溶胶凝胶制备氧化钒薄膜的生长机理及光电特性

采用溶胶凝胶法, 在不同的退火温度下制备了不同的氧化钒薄膜. 利用扫描电子显微镜、X射线衍射仪、高阻仪、紫外-可见分光光度计和傅里叶红外光谱仪等, 对薄膜的形貌、晶态、电学和光学特性进行了分析. 结果表明, 溶胶凝胶法获取V₂O₅薄膜的最佳退火温度为430 ℃, 低于此温度不利于使有机溶剂充分分解, 高于此温度则V–O键发生裂解、形成更多的低价态氧化钒. 本文制备的氧化钒薄膜具有较高的电阻温度系数和光吸收率, 适合应用在非制冷红外探测器中. 本文揭示了溶胶凝胶法制备氧化钒薄膜的生长机理. 关键词： 氧化钒薄膜 溶胶凝胶 光电特性 生长机理     

Physical and electrochemical properties of Li-intercalated Sn oxide films made by sputtering

Sn oxide films were made by reactive rf magnetron sputtering under conditions that led to both electronic and ionic conductivity. The film structure was studied by X-ray diffraction and Atomic Force Microscopy (AFM). Li⁺ intercalation produced electrochromism with coloration efficiency peaked in the infrared. Cyclic voltammograms taken at different sweep rates were interpreted in terms of a unique structural parameter related to the fractal dimension of a self-affine surface relief and in excellent agreement with the fractal dimension as obtained with AFM. Mössbauer spectroscopy was used to determine the valence state of the Sn-atoms; a change from Sn⁴⁺ to Sn²⁺ was detected after electrochemical intercalation of Li⁺.     

Structural and optical features of nanoporous silicon prepared by electrochemical anodic etching

Nanoporous silicon (NPS) samples were prepared by electrochemical anodic etching of p-type (0 0 1) silicon wafers in HF solution, and some of them were aged in air. The nanostructural, optical and chemical features of the NPS were investigated in terms of etching and aging conditions. The surface of the porous Si exhibits an etched layer with a thickness of 30–40 nm; this layer appears to consist of aggregates of 5–10 nm size nano-crystallites. The NPS exhibited broad photoluminescence (PL) spectra with its peak in the red light region (740 nm). After aging the porous samples for 4 weeks in air, we observed the PL intensity became approximately a fifth of that of the as-prepared one, along with a blue shift. It is very likely that the blue shift of the PL peak was caused by the shrinkage of the Si nano-crystallites due to the oxidation in the surface of the nano-crystallites.     

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.     

Optical and electrochemical properties of Cu-doped NiO films prepared by electrochemical deposition

Cu-doped nickel oxide (NiO) thin films were prepared by electrochemial deposition (cathodic deposition) technique onto the fluorine doped tin oxide (F: SnO₂; FTO) coated glass substrates from organic solutions. Effects of Cu content on the morphology, structure, optical and electrochromic properties of NiO films were investigated by means of scanning electron microscope (SEM), X-ray diffraction (XRD), ultraviolet-visible spectrophotometer (UV-vis) and cyclic voltammetry (CV), respectively. SEM images indicated the formation of nanorods after Cu was added. The films were formed with amorphous or short-range ordered NiO grains and a trace of face-centered cubic Ni_xCu_1−xO confirmed by XRD. The transmittances of both bleached state and colored state were significantly lowered when Cu was added. The NiO films doped with Cu (the molar ratio was 1/8) exhibited the optimum electrochromic behavior with a variation of transmittance (ΔT) up to ∼80% at the wavelength range of 350-600 nm. Cu doping reduces the response time for both the coloring and bleaching states, and the reversibility of the redox reaction was increased as well.     

Optical properties of alumina membranes prepared by anodic oxidation process

The luminescence property of anodic alumina membranes (AAMs) with ordered nanopore arrays prepared by electrochemically anodizing aluminum in oxalic acid solutions have been investigated. Photoluminescence emission (PL) measurement shows that a blue PL band occurs in the wavelength ranges of 300-600 nm. The PL intensity and peak position of AAMs depend markedly on the excitation wavelength. A new peak located at 518 nm can be observed under a monitoring wavelength at 429 nm in the photoluminescence excitation (PLE) spectra. Convincing evidences have been presented that the PLE would be associated with the residual aluminum ions in the membrane. The PLE and PL of AAMs, as a function of anodizing times, have been discussed. It is found that the oxalic impurities incorporated in the AAMs would have important influences on the optical properties of AAMs in the initial stage of anodization. The PL and PLE spectra obtained show that there are three optical centers, of which the first is originated from the F⁺ centers in AAMs, the second is correlated with the oxalic impurities incorporated in the AAMs, and the third is associated with the excess aluminum ions in the membrane.     

Gadolinium oxide high-k gate dielectrics prepared by anodic oxidation

The growth and properties of gadolinium oxide (Gd₂O₃) films prepared by anodic oxidation were investigated. Uniform Gd₂O₃ thin film with good oxide quality was obtained. The X-ray diffraction (XRD) pattern of the Gd₂O₃ films showed that they had a poly-crystalline structure. The dielectric constants of Gd₂O₃ films oxidized at 30 and 60 V are 9.4 and 12.2, respectively. The equivalent oxide thickness (EOT) of the Gd₂O₃ stacked oxide is in the range of 5.8-9.4 nm. The MOS capacitor with Gd₂O₃ exhibits interesting electrical properties. Longer oxidation time reduced the leakage current density for 30 V anodic oxidation but increased the leakage current density for 60 V anodic oxidation. This work reveals that Gd₂O₃ could also be an alternative dielectric for Si substrate and therefore, might pave the way to fabricate CMOS devices in the future.     

Magnetic and electromagnetic properties of composites of iron oxide and Co-B alloy prepared by chemical reduction

Magnetic and electromagnetic properties were investigated on the composites of iron oxide and Co-B alloy, which were prepared by a modified chemical reduction method. The composites are characterized by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDXA), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and vibrating sample magnetometry (VSM). The complex electromagnetic parameters (permittivity ε_r=ε_r′+jε_r″ and permeability μ_r=μ_r′+jμ_r″) of paraffin mixed composite samples (paraffin:composites=1:1 in mass ratio) were measured in the frequency range 2-18 GHz by vector network analyzer. The measured real part (ε_r′) and imaginary part (ε_r″) of the relative permittivity show two resonant peaks in the range of 2-18 GHz. The imaginary parts of relative permeability (μ_r″) of all samples exhibited one broad resonant peak over the 2-8 GHz range. The μ_r″ of samples with higher molar ratio of Co to Fe (C and D) shows negative values within 13-18 GHz, which exhibit resonant and antiresonant permeabilities simultaneously. Calculation results indicated that the reflection loss values of the composites and paraffin wax mixtures are less than −10 dB with frequency width of about 6 GHz at the matching thickness.     

Modeling and experiments of N-doped vanadium oxide prepared by a reactive sputtering process

An original numerical model, based on the standard Berg model, is used to simulate the growth mechanism of Ndoped VOx deposited with changing oxygen flow in the reactive gas mixture. In order to compare with the numerical model, N-doped VOx films are prepared by reactive magnetron sputtering from a metallic vanadium target immersed in a reactive gas mixture of Ar+O2+N2. Both experimental and numerical results show that the addition of N2 to the process alleviates the hysteresis effect with respect to the oxygen supply. Film compositions obtained from the XPS analysis are compared to the numerical results and the agreement is satisfactory. The results also show that the compound of VN is only found at very low O concentration because of the replacement reaction of VN by O2 atoms with higher oxygen flow rate.     

Electrical and optical properties of polythiophene prepared by electrochemical polymerization

Electrical conductivities and optical absorptions of neutral and oxidized polythiophene films polymerized by the electrochemical method are reported. The electrical conductivity of polythiophene borofluoride film shows metallic value of ca. 100 S cm^?1 at room temperature and decreases over 10¹⁰ times into semiconductive regime by the electro-chemical or chemical undoping. Absorption spectrum of polythiophene changes by the undoping from the characteristic of metal to interband transition with absorption edge ca. 2.0 eV and maximum absorption coefficient of ～ 10⁵ cm^?1 at 2.7 eV.     

Characterization of native and anodic oxide films formed on commercial pure titanium using electrochemical properties and morphology techniques

Potentiostatically anodized oxide films on the surface of commercial pure titanium (cp-Ti) formed in sulfuric (0.5 M H₂SO₄) and in phosphoric (1.4 M H₃PO₄) acid solutions under variables anodizing voltages were investigated and compared with the native oxide film. Potentiodynamic polarization and electrochemical impedance spectroscopy, EIS, were used to predicate the different in corrosion behavior of the oxide film samples. Scanning electron microscope, SEM, and electron diffraction X-ray analysis, EDX, were used to investigate the difference in the morphology between different types of oxide films. The electrochemical characteristics were examined in phosphate saline buffer solution, PSB (pH 7.4) at 25 °C. Results have been shown that the nature of the native oxide film is thin and amorphous, while the process of anodization of Ti in both acid solutions plays an important role in changing the properties of passive oxide films. Significant increase in the corrosion resistance of the anodized surface film was recorded after 3 h of electrode immersion in PSB. On the other side, the coverage (θ) of film formed on cp-Ti was differed by changing the anodized acid solution. Impedance results showed that both the native film and anodized film formed on cp-Ti consist of two layers. The resistance of the anodized film has reached to the highest value by anodization of cp-Ti in H₃PO₄ and the inner layer in the anodized film formed in both acid solutions is also porous.     

Antibacterial properties of Ag-doped hydroxyapatite layers prepared by PLD method

Thin hydroxyapatite (HA), silver-doped HA and silver layers were prepared using a pulsed laser deposition method. Doped layers were ablated from silver/HA targets. Amorphous and crystalline films of silver concentrations of 0.06 at.%, 1.2 at.%, 4.4 at.%, 8.3 at.% and 13.7 at.% were synthesized. Topology was studied using scanning electron microscopy and atomic force microscopy. Contact angle and zeta potential measurements were conducted to determine the wettability, surface free energy and electric surface properties. In vivo measurement (using Escherichia coli cells) of antibacterial properties of the HA, silver-doped HA and silver layers was carried out. The best antibacterial results were achieved for silver-doped HA layers of silver concentration higher than 1.2 at.%.     

Effects of reducing agents on the electrochemical properties of the prepared manganese oxide powders

Manganese oxide powders with high specific capacitance were successfully fabricated via a simple redox reaction at room temperature. The reducing agents used for the redox reaction significantly affected the oxidation states and the electrochemical properties of the prepared manganese oxide powders. As C₂H₅OH was used as the reducing agent, high Mn³⁺ content and high amount of hydroxide were observed in the prepared manganese oxide powders. In addition, the molar ratios of KMnO₄ and C₂H₅OH also influenced the electrochemical properties of the prepared manganese oxide powders. When the molar ratio of KMnO₄ and C₂H₅OH was 1:40, the specific capacitance of the prepared manganese oxide was as high as 402 F/g. These results of the electrochemical analysis showed that, adjusting the molar ratios of KMnO₄ and C₂H₅OH demonstrated to be an effective method for controlling the electrochemical characteristics of manganese oxide powders.     

Optical and magnetic properties of InFeP layers prepared by Fe~+ implantation

InFeP layers are prepared by ion implantation of InP with 100-keV Fe＋ ions to a dose of 5 ×10^16 cm-2 and investigated by optical, magnetic, and ion beam analysis measurements. Photoluminescence measurements show a deep-level peak at 1.035 eV due to Fe in InP and two exciton-related luminescences at 1.426 eV and 1.376 eV in the implanted samples annealed at 400℃. Conversion electron Mossbauer spectroscopy reveals a doublet corresponding to Fe3＋ ions in the indium sites. Atomic force microscopy and magnetic force microscopy show that magnetic clusters are formed in the annealing process. The magnetization-field hysteresis loops show ferromagnetic properties persisting up to room temperature with a coercive field of 100 0e （10e = 79.5775 A-m-1）, saturation magnetization of 4.35 × 10-5 emu, and remnant magnetization of 4.4× 10 6 emu.     

Structural characterization of titanium oxide layers prepared by plasma based ion implantation with oxygen on Ti6Al4V alloy

Ti6Al4V alloy was implanted with oxygen by using plasma based ion implantation (PBII) at pulsed voltage ranging from −10 to −50 kV with a frequency of 100 Hz. In order to maintain a lower implantation temperature, an oil cooling working table was employed. The structure of the modified layers was characterized by X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. The results show that the thickness of the titanium oxide layer increases significantly with the increase of implanted voltage. The structure of the modified layer changes along depth. It is found that the surface layer consists of TiO₂, and the subsurface layer is a mixing structure of TiO_2, Ti₂O₃ and TiO. There is crystalline rutile phase existing in the modified layer of sample implanted at high implanted voltage. In addition, in the outmost modified surface, aluminum present as oxidized state, and vanadium could not be detected.     

Field-emission properties of diamond-like-carbon and nitrogen-doped diamond-like-carbon films prepared by electrochemical deposition

Field-emission studies were carried out on diamond-like-carbon (DLC) and nitrogen-doped diamond-like-carbon (N-DLC) films deposited by an electro-deposition technique. The films were deposited on Si(100) substrates by electrolysis of methanol–urea solution under high voltage, at atmospheric pressure, and low temperature. The microstructure and morphology of the resulting films were analyzed by means of Raman spectroscopy, X-ray photoelectron spectroscopy, and atomic force microscopy. The field-emission measurements were carried out with a parallel plate configuration using the deposited DLC and N-DLC films as the cathode and indium tin oxide coated glass as the anode. The field-emission measurements indicated that the electro-deposited films exhibited good field-emission properties and the nitrogen doping could increase the current density. These behaviors were demonstrated to mainly relate to changes in the microstructure of the samples, in connection with the difference of surface morphology. PACS 79.70.+q; 81.05.Uw; 81.15.Pq     

Optimization of effective parameters in the synthesis of nanopore anodic aluminum oxide membrane and arsenic removal by prepared magnetic iron oxide nanoparicles in anodic aluminum oxide membrane via ultrasonic-hydrothermal method

In this study, a new anodized aluminum oxide (AAO) nanostructure membrane was synthesized by anodization process under a constant voltage, in oxalic acid solution that was improved with trace amounts of sulfuric acid at room temperature. The effect of various parameters on the morphology of the synthesized nanostructures such as voltage, electrolyte composition, anodization time and type of stripping solution were investigated. According to the results, corrosion of the walls, size regularity, diameter and number of the pores increased in the presence of sulfuric acid (0.018 mol.L⁻¹). Nitrogen adsorption-desorption analysis confirmed significant porosity, array and uniformity of the pore size in the synthesized nanoporous membrane. A new modification method was used based on ultrasonic-hydrothermal method to modify the synthesized AAO with Fe₃O₄/SiO₂ nanoparticles for metals and metalloids removal from aqueous solution. In this method, Fe₃O₄/SiO₂ nanoparticles were placed very regularly and uniformly on the surface and inside the pores. This modification was confirmed by characterization techniques. The modified AAO@Fe₃O₄/SiO₂ membrane showed excellent results for removing arsenic from aqueous media.     

电磁复合场制备匀质Zn-Bi偏晶合金的物理模拟

本文通过物理模拟的方法研究了强磁场复合交变电流作用对过偏晶合金凝固组织的影响机理,考察了电磁复合场下第二相初生液滴直径的演变规律,以及洛伦兹力作用下已分层少数相被"打碎"进入基体相的过程.结果表明:电磁体积力的增加,有利于液滴初始直径的减小;而交变电流频率的影响存在最佳值,偏离该值对初生液滴直径的抑制效果下降,这与实际试验规律一致;在电磁复合场作用下,已经分层的两液相可以重新实现均匀混合.这些效应有效缓解了偏晶合金凝固前第二相由于各种因素导致的偏聚,模拟结果直观地揭示了电磁复合场制备匀质偏晶合金的主要机理 关键词： 电磁复合场 偏晶合金 物理模拟     

Effect of thermal treatment on the structural characteristics and electrochemical properties of amorphous Mn oxide prepared by an ethanol-based precipitation method

Nanostructured amorphous Mn oxide, for use as an electrode material in supercapacitors, was prepared by a facile precipitation method using ethanol. After thermal treatment at various temperatures, the structural characteristics and electrochemical properties of the prepared Mn oxide were investigated. Importantly, the experimental results revealed that the alkyl chain of ethanol prevented the excessive crystallization of Mn oxide, resulting in the production of nanostructured Mn oxide. In addition, electrochemical properties of synthesized material were highly dependent on the structural characteristics. Mn oxide thermally treated at 300 °C, which had an optimized crystalline structure, showed the highest specific capacitance of 161 F/g in this study.     

Growth and properties of epitaxial iron oxide layers

Epitaxial layers of iron oxides have been grown on a MgO(001) substrate by evaporating natural Fe or⁵⁷Fe from Knudsen cells in the presence of a NO₂ flow directed to the substrate. The resulting layers have been investigated in situ with LEED, RHEED, AES and XPS and ex situ with CEMS and ion beam analysis. For substrate temperatures between 200 and 400°C we observe RHEED oscillations during deposition, indicative of layer-by-layer growth. By adjusting the flux of NO₂ at the surface, all stable and metastable cubic phases in the Fe-O system could be grown: FeO (wustite), Fe₃O₄ (magnetite), -Fe₂O₃ (maghemite) and solid solutions between the latter two phases. Rutherford backscattering spectra show a relatively high minimum yield in the channel directions.