温度对溶剂热改性C/C复合材料显微结构和氧化性能的影响

以硼酸三正丁酯、乙酸、B2O3粉体为原料,无水乙醇为溶剂,采用一种新颖的溶胶/凝胶结合溶剂热法对C/C复合材料基体进行了抗氧化改性.采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、能量色散谱仪(EDS)及X射线光电子能谱(XPS)对改性后试样进行了表征.重点研究了溶剂热反应温度对改性后试样的物相组成、微观结构和氧化性能的影响.结果表明:经过溶剂热改性处理后,C/C复合材料表面缺陷被玻璃相B2O3组成的涂层所覆盖,材料内部一部分孔隙也被B2O3相填充,且随着溶剂热温度的上升,试样表面的微裂纹逐渐消失,B2O3涂层的致密度上升;C/C基体的抗氧化性能随着溶剂热改性温度(范围353～433 K)的升高而提高;经433 K溶剂热改性后的C/C复合材料在873 K的空气中氧化16 h后的质量损失仅为4.09％.     

Preparation and Microstructure of Highly-Oriented LaNiO_3 Thin Films by RF Sputtering Method

In an attempt of being used as buffer layers and electrodes for the textured BaTiO3 (BTO) ferroelectric thin films, highly (100)-oriented LaNiO3 (LNO) thin films of different thicknesses were deposited directly on Si (100) substrate with radio-frequency (RF) magnetron sputtering method. It is observed that the substrate temperatures and the film thicknesses bring main influences on the micro-structures and orientation of the thin film. The effects of the thicknesses and substrate temperatures on the orientation of the films were studied on the LNO films of different thicknesses. The highly (100)-oriented LNO thin films were obtained at the substrate temperature of 600 ℃. The existence of epitaxially grown BTO films indicates that the oriented LNO thin films obtained in this work could be used as a buffer layer for epitaxial growth.     

特种材料表面镀TiN薄膜的结构与应力研究

本文采用多弧离子镀技术在特种材料表面制备TiN薄膜。利用扫描电镜和X射线衍射仪对TiN薄膜的形貌、成分结构、残余应力进行研究,结果表明：薄膜表面粗糙度较大;薄膜由TiN单相组成,以（111）晶面为主;TiN薄膜存在较大残余压应力,经过保温热处理后,薄膜的残余应力显著下降。     

工艺参数对2A12铝合金微弧氧化陶瓷层生长的影响

研究了正／负向电流密度、频率和正／负向占空比对铝合金微弧氧化陶瓷层生长的影响,采用扫描电子显微镜（SEM）和X射线衍射仪（XRD）,分析了不同氧化时间陶瓷层表面和截面形貌、成分和相组成,讨论了陶瓷层的生长过程。研究表明,正／负向电流密度相同时,随电流密度的增加膜层厚度增大;而当正向电流密度相同时,负向电流密度增加有利于膜层的生长;成膜速率随脉冲频率和负向占空比增加,均呈现先增大后减小的趋势;陶瓷层总厚度随氧化时间接近于线性增长,致密层占总膜层的比例先快速增加,其后略微下降。SEM结果显示,随氧化时间延长,样品表面膜厚度趋于均匀,界面处氧化膜变得比较平坦。陶瓷层主要由α—Al2O3和γ-Al2O3相组成,随氧化时间的延长,γ-Al2O3相在陶瓷层中的相对含量逐渐减少。而α-Al2O3相的含量逐渐提高。     

Microstructure and Optical Characterization of Magnetron Sputtered NbN Thin Films

Some fundamental studies on the preparation, structure and optical properties of NbN films were carried out. NbN thin films were deposited by DC reactive magnetron sputtering at different N2 partial pressures and different substrate temperatures ranging from –50 ℃ to 600 ℃. X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM) were employed to characterize their phase com- ponents, microstructures, grain sizes and surface morphology. Optical properties inclusive of refractive indexes, extinction coefficients and transmittance of the NbN films under different sputtering conditions were measured. With the increase in the N2 partial pressure, δ-NbN phase structure gets forming and the grain size and lattice constant of the cubic NbN increasing. The deposited NbN film has relatively high values of refractive index and extinction coefficient in the wavelength ranging from 240 nm to 830 nm. Substrate tem- perature exerts notable influences on the microstructure and optical transmittance of the NbN films. The grain sizes of the δ-NbN film remarkably increase with the rise of the substrate temperature, while the transmittance of the films with the same thickness decreases. Ultra-fine granular film with particle size of several nanometers forms when the substrate is cooled to –50 ℃, and a remarkable aug- mentation of transmittance could be noticed under so low a temperature.     

溅射工艺对TiAlN薄膜摩擦学性能的影响

研究利用反应磁控溅射法在高速钢基体上制备TiAlN薄膜材料,采用XRD测试薄膜晶体结构,用UMT显微力学测试仪测试薄膜摩擦系数.在此基础上讨论铝含量、直流偏压及后期处理对薄膜摩擦系数的影响.结果表明,不同铝含量的TiAlN薄膜中都存在面心立方相和六方相,随着铝含量的增高,面心立方相比例逐渐减小,六方相增多.铝的引入使膜层的硬度明显提高.随着Al含量增加,GCr15与TiAlN膜层之间的摩擦系数下降.另外,直流偏压和后期处理亦可显著改善薄膜的抗摩擦性能.     

Plasma Niobium Surface Alloying of Pure Titanium and its Oxidation at 900 ℃

A niobium-modified layer on pure titanium surface was obtained by means of double glow plasma surface alloying technique. The modified layer was uniform, continuous, compact and well adhered to the substrate. The niobium composition in the modified layer decreased gradually from the surface to the substrate. The oxidation behavior of the niobium-modified layer was investigated and compared with the untreated surface at 900 ℃ for 100 h. Characterization of the layers was performed using X-ray diffraction and scanning electron microscope, respectively. The test results show that the oxidation behavior of pure titanium was improved by niobium alloying process. Niobium has a positive influence on the oxidation resistance.     

Plasma Niobium Surface Alloying of Pure Titanium and its Oxidation at 900℃

A niobium-modified layer on pure titanium surface was obtained by means of double glow plasma surface alloying technique. The modified layer was uniform, continuous, compact and well adhered to the substrate. The niobium composition in the modified layer decreased gradually from the surface to the substrate. The oxidation behavior of the niobium-modified layer was investigated and com- pared with the untreated surface at 900 ℃ for 100 h. Characterization of the layers was performed using X-ray diffraction and scanning electron microscope, respectively. The test results show that the oxidation behavior of pure titanium was improved by niobium alloying process. Niobium has a positive influence on the oxidation resistance.     

Study on the Microstructure and Dielectric Properties of Barium Strontium Titanate Thin Films Prepared by Sol-gel Method

Sr0.5Ba0.5–xBixTiO3 (BST) thin films were fabricated on a Pt/SiO2/Si substrate by the sol-gel method. Then follows an investigation of the influences of bismuth (Bi) on the microstructures and the dielectric properties of Sr0.5Ba0.5-xBixTiO3 (BST) thin films. The micro-structures of the BST thin films were examined by the XRD and the TEM techniques. Tetragonal perovskite crystal grains were observed in BST thin films. Increasing Bi3 doping ration in BST will lead to decrease of the grain size. It is found that Bi3 doping decreases the dielectric loss and improves the frequency dispersion of the BST thin films. Not only is compressed the peak of temperature-dependence of dielectric constant of Bi3 -doped BST thin films but also moves into the low-temperature region. Moreover, the average Curie tem-perature decreases gradually with the Bi3 contents increasing.     

过滤式阴极电弧沉积类金刚石薄膜的特性分析

利用自行研制的过滤式阴极电弧沉积装置,在硅片和高速钢基体材料上获得了类金刚石薄膜,分别采用扫描电镜、原子力显微镜、喇曼光谱以及磨损实验等手段对薄膜进行了分析研究。结果表明,所获得的类金刚石薄膜为非晶态,sp3含量最高达70%;基体材料对成膜质量影响较大,在硅片上薄膜的摩擦系数可达0.08;同时偏压的变化会引起喇曼谱线中D峰和G峰位置向低频移动,半高宽σG增大、σD减小。     

Effects of the Fabrication Processes of NC-Si:H Films on Their Mechanical Properties

Studies of nanoindentation were performed on nc-Si:H films to evaluate the effects of the fabrication processes on their mechani-cal properties. It is observed that with the decrease of the SiH4 contents, the grain size of the films increases gradually, and as does the crystalline volume fraction. The smaller the grains become, the more homogeneous the films, and the more even the hardness as well as the modulus will be. The hardness and the modulus will increase with the substrate’s temperature rising. The hardness and the modulus of the nc-Si:H films on the Si substrate prove to be higher than those on the glass substrate given the same technology parameters. How-ever, the films on the glass substrate appear to be more homogeneous.     

Kinetic Monte Carlo Simulation of EB-PVD Film:Effects of Substrate Temperature

The 2D kinetic Monte Carlo (KMC) simulation was used to study the effects of different substrate temperatures on the microstruc-ture of Ni-Cr films in the process of deposition by the electron beam physical vapor deposition (EB-PVD). In the KMC model, substrate was assumed to be a “surface” of tight-packed rows, and the simulation includes two phenomena: adatom-surface collision and adatom diffusion. While the interaction between atoms was described by the embedded atom method, the jumping energy was calculated by the molecular static (MS) calculation. The initial location of the adatom was defined by the Momentum Scheme. The results reveal that there exists a critical substrate temperature which means that the lowest packing density and the highest surface roughness structure will be achieved when the temperature is lower than the smaller critical value, while the roughness of both surfaces and the void contents keep decreasing with the substrate temperature increasing until it reaches the higher critical value. The results also indicate that the critical substrate temperature rises as the deposition rate increases.     

一种用于电子薄膜导热系数和发射率测量的实验方案

薄膜传热性能对微电子设备的传热能力及其性能和可靠性有重大影响,测量薄膜的热物性参数并进一步研究其影响因素,可为微电子电路的设计和发展提供科学依据。评述了薄膜导热系数测量和研究的现状,在此基础上提出了一种新的能同时测量衬底薄膜导热系数和发射率的实验方案,并通过建立衬底薄膜试样传热的数学模型和分析推导,论证了该实验方案的可行性。本实验方案可推广应用于确定淀积在衬底薄膜上各种极小厚度薄膜的导热系数和发射率。     

TiNi基形状记忆合金薄膜的相变特征研究

利用磁控溅射的方法在单晶Si和非晶SiO2基片上制备了TiNi和TiNiCu形状记忆合金薄膜,并利用示差扫描量热法和基片曲率法研究了薄膜的相变特征及应力随温度的变化.研究结果表明450℃溅射形成的记忆合金薄膜具有良好的形状记忆效应,在微电子机械系统有很好的应用前景.TiNi薄膜降温时出现R相变,因而发生两步相变,而TiNiCu薄膜中马氏体和奥氏体间直接转变.基片以及薄膜成份对相变点有很大的影响.单晶Si片作为基片时,记忆合金薄膜和基片间有很好的结合力,而SiO2作为基片时,记忆合金薄膜容易剥落.     

可见光迷彩低红外发射率薄膜制备及其特性

采用多弧离子镀技术,在Al基底上制备了TiO2/TiN多层膜。通过控制基底材料的粗糙度使制备出的薄膜在可见波段具有非镜面反射效果。采用扫描电镜、红外辐射率测量仪、紫外-可见-近红外光光度计等测试手段对薄膜样品进行了表征。结果表明,采用多弧离子镀法在Al基底上制备了结合力良好、具有迷彩效果的低红外发射率薄膜。研究发现,随氧化层厚度增加,薄膜发射率趋向稳定(0.2左右)。薄膜电阻随氧化层厚度的变化无明显变化。     

热障涂层喷涂质量微焦点CT检测

采用微焦点X射线源对热障涂层样品进行了高分辨率X射线成像研究,采用多尺度对比度增强算法提高了热障涂层与基体之间的对比度.X射线图像显示热障涂层各处厚度差异较大,热障涂层内部可能存在大量孔隙.通过微焦点计算机层析成像(CT)对样品进行了高分辨率CT扫描与重建,得到了样品的CT重建图像.从热障涂层CT图像观察到热障涂层内部存在大量孔隙,且不同层孔隙尺寸、数量不同.结合3个坐标方向的切片图像分析了热障涂层深度方向的热障涂层厚度,得到了热障涂层厚度的二维分布,测量得到热障涂层平均厚度约为40μm.对沿热障涂层深度方向850~1131层切片图像,利用可视化软件VGstudio MAX得到了热障涂层内部孔隙三维分布.研究结果表明:微焦点CT可用于热障涂层制备工艺质量检测.      

离子束辅助沉积WS_2-Ti-Ag复合薄膜的摩擦性能

采用ZDH-100型号离子束复合沉积设备沉积WS_2-Ti-Ag复合薄膜,基材为轴承钢和单晶硅(100).采用场发射扫描电子显微镜、XRD衍射仪,检测复合薄膜的表面形貌、微观结构.采用球-盘式摩擦磨损试验机,对复合薄膜在大气环境中的摩擦性能进行了研究.结果表明:采用离子束辅助沉积技术制备的WS_2-Ti-Ag复合薄膜是非晶态薄膜;并且随法向载荷的增加,复合薄膜的摩擦因数减小,摩擦状态越稳定,耐磨寿命越短.     

沉积含Si过渡层对于不锈钢上沉积的DLC薄膜的性能影响

本文介绍了采用RF-PECVD法在3Cr13不锈钢基体圆片上沉积制备类金刚石多层膜,其内层薄膜为掺Si的过渡层,外层为不同厚度的在50～1000 nm之间的类金刚石薄膜（DLC）。实验结果表明沉积过渡层可以有效提高薄膜与基体的结合力。类金刚石薄膜的摩擦系数和薄膜在摩擦过程中的损坏情况都与外层薄膜的厚度有关。     

极性面导致新型纳米结构的生长

以氧化锌粉为原料,采用化学气相沉积的方法,通过控制沉积温度、压强、沉积时间等实验条件获得了2种氧化锌纳米材料的新形貌。利用扫描电镜、X射线衍射、X射线能谱仪等仪器进行了表征,并对氧化锌纳米材料的生长机制进行了探讨。     

IBAD法沉积TiN薄膜的机械和耐腐性

用离子束辅助沉积(IBAD)方法在医用不锈钢317L基底上沉积TiN陶瓷薄膜。通过X射线衍射(XRD)和俄歇电子能谱(AES)分析研究了薄膜的微结构；测试了薄膜的耐磨性及薄膜与基底的附着力：运用电化学腐蚀的方法检测了薄膜在Hank’s模拟体液中的耐腐蚀性能。研究结果表明：用高、低能氮离子束兼用的IBAD方法沉积TiN多晶薄膜后，材料表面结构和性能发生明显改变。表面硬度和耐磨性有明显提高，在Hank’s模拟体液中显示出更强的抗腐蚀能力。