磁控溅射沉积薄膜实验参数优化光谱诊断

采用磁控溅射仪、Omni-λ300系列光栅光谱仪、CCD数据采集系统和光纤导光系统等构成的等离子体光谱分析系统,采集了以Cu和Al为靶材、氩气为工作气体,射频磁控溅射法沉积硅基薄膜时的等离子体发射光谱。以CuⅠ324.754 nm,CuⅠ327.396 nm,CuⅠ333.784 nm,CuⅠ353.039 nm,AlⅠ394.403 nm和AlⅠ396.153 nm为分析线,研究了Cu和Al等离子体发射光谱强度随溅射时间、溅射功率、靶基距和气体压强等实验参数的变化。并与射频磁控溅射沉积薄膜实验参数的选择进行对比,表明发射光谱法对射频磁控溅射薄膜生长条件的优化有着很好的指导作用。     

Electron microprobe compositional analysis of sputtered tantalum-aluminium films

In the present paper the methods for measurement of the composition of two or more component tantalum-based thin sputtered films are summarized. The influence of the target construction on the composition of the films is discussed. The Ta-Al films were sputtered from composite Ta-Al targets. The composition of films was measured by means of the electron microprobe technique. From results it follows that using the composite targets for sputtering in argon at a pressure of 2×10^?2 torr and in its mixture with nitrogen (10^?3 torr), the composition of Ta-Al films is proportional to the ratio of the Ta and Al exposed surfaces on the target. The proportionality factor equals to the ratio of “effective” sputtering yields of target components measured at given sputtering conditions. The presence of nitrogen in sputtering gas decreases the value of Ta yield 2.2 times. If a small Al surface is sputtered together with much larger Ta surface, the sputtering yield of Al remains unchanged. In Ta-Al films the occluded argon was qualitatively determined. The presence of nitrogen was not proved. This seems to be caused by the absorption of nitrogen characteristic radiation in the investigated films.     

Specific features of the ferroelectric state in two-layer barium strontium titanate-based heterostructures

The structural properties of one- and two-layer heterostructures based on the barium–strontium titanate of various compositions deposited by the Frank–Van der Merve on a magnesium oxide substrate have been studied. The heterostructures have been prepared by the rf sputtering of the stoichiometric ceramic targets in a Plazma 50 SE deposition system. The principal difference of this method of deposition from known analogs is that the growth of single-crystal films occurs from a disperse oxide phase formed in the plasma of a high-current rf discharge during the ceramic target sputtering at the cluster level. The peculiarities of the manifestation of the ferroelectric state in the two-layer heterostructures when changing the sequence order of the films with various compositions of barium–strontium titanate.     

Influence of direct current plasma magnetron sputtering parameters on the material characteristics of polycrystalline copper films

Physical vapor processes using glow plasma discharge are widely employed in microelectronic industry. In particular magnetron sputtering is a major technique employed for the coating of thin films. This paper addresses the influence of direct current (DC) plasma magnetron sputtering parameters on the material characteristics of polycrystalline copper (Cu) thin films coated on silicon substrates. The influence of the sputtering parameters including DC plasma power and argon working gas pressure on the electrical and structural properties of the thin Cu films was investigated by means of surface profilometer, four-point probe and atomic force microscopy.     

Description of a hybrid PECVD-PVD process: Application to Zn-Si-O and Ti-Si-O composites thin films

A radio frequency hybrid process where sputtering and plasma enhanced chemical vapour deposition (PECVD) occur simultaneously is studied to describe the specificity it gains when the two techniques are merged. A model is developed to describe how the deposition rate evolves when the flow rate of the PECVD precursor increases. First, it is shown that it is constant below a critical value of the precursor flow rate because of the wind effect due to sputtering that strongly limits the transport of the precursor. Then it increases almost linearly with the precursor flow rate when PECVD and sputtering simultaneously occur. Finally, above a certain threshold in the precursor flow rate, the surface of the target is poisoned by the precursor and composite thin films can no longer grow. The previous model is deduced from results obtained in deposition of Zn-Si-O and Ti-Si-O thin films. These composites are synthesised respectively by sputtering of zinc and titanium targets in a vapour of oxygen and hexamethyldisiloxane (HMDSO-Si₂C₆H₁₈O). Limitations of the model used are also discussed.     

FEB偏滤器等离子体温度及靶板运行温度的优化

本文以石墨偏滤器靶板材料为例，用喷气或杂质注入对偏滤器靶板前等离子体温度进行控制，要刻薄虎器等离子体的各种变标关系及石墨靶板被腐蚀的程度、优化了ＦＥＢ偏滤器靶板前等离子体温度和靶板运行温度。     

The Radio Frequency Hollow Cathode Discharge Induced by the RF Discharge in the Plasma‐Jet Chemical Reactor

In the recent decade an RF driven, low‐pressure plasma reactor with supersonic plasma jet was developed (RPJ). This reactor was successfully used for deposition of thin films of various materials. The deposition of thin films indicates that the properties of the deposited films are dependent on the sputtering or reactive sputtering processes appearing inside the nozzle (hollow athode). The nozzle (hollow athode) fabricated of different kinds of materials and alloys works both as a cathode of the radio frequency (RF) hollow cathode discharge and as a nozzle for plasma jet channel generation as well. The RF hollow cathode discharge is a secondary discharge, which is induced by the primary RF plasma generated in the reactor chamber. The present paper deals with the experimental study of this RF hollow cathode discharge. The stress is laid on the investigation of the axial distribution of discharge parameters and sputtering processes inside the nozzle. On the base of experiments, the simple model of the axial distribution of the investigated RF hollow cathode discharge has been developed.     

Study of hydrogenated amorphous silicon nitride films prepared by RF magnetron sputtering

Hydrogenated amorphous silicon nitride films have been deposited by the rf magnetron sputtering method with non-stoichiometric and stoichiometric compositions using a poly-Si target and a mixture of Ar, H₂ and N₂ as the sputtering gas. Data on optical and infrared absorption, electrical conductivity, breakdown voltage, capacitance measurements and thermal evolution of hydrogen have been presented as a function of nitrogen concentration in the films, especially in the stoichiometric region of composition. Attempts have been made to identify the roles of hydrogen and nitrogen in determining the electrical and optical properties and thermal stability exhibited by the films. Properties relevant for device application of the material have been shown to be comparable to those obtained by glow discharge or electron cyclotron resonance plasma chemical vapour deposition methods of deposition. RF magnetron sputtering has therefore been suggested as a viable alternative to the more widely adopted CVD methods for device applications of silicon nitride, where the use of hazardous process gases can be avoided.     

Properties of permalloy films produced in low-temperature plasma flows with a controlled composition

A simple version of a flow-forming plasma sputtering system is proposed. The causes that determine the properties of the deposited films are revealed when the composition, energy, and particle density of the flow are controlled. The electron component of the plasma flow and an increase in its ion component are found to degrade the magnetic properties of the films. The ferromagnetic resonance (FMR) line half-width of 10- to 150-nm-thick films is shown to mainly depend on the energy of the neutral flow component, which is specified by the sputtering conditions at an anode voltage of 400–700 V. In this rather narrow energy range, the FMR line half-width is 25 Oe for cold substrates.     

Ion-plasma technologies for the preparation and modification of nanosized LiF layers

The characteristics of LiF films containing Ag nanoparticles prepared via vacuum thermal deposition and magnetron sputtering, and then painted in microwave discharge plasma, are investigated. It is shown that simple and freely available ion-plasma technologies allow us to obtain nanosized LiF layers promising for use in photonics.     

Heteroepitaxial growth of complex-oxide films from a self-organized system formed in a gas-discharge plasma

New experimental data on the characteristic features of the synthesis and crystallization of films of solid solutions of lead zirconate-titanate, deposited by means of rf diode sputtering of ceramic targets, are presented. Such a deposition system possesses threshold states, transition through which leads to a qualitative change in the processes occurring in the system and to the appearance of self-organization effects. The basic feature of this change is determined by the appearance of a new structured system, consisting of the sputtered particles and particles formed in the plasma, in the plasma of an rf discharge. Zh. Tekh. Fiz. 69, 87–91 (December 1999)     

Microwave plasma enhanced low pressure d.c. sputtering of copper films

This paper reports on d.c. sputtering of copper films using a cylindrical magnetron (CyM) with the discharge enhanced and/or ignited by a microwave plasma produced in an external magnetic fieldB _e . The sputtering system was optimized with the aim to achieve high deposition rate of films at low argon pressures. It was achieved by enhancing the ionization degree of the discharge plasma by microwaves absorbed in the plasma and by the control of the distribution ofB _e (z) along the device axis, i.e. by controlling the transport of the plasma to within a close vicinity of the sputtered target of the CyM. The optimized sputtering system can sputter films at low argon pressures from about 0.1 Pa down to 0.005 Pa and at quite large discharge currentsI _d up to 1 A, i.e. at quite large deposition ratesa _D of about several hunderds of nanometers per minute. The sputtering system operates at pressures lower than conventional magnetrons, i.e., under conditions when fast neutrals play a significant role. It opens the possibility to produce films of new properties. As an example, the microwave enhanced sputtering discharge was used to deposit Cu films. Resistivity and preferred crystal orientation of Cu films prepared under different argon pressures and at microwave powers ranging from about 100 W to 800 W is reported.This work was supported in part by the Grant Agency of Czech Republic under Grant No. 202/93/0508.     

直流三极溅射法制备CuInS2 薄膜

采用直流三极溅射装置制备获得了CuInS₂薄膜, 其中溅射靶采用一定面积比的[Cu]/[In]混合靶,反应气体采用CS₂气体. 本文中主要研究了0.02 Pa分压反应气体条件下不同面积比的[Cu]/[In]混合靶和沉积基板温度对CuInS₂薄膜结构和成分的影响, 其中CuInS₂薄膜制备所用时间为2 h生长的厚度为1—2 μm. 通过对CuInS₂薄膜的EPMA, X射线衍射测试分析表明, 最佳的CuInS₂薄膜可在面积比[Cu]/[In]混合靶为1.4:1和可控温度(150, 250和350 ℃)的条件下制备获得, 并且其结构被确认为黄铜矿结构. 通过实验结果计算出CuInS₂薄膜层有约为8.9%的C杂质含量.     

Intrinsic ZnO films fabricated by DC sputtering from oxygen-deficient targets for Cu(In,Ga)Se_2 solar cell application

Intrinsic zinc oxide films,normally deposited by radio frequency(RF) sputtering,are fabricated by direct current(DC) sputtering.The oxygen-deficient targets are prepared via a newly developed double crucible method.The 800-nm-thick film obtaines significantly higher carrier mobility compareing with that of the 800-nm-thick ZnO film.This is achieved by the widely used RF sputtering,which favors the prevention of carrier recombination at the interfaces and reduction of the series resistance of solar cells.The optimal ZnO film is used in a Cu(ln,Ga) Se2(CIGS) solar cell with a high efficiency of 11.57%.This letter demonstrates that the insulating ZnO films can be deposited by DC sputtering from oxygen-deficient ZnO targets to lower the cost of thin film solar cells.     

Novel type of indium oxide thin films sputtering for opto-electronic applications

Transparent conductive oxide (TCO) thin films play a significant role in recent optical technologies. Displays of various types, photovoltaic systems, and opto-electronic devices use these films as transparent signal electrodes. They are used as heating surfaces and active control layers. Oxides of TCO materials such as: tin, indium, zinc, cadmium, titanium and the like, exhibit their properties. However, indium oxide and indium oxide doped with tin (ITO) coatings are the most used in this technology.In this work, we present conductive transparent indium oxide thin films which were prepared using a novel triode sputtering method. A pure In₂O₃ target of 2 in. in diameter was used in a laboratory triode sputtering system. This system provided plane plasma discharge at a relatively low pressure 0.5-5 mTorr of pure argon. The substrate temperature was varied during the experiments from room temperature up to 200 °C. The films were deposited on glass, silicon, and flexible polyimide substrates. The films were characterized for optical and electrical properties and compared with the indium oxide films deposited by magnetron sputtering.     

感应耦合等离子体增强射频磁控溅射沉积ZrN薄膜及其性能研究

利用感应耦合等离子体(ICP)增强射频磁控溅射技术在Si(111)片和M2钢表面制备了ZrN薄膜,研究了基片的温度和ICP功率对ZrN薄膜的结构以及性能影响.研究发现：在基片温度≤300℃沉积的ZrN薄膜择优取向为(111);基片温度达到450℃时薄膜出现ZrN(200)衍射峰,ZrN(111)晶面的织构系数明显降低.传统磁控溅射沉积薄膜为柱状结构,当ICP为200 W,基片温度为300℃时沉积薄膜中柱状晶体消失;随着基片温度的升高,N/Zr元素比例降低,并且薄膜的电阻率下降;相对于传统溅射,ICP增强射 关键词： 感应耦合等离子体 磁控溅射 ZrN 微结构     

Optical and mechanical properties of AlF3 films produced by pulse magnetron sputtering of Al targets with CF4/O2 gas

In this study, AlF₃ thin films were deposited by pulse magnetron sputtering of Al targets with different ratios of CF₄/O₂ gas and at different sputtering powers. The optical and mechanical properties of the AlF₃ thin films were analyzed. The transmittance spectra showed no obvious negative inhomogeneous refractive indices. Denser films with a low optical absorption were obtained when high sputtering powers were used (larger than 30 W). The lowest extinction coefficient (7.3 × 10⁻⁴ at 193 nm) of the films can be reached with 12 sccm O₂ flow rate and at 160W sputtering power. All of the residual stresses were compressive and their trends were consistent with the refractive indices. The lowest compressive stress (0.068 GPa) was obtained when the AlF₃ films were prepared at 160W sputtering power.     

微通道板电子透射膜工艺的AES研究

用冷基底溅射方法和静电贴膜方法分别在微通道板表面制备了电子透射膜,采用俄歇电子能谱(AES)研究了两种工艺制备的微通道板电子透射膜的薄膜成分,微通道板电子透射膜工艺失败微通道板通道表面的成分和通道内壁的成分随深度的变化. 结果表明,冷基底溅射方法制膜工艺的失败对MCP造成了严重的碳污染,污染的MCP不可回收;静电贴膜方法制膜工艺的失败对MCP通道表面没有明显影响,MCP可回收利用.     

Preparation and characterization of Cu-Cu2O cermet films

Metal-insulator composites (cermets) find use in a wide range of applications. In this paper the preparation of cermet films by dc reactive magnetron sputtering is presented. These cermets have been characterised by measuring their electrical resistance and the properties have been correlated to the microstructure and composition. Magnetron sputtering is found to be very effective in controlling the composition of the deposited films, enabling the preparation of films with tailored properties.     

偏滤器等离子体中杂质对钨壁材料的侵蚀模拟研究

偏滤器是托卡马克中与等离子体直接接触的部件,为了保证装置的寿命,需要尽可能地减小等离子体对偏滤器靶板的侵蚀.本文用粒子模拟的方法研究了不同等离子体温度情况下碳和铍两种杂质离子对钨偏滤器侵蚀速率的影响.模拟首先得到稳定的鞘层结构、入射到靶板的离子流和能流密度,并通过统计获得了入射离子的能量和角度分布,最终根据这些物理参量,采用经验公式计算出钨靶板的侵蚀速率.研究表明,在等离子体温度不太高的情况下,钨靶板的热侵蚀几乎不起作用,而由于杂质离子对钨的物理溅射阈值较低,并且会通过鞘层加速获得能量,因此其对钨壁材料的物理溅射是导致靶板侵蚀的主要原因,另外靶板材料的侵蚀速率随着等离子体温度升高以及杂质含量增大而急剧增大.