Deposition and characterization of TiAlSiN nanocomposite coatings prepared by reactive pulsed direct current unbalanced magnetron sputtering

This work reports the performance of high speed steel drill bits coated with TiAlSiN nanocomposite coating at different Si contents (5.5-8.1 at.%) prepared using a four-cathode reactive pulsed direct current unbalanced magnetron sputtering system. The surface morphology of the as-deposited coatings was characterized using field emission scanning electron microscopy. The crystallographic structure, chemical composition and bonding structure were evaluated using X-ray diffraction, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, respectively. The corrosion behavior, mechanical properties and thermal stability of TiAlSiN nanocomposite coatings were also studied using potentiodynamic polarization, nanoindentation and Raman spectroscopy, respectively. The TiAlSiN coating thickness was approximately 2.5-2.9 μm. These coatings exhibited a maximum hardness of 38 GPa at a silicon content of approximately 6.9 at.% and were stable in air up to 850 °C. For the performance evaluation, the TiAlSiN coated drills were tested under accelerated machining conditions by drilling a 12 mm thick 304 stainless steel plate. Under dry conditions the uncoated drill bits failed after drilling 50 holes, whereas, TiAlSiN coated drill bits (Si = 5.5 at.%) drilled 714 holes before failure. Results indicated that for TiAlSiN coated drill bits the tool life increased by a factor of more than 14.     

Emission properties of Ti-DLC films prepared by unbalanced magnetron sputtering

The field emission properties of Ti-DLC films in diode and coplanar device structures were studied. An emission current density of 1.14 A/cm² could be obtained at an applied field of 33 V/μm and the threshold field was 24 V/μm for the coplanar emission structure. The silicon substrate was found to limit the emission current in the diode structure because of its high resistivity.     

非平衡磁控溅射法类金刚石薄膜的制备及分析

利用非平衡磁控溅射物理气相沉积技术制备了光滑、致密、均匀的类金刚石薄膜.分析沉积工艺参数对所得类金刚石薄膜的电学特性的影响以及溅射粒子的大小、能量、碰撞及沉积过程中的相变机理后认为：溅射粒子越小、与环境气体分子的碰撞次数越多、与衬底相互作用时具有适当动量等，能够有效提高薄膜中sp^３杂化碳原子的含量.利用拉曼光谱 、纳米力学探针、红外光谱、扫描电镜等分析了所得类金刚石膜的结构、力学及光学性能、 表面形貌等特征.结果表明，类金刚石膜中sp^３杂化碳原子的含量较高，显微硬 度大于11GPa，薄膜光学透过率达到89.4％，折射系数为1.952，沉积速率为0.724μm/h，表 面光滑、致密、均匀，不存在明显的晶粒特征. 关键词： 非平衡磁控溅射 类金刚石膜 拉曼光谱 红外光谱     

Growth characteristics and properties of ZnO:Ga thin films prepared by pulsed DC magnetron sputtering

Transparent conductive ZnO:Ga thin films were deposited on Corning 1737 glass substrate by pulsed direct current (DC) magnetron sputtering. The effects of process parameters, namely pulse frequency and film thickness on the structural and optoelectronic properties of ZnO:Ga thin films are evaluated. It shows that highly c-axis (0 0 2) oriented polycrystalline films with good visible transparency and electrical conductivity were prepared at a pulsed frequency of 10 kHz. Increasing the film thickness also enlarged the grain size and carrier mobility which will subsequently lead to the decrease in resistivity. In summary, ZnO:Ga thin film with the lowest electrical resistivity of 2.01 × 10⁻⁴ Ω cm was obtained at a pulse frequency of 10 kHz with 500 nm in thickness. The surface RMS (root mean square) roughness of the film is 2.9 nm with visible transmittance around 86% and optical band gap of 3.83 eV.     

Magnetic properties of Er-doped ZnO films prepared by reactive magnetron sputtering

All Zn_1−x Er _x O (x=0.04, 0.05, and 0.17) films deposited on glass substrates by radio-frequency reactive magnetron sputtering exhibit the mixture of ferromagnetic and paramagnetic phases at room temperature. The estimated magnetic moment per Er ion decreases with the increase of Er concentration. The temperature dependence of the magnetization indicates that there is no intermetallic ErZn buried in the films. The ferromagnetism is attributed to the Er ions substitution for Zn²⁺ in ZnO lattices, and it can be interpreted by the bound-magnetic-polaron model.     

Kinetic properties of TiN thin films prepared by reactive magnetron sputtering

Results of investigations of kinetic properties of TiN thin films prepared by dc reactive magnetron sputtering are presented. It is established that the TiN thin films are polycrystalline and possess semiconductor n-type conduction. The carrier concentration is ～10²² cm^?3, while electron scattering occurs at ionized titanium atoms.     

Nanolayered multilayer coatings of CrN/CrAlN prepared by reactive DC magnetron sputtering

Single-phase CrN and CrAlN coatings were deposited on silicon and mild steel substrates using a reactive DC magnetron sputtering system. The structural characterization of the coatings was done using X-ray diffraction (XRD). The XRD data showed that both the CrN and CrAlN coatings exhibited B1 NaCl structure with a prominent reflection along (2 0 0) plane. The bonding structure of the coatings was characterized by X-ray photoelectron spectroscopy and the surface morphology of the coatings was studied using atomic force microscopy. Subsequently, nanolayered CrN/CrAlN multilayer coatings with a total thickness of approximately 1 μm were deposited on silicon substrates at different modulation wavelengths (Λ). The XRD data showed that all the multilayer coatings were textured along {2 0 0}. The CrN/CrAlN multilayer coatings exhibited a maximum nanoindentation hardness of 3125 kg/mm² at a modulation wavelength of 72 Å, whereas single layer CrN and CrAlN deposited under similar conditions exhibited hardness values of 2375 and 2800 kg/mm², respectively. Structural changes as a result of heating of the multilayer coatings in air (400-800 °C) were characterized using XRD and micro-Raman spectroscopy. The XRD data showed that the multilayer coatings were stable up to a temperature of 650 °C and peaks pertaining to Cr₂O₃ started appearing at 700 °C. These results were confirmed by micro-Raman spectroscopy. Nanoindentation measurements performed on the heat-treated coatings revealed that the multilayer coatings retained hardness as high as 2250 kg/mm² after annealing up to a temperature of 600 °C.     

Electrical and optical properties of silver doped indium oxide thin films prepared by reactive DC magnetron sputtering

Silver doped indium oxide (In_2−x Ag_x O_3−y) thin films have been prepared on glass and silicon substrates at room temperature (300 K) by reactive DC magnetron sputtering technique using an alloy target of pure indium and silver (80: 20 atomic %. The magnetron power (and hence the metal atom sputter flux) is varied in the range 40-80 W. The energy dispersive analysis of X-ray (EDAX) results show that the silver content in the film decreases with increasing magnetron power. The grain size of these films is of the order of 100 nm. The resistivity of these films is in the range 10⁻²-10⁻³ Ω cm. The work function of the silver-indium oxide films (by Kelvin Probe) are in the range: 4.64-4.55 eV. The refractive index of these films (at 632.8 nm) varies in the range: 1.141-1.195. The optical band gap of indium oxide (3.75 eV) shrinks with silver doping. Calculations of the partial ionic charge (by Sanderson's theory) show that silver doping in indium oxide thin films enhance the ionicity.     

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用线圈电流控制非平衡磁场,用汤森放电击穿形成深度自触发放电,用磁阱捕获放电形成的二次电子和导致漂移电流,形成了高功率非平衡磁控溅射放电。采用偏压为-100V相对磁控靶放置的圆形平面电极收集饱和离子电流;在距离磁控靶14cm的位置由Langmuir探针测量浮置电位;示波器测量磁控靶的脉冲电压、电流、浮置电位和饱和离子电流信号。装置的放电脉冲功率达到0.9MW,脉冲频率最大值为40Hz左右,空间电荷限制条件是控制电子电流和离子电流的主要机制。     

高功率脉冲非平衡磁控溅射放电特性和参数研究

用线圈电流控制非平衡磁场,用汤森放电击穿形成深度自触发放电,用磁阱捕获放电形成的二次电子和导致漂移电流,形成了高功率非平衡磁控溅射放电。采用偏压为-100V相对磁控靶放置的圆形平面电极收集饱和离子电流;在距离磁控靶14cm的位置由Langmuir探针测量浮置电位;示波器测量磁控靶的脉冲电压、电流、浮置电位和饱和离子电流信号。装置的放电脉冲功率达到0.9MW,脉冲频率最大值为40Hz左右,空间电荷限制条件是控制电子电流和离子电流的主要机制。     

直流磁控溅射制备氧化钒薄膜

讨论了在低温下以高纯金属钒作靶材,用直流磁控溅射的方法制备出了氧化钒薄膜。通过设计正交试验,分析了氩气和氧气的流量比,溅射功率,工作压强,基底温度对氧化钒薄膜沉积速率和电阻温度系数TCR的影响,采用RTP-500型快速热处理机对氧化钒薄膜样品进行了退火热处理,实验结果表明:当Ar与O2的比例为100:4,溅射功率为120W,工作压强为2Pa时,所获得薄膜TCR较大,都在-2%/K附近,最高的可达-3.6%/K。     

Transparent conductive ZnO:Ga films prepared by DC reactive magnetron sputtering at low temperature

Ga-doped ZnO (ZnO:Ga) transparent conductive films were deposited on glass substrates by DC reactive magnetron sputtering. The structural, electrical, and optical properties of ZnO:Ga films were investigated in a wide temperature range from room temperature up to 400 °C. The crystallinity and surface morphology of the films are strongly dependent on the growth temperatures, which in turn exert an influence on the electrical and optical properties of the ZnO:Ga films. The film deposited at 350 °C exhibited the relatively well crystallinity and the lowest resistivity of 3.4 × 10⁻⁴ Ω cm. More importantly, the low-resistance and high-transmittance ZnO:Ga films were also obtained at a low temperature of 150 °C by changing the sputtering powers, having acceptable properties for application as transparent conductive electrodes in LCDs and solar cells.     

Study of microstructure and nanomechanical properties of Zr films prepared by pulsed magnetron sputtering

The present work studies the effect of substrate temperature on the growth characteristics of zirconium films prepared by pulsed magnetron sputtering. Formation of α-phase of zirconium was observed in the temperature range 300-873 K. X-ray diffraction of Zr films revealed predominantly [0 0 1] texture. It is noticed that crystallite size increases with increasing substrate temperature. Hexagonal shaped crystallites seem to grow along the surface normal of the substrate for the films deposited at 773 K. Nanoindentation measurements showed that the hardness of the films is in the range 6-10 GPa. The scratch test indicated that the films deposited at higher substrate temperatures had excellent bonding with the substrate and no significant critical failure was noticed up to an applied load of 20 N.     

磁控反应溅射法制备渐变折射率薄膜的模型分析

阐述了磁控反应溅射法制备渐变折射率薄膜的机理;探讨了磁控反应溅射法制备渐变折射率薄膜的理论模型,给出了渐变折射率薄膜的折射率与反应气体分压的关系,在一定的沉积参数下,由要得到的膜层折射率随膜层几何厚度的变化规律可推导出反应气体分压比随时间的变化规律;最后以制备折射率线性变化的薄膜为例说明了如何推导得到反应气体分压比随时间的变化规律. 关键词： 渐变折射率 磁控反应溅射 模型     

Structural and optical properties of the SiCN thin films prepared by reactive magnetron sputtering

Silicon carbonitride (SiCN) thin films were deposited on n-type Si (1 0 0) and glass substrates by reactive magnetron sputtering of a polycrystalline silicon target in a mixture of argon (Ar), nitrogen (N₂) and acetylene (C₂H₂). The properties of the films were characterized by scanning electron microscope with an energy dispersive spectrometer, X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectrometry and ultraviolet-visible spectrophotometer. The results show that the C₂H₂ flow rate plays an important role in the composition, structural and optical properties of the films. The films have an even surface and an amorphous structure. With the increase of C₂H₂ flow rate, the C content gradually increases while Si and N contents have a tendency to decrease in the SiCN films, and the optical band gap of the films monotonically decreases. The main bonds are Si-O, N-H_n, C-C, C-N, Si-N, Si-C and Si-H in the SiCN films while the chemical bonding network of Si-O, C-C, C-O, C-N, N-Si and CN is formed in the surface of the SiCN films.     

射频反应磁控溅射法制备的氟化类金刚石薄膜摩擦特性研究

以高纯石墨做靶,CHF3和Ar气为源气体,采用射频反应磁控溅射法在不同流量比条件下制备了氟化类金刚石(F-DLC)薄膜.利用原子力显微镜、纳米压痕仪、拉曼光谱和红外光谱、摩擦磨损测试仪对薄膜的表面形貌、硬度、键结构以及摩擦性能做了具体分析.表面形貌测试结果表明,制备的薄膜整体均匀致密,表现出了良好的减摩性能.当CHF3与Ar气流量比r为1:6时,所得薄膜的摩擦系数减小至0.42,而纳米压痕结果显示,此时薄膜的硬度也最高.拉曼和红外光谱显示,随着r的增加,薄膜中的F浓度呈上升趋势,薄膜中的芳香环比例减小.研究表明,F原子的键入方式是影响F-DLC薄膜摩擦系数的一个重要因素,CF2反对称伸缩振动强度的减弱和CC中适量碳氢氟键的形成都能导致薄膜具有相对较低的摩擦系数.     

Cu-In-O composite thin films deposited by reactive DC magnetron sputtering

Cu-In-O composite thin films were deposited by reactive DC magnetron sputtering at room temperature. The samples were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), UV/vis spectrophotometer, four-probe measurement and Seebeck effect measurement, etc. The samples contain Cu, In and O. The ratios of Cu to In and O to In increase with increase in O₂ flow rates. The ratio of Cu to In is over 1 and this suggests that Cu is in excess. The obtained Cu-In-O thin films are very possibly made of rhombohedral In₂O₃ and monoclinic CuO. Transmittance of the films decreases with increase in O₂ flow rate. The decrease in transmittance results from increase in Cu content in the films. The optical band gap of all the samples is estimated to be 4.1-4.4 eV, which is larger than those of In₂O₃ and CuO. The sheet resistance of the films decreases with increase in O₂ flow rate. Conductivity of the films is a little low, due to the addition of Cu and the poor crystalline quality of the film. The conduction behavior of the films is similar to that of In₂O₃ and the conduction mechanism of Cu-In-O thin films is through O vacancy.     

Pulsed DC magnetron sputtering of transparent conductive oxide layers

A comprehensive material study of different transparent conductive oxides （TCOs） is presented. The layers are deposited by pulsed direct current （DC） magnetron sputtering in an inline sputtering system. Indium tin oxide （ITO） films are studied in detail. The optimum pressure of 0.33 Pa （15Ar：202） produces a 300- nm thin film with a specific resistivity p of 2.2 × 10-6 Ωm and a visual transmittance of 81%. Alternatively, ZnO：A1 and ZnO：Ga layers with thicknesses of 200 and 250 nm are deposited with a minimum resistivity of 5.5× 10-6 and 6.8× 10-6Ωm, respectively. To compare the optical properties in the ultraviolet （UV） range, the optical spectra are modeled and the band gap is determined.     

Hydrogenation of Pd-capped Mg thin films prepared by DC magnetron sputtering

Structural and optical properties of pure Mg thin film coated with Pd have been investigated. Pd-capped Mg thin films had been prepared by DC magnetron sputtering. This work presents an ex situ study on hydrogenation and dehydrogenation kinetics of Pd/Mg films at different conditions using XRD, AFM and optical spectrophotometer. We have succeeded to load thin films of Mg to MgH₂ at normal temperature and normal pressure of hydrogen gas. In hydrogenation, α-MgH₂ phase of magnesium hydride was observed in hydrogenated films at 200 °C and γ-MgH₂ at 250 °C respectively. The desorption kinetics in vacuum also revealed the phase transformation α-MgH₂ to γ-MgH₂. A reflectance change was observed in hydrogenated films in comparison of as deposited thin film. Hydrogenated (H loaded) samples were observed partially transparent in comparison of as deposited.