离子轰击对致密T区结构Cr薄膜残余应力的影响

对于能量沉积技术,离子轰击是独立于晶粒尺寸之外影响残余应力的重要因素,沉积束流能量和通量是决定残余应力演化的关键参数。本文分别采用高功率调制脉冲磁控溅射 (Modulated Pulsed Power magnetron sputtering, MPPMS) 和高功率深振荡磁控溅射 (Deep Oscillation magnetron sputtering, DOMS) 控制沉积Cr薄膜的束流能量和通量,在相近的平均功率下调节微脉冲参数对峰值电流和峰值电压进行控制,进而实现离子轰击对本征残余应力控制。MPPMS和DOMS沉积的Cr薄膜厚度分别控制在 0.1、0.2、0.5、1.0、1.5 和 3.0 μm,并对残余应力进行对比研究。所有沉积的Cr薄膜均呈现 Cr(110) 择优取向,且形成了晶粒尺寸相当的致密T区结构。较之MPPMS,DOMS沉积Cr薄膜更呈现残余压应力特征。当Cr薄膜小于0.5 μm时,DOMS沉积Cr薄膜的残余应力表现出较高的压应力;进一步增加膜厚,残余应力逐渐受残余拉应力控制。在薄膜生长过程中,离子轰击在薄膜生长初期对残余应力贡献不大,当薄膜生长较厚时,离子能量对薄膜残余应力影响明显。离子能量是影响残余压应力形成的重要因素,高能量离子轰击有利于残余压应力的形成和控制。     

等离子体增强磁控溅射制备Ti(Cr)SiC(O)N涂层的结构和机械性能研究

采用等离子体增强磁控溅射(PEMS)方法分别在硬质合金和硅片上制备了TiSiCN, TiSiCON, TiCrSiCN, TiCrSiCON, CrSiCN 和 CrSiCON涂层。采用XRD、SEM、EDS、显微硬度计及销盘式摩擦磨损试验机对含氧涂层和不含氧涂层的微观结构、成分和机械性能进行了研究。研究结果表明,TiSiCON, TiCrSiCON和 CrSiCON含氧涂层为TiN型（或CrN型）面心立方(fcc)结构,但是TiSiCON, TiCrSiCON, 和 CrSiCON涂层中氧的存在会导致产生疏松的结构以及相比于不含氧涂层TiSiCN, TiCrSiCN和CrSiCN更多的缺陷;氧的加入会导致Ti(Cr)SiCN涂层硬度和弹性的下降;TiCrSiCON和 CrSiCON两种含氧涂层相比于不含氧涂层TiCrSiCN和CrSiCN有更低的摩擦系数和磨损率;然而,TiSiCON相比于TiSiCN却表现出更高的摩擦系数和磨损率。     

Nd-Fe-B薄膜的磁控溅射法制备与组织结构

对直流磁控溅射法制备Nd-Fe-B薄膜工艺进行了研究.在不同的溅射功率、溅射气压、溅射时间等条件下制备薄膜,并对薄膜进行了AFM、XRD分析.结果表明,Nd-Fe-B薄膜的沉积速率、表面形貌及相结构与溅射功率、溅射气压、溅射时间密切相关.薄膜的沉积速率随磁控溅射功率的增加而增加,薄膜表面晶粒尺寸和表面粗糙度随溅射功率增加而增大.沉积速率随溅射气压的升高先增大后减小.低功率溅射时,薄膜中出现α-Fe、Nd2Fe14B相相对较少,随溅射功率增加,α-Fe相消失,Nd2Fe14B相增多.综合考虑各种因素,最佳溅射功率为100～130 W.     

Effect of the PbOx thickness on the microstructure and electrical properties of PLT thin films prepared by RF magnetron sputtering

The (Pb_0.90La_0.10)Ti_0.975O₃ (PLT) thin films with different thicknesses of PbO_x buffer layers were deposited on the Pt(111)/Ti/SiO₂/Si(100) substrates by RF magnetron sputtering technique. The PbO_x buffer layer leads to the (100) orientation of the PLT thin films. Effects of the PbO_x thickness on the microstructure and electrical properties of the PLT thin films were investigated. The experimental results show that the PbO_x thickness plays an important role on the orientation, phase purity, domain structure, and electrical properties of the PLT thin films. The PLT thin films with proper PbO_x thickness possess highly (100) orientation, high phase purity, strong intensity of out of plane polarization, and good electrical properties. It is concluded that the PbO_x thickness between PLT thin films and Pt coated Si substrate is very critical to obtain good electrical properties.     

磁控溅射沉积W-Ti薄膜的结构与性能

采用复合靶磁控共溅射方法在p型(100)单晶硅衬底上制备了不同Ti含量的W-Ti薄膜,并与纯W和纯Ti薄膜作对比。采用XRD、SEM、AFM、显微硬度计和四探针电阻仪对薄膜的结构、成分及性能进行分析表征。结果表明,W-Ti薄膜呈细晶粒多晶结构,Ti含量较低时,W-Ti薄膜呈体心立方相结构,存在W基W(Ti)固溶体。Ti含量较高时,还出现hcp富Ti相。W-Ti薄膜的显微硬度随Ti含量的增加先增后减,而电阻率则随Ti含量的增加而增大。W-Ti薄膜显微硬度均高于纯Ti薄膜,电阻率则高于纯W而低于纯Ti薄膜。     

退火处理对不同RF功率下制备ZnO薄膜的结晶性能的影响

采用RF磁控溅射法,在不同溅射功率下在玻璃衬底上制备了ZnO薄膜,并对所制备的ZnO薄膜在空气气氛中进行了不同温度（350-600℃）的退火处理.利用X射线衍射仪（XRD）、扫描电子显微镜（SEM）等研究了退火对不同溅射功率条件下制备的ZnO薄膜晶体性能和应力状态的影响.研究表明,在衬底没有预热的情况下,较低功率（190W）下制备的ZnO薄膜,当退火温度为500℃时,能获得单一c轴择优取向和最小半高宽,张应力在350℃退火时最小;较高功率（270W）下,薄膜最佳c轴取向和晶粒度在600℃退火温度获得,张应力最小的退火温度在350-500℃之间.当衬底预热至300℃时,退火处理对两种功率下制备的薄膜的结晶性能和应力的影响基本一致.     

溅射沉积Cu-Mo薄膜的结构和性能

用磁控溅射法制备含钼2.19%～35.15%(摩尔分数)的Cu-Mo合金薄膜,运用能谱仪(EDX)、X射线衍射仪(XRD)、透射电镜(TEM)、扫描电镜(SEM)、显微硬度仪和电阻计对薄膜成分、结构和性能进行研究.结果表明Mo添加使Cu-Mo薄膜晶粒显著细化,Cu-Mo膜呈纳米晶结构,存在Mo在Cu中的FCCCu(Mo)非平衡亚稳过饱和固溶体;随Mo含量的增加,Mo固溶度逐渐增加,而薄膜微晶体尺寸则逐渐减小,Mo的最大固溶度为30.6%.与纯Cu膜对比表明,Cu-Mo膜的显微硬度和电阻率随Mo含量的上升而持续增加.经200、400和650℃热处理1h后,Cu-Mo膜的显微硬度和电阻率均降低,降幅与热处理温度呈正相关;经650℃退火后,Cu-Mo膜基体相晶粒长大,并出现亚微米-微米级富Cu第二相.在Cu-Mo膜的XRD谱中观察到Mo(110)特征峰,Cu-Mo薄膜结构和性能形成及演变的主要原因是添加Mo引起的晶粒细化效应以及热处理中基体相晶粒的生长.     

磁控溅射法制备SnS薄膜的结构和光学性能

利用磁控溅射法在FTO玻璃上制备了Sn S薄膜。采用X射线衍射仪、扫描电子显微镜和紫外可见分光光度计对不同溅射参数下制备的Sn S薄膜的晶体结构、表面形貌和光学性能进行研究,确定出制备Sn S薄膜的最优溅射参数。结果表明:溅射功率为28 W,沉积气压在2.5 Pa时,制备出的Sn S薄膜在(111)晶面具有最好的择优取向,薄膜微观形貌呈单片树叶状,晶粒粒径约370 nm,晶粒分布均匀,薄膜表面光滑致密;最优溅射参数下制备的Sn S薄膜的吸收系数可达到105cm-1,比其他方法制备的Sn S薄膜的吸收系数值高,禁带宽度为1.48 e V,与半导体太阳能电池所要求的最佳禁带宽度(1.5 e V)十分接近。     

Effects of processing parameters on the properties of tantalum nitride thin films deposited by reactive sputtering

The effects of processing parameters on the properties of tantalum nitride thin films deposited by radio frequency reactive sputtering have been investigated. The influence of the N₂ partial and (Ar + N₂) total gas pressures as well as the sputtering power on the microstructure and electrical properties is reported. Rising the N₂ partial pressure, from 2 to 10.7%, induces a change in the composition of the δ-TaN phase, from TaN to TaN_1.13. This composition change is associated with a drastic increase of the electrical resistivity over a 7.3% N₂ partial pressure. The total gas pressure is revealed to strongly affect the film microstructure since a variation in both composition and grain size is observed when the gas pressure rises from 6.8 to 24.6 Pa. When the sputtering power varied between 50 and 110 W, an increase of the grain size related to a decrease of the electrical resistivity is observed.     

Synthesis and high temperature XRD studies of tantalum nitride thin films prepared by reactive pulsed dc magnetron sputtering

In the present work, the growth characteristics of tantalum nitride (TaN) thin films prepared on (1 0 0) Si substrates by reactive pulsed DC magnetron sputtering are investigated. XRD analyses indicated the presence of α-Ta and β-Ta in the films deposited in pure argon atmosphere, while β-TaN and fcc-TaN phases appeared for 2 sccm of nitrogen, and cubic TaN for 5-25 sccm of nitrogen in the sputtering gas mixture of argon and nitrogen at a substrate temperature of 773 K. The TaN films obtained with increasing substrate temperature and pulse width showed a change in the texture from [1 1 1] to [2 0 0] orientation. Atomic force microscopy (AFM) results indicated that the average surface roughness was low for films deposited in pure argon than for the films deposited in a mixed Ar + N₂ atmosphere. Nanocrystalline phase of the deposited material was identified from the high-resolution transmission electron microscopy (HRTEM) images. X-ray photoelectron spectroscopy (XPS) core level spectra confirmed the formation of TaN phase. The high temperature X-ray diffraction analysis of the optimized TaN thin film was performed in the temperature range 298-1473 K. The lattice parameter of the TaN films was found to increase from 4.383 to 4.393 Å on increasing the temperature from 298 to 823 K and it reduced to 4.345 Å at 1473 K. The thermal expansion coefficient value was found to be negative for the TaN films.     

Conductive and transparent Bi-doped ZnO thin films prepared by rf magnetron sputtering

Bi-doped ZnO thin films were grown on glass substrates by ratio frequency (rf) magnetron sputtering technique and followed by annealing at 400 °C for 4 h in vacuum (~ 10^− 1 Pa). The effect of argon pressure on the structural, optical, and electrical properties of the Bi-doped films were investigated. The XRD patterns show that the thin films were highly textured along the c-axis and perpendicular to the surface of the substrate. Some excellent properties, such as high transmittance (about 85%) in visible region, low resistivity value of 1.89 × 10^− 3 W cm and high carrier density of 3.45 × 10²⁰ cm^− 3 were obtained for the film deposited at the argon pressure of 2.0 Pa. The optical band gap of the films was found to increase from 3.08 to 3.29 eV as deposition pressure increased from 1 to 3 Pa. The effects of post-annealing treatments had been considered. In spite of its low conductivity comparing with other TCOs, Bi-doping didn't appreciably affect the optical transparency in the visible range of ZnO thin films.     

Measuring residual stresses in linear friction welded joints composed by dissimilar titanium

The Ti–5Al–2Sn–2Zr–4Mo–4Cr (Ti17) titanium alloy is the main material used in manufacturing blades and disks of aero engines, and it is always jointed with different microstructures for the design constraints. In this work, the residual stresses of linear friction welding of β Ti17 and α?+?β Ti17 are measured by contour method and the X-ray diffraction method. The welding-induced tensions were found to be greater on the β side than that on the α?+?β side, and had an obvious reduction in the weld centre. After the post weld heat treatment (PWHT) of 630°C for 3?h, all tensions on the β side relax to a very limited value while some new PWHT-induced compressions are found on the α?+?β side.     

Sensitivity to humidity of TiO2 thin films obtained by reactive magnetron sputtering

This study presents results on the humidity-sensing properties of titanium dioxide thin films measured by a quartz microbalance. A novel two-layer structure, consisting of a polymer sub-layer and a sensing titanium dioxide layer, was fabricated on a quartz resonator. The polymer sub-layer was synthesized by a plasma process from hexamethyldisiloxane to protect the resonator's surface during the deposition of the titanium dioxide film by magnetron sputtering. The TiO₂ films were characterized by X-ray diffraction and Auger Electron Spectroscopy. The film composition was determined to be close to that of stoichiometric TiO₂. The sensitivity to humidity varied from 5 Hz/%RH to 7 Hz/%RH for TiO₂ film thickness lying in the range of 18-70 nm. An increase of film thickness in this interval led to a slight decrease in sensitivity, which is explained by water sorption occurring principally at the surface of the titanium dioxide film and a change of the morphology to a higher surface smoothness for thicker films. It was found that 30-60 min of sorption time is necessary to completely eliminate hysteresis, which suggests that the process is reversible.These results are promising for the development of sensor devices for measuring the relative humidity of air.     

Preparation of epitaxial and polycrystalline bismuth titanate thin films on single crystal (100) MgO by chemical solution deposition

Epitaxial and polycrystalline Bi₄Ti₃O₁₂ thin films were prepared on single crystal (100) MgO substrates by a chemical solution deposition process using metal naphthenates as starting materials. Pyrolyzed films (at 500°C) were annealed for 30 min in air at 650, 700, 750 and 800°C, respectively. The effects of annealing temperature on the crystallinity, epitaxy and surface morphology of the films were investigated by X-ray diffraction θ-2θ scans, pole-figure analysis, and atomic force microscopy (AFM). Epitaxially grown films annealed at 700 and 750°C, respectively, showed growth of three-dimensional needle-shaped grains. During annealing at 800°C, grain growth of Bi₄Ti₃O₁₂ may be suppressed by the formation of a titanium-rich phase such as Bi₂Ti₂O₇ owing to Bi volatilization, resulting in lower root mean square roughness than that of film annealed at 750°C.     

X-ray diffraction measurement of residual stress and crystal orientation in Au/NiCr/Ta films prepared by plating

Au/NiCr/Ta films were prepared by plating and then annealed at 400 °C in Ar gas for an hour. The Au diffraction peak positions including incidence angles 0°, 15°, 30°, and 45° were measured by a glancing incidence X-ray diffraction (GIXRD) method. Residual stresses were then calculated using the sin²ψ method. The results indicate that the residual stress in the as-deposited Au/NiCr/Ta films was about 50 MPa, but was decreased down to − 5 MPa in average after samples annealing. The XRD analysis on crystal orientation shows that only the diffraction peaks of Au were found. There are no alloying phases in the plating Au film, and the interlayer of NiCr and Ta is too thin to be detected by the conventional XRD. The XRD also revealed that the films are highly textured with Au-(111) or a mixture of Au-(111) and Au-(200) orientation, and the (111)/(200) intensity ratio decreases after samples annealed.     

Origins of microstructure and stress gradients in nanocrystalline thin films: The role of growth parameters and self-organization

The development of depth gradients of texture, morphology and stresses in thin nanocrystalline films was experimentally demonstrated for a nanocrystalline CrN film by means of position-resolved synchrotron X-ray nanodiffraction and explained by atomistic processes at the growing film surface and the effect of interfaces, both controlled by the deposition conditions. Controllable changes in the energy of incident particles adjusted by bias voltages ranging from ?40 to ?120 V affect the competitive growth of grains with different orientations, induce disruption of grain growth and thus give rise to structural variations across the film thickness. Subsequent changes in the volume fraction of grain boundaries and film texture were found to be responsible for changes in the residual stress state as defect generation proceeds to different extents in the interior of differently oriented grains and in the interfacial area. While the defect density predominantly affects the development of intrinsic stress, the variation in the number of weakly bonded atoms of grain boundaries determines the thermal stress component. The structural dependence of both stress components thus contributes to the characteristic development of stress gradients in thin nanocrystalline films.     

Effect of bias voltage on microstructure and properties of Ti-doped graphite-like carbon films synthesized by magnetron sputtering

Ti-doped graphite-like carbon (GLC) films with different microstructures and compositions were fabricated using magnetron sputtering technique. The influence of bias voltages on microstructure, hardness, internal stress, adhesion strength and tribological properties of the as-deposited GLC films were systemically investigated. The results showed that with increasing bias voltage, the graphite-like structure component (sp² bond) in the GLC films increased, and the films gradually became much smoother and denser. The nanohardness and compressive internal stress increased significantly with the increase of bias voltage up to −300 V and were constant after −400 V. GLC films deposited with bias voltages in the range of -300--400 V exhibited optimum adhesion strength with the substrates. Both the friction coefficients and the wear rates of GLC films in ambient air and water decreased with increasing voltages in the lower bias range (0--300 V), however, they were constant for higher bias values (beyond −300 V) . In addition, the wear rate of GLC films under water-lubricated condition was significantly higher for voltages below −300 V but lower at high voltage than that under dry friction condition. The excellent tribological performance of Ti-doped GLC films prepared at higher bias voltages of −300--400 V are attributed to their high hardness, tribo-induced lubricating top-layers and planar (2D) graphite-like structure.     

CVD掺硅金刚石残余应力的X射线衍射和拉曼光谱分析(英文)

采用X射线衍射(XRD)和拉曼光谱2种方法测量了不同硅碳比的CVD掺硅金刚石薄膜的残余应力。采用偏压增强热丝化学气相沉积装置在硬质合金基底上制备了掺硅金刚石薄膜,将正硅酸乙酯以不同的体积比溶解在丙酮中以使得反应气体中的硅碳比从0.1%变化到1.4%,从而控制掺硅金刚石薄膜的掺杂浓度。SEM和XRD的表征结果显示,随着硅掺杂浓度的增加,金刚石薄膜的晶粒尺寸减小,而金刚石(110)的晶面则逐渐占优。XRD法是测量入射角从0°到45°变化时对应的金刚石(220)面XRD衍射峰,并采用sin2ψ方法计算掺硅金刚石薄膜的残余应力。拉曼谱法则是通过检测金刚石特征峰偏移1332cm1位置的偏移量来测量残余应力。2种方法测得的残余应力随着硅掺杂含量的升高显示出良好的一致性,所有的硅掺杂金刚石的残余应力均为压应力,Si/C摩尔比为0.1%的薄膜具有最高的残余应力,为~1.75GPa(拉曼谱法)或~2.3GPa(XRD法)。随着硅掺杂浓度的进一步升高,薄膜的残余应力则稳定在~1.3GPa左右。     

Substrates effect on Zn1−xMnxO thin films grown by RF magnetron sputtering

In this paper, we have presented the surface effect of the substrates on Mn doped ZnO (Zn_1−xMn_xO) thin films grown on Si(1 0 0) and sapphire [i.e. Al₂O₃(0 0 0 1)] by RF magnetron sputtering. These grown films have been characterized by X-ray diffraction (XRD), photoluminescence (PL) and vibrating sample magnetometer (VSM) to know its structural, optical and magnetic properties. All these properties have been found to be strongly influenced by the substrate surface on which the films have been deposited. The XRD results show that the Mn doped ZnO films deposited on Si(1 0 0) exhibit a polycrystalline nature whereas the films on sapphire substrate have only (0 0 2) preferential orientations indicating that the films are single crystalline. The studies of room temperature PL spectra reveal that the Zn_1−xMn_xO/Si(1 0 0) system is under severe compressive strain while the strain is almost relaxed in Zn_1−xMn_xO/Al₂O₃(0 0 0 1) system. It has been observed from VSM studies that Zn_1−xMn_xO/Al₂O₃(0 0 0 1) system shows ferromagnetic nature while the paramagnetic behaviour observed in Zn_1−xMn_xO/Si(1 0 0) system.     

MmM5/Mg multi-layer hydrogen storage thin films prepared by dc magnetron sputtering

MmNi_3.5(CoAlMn)_1.5/Mg (here Mm denoted for mischmetal) multi-layer thin films were deposited on (0 0 1) Si substrate by direct current (dc) magnetron sputtering with dual-target. X-ray diffraction (XRD) and scanning electron microscopy analysis revealed that the microstructure of the MmNi_3.5(CoAlMn)_1.5 layer is amorphous and/or nanocrystalline and that the microstructure of the Mg layer is fine grained crystalline with preferential orientation. Phase analysis of hydrogenated and dehydrogenated MmNi_3.5(CoAlMn)_1.5/Mg multi-layer thin films proved that an apparent absorption of hydrogen in the Mg layer occurs at temperatures higher than 200 °C and that the hydrogen absorbed can be fully released at 250 °C.