Deposition of Ti/C nano-composite DLC films by magnetron DC sputtering with dual targets

Deposition of Ti/C nano-composite DLC films by magnetron DC sputtering was examined using dual targets of titanium and carbon, in order to in order to investigate the effects of Ti/C nano-composite structure on its mechanical properties such as hardness or physical properties such as electrical resistivity. The deposition of DLC films or Ti/C nano-composite DLC films was respectively carried out in the atmosphere of argon at the pressure of 0.4 Pa by sputtering of only the carbon target or by co-sputtering of both the carbon one and the titanium one. The DLC film obtained in this study looked semitransparent and dark brown, while the Ti/C nano-composite DLC one looked metallic and light gray. According to Raman spectroscopy, a typical spectrum for DLC was detected for the metal-like titanium containing composite DLC films even though it's intensity was rather small. And it was found that the G band slightly shifted to higher wave numbers and the shoulder D band was enhanced, compared to the spectrum for the DLC films. Furthermore, based on both the indentation hardness and the electrical resistivity of the obtained films, it was assumed that the miniaturization of titanium phase might bring the increase in hardness.     

Multilayer DLC coatings via alternating bias during magnetron sputtering

To combat the high residual stress problem in monolayer diamond-like carbon coatings, this paper fabricated multilayer diamond-like carbon coatings with alternate soft and hard layers via alternating bias during magnetron sputtering. The surface, cross sectional morphology, bonding structures and mechanical properties are investigated. The atomic force microscopy images indicate low bias results in rougher surface with large graphite clusters and voids suggesting low coating density. The multilayered coatings demonstrate relatively smooth surface stemming from higher bias. The cross sectional images from field emission scanning electron microscopy indicate coating thickness decreases as substrate bias increases and confirm that higher bias results in denser coating. Delamination is observed in monolayer coatings due to high residual stress. The trend of sp³/sp² fraction estimated by X-ray photoelectron spectroscopy is consistent with that of I_D/I_G ratios from Raman spectra, indicating the change of bonding structure with change of substrate bias. Hardness of multilayer diamond-like carbon coating is comparable to the coatings deposited at low constant bias but the adhesion strength and toughness are significantly improved. Alternately biased sputtering deposition provides an alternative when combination of hardness, toughness and adhesion strength is needed in an all diamond-like carbon coating.     

Synthesis of DLC films by PECVD combined with hollow cathode sputtering

The mechanical and electrical properties of aluminium-doped diamond-like carbon (DLC) thin films obtained with a hybrid method combining hollow magnetron discharge sputtering and plasma-enhanced chemical vapour deposition (PECVD) are reported. The ratio between the mass flows of methane reactive gas and argon inert gas was found to have a big influence on the properties of doped DLC films. For low mass flow of methane gas the cathode surface was kept in a metallic state. By increasing methane mass flow the cathode surface became to be covered with DLC and the behaviour of the discharge changed, influencing the properties of deposited films. The lowest resistivity (10⁻⁴ Ω cm) of thin films was obtained in the metallic state of the cathode but without DLC character, as indicated by Raman measurements. The resistivity increased in the intermediate mode (0.01 Ω cm) and attained higher value (1 Ω cm) in the poisoned state of the cathode. These films presented DLC character, with D and G bands, as revealed by Raman measurements.     

Hydrogen-free diamond-like carbon films prepared by microwave electron cyclotron resonance plasma-enhanced direct current magnetron sputtering

Hydrogen-free diamond-like carbon (DLC) films were prepared by means of microwave electron cyclotron resonance plasma enhanced direct current magnetron sputtering. To study the influence of enhanced plasma on film fabrication and properties, the structures as well as mechanical and electrical properties of these films were studied as a function of applied microwave power. Results showed that higher microwave power could induce higher plasma density and electron temperature. The hardness increased from 3.5 GPa to 13 GPa with a variation of microwave power from 0 W to 1000 W. The resistivity showed a drastic increase from 4.5 × 10⁴ Ωcm at 0 W to 1.3 × 10¹⁰ Ωcm at 1000 W. The variation of the intensity ratio I(D)/I(G) and the position of the G-peak of the DLC films with respect to changes in microwave power were also investigated by Raman spectroscopy.     

非平衡磁控溅射无氢DLC增透膜的研制

非平衡磁控溅射(UBMS)技术近年来得到了广泛地应用.采用该技术制备的类金刚石薄膜(DLC)具有许多独特的性质.本文利用正交实验方法,对非平衡磁控溅射技术制备无氢DLC膜增透膜进行了研究,得到了影响薄膜光学性能的主要因素和最佳的制备工艺.结果表明,非平衡磁控溅射制备的无氢DLC膜具有较宽的光谱透明区,锗基底单面沉积DLC膜,其峰值透射率达到61.4%,接近理论值.     

直流磁控溅射制备PbTe薄膜

采用直流磁控溅射的方式，用PbTe靶材溅射沉积在玻璃基底上得到了PbTe薄膜，薄膜生长速率约为100nm／min，通过控制溅射时间可沉积几纳米到几微米的不同厚度的薄膜。PbTe薄膜是面心立方结构的纤维状生长的薄膜，溅射沉积时间对薄膜的晶粒大小和结构有较大影响，溅射时间越长薄膜的晶粒越大，薄膜结构越致密，具有片层状结构。得到的PbTe薄膜是富Te的P型半导体薄膜，其电阻率随着薄膜厚度的增大而减小。     

微波ECR等离子体源增强非平衡磁控溅射DLC膜的制备与表征

介绍了微波ECR等离子体源增强非平衡磁控溅射设备的结构和工作原理,详细叙述了利用该设备制备类金刚石膜的过程。Raman光谱证实了薄膜的类金刚石特性;采用原子力显微镜(AFM)观察薄膜的微观表面形貌,均方根粗糙度大约为1．9nm,结果表明薄膜表面非常光滑;利用CERT微摩擦计进行摩擦、磨损和划痕实验,薄膜的平均摩擦系数较小,大约为0．175;DLC膜和Si衬底磨损情况的扫描电镜图片相对比,可以看到DLC膜的磨痕小的多,说明薄膜有较好的耐磨性能;划痕测试结果表明制备薄膜临界载荷大约为40mN。     

Electrical and structural characterization of DLC films deposited by magnetron sputtering

In this work diamond-like carbon (DLC) films were deposited by d.c. magnetron sputtering using a graphite target and argon as the discharge gas. Hydrogen gas was introduced in the discharge chamber to produce hydrogenated DLC films. By increasing the hydrogen flow from zero to 22% of the total flow, the following modifications of the film properties were observed: a decrease in the r.m.s. roughness (from 0.45 to 0.21 nm); an increase in the electrical resistivity (from 5×10⁶cm to 2.55×10⁸cm , while the relative dielectric constant remained almost constant at about 3.3. Increasing the substrate temperature, we observed a logarithmic decrease of the electrical resistivity of the films, caused by a self-annealing process of the DLC film during the deposition. This decrease was faster for the hydrogenated films, due to the additional effect of the dehydrogenation. The Raman spectra analyses of these films are in agreement with these observations.     

非平衡磁控溅射DLC薄膜应力研究

类金刚石（DLC）薄膜可用作红外增透保护膜,高的薄膜残余应力造成薄膜附着力下降是目前应用中存在的主要问题之一。本文从DLC薄膜作为红外增透保护膜的需求出发,采用非平衡磁控溅射技术生长DLC薄膜。实测了薄膜的残余应力,分析研究了薄膜残余应力在不同工艺条件下的变化情况。探讨了薄膜残余应力与薄膜厚度、光学透过率、离子能量、沉积速率以及能流密度之间的关系。研究结果表明,薄膜残余应力平衡值在0．9～2．2GPa之间,相应的单面镀膜样片的透过率在4μm波长处为69％～63％,随工艺的不同而变化。工艺优化后薄膜残余应力显著下降。硅基底上薄膜与基底剥离的力的临界值大于2160GPa．nm,最大薄膜厚度≥2400nm;锗基底上最大薄膜厚度≥2000nm,可以满足整个红外波段的需求。     

直流磁控溅射制备TiNxOy薄膜的性能研究

利用直流磁控溅射技术在玻璃衬底上制备了TiNxOy薄膜样品,研究了溅射过程中电压与N2流量之间的迟滞效应,通过X射线衍射（XRD）、UV-Vis分光光度计、四探针电阻仪等测试手段表征了样品的物相、光吸收谱、电阻等性能。结果表明：随着N2含量的提高和薄膜厚度的增加,XRD显示薄膜样品出现明显的衍射峰,吸收光谱向可见光方向展宽至500nm,电阻随着N2含量的提高呈逐渐下降的趋势。     

直流磁控溅射制备大面积AZO透明导电薄膜

采用直流磁控溅射工艺于200℃的玻璃基板制备了大面积AZO透明导电薄膜。重点研究了样品晶体结构、方阻、可见光透过率、样品形貌等随其位置变化的情况。研究表明,大面积AZO薄膜的晶体结构、可见光透过率、样品形貌等随样品位置变化比较小,大面积AZO样品均按C轴取向生长,表面平整,晶粒尺寸为20 nm左右。在本实验条件下获得的大面积AZO薄膜方阻在86～110Ω/□范围内,方阻线性变动率为28%,样品电阻率为6.34～7.26×10-4Ω·cm,可见光平均透过率均高于87%。     

Surface plasmon characteristics of nanocrystalline gold/DLC composite films prepared by plasma CVD technique

Composite films containing gold nanoparticles embedded in diamond-like carbon (Au–DLC) matrix were deposited on glass and Si (1 0 0) substrates by using capacitatively coupled plasma (CCP) chemical vapour deposition technique (CVD). Particle size and metal volume fraction varied between 2.7–3.5 nm and 0.04–0.7, respectively with the amount of argon in the methane + argon gas mixture in the plasma. Bonding environment in these films were obtained from XPS, Raman and FTIR studies. Microstructural studies were carried out by SEM, XRD and TEM studies. Blue-shift of the surface plasmon resonance peak (located 540–561 nm) in the optical absorbance spectra of the films could be associated with the reduction of the particle size while red shift was associated with the increase in volume fraction of metal particles. The experimental results have been discussed in light of the core–shell model.     

Mn-doped ZnO transparent conducting films deposited by DC magnetron sputtering

Mn-doped zinc oxide (ZnO:Mn) thin films with low resistivity and relatively high transparency were firstly prepared on glass substrate by direct current (DC) magnetron sputtering at room temperature. Influence of film thickness on the properties of ZnO:Mn films was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) show that all the deposited films are polycrystalline with a hexagonal structure and have a preferred orientation along the c-axis perpendicular to the substrate. As the thickness increases from 144 to 479 nm, the crystallite size increases while the electrical resistivity decreases. However, as the thickness increases from 479 to 783 nm, the crystallite size decreases and the electrical resistivity increases. When film thickness is 479 nm, the deposited films have the lowest resistivity of 2.1 × 10^− 4 Ω cm and a relatively high transmittance of above 84% in the visible range.     

磁控溅射ITO薄膜的退火处理

采用直流磁控溅射方法在室温下玻璃基板上制备ITO(Indium tin oxide)薄膜,并在真空中不同温度(100℃~400℃)下退火处理.研究了退火对薄膜表面形貌、电光特性的影响.XRD测试发现薄膜在200℃退火后结晶,优选晶向为(222).随退火温度升高,方块电阻迅速下降,表面更加平整,薄膜在可见光范围平均透过率提高到85%.     

Amorphous indium tungsten oxide films prepared by DC magnetron sputtering

Indium-tungsten-oxide (IWO) films were prepared by dc magnetron sputtering at ambient substrate temperature (T_s). Characteristics of the films were compared with those of In₂O₃–SnO₂ (ITO) thin films prepared under the same condition. The sputter-deposited IWO films have entirely amorphous structure with an average transmittance of over 85% in the visible range and exhibit a minimum resistivity of 3.2 × 10^–4cm at W content [W/(In + W)] of 0.57 at.%. An in-situ heating X-ray diffraction measurement have shown that the crystallization temperature of IWO films is higher than those of ITO films (150–160C) and increases with increasing W content. This enabled a smooth amorphous surface of IWO films as compared with a rough surface of partially crystallized ITO films as revealed by an atomic force microscopy. IWO films are useful for transparent electrode of organic light emitting diode and polymer LCDs because of the low resistivity, high transparency and smooth surface obtainable by the conventional dc magnetron sputtering at room temperature.     

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.     

Electrical characterisation of AlCuMo thin films prepared by DC magnetron sputtering

Thin film resistors have been manufactured to evaluate the electrical performance characteristics of AlCuMo thin films. The films were prepared on Al2O3 substrates at room temperature as a function of Mo concentration by DC magnetron sputtering and were then annealed at various temperatures in air and N2 atmospheres. The effect of annealing temperature on the electrical properties of the films was systematically investigated. Increase in Mo content produced a decrease in temperature coefficient of resistance (TCR), an increase in resistivity (r) and an improvement in long term stability (DV/V) of the films. TCR varied from negative to positive and further improvements in resistance stability of the films were also achieved through increasing annealing temperature in both air and N2 atmospheres. A temperature region is proposed where `near zero? TCR (ppm/8C) and long term stability of better than 0.2% can be realised.     

直流磁控溅射铝纳米颗粒膜的微结构及电学特性

采用直流磁控溅射法,以高纯铝(99.99%)为靶材,高纯氩气(99.999%)为起辉气体,在经机械抛光的单晶Si衬底上制备铝纳米颗粒薄膜。利用X射线衍射仪(XRD)、光学薄膜测厚仪、扫描电子显微镜(SEM)和四探针测试仪分别测试了铝纳米颗粒薄膜的晶相结构、薄膜厚度、表面形貌及电阻率。XRD衍射图谱表明此薄膜为面心立方的多晶结构,择优取向为Al(111)晶面。随溅射功率由30 W增至300 W,铝纳米颗粒薄膜的沉积速率由3.03 nm/min增加至20.03 nm/min;而随溅射压强由1 Pa增加至3 Pa,沉积速率由2.95 nm/min降低到1.66 nm/min。在溅射功率为150 W,溅射压强为1.0 Pa条件下制备的样品具有良好的晶粒分布。随溅射功率从80 W增大到160 W,样品电阻率由4.0×10-7Ω·m逐渐减小到1.9×10-7Ω·m;而随溅射压强从1 Pa增至3 Pa,样品电阻率由1.9×10-7Ω·m增加到7.1×10-7Ω·m。     

基体偏压对中频磁控溅射沉积DLC膜结构的影响

利用中频非平衡磁控溅射技术,以氩气和甲烷混合气体为工作气体,在载玻片和单品硅片上沉积含氢的类金刚石簿膜.改变加载在基体上的负偏压,在0～400 V范围内,制备5种偏压值下的薄膜,研究偏压对薄膜结构的影响.用光学显微镜和AFM考察薄膜的光学形貌;激光Raman谱定性分析膜的化学组分;VFIR分析其C-H键合类型;纳米压痕法测量膜的硬度.结果表明:当基体上施加偏压-100 V时,可以有效地提高沉积粒子与基体结合力以及溥膜的致密性,薄膜中正四面体的sp3结构和sp3CHn含最增加,纳米硬度提高.     

磁控溅射制备ZrN_x薄膜离子导体性能研究

采用射频反应磁控溅射工艺,以纯Zr为靶材,在WO3/ITO/Glass基片上采用不同工艺参数沉积ZrNx薄膜,用紫外-可见分光光度计、循环伏安法、X射线衍射仪、扫描电镜等研究了ZrNx薄膜的离子导电性能。研究结果表明,所制备的ZrNx薄膜为非晶态,ZrNx/WO3/ITO/Glass复合膜的光学调节范围最大达57%以上,在离子传导过程中表现出良好的离子导电性能。