高功率调制脉冲磁控溅射沉积TiAlSiN纳米复合涂层结构调控与性能研究

采用高功率调制脉冲磁控溅射Al/(Al+Ti)原子比(x)分别为0.25、0.5和0.67的TiAlSi合金靶, 溅射功率1~4 kW, 氮气分压25%, 工作气压0.3 Pa, 在Si(100)和AISI 304奥氏体不锈钢基片上沉积了TiAlSiN纳米复合涂层。TiAlSiN涂层中氮含量保持在52.0at%~56.7at%之间, 均形成了nc-TiAlN/a-Si₃N₄/AlN纳米晶/非晶复合结构。随着原子比x增加, 非晶含量增加, 涂层硬度先升高而后降低。当x=0.5时, 硬度最高可达28.7 GPa。溅射功率升高可提高溅射等离子体中金属离化程度, 促进涂层调幅分解的进行, 形成了界面清晰的非晶包裹纳米晶结构, 且晶粒尺寸基本保持不变。当x=0.67时, 溅射功率由1 kW上升到4 kW时, 硬度由16.4 GPa升至21.3 GPa。不同靶材成分和溅射功率条件下沉积的TiAlSiN涂层的磨损率为(0.13~6.25)×10^-5 mm³/(N·m), 具有优良的耐磨性能。当x=0.67, 溅射功率2 kW时, nc-TiAlN/a-Si₃N₄纳米复合涂层具有最优的耐磨性能。     

高功率脉冲磁控溅射制备ZnO薄膜的研究进展

氧化锌薄膜材料由于具有高电导率、良好的光学透过率、原料储存丰富、成本低廉的特点,被认为是最具有潜力的透明导电薄膜.特别是其宽禁带(3.37eV)和高达60meV的激子束缚能,使其在环境温度制备同质结发光器件、太阳能电池电子传输层具有巨大的应用前景.然而,传统制备方法难以实现薄膜质量的综合调控,存在p-ZnO稳定性差、制...     

高功率脉冲磁控溅射电源的研制

高功率脉冲磁控溅射(HPPMS)因其高离化率而得到广泛关注.高压大电流脉冲电源是实现该技术的重要环节之一.本论文介绍了一种HPPMS电源,该电源由充电电源、斩波输出两部分组成,给出了主电路框图.分析了大电流对斩波开关过电压的影响,采用RC吸收和续流有效地抑制了电压过冲,用所研制的电源进行HPPMS镀膜试验,结果表明电源运行稳定可靠,制备的薄膜表面清洁、致密,其平均表面粗糙度很低.可以预见HPPMS技术将会促进镀膜技术的发展.     

高功率脉冲磁控溅射试验平台设计及放电特性研究

高功率脉冲磁控溅射(HPPMS)因其高离化率而得到广泛关注,是目前的热点研究方向,为此我们搭建了试验平台并对HPPMS的放电特性进行了研究.结果表明:脉冲峰值电流随脉冲电压的增加而增加,随着气压的增加而增加.本文为进一步研究高功率脉冲磁控溅射提供了硬件条件和参考.     

复合高功率脉冲磁控溅射放电等离子体特性

高功率脉冲磁控溅射具有高的金属离化率,在薄膜制备表现出巨大的优势,成为当前磁控溅射技术领域一个新的发展趋势。高功率脉冲磁控溅射的放电特性、等离子体特性等微观参数对薄膜质量控制具有决定性作用,分析宏观参数如何影响微观参数,有利于提高薄膜质量,稳定工艺。因此,本文研究了脉冲与直流电源并联模式的复合高功率脉冲磁控溅射过程中,脉冲电压(400~800 V)对Ti、Cr靶在Ar气氛中的放电特性、等离子体参数(等离子体电势、电子温度、电子密度)、基体电流的影响。结果表明:复合高功率脉冲磁控溅射Ti、Cr靶放电过程中,脉冲电压的增加有利于脉冲作用期间的靶电压、靶电流、基体电流增加;当Ti靶脉冲电压为600 V或Cr靶脉冲电压为700 V时,电子密度出现较大值。Cr靶与Ti靶放电相比,前者的靶电流、基体电流、等离子体电势、电子温度比后者更高,而电子密度却更低。     

高功率脉冲磁控溅射ZrN纳米薄膜制备及性能研究

采用高功率复合脉冲磁控溅射的方法(HPPMS)在不锈钢基体上制备ZrN纳米薄膜,并研究了不同的工作气压对薄膜形貌、相结构及各种性能的影响。采用SEM、XRD对其表面形貌和结构进行分析,发现制备的薄膜表面光滑、致密,无大颗粒,主要以ZrN(111)和ZrN(220)晶面择优生长,并呈现出多晶面竞相生长的现象。对薄膜硬度、弹性模量、耐磨性和耐腐蚀性的测试发现薄膜具有很高的硬度,最高可达33.1 GPa,同时摩擦系数均小于0.2,耐腐蚀性也都有很大提高,腐蚀电位比基体提高了0.28 V,腐蚀电流下降到未处理工件的1/5。工作气压较低时,薄膜耐磨耐蚀性能都较好,但在较高气压时,耐磨耐蚀性能出现一定的下降。     

高功率脉冲磁控溅射技术的发展与研究

高功率脉冲磁控溅射技术(HPPMS)作为一种溅射粒子离化率高、可以沉积致密、高性能薄膜的新技术已经在国外广泛研究,但在国内尚未见研究报道.本文介绍了近十年来HPPMS技术在电源、脉冲形式、放电行为和薄膜沉积等方面的研究进展.在HPPMS过程中,粒子随脉冲开关通过电子冲击和电荷交换电离,并按照双极扩散理论向基体附近传输,离子能量分布随工作气压的不同而呈现不同的分布特征.这些放电特征有利于获得更宽的工艺范围和优异的膜层性能,最后介绍了我们实验室在HPPMS方面的研究工作.     

强流脉冲电子束作用下TiCN涂层微观结构变化与性能研究北大核心CSCD

采用化学气相沉积(CVD)技术在硬质合金基体表面制备TiCN涂层,随后利用强流脉冲电子束(HCPEB)对TiCN涂层表面进行辐照处理。通过X射线衍射仪(XRD)、扫描电子显微镜(SEM)等仪器观察了HCPEB辐照前后TiCN涂层的微观结构变化,并对比分析了其显微硬度和耐磨性能。结果表明:HCPEB辐照前后TiCN涂层的相组成保持不变,但相衍射峰的位置发生偏移且有所宽化,表明涂层晶粒细化,同时涂层内部应力状态发生改变;辐照后涂层表面粗大的晶粒消失,涂层变得光滑平整;随着辐照次数的增加,涂层的厚度逐渐减小。显微硬度和摩擦磨损试验结果表明,HCPEB辐照显著增加了TiCN涂层的表面显微硬度,其耐磨性能得到显著提升。涂层表面粗糙颗粒的消除、涂层晶粒细化、高密度晶体缺陷的形成以及涂层内部残余应力的改变是HCPEB辐照TiCN涂层性能改善的主要原因。     

工作参数对磁场增强高功率脉冲磁控溅射放电特性的影响

研究磁场增强高功率脉冲磁控溅射技术的放电特性在不同工作参数下的演变规律。利用数字示波器采集HiPIMS的基体离子电流用于表征其放电特性的变化。结果表明:靶放电电压不同时基体离子电流对工作气压的响应不同, 较低靶电压时基体离子电流平均值随工作气压的增加逐渐增加;而较高靶电压时基体离子电流平均值随工作气压增加迅速增加后趋于稳定。基体离子电流随基体偏压的变化表现出两个特征, 较低基体偏压时的基体离子电流在脉冲开始阶段呈现出较强的电子流波段, 而基体偏压较高时则未出现电子流。不同脉冲频率及靶电压下的基体离子电流的波形形状大致相似, 但当处于较高靶电压时存在一个明显特征, 即当脉冲结束后离子流会出现一个尖锐峰值。随脉冲宽度的增加, 基体离子电流负向电子流和正向离子流均逐渐增大。     

高功率脉冲磁控溅射氩氮比对ZrN薄膜结构及性能的影响

采用高功率复合脉冲磁控溅射的方法(HPPMS)在不锈钢基体上制备ZrN薄膜,对比DCMS方法制备的ZrN薄膜,得出HPPMS制备的薄膜表面更平整光滑、致密,既无空洞、又无大颗粒等缺陷。Ar/N对薄膜相结构及硬度、耐磨耐蚀等有较大影响。XRD结果显示,薄膜主要以ZrN(111)和ZrN(220)晶面择优生长,并呈现出多晶面竞相生长的现象。制备的ZrN薄膜的硬度最高可达33.1 GPa,同时摩擦系数小于0.2,耐腐蚀性也有很大提高,腐蚀电位比基体提高了0.27 V,腐蚀电流下降到未处理工件的1/5。存在一个合适的Ar/N比,使得制备的ZrN薄膜具有较好的耐磨性和耐腐蚀性。     

Mitigating the geometrical limitations of conventional sputtering by controlling the ion-to-neutral ratio during high power pulsed magnetron sputtering

High power pulsed magnetron sputtering has been used to grow thin chromium layers on substrates facing and orthogonal to the target. It is demonstrated that at low peak target current density, j_T < 0.6 A/cm² corresponding to a low ion-to-neutral flux ratio, films grown on substrates facing the target exhibit in-plane alignment. This is due to the rectangular shape of the target that yields an asymmetry in the off-normal flux of sputtered species. With increasing j_T the biaxial alignment degrades, as the major portion of the incoming flux (ions) can be effectively steered by the electric field of the substrate to remove asymmetry imposed by geometrical restrictions. Eventually, at j_T = 1.7 A/cm² a fiber texture is obtained. For films grown on substrates orthogonal to the target, the large column tilt characteristic for growth at low j_T, decreases with increasing ion content in the flux and almost disappears at the highest value of j_T. The latter indicates that material flux to the substrate is highly ionized so that deposition takes place along substrate normal despite the high nominal inclination angle. Thus, in the limit of high j_T the artifacts of conventional physical vapor deposition, resulting from the line-of-sight deposition, are effectively eliminated and the film growth proceeds more or less unaffected by the substrate orientation. Samples mounted orthogonally thus possess a similar texture, morphology, and topography as those facing the target.     

Thermochromic properties of vanadium oxide films prepared by dc reactive magnetron sputtering

A transparent vanadium oxide film has been one of the most studied electrochromic (EC) and Thermochromic (TC) materials. Vanadium oxide films were deposited at different substrate temperatures up to 400 °C and different ratios of the oxygen partial pressure (P_O2). SEM, AFM and X-ray diffraction's results show detail structure data of the films. IR mode assignments of the films measured by IR reflection-absorbance in NGIA (near grazing incidence angle) are given. It is found that the film has V₂O₅ and VO₂ combined structures. The films exhibit clear changes in transmittance when the environment temperature (T_e) is varied, especially in the 3600-4000 cm^− 1 range. Applying a T_e that is higher than a critical temperature (T_c) to the samples, the as-RT (room temperature) deposited film with 9% P_O2 has a transmittance variation of 30%, but the films that were deposited on a heated substrate of 400 °C have little variation. There is tendency of bigger variation in transmittance for the sample deposited at a larger P_O2, when it is applied by 200 °C T_e.     

利用脉冲直流磁控溅射制备ZnO:Al薄膜的研究

利用中频脉冲直流磁控溅射法制备了平面ZnO:Al(AZO)透明导电薄膜,研究了沉积压力、衬底温度和溅射功率对AZO薄膜光电性能、薄膜稳定性的影响.结果表明:在较低沉积压力、衬底温度及溅射功率下,可获得具有低电阻率、高透过率、高稳定性的AZO薄膜.     

磁控溅射TiAlNO薄膜的结构与力学性能

采用独立的Ti靶和Al靶,用射频反应磁控溅射方法,逐步控制氧流量在高速钢（W18Cr4V）基体上沉积了一系列具有不同氧含量的TiAlNO薄膜。研究了氧流量对薄膜组织结构、硬度和摩擦性能的影响。结果表明,在（Ti,Al）N中加入氧形成由（Ti,Al）（N,O）纳米晶和（TiO2,Al2O3）非晶组成的复合结构。随着氧流量的增加,薄膜中晶体相晶格常数逐步减小,其取向则逐步从（111）为主转变为（111）和（200）混合。同时薄膜硬度缓慢地下降,摩擦系数和磨损量先减少后增大,在氧流量为0．9sccm时达到最小值。研究同时表明,当氧流量为0．9sccm时薄膜具有最小摩擦系数和高耐磨性,同时保持了高硬度,综合性能最好。     

磁控溅射制备ITO薄膜光电性能的研究

采用直流磁控溅射方法在玻璃基底上制备了ITO薄膜.分别用分光光度计和四探针仪测试了所制备ITO薄膜在可见光区域内的透过率和电阻率,研究了溅射气压、氧氩流量比和溅射功率三个工艺参数对ITO薄膜光电性能的影响.研究结果表明,制备ITO薄膜的最佳工艺参数为:溅射气压0.6 Pa,氧氩流量比1:40,溅射功率108 W.采用此工艺参数制备的ITO薄膜在可见光区平均透过率为81.18％,薄膜电阻率为8.9197×10-3Ω·cm.     

Hysteresis-free reactive high power impulse magnetron sputtering

High power impulse magnetron sputtering (HIPIMS) of an Al target in Ar/O₂ mixtures has been studied. The use of HIPIMS is shown to drastically influence the process characteristics compared to conventional sputtering. Under suitable conditions, oxide formation on the target as the reactive gas flow is increased is suppressed, and the hysteresis effect commonly observed as the gas flow is varied during conventional sputtering can be reduced, or even completely eliminated, using HIPIMS. Consequently, stoichiometric alumina can be deposited under stable process conditions at high rates. Possible explanations for this behavior as well as a model qualitatively describing the process are presented.     

Structural properties of Eu-doped GaN films prepared by RF magnetron sputtering

Films of Eu-doped GaN (GaN:Eu) were grown on c-plane of sapphire (c-Al₂O₃), GaAs(1 0 0), Si(1 0 0) and glass substrates by RF magnetron sputtering method. The X-ray diffraction (XRD) measurement of the sputtered film was carried out. For GaN:Eu and undoped GaN, the lattice constants c and a of as-grown films were larger than those of the bulk GaN. After annealing, the lattice constants c and a of the films decreased.     

Effects of heat treatment on properties of ITO films prepared by rf magnetron sputtering

Indium tin oxide (ITO) films were deposited on glass substrates by rf magnetron sputtering using a ceramic target (In₂O₃-SnO₂, 90-10 wt%) without extra heating. The post annealing was done in air and in vacuum, respectively. The effects of annealing on the structure, surface morphology, optical and electrical properties of the ITO films were studied. The results show that the increase of the annealing temperature improves the crystallinity of the films, increases the surface roughness, and improves the optical and electrical properties. The transmittance of the films in visible region is increased over 90% after the annealing process in air or in vacuum. The resistivity of the films deposited is about 8.125×10⁻⁴ Ω cm and falls down to 2.34×10⁻⁴ Ω cm as the annealing temperature is increased to 500°C in vacuum. Compared with the results of the ITO films annealed in air, the properties of the films annealed in vacuum is better.     

钢基耐磨SiC薄膜制备研究

用磁控溅射的方法在40Cr钢的表面制得了SiC薄膜.通过X射线衍射、傅里叶红外光谱分析、摩擦磨损以及划痕试验研究了工艺参数、溅射方式对薄膜性能的影响.结果表明:室温下,用磁控溅射法制备的SiC薄膜具有非晶态结构;傅立叶红外光谱证实了薄膜中除了Si-C键的存在外还有大量的Si-Si键;在相同的工艺参数下用射频溅射法制备的薄膜表面更为光滑致密,与基体结合更好;采用射频溅射法,在功率200W,时间为2h,工作气压为0.1Pa条件下制备的SiC薄膜性能最佳.     

非平衡磁控溅射沉积Ta-N薄膜的结构与电学性能研究

采用直流反应非平衡磁控溅射技术在单晶Si(100)和玻璃表面沉积氮化钽(Ta-N)薄膜,分别测试了薄膜的结构、成分、电阻率和吸收光谱,研究了氮氩流量比(N2∶Ar)变化对Ta-N薄膜的结构和电学性能的影响.研究结果表明随N2∶Ar增加,依次生成六方结构的γ-Ta2N、面心立方结构(fcc)的δ-TaNx、体心四方结构(bct)的TaNx;N2∶Ar在0.2～0.8的范围内,Ta-N薄膜中只存在着fcc δ-TaNx;当N2∶Ar＞1之后,Ta-N薄膜中fcc δ-TaNx和bct TaNx共存.Ta-N薄膜电阻率随N2∶Ar流量比增加持续增加,当N2∶Ar为1.2时,薄膜变为绝缘体,光学禁带宽度为1.51eV.