Anomalous magnetic properties of an iron film system deposited on fracture surfaces of α-Al_2O_3 ceramics

An iron film percolation system is fabricated by vapour-phase deposition on fracture surfaces of α-Al2O3 ceramics. The zero-field-cooled （ZFC） and field-cooled （FC） magnetization measurement reveals that the magnetic phase of the film samples evolve from a high-temperature ferromagnetic state to a low-temperature spin-glass-like state, which is also demonstrated by the temperature-dependent ac susceptibility of the iron films. The temperature dependence of the exchange bias field He of the iron film exhibits a minimum peak around the temperature T=5 K, which is independent of the magnitude of the cooling field Hcf. However, for T 〉 10K, （1） He is always negative when Hcf=2kOe and （2） for Hcf= 20 kOe （1Oe≈80 A/m）, He changes from negative to positive values as T increases. Our experimental results show that the anomalous hysteresis properties mainly result from the oxide surfaces of the films with spin-glass-like phase.

X-ray absorption near the edge structure and x-ray photoelectron spectroscopy studies on pyrite prepared by thermally sulfurizing iron films

This paper reports how pyrite films were prepared by thermal sulfurization of magnetron sputtered iron films and characterized by X-ray absorption near edge structure spectra and X-ray photoelectron spectroscopy on a 4B9B beam line at the Beijing Synchrotron Radiation Facility. The band gap of the pyrite agrees well with the optical band gap obtained by a spectrophotometer. The octahedral symmetry of pyrite leads to the splitting of the d orbit into t2g and eg levels. The high spin and low spin states were analysed through the difference of electron exchange interaction and the orbital crystal field. Only when the crystal field splitting is higher than 1.5 eV, the two weak peaks above the white lines can appear, and this was approved by experiments in the present work.

Domain Structure of Iron Thin Films Prepared by Sputtering

Microstructure and magnetic domain structure of thin iron film prepared by sputtering were studied by magnetic force microscopy (MFM). Owing to the high lateral resolution of MFM magnetic structure of a single domain is able to be studied. Two series of iron thin films were grown on microcrystalline glass substrate by DC magnetron sputtering. They were prepared at different Ar pressure and annealing time. The results by magnetic force microscopy show both surface topography of the films and their local magnetic domain structure. It is suggested that the pin effect by single domain wall influence magnetic properties of the iron thin films.

Electrodeposited Cobalt-Iron Alloy Thin-Film for Potentiometric Hydrogen Phosphate-Ion Sensor

A cobalt-iron alloy thin-film electrode-based electrochemical hydrogen-phosphate-ion sensor was prepared by electrodepositing on an Au-coated Al2O3 substrate from an aqueous solution of metal-salts. The use of a cobalt-iron alloy electrode greatly improved the hydrogen-ion sensor response performance, i.e., the sensor worked stably for more than 7 weeks and showed a quick response time of several seconds. Among the cobalt and iron alloy systems tested, the electrodeposited Co58Fe42 thin-film electrode showed the best EMF response characteristics, i.e., the sensor exhibited a linear potentiometric response to hydrogen-phosphate ion at the concentration range between 1.0 × 10–5 and 1.0 × 10–2 M with the slope of –43 mV/decade at pH 5.0 and at 30℃. A sensing mechanism of the Co-based potentiometric hydrogen-phosphate ion sensor was proposed on the basis of results of instrumental analysis.

High Resolution Electron Microscopy Observations of Structural Changes in Iron Nitride Films Annealed in Vacuum

Iron-nitride films were prepared by reactive sputtering, and the effect of annealing treatment on the structures was investigated by means of in-situ electron microscopy and high resolution electron microscopy (HREM). As-deposited films were observed to be a mixed structure of a few ultrafine epsilon-Fe2-3N particles existing in the amorphous matrix. it was found that the structure-relaxation in the amorphous occurred at 473 K, and the ultrafine grains began to grow at the higher annealing temperatures. The transition of the amorphous to epsilon-Fe2-3N was almost completed at 673 K. It is considered that the formation of the ideal epsilon-Fe3N is originated from the ordering of the nitrogen atoms during the annealing in vacuum. On the other hand, gamma'-phase (Fe4N) was seen to precipitation of epsilon-phase at 723 K. Two possible modes are proposed in the precipitation of gamma'-phase, depending on the heating rate and crystallographic orientation relationships, i.e. [121](epsilon)//[001](gamma), (2(1) over bar0$)(epsilon)//(110)(gamma) and [100](epsilon)//[110](gamma), (001)(epsilon)//(111)(gamma). In addition, alpha-Fe particles were observed to form from the gamma'-phase at high temperatures. We assumed that these structural changes are due to the diffusion of nitrogen and iron atoms during the annealing, except for the case of the precipitation of the gamma'-phase as depicted above. The results obtained in this work are in a good agreement with the assumption.

PHOTOSPLITTING OF WATEM AT THIN FILM IRON OXIDE ELECTRODES

both theoretical and experimental findings of the photoresponse for water spliting of the pyrolytically prepared thin film iron oxide electrodes are given.Fur- ther,the spray time and the corresponding thickness of the Fe_2O_3 thin film were opti- mized to have maximum photoresponse.The effect of iodine doping on photoresponse of iron oxide was investigated.

Dynamic scaling behavior of iron nitride thin films prepared by magnetron sputtering and ion implantation

Under far from equilibrium conditions, the formation mechanism of solid can be studied in terms of the dynamic scaling theory. The roughness and dynamic scaling behavior of the Fe-N thin films were studied by atomic force microscopy and grazing incidence X-ray scattering. The results indicate that the roughness of the surface increases with increasing sputtering time during the course of magnetron sputtering, and the surface exhibits a fractal characteristic. While the Fe-N films prepared by compound technology—combining magnetron sputtering with plasma based ion implantation are not in agreement with the fractal theory.

Influence of process parameters on electrochemical and physical properties of sputtered iron-doped nickel oxide thin films

The iron-doped nickel oxide films used as oxygen evolution catalysts in the photoelectrochemical production of hydrogen from solar energy were deposited by means of RF reactive magnetron sputtering from a Ni-Fe alloy target in oxygen and argon atmosphere.The effects of processing parameters on the film properties,such as overpotential,composition,surface morphology and preferred orientation,were investigated.The electrochemical experiment,structural and compositional measurements indicate that the relative lower substrate temperature,higher RF power,higher working pressure and oxygen content are necessary to gain lower overpotential.The lowest overpotential of 251 mV is obtained at a current density of 80 mA/cm2.The existence of iron,which acts as activity site,and Ni3+ ion is responsible for lowering overpotential.By analyzing SEM and XRD data,it is also noticed that an improvement in crystallinity,appropriate grain size and less crystalline phase contribute to an increased electrocatalytic activity in oxygen evolution reaction.These results mentioned above indicate that iron-doped nickel oxide is promising as an oxygen catalyst.

Growth of a Pure and Single Phase Iron Sulfide (Pyrite) Thin Film by Electrochemical Deposition for Photovoltaic Applications

Single phase iron pyrite (FeS2) films have been successfully deposited on ITO-coated glass substrates using a 3-electrode electrochemical system with graphite as the counter electrode and Ag/AgCl as the reference electrode. In this single-step electrodeposition, the FeS precursor thin film was directly electrodeposited on the conductive substrate from the electrolytic bath solution which contained FeSO4.7H2O as an iron source, and Na2S2O3.5H2O as a sulfur source. The deposition was carried out potentiostatically at a constant potential of -0.9 V vs. Ag/AgCl at room temperature. The growth of the iron pyrite phase was achieved by annealing the as-deposited at 500°C for an hour in an ambient of sulfur to form the pyrite phase. For sulfurization, two different techniques, one using the Kipp’s apparatus and a second, which involved heating elemental sulfur at 200°C, were used for the production of the sulfur gas. X-ray diffraction analyses of the sulfurized films showed that both sulfurization techniques appeared to form the pyrite phase, however, the second method yielded films with maximum crystalline order and stoichiometry with no discernable impurity peaks. Optical absorption measurements revealed the existence of a direct transition with an estimated band gap of 1.75 eV. SEM micrograph showed a compact morphology with a rough surface made up of crystallites of irregular shapes and sizes with well-defined edges, covering the entire substrate. EDAX analysis of the film was consistent with the formation of FeS2 pyrite thin films.

Diffusion in the aged aluminium film on iron

Metallic coatings of many types can be applied to steel to provide outstanding, long-term corrosion protection. A thin A1 film is studied at an Fe substrate by the molecular dynamics method at temperatures ranging from 300 K to 1173 K. A1 atoms are found to penetrate the Fe matrix at a temperature of 873 K. The potential energy of the system changes step-like at a temperature of 1173 K. At such temperature mean square atomic displacement significantly changes. The behaviors of the A1 and Fe diffusion coefficients are mainly determined by the temperature dependence of the diffusion activation energy.

Gas-sensing Properties of Bismuth Iron Molybdate Thin Films

The thin film gas sensors of bismuth iron molybdate were prepared by ion beam sputtering technique. The prototype gas sensors studied have high sensitivity and selectivity to reducing gases, such as ethanol vapor, show a long term stability of response under most operating conditions and insensitivity to atmospheric humidity, and respond quickly comparing to traditional sintered gas sensors. The crystallographic structure and phase composition of these thin films were investigated with XRD, XPS and SEM techniques.

生物炭负载纳米零价铁对废旧薄膜太阳能电池中稀贵金属富集分离

本研究采用废弃生物秸秆作为原料,通过高温热解制备生物炭。随后,通过加入还原剂将零价铁纳米粒子修饰在生物炭材料上,获得零价磁性生物炭纳米复合材料。基于废旧薄膜太阳能电池中稀贵金属的有效回收问题,利用该复合材料实现了废旧薄膜太阳能电池中稀贵金属铟、镓、硒高效富集与分离。通过实验分析,复合材料对铟、镓、硒富集效率分别为13.5、23.4、18.9 mmol/g,铟、镓、硒加标平均回收率在93.0%~97.4%范围,相对标准偏差<10%,证实该方法在提取和回收废旧薄膜太阳能电池中的稀贵金属方面具有显著优势。

LDPE/m-nZVI复合膜的制备及性能

为克服脱氧剂小袋包装与食品混装带来的安全问题,采用硼氢化钾(KBH4)液相还原法制备了油酸钠(NaOl)改性纳米零价铁(m-nZVI),将其与低密度聚乙烯(LDPE)熔融共混后热压成膜,制备了包装用LDPE/m-nZVI阻氧复合膜。利用傅里叶变换红外光谱仪、热重分析仪、差示扫描量热仪、万能拉伸试验机和气体渗透仪对复合膜的结构与性能进行表征和测定。结果表明:m-nZVI和LDPE的复合是物理共混;加入m-nZVI后,LDPE的热稳定性基本不变;随着m-nZVI含量的增加,复合膜的抗拉强度和断后伸长率先增大后减小,m-nZVI质量分数为2%时,抗拉强度和断后伸长率达到最大,较LDPE膜分别提高了41.4%和23.4%;复合膜的氧气透过系数也呈现出先减小后增大,当m-nZVI质量分数为3%时,复合膜的氧气透过系数最小,较LDPE膜降低了40.9%。复合膜结晶过程中,m-nZVI起异相成核的作用,改善了复合膜的结晶行为,使复合膜的结构和性能得到改善,力学性能和阻隔性能都得到提高。

周期性铁薄膜-羰基铁@环氧树脂涂层的制备及其雷达红外兼容隐身性能优化

随着侦查技术的快速发展,亟需兼具雷达/红外隐身性能的兼容隐身材料。以羰基铁为吸收剂,环氧树脂为粘结剂,采用刮涂法制备了羰基铁@环氧树脂吸波涂层,随后采用磁控溅射及激光雕刻技术在吸波涂层表面制备了具有周期性结构的铁薄膜,得到了兼具雷达/红外隐身性能的兼容隐身涂层,探究了铁薄膜厚度及面积占比及羰基铁含量对兼容涂层吸波/红外发射率的影响规律。研究表明:当片状羰基铁粉含量为75wt%、铁薄膜厚度为100 nm、铁薄膜面积分数为80%时,兼容隐身涂层性能最好,在8.2~12.4 GHz频段内,反射率小于-8.75 dB,中、远红外两个波段红外发射率分别为0.279和0.338。

关于M5合金燃料包壳表面材料在堆内流致振动下脱落共性问题的研究

M5锆合金包壳是由法国法马通公司设计研发的,目前广泛应用于核电厂AFA-3G等系列的燃料组件。本文分析了国内外核电厂使用M5合金燃料包壳表面材料在堆内流致振动下脱落共性问题的研究现状,包括燃料组件外观检查情况、氧化膜厚度测量情况等,从而得出研究结论并提出合理建议。

Mechanism of protective film formation during CO_2 corrosion of X65 pipeline steel

Electrochemical techniques, X-ray diffraction （XRD）, and scanning electron microscopy （SEM） were applied to study the corrosion behaviors of X65 steel in static solution with carbon dioxide （CO2） at 65℃. The results show that iron carbonate （FeCO3） deposits on the steel surface as a corrosion product scale. This iron carbonate scale acts as a barrier to CO2 corrosion, and can reduce the general corrosion rate. The protection ability of the scale is closely related to the scale morphological characteristics.

Microstructure and properties of hydrophobic films derived from Fe-W amorphous alloy

Amorphous metals are totally different from crystalline metals in regard to atom arrangement. Amorphous metals do not have grain boundaries and weak spots that crystalline materials contain, making them more resistant to wear and corrosion. In this study, amorphous Fe-W alloy films were first prepared by an electroplating method and were then made hydrophobic by modification with a water repellent （heptadecafluoro-1,1,2,2-tetradecyl） trimethoxysilane. Hierarchical micro-nano structures can be obtained by slightly oxidizing the as-deposited alloy, accompanied by phase transformation from amorphous to crystalline during heat treatment. The mi-cro-nano structures can trap air to form an extremely thin cushion of air between the water and the film, which is critical to producing hydrophobicity in the film. Results show that the average values of capacitance, roughness factor, and impedance for specific surface areas of a 600°C heat-treated sample are greater than those of a sample treated at 500°C. Importantly, the coating can be fabricated on various metal substrates to act as a corrosion retardant.

Thickness dependent manipulation of uniaxial magnetic anisotropy in Fe-thin films by oblique deposition

The uniaxial magnetic anisotropy of obliquely deposited Fe（001）/Pd film on MgO（001） substrate is investigated as a function of deposition angle and film thickness. The values of incidence angle of Fe flux relative to surface normal of the substrate are 0°, 45°, 55°, and 70°, respectively. In-situ low energy electron diffraction is employed to investigate the surface structures of the samples. The Fe film thicknesses are determined to be 50 ML, 45 ML, 32 ML, and 24 ML（1 ML = 0.14 nm） by performing x-ray reflectivity on the grown samples, respectively. The normalized remanent magnetic saturation ratio and coercivity are obtained by the longitudinal surface magneto-optical Kerr effect. Here, the magnetic anisotropy constants are quantitatively determined by fitting the anisotropic magnetoresistance curves under different fields.These measurements show four-fold cubic anisotropy in a large Fe film thickness（50 ML） sample, but highly in-plane uniaxial magnetic anisotropies in thin films（24 ML and 32 ML） samples. In the obliquely deposited Fe films, the coercive fields and the uniaxial magnetic anisotropies（UMAs） increase as the deposition angle becomes more and more tilted. In addition, the UMA decreases with the increase of the Fe film thickness. Our work provides the possibility of manipulating uniaxial magnetic anisotropy, and paves the way to inducing UMA by oblique deposition with smaller film thickness.

Thickness-dependent magnetic anisotropy in obliquely deposited Fe(001)/Pd thin film bilayers probed by VNA-FMR

The thickness-dependent magnetic anisotropy of obliquely deposited Fe(001)/Pd thin films on Mg(001) is investigated by fitting the field-dependent resonant field curve using the Kittel equation.In this study, three Fe film samples with thicknesses of 50 monolayers(ML), 45 ML, and 32 ML deposited at 0°, 45°, and 55°, respectively, are used.The magnetic anisotropy constant obtained from ferromagnetic resonance(FMR) spectra exhibits a dominant fourfold magnetocrystalline anisotropy(MCA) at the normal deposition angle with larger Fe thickness.However, the in-plane uniaxial magnetic anisotropy(UMA) is induced by a higher oblique deposition angle and a smaller thickness.Its hard axis lies between the [100] and [010] directions.The FMR data-fitting analysis yields a precise measurement of smaller contributions to the magnetic anisotropy, such as in-plane UMA.Due to MCA, when the magnetic field is weaker than the saturated field,the magnetization direction does not always align with the external field.The squared frequency-dependent resonant field measurement gives an isotropic Landé g-factor of 2.07.Our results are consistent with previous experiments conducted on the magneto-optical Kerr effect(MOKE) and anisotropic magnetoresistance(AMR) systems.Thus, a vector network analyzer ferromagnetic resonance(VNA-FMR) test-method for finding UMA in obliquely deposited Fe(001)/Pd bilayer ferromagnetic thin films, and determining the magnetic anisotropy constants with respect to the film normal deposition, is proposed.