SiO2薄膜制备的现行方法综述

在导电基体上制作薄膜传感器的过程中,需要在基体与薄膜电极之间沉积一层绝缘膜.二氧化硅薄膜具有良好的绝缘性能,并且稳定性好,膜层牢同,长期使用温度可达1000℃以上,应用十分广泛.通常制备SiO2薄膜的现行方法主要有磁控溅射、离子束溅射、化学气相沉积、热氧化法、凝胶-溶胶法等.本文系统阐述了各种方法的基本原理、特点及适用场合,并对这些方法做了比较.     

Niederenergie-IBAD: Zusammenhang zwischen Prozeßparametern und Schichteigenschaften bei ionenstrahlunterstützten Aufdampf-und Sputtertechniken

Low energy IBAD: correlation between process parameters ans film properties for ion beam assisted evaporation and sputter deposition Binary nitride films with Al, Cr and Ti as metal components have been deposited with ion beam assisted evaporation and sputtering (IBAD) and the film properties are investigated in terms of the individual deposition parameters. In the case of ion beam assisted evaporation the flux ratio between the film forming metal atoms and the nitrogen ions from the ion source was shown to enable a quantitative control of the composition and the chemical phases of the films. Detailed studies for TiN reveal the possibilities to manipulate texture and stress, the average grain size and the morphology of the films. Such results are discussed with an extended structure zone model, introducing the energy input per film forming particle as the relevant parameter. Also, the structural film properties and the deposition parameters are quantitatively correlated with the hardness and the beginning of TiN deposition on stainless steel resulted in distinctly improved adhesion properties. For the deposition of TiN with a dual ion beam arrangement in which one beam bundle was directed onto a Ti-target and an other onto the substrate with the growing film, a strong influence of the particle energies and the incidence angles on the film texture and its directional orientation was found. Such effects are quantitatively related to the minimization of the free energy of the films and the influence of preferential re-sputtering effects. For ion beam sputter deposition without simultaneous ion bombardment of the growing film, the texture and the film stress are found to be controlled by energetic particles resulting from elastic backscattering at the target surface.     

The nucleation and initial growth of gold films deposited onto sodium chloride by ion-beam sputtering

Data are presented for the initial growth of sputtered films of gold on vacuum-cleaved rocksalt substrates. The films were grown in high vacuum by means of an ion-beam sputtering system, so that no plasma effects were present.The experimental variations of island density with such parameters as deposition time, substrate temperature and deposition rate are reported. These results have been compared with existing data for evaporated films and differences have been found.A simplified treatment of the nucleation and growth kinetics has been used to correlate the results by sputtering to those by evaporation. In the case of sputtering, it has been necessary to postulate a constant density of preferred adsorption sites on the substrate. More detailed theories have been used to confirm the analysis.Apart from the influence of the preferred sites, growth apparently proceeds in the same way for deposition by sputtering and for deposition by evaporation.     

Mg-PbO2-Ti-PbO2-PTFE复合薄膜烟火材料的制备及性能

采用磁控溅射和真空蒸镀结合的方法,制备了Mg-PbO2-Ti-PbO2-PTFE复合薄膜烟火材料,利用X射线光电子能谱(XPS)分析了真空蒸镀的薄膜成分,并测定了薄膜材料与基底间的附着力.采用光纤法测量薄膜材料的燃烧线速度,分析了其燃烧过程.结果表明,利用真空蒸镀法可得到PbO2薄膜,复合薄膜烟火材料与基底有较好的附着...     

Processes of the activated reactive evaporation type and their tribological applications

Plasma-assisted deposition processes have created a breakthrough in the deposition of compounds particularly the refractory compounds such as oxides, carbides, nitrides etc. Processes such as sputtering or ion plating inherently contain a plasma in the space between the target and the substrate. Evaporation and chemical vapor deposition processes have to be modified to include a plasma. In all of these reactive deposition processes the plasma plays a vital role in providing the activation energy necessary to carry out the process or to enhance its efficiency. All types of vapor sources can be used in these processes. The original development in 1971 used a thermionic electron beam evaporation source. Subsequently, resistance- heated, arc, induction, plasma electron beam and sputtering sources have all been used. In this paper we shall discuss the processes and the influence of deposition parameters on the microstructure and properties of compounds. Specific examples of the use of these compounds in tribological applications are considered.     

Vacuum deposited polymer/metal multilayer films for optical application

Vacuum-deposited polymer/silver/polymer reflectors and tantalum/polymer/aluminum Fabry-Perot interference filters were fabricated in a vacuum web coating operation on polyester substrates with a new, high-speed deposition process. Reflectivities were measured in the wavelength range from 0.3 μm to 0.8 μm. This new vacuum processing technique has been shown to be capable of deposition line speeds in excess of 500 linear m min⁻¹ (D.G. Shaw and M.G. Langlois, Proc. 7th Int. Conf. Vacuum Web Coating, November 1993, p. 268). Central to this technique is a new vacuum deposition process for the high-rate deposition of polymer films. This polymer process involves the flash evaporation of an acrylic monomer onto a moving substrate. The monomer is subsequently cured by an electron beam or ultraviolet light. This high-speed polymer film deposition process has been named the polymer multi-layer process. Also, vacuum-deposited, index-matched, polymer/CaF₂ composites were fabricated from monomer slurries that were subsequently cured with ultraviolet light. This second technique is called the liquid multi-layer process. Each of these polymer processes is compatible with each other and with conventional vacuum deposition processes such as sputtering or evaporation.     

Vacuum-deposited carbon coatings

In recent years, highly favorable results have been obtained using low temperature isotropic pyrolytic carbons in prosthetic devices requiring a high degree of thromboresistance. The development of vacuum-deposited carbon coatings was undertaken to extend the application of carbon to geometries and configurations that cannot be fabricated from low temperature isotropic carbon. Vacuum-deposited coatings have been produced on a variety of metallic and polymeric substrates.The different vacuum deposition processes which have been investigated include electron beam gun evaporation using high vacuum, gas scattering and ion- plating conditions. In addition, sputtering processes using ion beams and magnetically confined plasmas were studied.The surface morphology, structure and preferred orientation of the coatings produced by the different processes were characterized by scanning and transmission electron microscopy. Film purity and interfacial characteristics were examined by Auger electron spectroscopy.The scanning electron microscopy study shows that thin carbon films generally have a smooth and featureless surface morphology. However, other surface morphology features are obtained in thicker films, depending on the processing conditions. The transmission electron micrographs show the absence of structure and growth features. Electron diffraction indicates that the films consist of a turbostratic phase and a non-crystalline phase. The apparent crystallite sizes are small, and there is no three-dimensional ordering. Generally, the films are isotropic and consist of relatively pure carbon, with the degree of disorder dependent on the process conditions.     

离子束溅射法制备碳氮薄膜及其结构表征

采用离子束溅射沉积技术,对不同氮离子束能量情况下制备的氮化碳薄膜,进行了拉曼(Raman)和红外光谱(FT-IR)分析,并采用透射电子显微镜(TEM)分析其表面形貌,研究所制备薄膜的化学组成和键合结构。结果显示:随着氮离子束能量增大,氮碳薄膜的沉积速率减小,薄膜结构中sp2含量增大,薄膜有序度增加,另外薄膜结构的团簇尺寸大幅下降,团簇趋于均匀分布。     

Studies of diamond-like carbon films prepared by ion beam-assisted deposition

Ion beam-assisted deposition offers a novel and unique process to prepare diamond-like carbon (DLC) films at room temperature, with particularly good interface adhesion. This advantage was explored in this study to deposit highly wear-resistant coating on bearing 52100 steel. Both dual ion beam sputtering and ion beam deposition were employed. Various bombarding species and energy were investigated to optimize the process. Raman, X-ray photoelectron and Auger electron spectroscopy were used to characterize the bonding structure of DLC. Extensive experiments were carried out to examine the tribological behaviour of the DLC/52100 system. A metal intermediate layer can help tremendously in wear resistance. The results are optimistic and may lead to useful applications.     

Herstellung und Untersuchung aufgedampfter Funktionsschichten zum Einsatz in modularen Mikrosensoren

Fabrication and characterization of functional layers evaporated for the application in modular micro sensors A new concept aims at the development of genetically intelligent (“gentelligent^TM”)devices, which bequeath production or application data to their next generation. To support such an approach, it is necessary to gather various data from the device. To do so, afamily of modular sensors is under development, which is capable of measuring strain, force, magnetic properties, and temperature. Such micro sensor sconsist of structural and functional patterned thin films. A technology particularly well suited for such thin films is the vacuum deposition. This process allows to deposit rather different materials for conductors, insulators, and alloys for creating functional films. This work describes the technology development for fabricating temperature sensitive metallic functional films of Cu and Pt by means of electron beam evaporation and of an insulating SiO₂ film by means of thermal evaporation. The latter film is deposited by evaporating SiO and its thermal oxidation to SiO₂.     

Effect of Ion Bombardment on the Structure and Properties of Polycrystalline Chromium Films

Polycrystalline chromium films were fabricated by electron beam evaporation with concurrent bombardment using argon ions from an ion gun or by sputtering with substrate bias. The microstructure and composition of the films were characterized using TEM/EDS. It was found that the grain size/shape, porosity, and argon content of the films strongly depend on the deposition parameters such as bombardment ion current density, deposition rate, argon pressure and substrate bias. Film properties including residual stress, resistivity, and reflectance were measured. A correlation of deposition, structure, and properties is discussed.     

An orientation competition in yttria-stabilized zirconia thin films fabricated by ion beam assisted sputtering deposition

A previously found orientation competition in ion beam sputtered yttria-stabilized zirconia thin films was studied in detail. The effects of sputtering energy and deposition angle were analyzed in ion sputtered films without assisting ions bombardment. It is found that for normally deposited films, (001) and (011) orientations are favored at low and high sputtering energy respectively. For inclined substrate deposited films, as deposition angle increases, (001), (011) and (111) orientations are advantaged in turn. The results can be attributed to the in-plane energy exchange of deposition atom and adatoms. In ion beam assisting deposited YSZ films of low assisting ions energy and current, a (001) oriented biaxial texture is gradually induced as ion energy increased. In the case of ion beam assisted inclined deposition of 45°, (001) orientation is enhanced and two preferential in-plane orientations are found coexist.     

气离溅射离子镀制氮化钛

本文详细介绍了气体离子源增强磁控溅射(气离溅射)反应离子镀膜技术和系统配置.特别是首次提出空分气离溅射的新概念,实现了磁控溅射金属镀膜过程和气体离子轰击化学反应过程在真空室内空间上的分离,从而保证空分气离溅射反应离子镀膜过程的长时间稳定性、重复性和一致性.当磁控溅射源采用中频电源驱动、最新开发的气体离子源采用脉冲直流电源后,实现了最佳的设备组合,可镀制出高品质的TiN膜层.     

超高真空中使用的高纯过渡金属蒸发源

设计了一种超高真空使用的低电流过渡金属蒸发源 ,它能产生高纯金属原子束 ,且具有一定的寿命。该蒸发源是将过渡金属Co,Ni或Cr电镀到一个由W丝弯成的U形加热器上构成的。装入超高真空中 ,利用W丝自身的电阻加热 ,去气后 ,可获得数小时的清洁蒸发。实验结果表明 ,在离蒸发源约 5cm处 ,其淀积速率最高可达 1 0nm/min ,总的淀积厚度超过 5 0 0nm ,而且Auger分析结果显示 ,在超高真空中淀积的上述几种过渡金属薄膜 ,其纯度相当高 ,杂质含量均小于仪器的检测灵敏度。本文详细介绍了这种过渡金属蒸发源的制作技术及性能     

离子束增强反应磁控溅射低温快速沉积AlN膜

本文采用氮离子束增强反应磁控溅射,在低温下沉积了 AlN 薄膜.用 X 射线衍射和 X 射线光电子谱对薄膜的晶体结构和电子结构进行了分析,结果表明,随着离子源中氮离子束流的增加,薄膜组成由面心立方的 Al 转变为密排立方的 AlN.氮离子在薄膜制备中的引入,有效地降低了沉积温度,提高沉积速率,并实现了薄膜 N/Al 化学计量比的控制.对 AlN 薄膜的紫外-可见光透射谱和红外吸收谱也进行了测定.     

Influence of the evaporation rate and the evaporation mode on the hydrogen sorption kinetics of air-exposed magnesium films

It has been shown that the hydrogen sorption properties of air-exposed magnesium films are influenced by the deposition parameters such as the evaporation rate or the evaporation mode used during their preparation. As the evaporation rate increases, the structure of the film tends to be highly oriented along the [002] direction and the kinetics of hydrogen absorption and desorption are faster. Moreover, the hydrogen sorption kinetics of magnesium films prepared with an electron beam source under a high vacuum are faster by almost a factor of two compared to those prepared using resistive heating under low vacuum. These two parameters reduce drastically the activation and the incubation period during hydrogen absorption and desorption, respectively.     

Ion beam sputtering of ZnS thin films

Ion beam sputtering was used to deposit adherent high quality ZnS films non-reactively. The optical properties of films thicker than 80.0 nm were found to be equivalent to those of bulk ZnS with a packing density of unity. Unlike that of evaporated films, the refractive index was insensitive to the substrate temperature but for thinner films was dependent on the substrate condition prior to deposition. The deposition of fully dense films is qualitatively explained using Muller's model of ion-assisted deposition. In the case of ion beam sputtering, the high energy species comprise energetic sputtered atoms and/or molecules, reflected beam ions and charge exchange neutrals.     

波长小于10nm的软X射线多层膜制备技术

软X射线短波段区域(1～10nm)高反射率多层膜的制备对软X射线光学的研究具有十分重要的意义.该波段要求镀膜过程中能减小界面扩散,实现膜厚控制,从而严格限制了制备技术的应用.介绍了软X射线短波段多层膜的发展现状和制备技术,主要包括蒸发沉积、溅射沉积、脉冲激光沉积技术和激光分子束外延,对这些方法进行了比较并提出了今后的研究方向.     

Preparation of silica thin films by novel wet process and study of their optical properties

Silicon dioxide (SiO2) thin films have gained considerable attention because of their various industrial applications. For example, SiO2 thin films are used in superhydrophilic self-cleaning surface glass, UV protection films, anti-reflection coatings, and insulating materials. Recently, many processes such as vacuum evaporation, sputtering, chemical vapor deposition, and spin coating have been widely applied to prepare thin films of functionally graded materials. However, these processes suffer from several engineering problems. For example, a special apparatus is required for the deposition of films, and conventional wet processes are not suitable for coating the surfaces of substrates with a large surface area and complex morphology. In this study, we investigated the film morphology and optical properties of SiO2 films prepared by a novel technique, namely, liquid phase deposition (LPD). Images of the SiO2 films were obtained by scanning electron microscopy (SEM) and atomic force microscopy (AFM) in order to study the surface morphology of these films: these images indicate that films deposited with different reaction times were uniform and dense and were composed of pure silica. Optical properties such as refractive index and transmittance were estimated by UV-vis spectroscopy and ellipsometry. SiO2 films with porous structures at the nanometer scale (100-250 nm) were successfully produced by LPD. The deposited film had excellent transmittance in the visible wavelength region.     

TiO2和SiO2薄膜应力在线测量与研究

研究了离子能量在薄膜制备过程中对TiO2和SiO2薄膜应力的影响。用电子束蒸发的方法制备TiO2和SiO2薄膜,使用实验室自行设计制作的基于哈特曼传感器的薄膜应力仪在线监测TiO2和SiO2薄膜应力随膜厚的变化。结果表明,离子辅助沉积的TiO2薄膜张应力值要比传统工艺低40 MPa,并且随着离子能量的增加,薄膜逐渐由张应力变为压应力,薄膜的最大折射率为2.56;而离子辅助的溅射效应在制备SiO2薄膜时比较明显,传统工艺制备的SiO2薄膜表现为压应力,而用离子辅助的方法制备的SiO2薄膜表现为张应力,并且随着离子能量的增加,薄膜变得疏松,折射率逐渐降低。