装饰薄膜氮化锆的中频反应磁控溅射沉积工艺的研究

发布时间：2018-01-22 04:30

本文关键词： 沉积工艺中频反应溅射:Zr-N薄膜颜色沉积速率俄歇深度分析　出处：《河北农业大学》2005年硕士论文　论文类型：学位论文

【摘要】：现代科学技术的发展对材料的性能的要求日益提高,利用溅射薄膜对材料表面防腐、表面装饰和各种工模具的表面强化是提高材料性能的一种经济实用的途径。近年来,仿金膜氮化锆(ZrN)由于有比氮化钛更好的耐磨性、抗腐蚀性,更优的力学性质,良好的化学和热学性能以及漂亮的金黄色和较高的硬度和熔点,已经在手表、眼睛架、金属家具、五金制品、陶瓷及玻璃制品等得到广泛的应用。目前关于氮化锆薄膜的制备方法很多,直流反应溅射技术由于存在着阳极消失和迟滞效应的缺陷,严重的影响了薄膜的沉积速率。因此如何使得靶面处于金属模式的溅射状态下维持较高的溅射速率,在基体上能够获得化学配比合适的氮化锆薄膜并有较高的沉积速率,是溅射氮化锆薄膜需要解决的一个关键问题。中频溅射技术是近些年来兴起的一门新技术,它是将辉光放电、等离子体与中频技术相结合的一种物理气相沉积技术,兼具蒸镀法沉积速率高和溅射法离子轰击清洁基体表面的优点。中频溅射能够显著的改善薄膜的性能,提高膜层和基底的结合力,绕射性能好、薄膜缺陷少以及可镀材料广泛等优点。另外中频溅射技术能够有效抑制弧光放电及根除阳极消失,从而保证溅射沉积过程能够稳定进行。因此中频溅射在装饰薄膜的工业化生产中发挥着重要作用。本研究利用工业化生产设备SP-1215,采用中频电源、孪生磁控靶、等离子体和质谱分析技术,在1Crl8Ni9Ti不锈钢基底上沉积氮化锆薄膜,改变试验的工艺参数,制备了不同工艺下的Zr-N薄膜。并对不同工艺下的薄膜试样进行了分析研究,得到了以下几点结论: 1、工作气压在0.3Pa附近的范围内,薄膜能够得到较高的沉积速率。Zr-N薄膜的沉积速率与溅射功率和反应气体分压强有密切的关系:沉积速率和溅射功率成正比,和反应气体分压强成反比。而基体偏压对沉积速率的影响很小。 2、反应气体分压强和溅射功率是影响Zr-N薄膜颜色的最主要的两个因素。氮气分压强由0～85%的变化范围内,Zr-N薄膜的颜色呈白色、浅黄色、金黄色、红金色和深红色的变化规律;在溅射功率3KW～10KW的范围内,Zr-N薄膜颜色呈金黄略微偏红、金黄色、浅黄色的变化规律,两者恰好相反。因此对薄膜颜色起决定作用的是溅射功率和反应气体分压强的比值。 3、通过对不同反应气体分压强下制备的Zr-N薄膜的俄歇深度分析,发现了N/Zr比例随氮气分压强的增加而增加,但是增加趋势趋缓。通过大量的氮化锆沉积试验数据,分析了中频反应磁控溅射沉积工艺参数对氮化锆的颜色和沉积速率的影响,从而在工业化生产设备上获得一
[Abstract]:With the development of modern science and technology, the performance of materials is becoming more and more important. Sputtering films are used to prevent corrosion on the surface of materials. Surface decoration and surface strengthening of various die tools are an economical and practical way to improve the properties of materials. In recent years, the gold-imitating film zirconium nitride ZrN has better wear resistance and corrosion resistance than titanium nitride. Better mechanical properties, good chemical and thermal properties as well as beautiful gold and high hardness and melting point, have been in watches, eye frames, metal furniture, hardware. Ceramics and glass products are widely used. At present, there are many preparation methods of zirconium nitride thin films. DC reactive sputtering technology has the defects of anodic disappearance and hysteresis. The deposition rate of the film is seriously affected, so how to keep the target surface in the metal mode of sputtering state to maintain a high sputtering rate. Zirconium nitride thin films with suitable chemical ratio and high deposition rate can be obtained on substrates, which is a key problem to be solved in sputtering zirconium nitride thin films. Intermediate frequency sputtering technology is a new technology developed in recent years. It is a physical vapor deposition technology which combines glow discharge, plasma and intermediate frequency technology. With the advantages of high deposition rate of evaporation and ion bombardment of clean substrate surface by sputtering, if sputtering can significantly improve the performance of the film, improve the adhesion between the film and substrate, and have good diffraction performance. In addition, if sputtering technology can effectively suppress arc discharge and eliminate anode disappearance. Therefore, if sputtering plays an important role in the industrial production of decorative films. In this study, the industrial production equipment SP-1215, if power supply, twin magnetic target, plasma and mass spectrometry analysis technology. Zirconium nitride thin films were deposited on 1Crl8Ni9Ti stainless steel substrate and the technological parameters were changed. Zr-N thin films were prepared under different processes, and the film samples under different processes were analyzed and studied, and the following conclusions were obtained: 1, the working pressure is in the range of 0.3 Pa. The deposition rate of Zr-N thin films is closely related to the sputtering power and reactive gas partial pressure: the deposition rate is directly proportional to the sputtering power. It is inversely proportional to the partial pressure of the reaction gas, while the substrate bias has little effect on the deposition rate. 2. The reactive gas partial pressure and sputtering power are the two most important factors affecting the color of Zr-N films. The color of Zr-N thin films is white in the range of 0 ~ 85% nitrogen partial pressure. Light yellow, golden yellow, red gold and deep red change law; In the range of sputtering power of 3KW ~ (10) KW, the color of Zr-N thin film is golden slightly red, golden yellow and light yellow. Therefore, it is the ratio of sputtering power to partial pressure of reactive gas that determines the color of the film. 3. By analyzing the Auger depth of Zr-N films prepared at different partial pressure of reaction gas, it is found that the ratio of N / Zr increases with the increase of nitrogen partial pressure, but the increasing trend is slower. Based on a large amount of experimental data of zirconium nitride deposition, the influence of deposition parameters of intermediate frequency reactive magnetron sputtering on the color and deposition rate of zirconium nitride was analyzed.
【学位授予单位】：河北农业大学
【学位级别】：硕士
【学位授予年份】：2005
【分类号】：TB43

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