron spectroscopy, such as the electron inelastic mean free path (IMFP) values. The IMFPs were measured in the electron kinetic energy range 200-1000 eV with the Cu standard. The surface excitation parameters using Chen and Werner et al. approaches were evaluated and applied for correcting these IMFPs. The discrepancies between the evaluated parameters obtained using the above quantitative and qualitative approaches for characterising the iron oxide layers were discussed.     

Physico-chemical, optical and electrochemical properties of iron oxide thin films prepared by spray pyrolysis

Iron oxide thin films were prepared by spray pyrolysis technique onto glass substrates from iron chloride solution. They were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and (UV-vis) spectroscopy. The films deposited at T_s ≤ 450 °C were amorphous; while those produced at T_sub = 500 °C were polycrystalline α-Fe₂O₃ with a preferential orientation along the (1 0 4) direction. By observing scanning electron microscopy (SEM), it was seen that iron oxide films were relatively homogeneous uniform and had a good adherence to the glass substrates. The grain size was found (by RX) between 19 and 25 nm. The composition of these films was examined by X-ray photoelectron spectroscopy and electron probe microanalysis (EPMA). These films exhibited also a transmittance value about 80% in the visible and infrared range. The cyclic voltammetry study showed that the films of Fe₂O₃ deposited on ITO pre-coated glass substrates were capable of charge insertion/extraction when immersed in an electrolyte of propylene carbonate (PC) with 0.5 M LiCLO₄.     

Effect of phase transformation on optical and dielectric properties of zirconium oxide nanoparticles

Zirconium oxide nanoparticle (ZrO₂) is synthesized by the hydrothermal method at different calcination temperatures. The structural analysis is carried out by X-ray diffraction and Raman spectra. The sample prepared at 400 °C and 1100 °C showed the cubic and monoclinic phase, respectively, and the sample calcined at 600 °C and 800 °C showed the mixed phase with co-existence of cubic and monoclinic phases. Furthermore, the morphology and particle size of these samples were investigated by scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis. The band gap estimated from UV–Vis spectra of ZrO₂ (zirconia) nanocrystalline materials calcined at different temperatures from 400 °C to 1100 °C was in the range of 2.6–4.2 eV. The frequency dependence of dielectric constant and dielectric loss was investigated at room temperature. The low frequency region of dielectric constant is attributed to space charge effects.     

Preparation of Bi2Fe4O9 particles by hydrothermal synthesis and functional properties

In the present study, particles with different Bi₂Fe₄O₉ micro/nanostructures with a few particular morphologies (flower-like nanoplatelets, hierarchical microstructures, perfectly square platelets single crystals, etc.) obtained under specific hydrothermal synthesis conditions were investigated. The role of the processing parameters (such as NaOH concentration, reaction temperature, and reaction duration time) on the phase formation mechanism and on the microstructural characteristics was investigated. All the Bi₂Fe₄O₉ morphologies showed orthorhombic symmetry with space group Pbam. The photocatalytic properties and magnetic behavior as a function of the micro/nanostructural characteristics of various Bi₂Fe₄O₉ powders were determined. In the presence of Bi₂Fe₄O₉, a degradation rate of Rose Bengal in the range of 52–61% was determined after 180?min under UV light irradiation (λ?=?254?nm). Magnetic activity with antiferromagnetic behavior and a transition at ～240?K slightly dependent on the microstructures was found. The role of Bi₂Fe₄O₉ microstructures in the photocatalytic activity and magnetic properties was discussed.     

High surface area thermally stabilized porous iron oxide/silica nanocomposites via a formamide modified sol-gel process

Iron oxide/silica (Fe:Si as 1:10 atomic ratio) composite materials have been prepared by calcination for 3 h at different temperatures (400-900 °C) of xerogel precursor obtained via a formamide modified sol-gel process. The process involved TEOS and iron(III) nitrate, nitric acid and formamide. Genesis of the composite materials from the xerogel precursor has been investigated by TGA, DSC, FTIR, XRD, SEM and EDX. Results indicated that all the calcined composites are mainly composed of amorphous iron oxide dispersed as finely divided particles in amorphous silica matrixes. Nitrogen adsorption/desorption isotherms revealed a reversible type I of isotherms indicative of microporosity. However, high S_BET surface area and microsporosity were observed for the calcined composite materials (e.g. S_BET = 625 m² g⁻¹, and S_αs = 556 m² g⁻¹ for the composite calcined at 400 °C). Formation of the porous texture was discussed in terms of the action of formamide, which enhanced strengthening of the silica gel network during evaporation of the more volatile components within the composite body during the drying process.     

One-step hydrothermal synthesis of highly water-soluble secondary structural Fe3O4 nanoparticles

Magnetite nanoparticles (MNPs) were prepared using the ferric acetylacetonate as the sole iron source in a facile hydrothermal route, while poly(acrylic acid) (PAA) was chosen as the stabilizer via one-step functionalized MNPs for better hydrophilic properties. The orthogonal was used in the paper for the experimental parameters optimization, including the solvent, the reaction time, the amount of stabilizer and the presynthesis. The obtained highly water dispersible MNPs with uniform size from about 50 to about 100 nm was individually composed of many monodisperse magnetite crystallites approximately 6 nm in size. And the MNPs show high magnetic properties, whose magnetite content was up to 76.76% and the saturation magnetization was 39.0 emu/g. Later the formation mechanism of MNPs was also discussed. Thus the MNPs proved to be very promising for biomedical applications.     

Sinterability of 8Y–ZrO2 powders hydrothermally synthesized at low temperature

Nanometric yttria (8 mol%)-stabilized zirconia powders were hydrothermally synthesized at 110 °C for 7 days in the presence of dilute (0.20 M) or concentrated (2.0 M) solutions of (KOH+K₂CO₃) mineralizer. Zirconia xerogel, crystalline Y(OH)₃, crystalline Y₂O₃ and a xerogel of coprecipitated (Y–Zr) hydroxide were used as starting materials. Setting the content of yttria constant and equal to 8 mol%, three types of mixtures were tested. Zirconia xerogel in mixture with crystalline Y₂O₃, zirconia xerogel in mixture with crystalline Y(OH)₃ and, finally, a xerogel of coprecipitated (Y–Zr) hydroxide were hydrothermally treated.The different characteristics of the resulting powders are discussed in terms of both the mineralizer concentration and the type of Y-based precursor used in the hydrothermal treatments, respectively.Weakly agglomerated cubic ZrO₂ powders with primary particles bigger in size and without any preliminary treatment show better performances when they are directly sintered at 1500 °C.     

Size-controlled synthesis of superparamagnetic iron oxide nanoparticles and their surface coating by gold for biomedical applications

The size mono-dispersity, saturation magnetization, and surface chemistry of magnetic nanoparticles (NPs) are recognized as critical factors for efficient biomedical applications. Here, we performed modified water-in-oil inverse nano-emulsion procedure for preparation of stable colloidal superparamagnetic iron oxide NPs (SPIONs) with high saturation magnetization. To achieve mono-dispersed SPIONs, optimization process was probed on several important factors including molar ratio of iron salts [Fe³⁺ and Fe²⁺], the concentration of ammonium hydroxide as reducing agent, and molar ratio of water to surfactant. The biocompatibility of the obtained NPs, at various concentrations, was evaluated via MTT (3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide) assay and the results showed that the NPs were non-toxic at concentrations <0.1 mg/mL. Surface functionalization was performed by conformal coating of the NPs with a thin shell of gold (∼4 nm) through chemical reduction of attached gold salts at the surface of the SPIONs. The Fe₃O₄ core/Au shell particles demonstrate strong plasmon resonance absorption and can be separated from solution using an external magnetic field. Experimental data from both physical and chemical determinations of the changes in particle size, surface plasmon resonance optical band, phase components, core–shell surface composition, and magnetic properties have confirmed the formation of the mono-dispersed core–shell nanostructure.     

ZnFe2O4的固相法和水热法制备及其电化学性能研究

本文用固相反应法和水热法制备了ZnFe₂O₄材料,X射线衍射(X-ray diffraction, XRD)表明制备出来的ZnFe₂O₄为尖晶石结构,表面形貌测试 (scanning electron microscopy, SEM) 显示两种方法制备的材料的平均粒径分别为500 nm和200 nm.比表面积测试结果表明,两种方法制备的样品的比表面积分别为136.7 m² g^{-1关键词： 2O₄')" href="#">ZnFe₂O₄ 尖晶石结构 电化学性能 锂离子电池}     

A Study on the Rheological and Magnetic Properties of Polymer-Bonded Magnets Using Polycarbonate as the Bonding Material

The effect of three metal oxides on the magnetic properties of polymer bonded magnets (PBMs) was studied. The three PBMs, using polycarbonate (PC) as binder and 5 wt% of Fe₃O₄, Fe₂O₃, or CuO nanoparticles, were prepared by melt extrusion in a twin screw extruder followed by compression molding. Transmission electron microscopic (TEM) images showed a better dispersion for the PC/Fe₃O₄ nanocomposite compared with that of the other nanocomposites. The dynamic intersection frequency (ω_c), which is related to the crossing of the G′ and G^″ curves, showed that there was more homogeneity in the PC/Fe₃O₄ and PC/Fe₂O₃ nanocomposites. The curves of saturation magnetization for the three nanocomposites showed that there was a relationship between the magnetic properties and the homogeneity of the nanoparticles studied by rheometry. Because the magnetic strength of PC/Fe₃O₄ was greater than that of the other nanocomposites, it was concluded that not only the intrinsic magnetic property of the filler was an important factor to increase the magnetic property, but also the homogeneity of the filler within the matrix had an important role.     

MOCVD of zirconium oxide thin films: Synthesis and characterization

The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO₂ thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.     

Preparation and characterization of iodine-doped mesoporous TiO2 by hydrothermal method

Iodine-doped mesoporous TiO₂ (I/TiO₂) was prepared by hydrothermal method, using tetrabutyl titanate as precursor, potassium iodate as iodine sources. The as-prepared I/TiO₂ catalysts were characterized by UV-vis, XRD, TEM, BET, TG/DTA, XPS and photoluminescence (PL) spectroscopy. Production of OH radicals on the I/TiO₂ surface was detected by the PL technique using terephthalic acid as a probe molecule. The effects of hydrothermal reaction temperature, calcination temperature and iodine doping content on the structure and properties of the catalysts were investigated. The results showed that iodine-doped TiO₂ calcinated at 300 °C have good anatase crystal. The optimal hydrothermal conditions have been determined to be that reaction temperature 120 °C, calcinated temperature 300 °C and added 1.16 mmol iodine dopants. The average particle size of I/TiO₂ synthesized under optimal condition (I-3 sample) is about 3.9 nm. The I-3 photocatalyst contains 100% anatase crystalline phase of TiO₂. BET specific surface area of I-3 sample is184.8 m² g⁻¹ and is 3.67 times that of pure TiO₂ (50.37 m² g⁻¹). Iodine in I/TiO₂ catalyst mainly exists in the form of I₂, and photoactivity of I/TiO₂ catalyst in visible light comes from photosensitize of I₂. I/TiO₂ catalysis shows very high efficiency for the degradation of phenol under visible light.     

Green synthesis and characterization of superparamagnetic Fe3O4 nanoparticles

In this paper, we have first demonstrated a facile and green synthetic approach for preparing superparamagnetic Fe₃O₄ nanoparticles using α-d-glucose as the reducing agent and gluconic acid (the oxidative product of glucose) as stabilizer and dispersant. The X-ray powder diffraction (XRD), X-ray photoelectron spectrometry (XPS), and selected area electron diffraction (SAED) results showed that the inverse spinel structure pure phase polycrystalline Fe₃O₄ was obtained. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) results exhibited that Fe₃O₄ nanoparticles were roughly spherical shape and its average size was about 12.5 nm. The high-resolution TEM (HRTEM) result proved that the nanoparticles were structurally uniform with a lattice fringe spacing about 0.25 nm, which corresponded well with the values of 0.253 nm of the (3 1 1) lattice plane of the inverse spinel Fe₃O₄ obtained from the JCPDS database. The superconducting quantum interference device (SQUID) results revealed that the blocking temperature (T_b) was 190 K, and that the magnetic hysteresis loop at 300 K showed a saturation magnetization of 60.5 emu/g, and the absence of coercivity and remanence indicated that the as-synthesized Fe₃O₄ nanoparticles had superparamagnetic properties. Fourier transform infrared spectroscopy (FT-IR) spectrum displayed that the characteristic band of Fe-O at 569 cm⁻¹ was indicative of Fe₃O₄. This method might provide a new, mild, green, and economical concept for the synthesis of other nanomaterials.     

Effect of hydrothermal treatment on the acidity distribution of γ-Al2O3 support

The influence of hydrothermal treatment on the total acidity and the acidity distribution of γ-Al₂O₃ were studied in this paper. The experimental results indicated that the hydrothermal treatment of γ-Al₂O₃ at moderate condition (140 °C, 1.0-24.0 h) led to the formation of the plate-like γ-AlOOH crystallites with different morphologies, which resulted in the change of the surface acidity of the corresponding γ-Al₂O₃ supports. The increase of the reaction time in the period of 1.0-2.0 h led to the increase of the specific surface area, the surface OH, the total acidity and the ratio of the weak acidity in the acidity distribution of γ-Al₂O₃. The further prolongation of reaction time caused the overgrowth of γ-AlOOH crystallites, leading to the decrease of the specific surface area, the surface OH and the total acidity of the corresponding γ-Al₂O₃.     

Influence of deposition conditions on the optical properties of erbium-doped yttrium oxide films grown by aerosol-UV assisted MOCVD

Erbium-doped Y₂O₃ films were prepared by aerosol-UV assisted metal-organic chemical vapour deposition (MOCVD) at 410 °C. The effects of humidity of carrier gas and UV-assistance on their structure and optical properties were investigated on the as-deposited and thermal annealed films using infrared spectroscopy, X-ray diffraction and transmission electron microscopy. It was found that the as-deposited Er:Y₂O₃ films crystallise in the Y₂O₃ cubic structure and present a very low organic contamination when the deposition takes place under high air humidity and, even better, with UV-assistance. After annealing, two different structural phases are observed corresponding to the cubic and the monoclinic structures of Y₂O₃. The Er³⁺ luminescence analysed in the visible and IR regions, shows the classical green transitions. The best optical properties were obtained with as-deposited and annealed Er:Y₂O₃ films grown under high air humidity with UV-assistance. Under such deposition conditions, ⁴I_13/2 lifetimes was found to be 3.07 and 6.1 ms for films annealed at 800 and 1000 °C, respectively, and up-conversion phenomena were underlined. This indicates that the deposition conditions, in particular air humidity, play an important role in the luminescent properties even after annealing.     

Structure and dielectric studies of nano-composite Fe2O3: BaTiO3 prepared by sol-gel method

Nano-structure pure barium titanate (BaTiO₃) and that was doped with iron oxide (Fe₂O₃), have been prepared by sol-gel method, using barium acetate (Ba(Ac)₂) and titanium butoxide (Ti(C₄H₉O)₄), as precursors. The as-grown prepared samples by sol-gel technique were found to be amorphous, which crystallized to the tetragonal phase after synthesized at 750 °C in air for 1 h as detected from the XRD patterns. The XRD data were confirmed by transmission electron microscope (TEM). The dielectric properties namely; dielectric constant (ε′) and loss tangent (tan δ) in the frequency range between 42 Hz and 1 MHz, at range of temperature 25-250 °C were investigated. The temperature dependence of ε′ and tan δ for the undoped and doped materials, at 1 kHz, was also investigated. As a result, tan δ increased rapidly with decreasing temperature below 125 °C (Curie temperature) while above this temperature, tan δ shows temperature independent. As a result, below and above Curie temperature, ferroelectric phase and paraelectric phase of BaTiO₃ can be obtained, respectively.     

Green synthesis of soya bean sprouts-mediated superparamagnetic Fe3O4 nanoparticles

Superparamagnetic Fe₃O₄ nanoparticles were first synthesized via soya bean sprouts (SBS) templates under ambient temperature and normal atmosphere. The reaction process was simple, eco-friendly, and convenient to handle. The morphology and crystalline phase of the nanoparticles were determined from scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD) spectra. The effect of SBS template on the formation of Fe₃O₄ nanoparticles was investigated using X-ray photoemission spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FT-IR). The results indicate that spherical Fe₃O₄ nanoparticles with an average diameter of 8 nm simultaneously formed on the epidermal surface and the interior stem wall of SBS. The SBS are responsible for size and morphology control during the whole formation of Fe₃O₄ nanoparticles. In addition, the superconducting quantum interference device (SQUID) results indicate the products are superparamagnetic at room temperature, with blocking temperature (T_B) of 150 K and saturation magnetization of 37.1 emu/g.     

Characterization and compositional study of a ZrO2 engineering ceramic irradiated with a fibre laser beam

Fibre laser surface treatment (FLST) of a cold isostatic pressed (CIP) ZrO₂ engineering ceramic (ZEC) was performed using various processing gas compositions. This is the first time that a surface treatment of ZEC has been employed hitherto by using the fibre laser (FL) radiation to observe the changes on and within the surface of the engineering ceramic; in particular, material removal, surface topography, chemical composition, changes in the surface hardness and distribution of the heat affected zone (HAZ). Bonding of the grain boundaries was found through surface melting with all FL irradiated samples to some extent, but the effect was more marked on the sample FL irradiated with an Ar assist gas and proved to be the most effective combination for modifying the surface morphology. The surface finish and the material removal were varied with the changes in the gas composition. Maximum material removal was observed when an O₂ assist gas was employed on account of the O₂ generating an exothermic reaction. This in turn, produced excessive heating. The compositional analysis revealed a chemical change occurring within the FL irradiated surfaces, regardless of the assist gas used, with the ZEC transforming to zirconia carbide (ZrC).     

Mössbauer characterization of calcium–ferrite oxides prepared by calcining Fe2O3 and CaO

Calcium ferrite oxides were prepared by calcining a mixture powder of iron- and calcium oxide. The ⁵⁷Fe-Mössbauer spectra of the calcium ferrites oxides were measured, revealing that the products should be Ca₂Fe₂O₅ and CaFe₂O₄, the ratio of which was dependent of the Fe/Ca atomic ratio of the mixture powder.     

Structural-optical study of high-dielectric-constant oxide films

High-k polycrystalline Pr₂O₃ and amorphous LaAlO₃ oxide thin films deposited on Si(0 0 1) are studied. The microstructure is investigated using X-ray diffraction and scanning electron microscopy. Optical properties are determined in the 0.75-6.5 eV photon energy range using spectroscopic ellipsometry. The polycrystalline Pr₂O₃ films have an optical gap of 3.86 eV and a dielectric constant of 16-26, which increases with film thickness. Similarly, very thin amorphous LaAlO₃ films have the optical gap of 5.8 eV, and a dielectric constant below 14 which also increases with film thickness. The lower dielectric constant compared to crystalline material is an intrinsic characteristic of amorphous films.