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Development of modulation reactive sputtering and its application for films with multilayr structures

调制反应溅射技术的发展及其在多层结构薄膜中的应用

基本信息

批准号：
07455029
负责人：
KINBARA Akira
金额：
$ 4.61万
依托单位：
Kanazawa Institute of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (B)
财政年份：
1995
资助国家：
日本
起止时间：
1995 至 1996
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-07455029/
关键词：
Thin Films Reactive Sputtering Titanium Oxide Titanium Nitride Compositional Gradient Multilayr Structure Microhardness

项目摘要

In this research a modulation reactive sputtering method has been developed by using an sputtering apparatus with a computer controlled process gas flow system. The method has been applied for the formation of TiOx/Ti and TiNx/Ti multiayr film with compositionally modulated structures.In the research of TiOx (where x continuously and periodically changed from nearly 0 to 2) compositionally modulated multilayr films the differences of the physical properties such as refractive index between TIOx (x<1 : metal-rich) layrs and TiO2 (dioxide) layrs result in novel properties. The target used in the experiments was a 6inch dia. 99.98% Ti. The O2 gas mass flow rate was controlled by a mass flow contorller to obtain a multilayr film with an optimum oxygen distribution. Ar flow rate was kept constant during film deposition. The pressure in the chamber was measured with a capacitance manometer to estimate O2 gas consumption by gettering actions during film deposition. Mass deposition rate was me … More asured with a quartz-crystal eposition monitro. The oxygen content depth profiles of deposited films were analyzed by Auger Electron Spectroscopy. The experimental result showed that when the O2 flow rate was changed sinusoidally during the film deposition the metal-rich layrs (x<=1 in TiOx) became almost 6 to 8 times thicker than monoxide and dioxide mixture layrs (1<x=2 in TiOx). This is due to the diference of the Ti sputtering yield between the two sputtering modes in reactive sputtering process : metal mode and oxide mode. To obtain films with an almost equivalent thickness of metal-rich layrs and of monoxide and dioxide mixture layrs, O2 flow rate was changed to extend the time of deposition in the oxide mode and to shorten it in the metal mode. By optimizing the flow control.the films with an almost equivalent thickness of the metal-rich layrs and the monoxide and dioxide mixture layrs were obtained. The relationship between oxygen distribution obtained by AES depth profile analysis and O2 gas consumption calculated from O2 partial presure and O2 mass flow rate data obtained during the film deposition has been revealed mechanisms involved in the gas flow rate modulated reactive sputtering method. In conclusion, it has been shown that the continuous and periodical, but non-sinusoidal, change in O2 flow rate generates graded and periodical component distribution of the material in films and that tha gas rate flow rate modulated reactive sputtering method is advantageous to produce multilayr films by a single target-single reactive gas sputtering.In the research of TiNx/Ti (where x continuously and periodically changed from nearly 0 to 1) compositionally modulated multilayr films effects of multilayr strnctures of compositionally modulated TiNx/Ti films on their hardness has been investigated. Compositionally modulated TiNx/Ti multilayr films were deposited by a modulated reactive sputtering using the same apparatus described above. In the formation of TiNx/Ti compositionally modulated multilayr film a N2 gas flow rate was automatically controlled by a computer-controlled mass flow controller to produce films with an optimized composition distribution. Borosilicate glass and alumina plate were used as substrates. Hardness of prepared films were measured by a nono-indentation method. Composition distribution of prepared films was estimated by Auger electron spectroscopy. TiN singlelayr films were also deposited to compare is hardness with those of the multilayr TiNx/Ti films. By changing N2 reactive gas flow rate modulation frequency, films with a modulation period of 5nm, 7.5nm, 10nm, and 20nm were deposited onto unheated substrates. It is found by nano-indentation measurements that the films with a modulation frequency of 5nm provide highest values of micro hardness among the single layr and multilayr films. The same results were obtained for the films both deposited on the two types of substrates. The results obtained in this study indicate that the hardness of compositionally modulated multilayr TiNx/Ti films strongly depends on modulation frequency Less

本研究发展了一种调制反应溅镀方法，使用一台溅镀装置，并以电脑控制制程气体流量系统。在TiOx（x从0到2连续周期性变化）组分调制多层膜的研究中，TiOx（x<1：富金属）层和TiO 2（dioxide）层之间的折射率等物理性质的差异导致了新的性质。实验中使用的靶是直径6英寸的。钛含量99.98%。通过质量流量控制器控制O2气体的质量流量，以获得具有最佳氧分布的多层膜。在薄膜沉积过程中，氩气流量保持恒定。用电容压力计测量腔室中的压力，以估计在膜沉积期间通过吸杂作用消耗的O2气体。质量沉积率是我 ...更多信息用石英晶体沉积监测仪测量。用俄歇电子能谱分析了沉积膜的氧含量深度分布。实验结果表明，当O2流量在薄膜沉积过程中呈正弦变化时，富金属层（TiOx中x<=1）的厚度几乎是一氧化物和二氧化物混合物层（TiOx中1<x=2）的6至8倍。这是由于在反应溅射过程中，金属溅射模式和氧化物溅射模式的钛溅射产额的差异。为了获得具有几乎相等厚度的富金属层和一氧化物和二氧化物混合物层的膜，改变O2流速以延长氧化物模式中的沉积时间并缩短金属模式中的沉积时间。通过优化流动控制，获得了富金属层与一氧化物和二氧化物混合层厚度几乎相等的薄膜。通过AES深度剖面分析得到的氧分布与由氧分压和氧流量数据计算得到的氧耗之间的关系，揭示了气体流量调制反应溅射法的机理。总之，已经表明，连续的和周期性的，但非正弦的，O_2流量的变化使薄膜中材料的成分呈梯度和周期性分布，气体流量调制反应溅射法有利于单靶单反应气体溅射制备多层膜（其中x从0到1连续周期性变化）成分调制多层膜研究了成分调制TiNx/Ti多层膜结构对其硬度的影响。使用与上述相同的装置通过调制反应溅射沉积成分调制的TiNx/Ti多层膜。在TiNx/Ti成分调制多层膜的形成中，通过计算机控制的质量流量控制器自动控制N2气体流速以产生具有优化的成分分布的膜。采用硼硅酸盐玻璃和氧化铝板作为基底。用非压痕法测量了薄膜的硬度。利用俄歇电子能谱估计了所制备薄膜的成分分布。还沉积了TiN单层膜以比较其与多层TiNx/Ti膜的硬度。通过改变N2反应气体流量调制频率，在未加热的衬底上沉积具有5 nm、7.5nm、10 nm和20 nm调制周期的薄膜。纳米压痕测试结果表明，在单层和多层薄膜中，调制频率为5 nm的薄膜的显微硬度最高。沉积在两种类型基底上的薄膜获得了相同的结果。研究结果表明，成分调制TiNx/Ti多层膜的硬度与调制频率密切相关。