Microstructure and electrochemical properties of electron-beam deposited Sn-Cu thin film anodes for thin film lithium ion batteries

Thin film Sn-Cu anodes with high Cu content were prepared by electron-beam evaporation deposition using Cu substrate as current collector. Annealing, with the condition being determined by DSC, was used to improve the performance of these electrodes. X-ray diffraction (XRD), scanning probe microscopy (SPM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) were used to characterize the structure and composition of the Sn-Cu thin film electrodes. Cyclic voltammetry and galvanostatical charge-discharge measurement were carried out to characterize the electrochemical properties of the as-deposited and annealed electrodes. ?-Cu₃Sn intermetallic phase was formed and interface strength between deposited active materials layer and current collector was enhanced by annealing the as-deposited film under suitable condition. The annealed thin film electrode showed good cycleability and had no phase change during cycling. Although large initial capacity loss was found associated with SEI formation due to increase of surface roughness of annealed electrode, a stable discharge capacity near 300 mAh/g with Coulomb efficiency of about 96% was obtained at voltage window of 0.1-2.0 V and a discharge capacity of about 200 mAh/g and Coulomb efficiency of 97% were kept stable up to 30th cycle at a narrower voltage window of 0.2-1.5 V versus Li/Li⁺.     

Effect of doped niobium pentoxide on structure and properties of hafnium oxide films deposited by ion beam assisted deposition

Hafnium oxide is widely used in optical coating materials because of its high refractive index, broad band gap, high laser damage threshold and its high transparency in the wavelength range from ultraviolet to middle infrared (0.20–12 μm). However, hafnium oxide has some defects such as strong crystallinity and poor surface quality, which results in enhanced absorption and reflection of light wave and limits its application in optical field. As a pentoxide with high transparency and excellent optical properties in the wavelength range from ultraviolet to mid-infrared(0.35–9 μm), the doping of niobium pentoxide can effectively improve the surface quality and optical properties of the films. Mixed films with different chemical compositions were prepared by ion beam assisted deposition, and the microstructure, crystallinity, surface quality, optical properties and mechanical properties of the mixed films with different chemical compositions were investigated. The doping of niobium pentoxide inhibits the crystallization of hafnium oxide, optimizes the surface quality of the films, and improves the refractive index and mechanical properties of mixed films, effectively broadens the application of hafnium oxide in the field of optical films.     

Effect of Au ion beam on structural,surface, optical and electrical properties of ZnO thin films prepared by RF sputtering

In the present work, ZnO thin films were irradiated with 700?keV Au⁺ ions at different fluence (1?× 10¹³, 1?× 10¹⁴, 2?× 10¹⁴ and 5?× 10¹⁴ ions/cm²). The structural, morphological, optical and electrical properties of pristine and irradiated ZnO thin films were characterized by X-ray diffraction (XRD), Fourier transforms infrared spectroscopy (FTIR), scanning electron microscope (SEM), spectroscopy ellipsometry (SE) and four point probe technique respectively. XRD results showed that the crystallite size decreased from pristine value at the fluence 1?×?10¹³ ions/cm², with further increase of ion fluence the crystallite size also increased due to which the crystallinity of thin films improved. SEM micrographs showed acicular structures appeared on the ZnO thin film surface at high fluence of 5?×?10¹⁴ ions/cm². FTIR showed absorption band splitting due to the growth of ZnO nanostructures. The optical study revealed that the optical band gap of ZnO thin films changed from 3.08?eV (pristine) to 2.94?eV at the high fluence (5?× 10¹⁴ ions/cm²). The electrical resistivity of ZnO thin film decreases with increasing ion fluence. All the results can be attributed to localized heating effect by ions irradiation of thin films and well correlated with each other.     

不同载体表面负载TiO2薄膜的离子掺杂研究

TiO₂薄膜是解决TiO₂回收的有效方法，缺点是TiO₂活性低，寻找合适的载体以及提高TiO₂薄膜的光催化活性,是TiO₂负载薄膜技术需要解决的核心问题。研究了13种离子对负载在釉面瓷砖、玻璃、陶瓷、钛片、铝片和不锈钢片6种载体上TiO₂薄膜的掺杂，并从界面材料结构、双电层结构等方面讨论了离子掺杂与载体对TiO₂薄膜光催化活性的影响。结果表明，TiO₂薄膜的离子掺杂效果不仅和离子掺杂浓度、种类有关，而且还与载体类型有关。TiO₂薄膜和非金属载体主要形成复合半导体结构，改善掺杂离子对载流子的捕获能力。金属载体与TiO₂薄膜之间主要形成肖特基势垒，有利于电子与空穴的分离。载体与TiO₂薄膜之间形成的界面双电层结构能改变离子捕获中心与TiO₂半导体费米能级间的相对位置，从而提高或降低离子对载流子的捕获能力。     

Effect of Ar:N2 flow rate on morphology,optical and electrical properties of CCTO thin films deposited by RF magnetron sputtering

Calcium copper titanate (CCTO) thin films were deposited on indium tin oxide (ITO) substrates using radio frequency (RF) magnetron sputtering, at selected Ar:N₂ flow rates (1:1, 1:2, 1:4, and 1:6 sccm) at ambient temperature. The effect of Ar:N₂ flow rate on the morphology, optical and electrical properties of the CCTO thin films were investigated using FESEM, XRD, AFM, Hall effect measurement, and UV–Vis spectroscopy. It was confirmed by XRD analysis that the thin films were produced is CCTO with cubic crystal structure. As the flow rate of Ar:N₂ increased up to 1:6 sccm, the thin film thickness reduced from 87 nm to 35 nm while the crystallite size of CCTO thin film decreased from 27 nm to 20 nm. Consequently, the surface roughness of thin film was halved from 8.74 nm to 4.02 nm. In addition, the CCTO thin films deposited at the highest Ar:N₂ flow rate studied, at 1:6 sccm; are having the highest sheet resistivity (13.27 Ω/sq) and the largest optical energy bandgap (3.68 eV). The results articulate that Ar:N₂ flow rate was one of the important process parameters in RF magnetron sputtering that could affect the morphology, electrical properties and optical properties of CCTO thin films.     

Photocatalytic decomposition of NO on titanium oxide thin film photocatalysts prepared by an ionized cluster beam technique

Transparent TiO₂ thin film photocatalysts were prepared on transparent porous Vycor glass (PVG) by an ionized cluster beam (ICB) method. The UV‐VIS absorption spectra of these films show specific interference fringes, indicating that uniform and transparent TiO₂ thin films are formed. The results of XRD measurements indicate that these TiO₂ thin films consist of both anatase and rutile structures. UV light (λ > 270 nm) irradiation of these TiO₂ thin films in the presence of NO led to the photocatalytic decomposition of NO into N₂, O₂ and N₂O. The reactivity of these TiO₂ thin films for the photocatalytic decomposition of NO is strongly dependent on the film thickness, i.e., the thinner the TiO₂ thin films, the higher the reactivity. This revised version was published online in July 2006 with corrections to the Cover Date.     

Suppression of radiation‐induced oxidation of polymers by sputtered silicon oxide coating

Oxygen barrier coating on polymers was attempted to obtain polymeric composite materials with improved radiation resistance. Silicon oxide (SiO_1.6) films ranging from 120 to 240 nm thick were formed on polypropylene (PP) and polyethylene (PE) by radio frequency (RF) magnetron sputtering. Oxygen permeability after SiO_1.6 deposition was reduced significantly in all samples studied, indicating that silicon oxide is a useful gas barrier. The oxygen permeability coefficient of deposited films for PP was 1.7–2.2 × 10^?14 cm³‐cm/cm²/s/cmHg and that for PE was 2.8–4.8 × 10^?13 cm³‐cm/cm²/s/cmHg. We studied the effect of such films on the radiation resistance of polymers in the presence of oxygen by microscopic infrared (IR) absorption spectroscopy. Silicon oxide films 180 nm thick were deposited on the surfaces of PP and PE, and the formation of carbonyl groups after irradiation in air was measured as a function of depth from the surface. Results compared with those for uncoated PE and PP showed that the radiation‐induced polymer oxidation is dramatically suppressed by silicon oxide coating. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 186–190, 2002     

Variable‐energy positron lifetime study of silicon‐oxide films plasma deposited from hexamethyldisiloxane and oxygen mixtures

Mixtures of hexamethyldisiloxane [HMDSiO, (CH₃)₃SiOSi(CH₃)₃] and oxygen are plasma polymerized at different oxygen pressures (P = 1.3–11.4 Pa) and a fixed monomer pressure (P_m = 2.6 Pa). The discharge power is kept at 100 W throughout the work. Nanometer‐size holes in the deposited films are characterized by variable‐energy positron annihilation lifetime spectroscopy (PALS). Additional information on the film composition and structure is obtained by X‐ray photoelectron spectroscopy and IR absorption spectroscopy. The ortho‐positronium lifetime τ₃ and intensity I₃ increase with the P up to 6.2 Pa and then decrease with the P. PALS measurements after annealing at 400°C show that films prepared at high oxygen pressure have a less stable structure than a film deposited at a lower oxygen pressure. These results are discussed in comparison with plasma deposition of pure HMDSiO, as are the possible effects of oxygen radicals on the film structure. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 79: 974–980, 2001     

Study the effect of thermal annealing on adhesion strength of Silver-Tantalum Oxide thin film deposited by reactive magnetron sputtering

Stainless steel (SS) are extensively used for healthcare, hygiene and surgical applications due to their excellent corrosion resistance and adequate mechanical strength. Among this class SS 316?L is employed most widely, due to highest corrosion resistance, good mechanical properties, resistance to sensitization and ease of fabrication. To incorporate antimicrobial characteristic in SS 316?L based surgical tools a nanocomposite layer comprising of Silver (Ag) and Tantalum oxide (Ta_xO_x) has been deposited by using Physical Vapor Deposition (PVD) magnetron sputtering. Delamination of ceramic layers on SS 316?L substrate is one of the major limitation arising from insufficient crystallization and poor adhesion strength. PVD magnetron sputtering has been employed to develop 5.49?µm thick Ag-Ta_xO_x nanocomposite layer on SS 316?L. Substantially improved adhesion strength has been achieved by controlling thermal treatment. The microstructure, surface and phase analysis of as-sputtered and annealed thin films has been carried out to determine the characteristics of the developed layer. A nanocomposite layer on SS 316?L substrate comprising of Ag and Ta_xO_x has been achieved by releasing O₂ during deposition. Thermal treatment was performed at 300, 400, 500 and 600?°C which progressively increased the crystallinity and segregation of Ag at the surface. Highest adhesion strength was achieved by annealing the coated samples at 400?°C, which exhibited four-fold increased adhesion strength when compared to as-deposited layer. The precipitation of a new phase Silver tantalum oxide (AgTaO₃) was observed for the samples annealed at temperature above 400?°C, which may be responsible for the decrease in adhesion strength.     

Preparation of oxygen gas barrier poly(ethylene terephthalate) films by deposition of silicon oxide films plasma‐polymerized from a mixture of tetramethoxysilane and oxygen

To prepare silicon oxide (SiOx)‐deposited poly(ethylene terephthalate) films with high oxygen gas barrier capability, SiOx deposition by plasma polymerization has been investigated from the viewpoint of chemical composition. Tetramethoxysilane (TMOS) is suitable as a starting material for the synthesis of the SiOx films. The SiOx deposition under self‐bias, where the etching action occurs around an electrode surface, is effective in eliminating carbonaceous compounds from the deposited SiOx films. There is no difference in the chemical composition between the SiOx films deposited under self‐bias and under no self‐bias. The SiOx films are composed of a main component of Si O Si networks and a minor component of carbonized carbons. The SiOx films deposited under no self‐bias from the TMOS/O₂ mixture show good oxygen gas barrier capability, but the SiOx films deposited under the self‐bias show poor capability. The minimum oxygen permeation rate for poly(ethylene terephthalate) films deposited SiOx film is 0.10 cm³ m⁻² day⁻¹ atm⁻¹, which corresponds to an oxygen permeability coefficient of 1.4 × 10⁻¹⁷ cm³‐cm cm⁻² s⁻¹ cm⁻¹ Hg for the SiOx film itself. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 2091–2100, 1999     

Quality enhancement of copper oxide thin film synthesized under elevated gravity acceleration by two-axis spin coating

Two-Axis spin coating as a new modified technique is employed to enhance the quality and surface leveling of thin films. The modified technology utilizes a synthetic centrifugal force perpendicular to the surface which generates an elevated gravity acceleration while spreading the coating on the entire wafer surface. In this paper, copper acetate sol-gel is coated by conventional and Two-Axis spin coating techniques. The coated layers are sintered in an air furnace at 275 °C. The fabricated layers are characterized by GIXRD, EDX, AFM and SEM devices. Wettability and Surface Free Energy (SFE) of sintered films using the contact angle technique are measured, and evaluated by the Owens-Wendt method. XRD and EDX spectra show a higher intensity of copper oxide phase using Two-Axis spin coating technology. AFM micrographs showed an improvement in the surface leveling within the Two-Axis spin coated layer. A comparison between the SFE of conventional and Two-Axis spin coated layers shows an increase in SFE of the layer synthesized under 200g artificial gravity acceleration.     

溶胶-凝胶法制备掺铝氧化锌薄膜及其近红外反射性能研究

采用溶胶-凝胶法制备了掺铝氧化锌(ZAO)薄膜,用X射线衍射(XRD)、紫外-可见光-近红外分光光度计等分析测试手段对薄膜进行了表征;通过正交试验探讨了镀膜层数、溶胶浓度、铝离子的摩尔分数以及退火温度等因素时掺铝氧化锌(ZAO)薄膜近红外反射率的影响,优选了制备具有高近红外反射率的薄膜的工艺参数.研究结果表明,当溶胶浓...     

Effect of post annealing treatment on electrochromic properties of spray deposited niobium oxide thin films

Niobium oxide thin films were deposited on the glass and fluorine doped tin oxide (FTO) coated glass substrates using simple and inexpensive spray pyrolysis technique. During deposition of the films various process parameters like nozzle to substrate distance, spray rate, concentration of sprayed solution were optimized to obtain well adherent and transparent films. The films prepared were further annealed and effect of post annealing on the structural, morphological, optical and electrochromic properties was studied. Structural and morphological characterizations of the films were carried out using scanning electron microscopy, atomic force microscopy and X-ray diffraction techniques. Electrochemical properties of the niobium oxide thin films were studied by using cyclic-voltammetry, chronoamperometry and chronocoulometry.     

High‐performance varistors prepared by hot‐dipping tin oxide thin films in Sb2O3 powder: Influence of temperature

A series of SnO_x–Sb₂O₃ thin film varistors were fabricated through hot‐dipping tin oxide films deposited by radio‐frequency magnetron sputtering in Sb₂O₃ powder at varied temperatures in air. With the increase in hot‐dipping temperature (HDT) from 200°C to 600°C, the nonlinear coefficient (α) of the samples increased first and then decreased, reaching the maximum at 500°C, which was mainly determined by the completeness of high‐resistant Sb₂O₃ layer at tin oxide grain boundary and the chemical composition of tin oxide films. Correspondingly, the leakage current (I_L) decreased first and increased later. The breakdown electric field (E_100 mA) decreased constantly with increasing HDT. The SnO_x–Sb₂O₃ film varistors prepared at 500°C exhibited the optimum nonlinear properties with the maximum α of 10.88, the minimum I_L of 36.3 mA/cm², and an E_100mA of 0.0188 V/nm. The obtained nanoscaled film varistors would be promising in electrical/electronic devices working in low voltage.     

元素成分对磁控溅射TiNi薄膜结构性能的影响及其控制

描述了TiNi形状记忆合金薄膜的一般特性及成分对其组织及性能的重要影响.磁控溅射法是应用最为广泛的制备TiNi基形状记忆薄膜的方法之一,但由于Ti与Ni的溅射产额不同,很难得到理想成分的TiNi薄膜.目前主要采用改变工艺参数或靶材成分补偿的方法控制薄膜的成分.借鉴反应磁控溅射沉积薄膜时成分控制方法,提出了一种利用溅射靶表面光发射谱的控制技术,理论上可以达到精确检测或控制TiNi形状记忆合金薄膜成分的目的.     

Effect of gamma irradiation on structural,morphological and optical properties of thermal spray pyrolysis deposited CuO thin film

This study reports the influences of gamma irradiation (GI) in the range of 20–100 kGy on CuO thin films via thermal spray pyrolysis technique on the glass substrates. The results demonstrate significant influences of GI on the crystallographic, microstructural and optical characteristics of CuO thin films. The obtained XRD results showed that the crystallinity of the films deteriorates by gradually decreasing crystallite size (from 59.13 to 46 nm) as applied gamma doses increases. However, the basic monoclinic crystal structure remains same. The dislocation density and lattice strain increased with the rise of GI absorbed dose due to the creation of defects. The values of number of crystallites per unit surface area increased as dose increased indicating the abundance of crystallization of nano CuO thin films. A UV–Vis–NIR spectrophotometer was utilized to determine the optical properties and obtained results indicated that the optical energy band gap (OBG) energies reduced from 2.00 to 1.72 eV as the doses increased from 0 to 100 kGy. No distinctions of the monoclinic phase of virgin CuO thin film have been perceived under applied absorbed doses, notwithstanding the slight deterioration of the crystallinity and narrowing the OBG.     

The dielectric properties and optical propagation loss of c-axis oriented ZnO thin films deposited by sol–gel process

The c-axis oriented ZnO thin films were prepared on various substrates by sol–gel processes. The stability of solution was examined through solvent and stabilizer. The c-axis orientation and grain size of films were increased with increasing of heat treatment temperature. The optical propogation losses of ZnO films deposited SiO₂/Si(111) substrates were measured using end-coupling method. The losses result in the scattering of the interface of ZnO/SiO₂, and the ZnO grain. Dielectric constant and resistivity of thin films deposited on Pt/SiO₂/Si(111) substrates are, respectively, in the range of 7–13 and 1.7×10⁴9.8×10⁵Ω cm.     

Effect of phosphate ion on the textural and catalytic activity of titania–silica mixed oxide

Phosphate-modified TiO₂-SiO₂ mixed oxide catalysts have been prepared by varying the method of preparation, source and concentration of phosphate ion. The prepared catalysts were compared for their catalytic activity/selectivity in nitration of toluene. The characterisation of the catalysts was performed using X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), thermal analysis (TG–DTA), nitrogen adsorption–desorption methods, surface acid strength measured by Hammett indicator method, surface acid sites measured by amine titration method, and phosphate content measured by UV–VIS spectrophotometry. The XRD patterns revealed that phosphate ion stabilises the anatase phase up to 1173 K activation. FT-IR results show that phosphate species strongly bound bidentately, and that both the internal weakly H-bonded hydroxyl groups and free hydroxyl groups are present on TiO₂–SiO₂ mixed oxide support. Surface area and surface acidity are found to increase with the increase in phosphate loading up to 7.5 wt.% and thereafter the values decrease drastically. However, average pore radius and total pore volume shows the reverse order. Phosphated samples prepared using H₃PO₄ as the source of phosphate ion exhibit higher acidity, and surface area but lower porosity than the samples prepared from (NH₄)₃PO₄, though both the samples contain the same amount of phosphate (7.5 wt.%). Similar results were also observed when varying the method of preparation. TiO₂–SiO₂ samples prepared at pH=3 exhibit higher acidity and surface area but lower porosity than the samples prepared at pH=7. The acid strength of 7.5P/TiO₂–SiO₂ (H) is found to be stronger than that of 100% concentrated H₂SO₄. The material modified with phosphate ion was found to be an efficient and selective catalyst for solvent-free mono-nitration of toluene. Selectivity to the para-product is correlated with the porosity of the material.     

Development of thin‐film composite membranes for carbon dioxide and methane separation using sulfonated poly(phenylene oxide)

Novel membranes based on sulfonated poly (phenylene oxide) (SPPO) was developed. SPPO membranes in the hydrogen form were converted to metal ion forms. The effect of exchange with metal ions including monovalent (Li⁺, Na⁺, K⁺), divalent (Mg²⁺, Ba²⁺, Ca²⁺) and trivalent (Al³⁺) ions was investigated in terms of permeation rate and permeation rate ratios for CO₂ and CH₄ gases. Both dense homogeneous membranes and thin‐film composite (TFC) membranes were studied for their gas separation characteristics. The effect of membrane preparation conditions and operating parameters on the membrane performance were also investigated. The selectivity of the TFC membrane increased as the cationic charge density increased as a result of electrostatic cross‐linking. TFC membrane of very high selectivity was achieved by coating a thin layer of SPPO‐Mg on a PES substrate. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 76: 735–742, 2000