激光制备类金刚石膜技术研究

现有技术制备的类金刚石(DLC)膜由于含氢、硬度低、内应力大、附着力差等特点,严重限制了其光学工程应用.激光法是近年发展的一种制备DLC膜的新方法,相比其他制备方法具有诸多优点.综合分析了激光制备DLC膜过程中,激光波长、脉宽、功率密度、衬底温度和偏压等因素对薄膜质量的影响规律.采用氧气氛辅助沉积、元素掺杂和双波长激光...     

硫化锌基底硬质红外保护薄膜技术研究

硫化锌在3~5μm和7.7~9.3μm两个波段具有较高透过率,但其脆性大、耐摩擦性能较差,在其表面镀制类金刚石膜保护膜可显著提高其使用性能。直接在硫化锌基底沉积类金刚石膜难以实现,采用匹配层与过渡层的设计思想,制备出类金刚石膜与硫化锌基底之间相互牢固结合的过渡层。通过等离子体化学气相增强法在过渡层上成功制备类金刚石膜。研究了射频功率、气压等对保护膜系力学性能的影响。结果表明,镀制了硬质保护薄膜的硫化锌窗口在3~5μm和7.7~9.3μm双波段的平均透过率均高于90%,膜层硬度为硫化锌窗口近5倍。经环境试验之后,膜层光学性能与机械性能均无变化。     

RF-PECVD法制备大面积类金刚石薄膜性能的研究

采用RF-PECVD法在锗、硅红外光学窗口上制备了大面积(基底直径φ=150～250mm)类金刚石薄膜.采用拉曼光谱分析了大面积DLC膜的结构组成,对RF-PECVD法制备的大面积DLC膜的均匀性、红外光学性能、机械力学性能以及其抗恶劣环境的能力进行了检测和分析.膜层厚度均匀性在3%以内.锗、硅红外窗口双面镀制DLC膜后,极值透过率分别达92%和96%以上,可显著提高红外光学窗口的显微硬度.膜层具有极强的抗盐雾、耐海水腐蚀和抗摩擦的能力.     

常温溅射DLC膜的工艺研究

常温下,采用磁控溅射技术成功地在Ge基底上制备了类金刚石膜,并研究了溅射功率、碳氢气体与氩气流量比、溅射频率、基底负偏压等工艺参数对类金刚石膜沉积速率的影响和薄膜的光学性能。结果表明：溅射功率、溅射频率、碳氢气体与氩气流量比对沉积速率有显著的影响。沉积速率随着溅射功率的增大而增大,随着溅射频率的减小而增大。随着碳氢气体与氩气流量比、基底负偏压的增大沉积速率先增大后降低。制备的类金刚石膜具有较宽的光谱透明区,Ge基底单面沉积的类金刚石膜其峰值透过率最高达到63．99％。     

W过渡层结合界面对金刚石薄膜在WC-6%Co上的附着力的影响

 在微波等离子体化学气相沉积装置中,采用负偏压形核等方法,研究两种不同的W过渡层/基体结合界面对金刚石薄膜与WC-6%Co附着力的影响。采用氢等离子体脱碳、磁控溅射镀W、高偏压碳化等方法,在YG6衬底表面形成化学反应型界面,W膜在碳化时和基体WC连为一体,极大地增加了W膜与基体的附着力,明显优于直接镀钨、碳化形成的物理吸附界面。在高负偏压下碳化,能提高表面粗糙度,增加膜与基体机械钳合,而负偏压形核增加核密度,从而增加膜与基体的接触面积,结果极大地提高了金刚石薄膜的附着力。     

不同方法制备的类金刚石薄膜的XPS和Raman光谱的研究

分别利用金属脉冲磁过滤真空阴极弧沉积法(FCVA)、直流磁控溅射法(SP)和脉冲辉光放电等离子体化学气相沉积法(PECVD)在硅片上沉积类金刚石膜层.并利用激光拉曼光谱法(Raman spectroscopy)和X射线光电子能谱法(XPS)对类金刚石膜层进行研究.通过研究分析发现,不同方法制备的类金刚石膜层的G峰位、D...     

脉冲激光沉积无氢钨掺杂类金刚石膜的摩擦与机械性能

采用脉冲激光沉积技术制备出无氢钨掺杂非晶态类金刚石膜.膜中的钨含量与靶材中的钨含量保持稳定的线性关系,显示了脉冲激光沉积在难熔金属掺杂技术方面的亮点.由于碳-钨结构的形成和表面粗糙度影响,膜层的干摩擦系数随着钨含量的增加显现出先减后增的趋势,钨含量为9.67 at.%时达到最低值0.091.钨含量的增大降低了类金刚石膜纳米硬度和杨氏模量,但最佳的膜层耐磨性参数并非表现在硬度最大(52.2 GPa)的纯类金刚石膜中,而是出现在低掺杂含量(6.28 at.%)的类金刚石膜中.研究为脉冲激光沉积技术制备低摩擦、高硬度无氢钨掺杂类金刚石膜的应用提供了技术实践.     

红外高效增透膜镀类金刚石膜的特性研究

外层为氟化物的红外高效膜、膜层软、易吸潮和氧化.本文提出使用类金刚石膜做红外高效膜的保护膜,讨论了镀制类金刚石膜后,镀膜件光谱特性的变化情况.     

蓝宝石基底可见光/激光/中红外多光谱窗口薄膜研究

研究了一种以蓝宝石为基底的可见光/激光/中红外"三光合一"窗口保护型硬质增透膜。首先开展了蓝宝石基底无吸收型硬质氧化物膜层的制备及其工艺最优化的研究,同时基于离子源工艺参数与反应气体流量的控制实现一种中波无吸收的低折射率Si_(1-x)O_x膜层,从而实现了全氧化物膜系在中红外波段上的应用。以此为基础,对蓝宝石基底可见光/激光/中红外三波段窗口膜系进行了优化设计与沉积仿真研究。经过大量镀制实验与工艺改进,最终制备出光学与机械性能良好的"三光合一"窗口薄膜,可见光至中红外波段上的平均透过率达到95%以上。镀膜样品一次性通过高低温试验、恒定湿热试验以及重度磨擦试验等。试验结果表明,膜层致密性和表面机械性能良好,具备一定强度的防潮防腐能力和抗激光损伤阈值水平,可适应海洋环境光电窗口的应用需求。     

激光技术的一种特殊应用--镀类金刚石膜的探讨

讨论了类金刚石膜的特性及应用，介绍了激光镀膜系统的结构原理．探讨了激光镀类金刚石膜的特点及金刚石膜生成工艺中的关键问题及解决途径．     

The effect of applied negative bias voltage on the structure of Ti-doped a-C:H films deposited by FCVA

Ti-doped hydrogenated diamond-like carbon (DLC) films were deposited on Si(1 0 0) substrates by a filtered cathodic vacuum arc (FCVA) method using Ar and CH₄ as the feedstock. The composition and microstructure of the films were investigated by Raman spectroscopy, X-ray photoelectron spectroscopy and IR spectroscopy. The internal stress was determined by the radius of curvature technique. The influence of the bias voltage on the microstructure of the as-deposited films was investigated. It was found that the graphite-like bonds was dominated in the Ti-doped DLC film deposited at 0 V bias voltage. When bias voltage was increased to −150 V, more diamond-like bond were produced and the sp³ content in film reached the maximum value, after which it decreased and more graphite-like bonds feature produced with further increase of the negative bias voltage. The compressive internal in the Ti-doped DLC films also exhibited a maximum value at −150 V bias voltage. IR results indicated that CH bonded intensity reduced, and H atoms bonded with C atoms were substituted for the Ti atoms as the negative bias voltage increasing. All the composition and microstructure change can be explained by considering the plasma conditions and the effect of negative bias voltage applied to the substrate.     

The microstructure, mechanical and friction properties of protective diamond like carbon films on magnesium alloy

Protective hard coatings deposited on magnesium alloys are believed to be effective for overcoming their poor wear properties. In this work, diamond-like carbon (DLC) films as hard protective films were deposited on AZ91 magnesium alloy by arc ion plating under negative pulse bias voltages ranging from 0 to −200 V. The microstructure, composition and mechanical properties of the DLC films were analyzed by scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and nanoindentation. The tribological behavior of uncoated and coated AZ91 magnesium alloy was investigated using a ball-on-disk tribotester. The results show that the negative pulse bias voltage used for film deposition has a significant effect on the sp³ carbon content and mechanical properties of the deposited DLC films. A maximum sp³ content of 33.3% was obtained at −100 V, resulting in a high hardness of 28.6 GPa and elastic modulus of 300.0 GPa. The DLC films showed very good adhesion to the AZ91 magnesium alloy with no observable cracks and delamination even during friction testing. Compared with the uncoated AZ91 magnesium alloy, the magnesium alloy coated with DLC films exhibits a low friction coefficient and a narrow, shallow wear track. The wear resistance and surface hardness of AZ91 magnesium alloy can be significantly improved by coating a layer of DLC protective film due to its high hardness and low friction coefficient.     

The protective properties of ultra-thin diamond like carbon films for high density magnetic storage devices

With the increase of magnetic storage density, the thickness of the protective diamond like carbon (DLC) film on the surfaces of head and disk is required as thin as possible. In this paper, the structure, mechanical properties and corrosion and oxidation resistance of ultra-thin DLC films are investigated. The ultra-thin DLC films were deposited by using filtered cathodic vacuum arc (FCVA) technique. The exact thickness of the ultra-thin DLC film was determined by high resolution transmission electron microscope (HRTEM). Raman analysis indicates that the ultra-thin DLC film presents ta-C structure with high sp³ fraction. In the wear test, a diamond tip was used to simulate a single-asperity contact with the film surface and the wear marks were produced on the film surface. The wear depths decrease with film thickness increasing. If the film thickness was 1.4 nm or above, the wear depth was much lower than that of Si substrate. This indicates that the ultra-thin DLC film with thickness of 1.4 nm shows excellent wear resistance. Corrosion tests in water and oxidation tests in air were carried out to investigate the diffusion barrier effect of the ultra-thin DLC films. The results show that the DLC film with thickness of 1.4 nm provides adequate coverage on the substrate and has good corrosion and oxidation resistance.     

Studies of diamond-like carbon （DLC） films deposited on stainless steel substrate with Si/SiC intermediate layers

In this work, diamond-like carbon （DLC） films were deposited on stainless steel substrates with Si/SiC intermediate layers by combining plasma enhanced sputtering physical vapour deposition （PEUMS-PVD） and microwave electron cyclotron resonance plasma enhanced chemical vapour deposition （MW-ECRPECVD） techniques. The influence of substrate negative self-bias voltage and Si target power on the structure and nano-mechanical behaviour of the DLC films were investigated by Raman spectroscopy, nano-indentation, and the film structural morphology by atomic force microscopy （AFM）. With the increase of deposition bias voltage, the G band shifted to higher wave-number and the integrated intensity ratio ID/IG increased. We considered these as evidences for the development of graphitization in the films. As the substrate negative self-bias voltage increased, particle bombardment function was enhanced and the sp^3-bond carbon density reducing, resulted in the peak values of hardness （H） and elastic modulus （E）. Silicon addition promoted the formation of sp^3 bonding and reduced the hardness. The incorporated Si atoms substituted sp^2- bond carbon atoms in ring structures, which promoted the formation of sp^3-bond. The structural transition from C-C to C-Si bonds resulted in relaxation of the residual stress which led to the decrease of internal stress and hardness. The results of AFM indicated that the films was dense and homogeneous, the roughness of the films was decreased due to the increase of substrate negative self-bias voltage and the Si target power.     

液相电化学法制备类金刚石薄膜及其摩擦性能研究

采用自行设计的液相法沉积装置,以甲醇有机溶剂作为碳源,利用液相电化学沉积技术在不锈钢及Si基底上制备了类金刚石薄膜;用扫描电镜、Raman光谱仪表征了沉积薄膜的表面形貌和结构;用UMT-2M摩擦磨损试验机对两种沉积薄膜进行了摩擦性能测试。结果表明:经电化学沉积的类金刚石薄膜均匀、致密,表面粗糙度小;Raman光谱在1 332cm-1处有强的谱峰,与金刚石的特征峰相吻合,其中不锈钢基底上薄膜的sp3含量更高;不锈钢基底沉积膜的摩擦系数为0.12,Si片基底沉积膜的摩擦系数为0.10;不锈钢基底沉积膜的耐磨性较Si片沉积膜高。     

高透过率红外窗口保护薄膜的研制

在Si、Ge红外窗口上利用离子辅助电子束蒸发技术和RF-PECVD技术制备了具有高透过率的AR／DLC保护薄膜,并与单层DLC保护薄膜的光学性能进行了对比。所制备的高透过率保护薄膜达到如下性能：在3～5μm波段,Si基底上一面镀高效红外增透膜一面镀AR／DLC增强型保护薄膜的平均透过率达到约96％,较之镀DLC膜平均透过率提高了约4％。在8～12μm波段,Ge基底上一面镀高效红外增透膜一面镀AR／DLC增强型保护薄膜的平均透过率达到约95％,较之镀DLC膜平均透过率提高了约5％。有关薄膜样品都通过了相应的环境试验。     

Characterization of the interfacial reaction between sputter-deposited Ni film and Si substrate

In the present work, we report the interfacial reaction characteristics between sputter-deposited Ni film and a single crystalline Si substrate. The effect of substrate bias during the deposition process on the interfacial reaction is also discussed. It was found that sputter deposition with a substrate bias can promote the interfacial reaction between Ni film and Si substrate. Under our experimental conditions, Ni₂Si (orthorhombic) with good crystallinity formed in the film when it was deposited at 200 °C and with a -80 V substrate bias. Such films had relatively low resistivity. Upon thermal annealing at 500 °C, NiSi formed through further reaction, however there is almost no change in resistivity. PACS 67.57.Np; 68.55.-a; 68.35.Fx     

激光加速实验超薄类金刚石碳靶的制备

采用过滤阴极真空弧法,制备了满足激光稳相加速机制要求的超薄自支撑类金刚石碳靶。室温下沉积,基片偏压为-32 V,薄膜沉积速率约为每脉冲0.002 nm。选取NaCl膜作脱膜剂,采用漂浮法进行脱膜。打捞板孔径为1 mm时,自支撑厚度范围为5~50 nm,自支撑成功率约为70%。利用拉曼光谱仪及原子力显微镜等仪器,测量了薄膜的结构、表面粗糙度等关键参数。     

Optical and Electrical Properties Evolution of Diamond-Like Carbon Thin Films with Deposition Temperature

Optical and electrical properties of diamond-like carbon （DLC） films deposited by pulsed laser ablation of graphite target at different substrate temperatures are reported. By varying the deposition temperature from 400 to 25℃, the film optical transparency and electrical resistivity increase severely. Most importantly, the transparency and resistivity properties of the DLC films can be tailored to approaching diamond by adjusting the deposition temperature, which is critical to many applications. DLC films deposited at low temperatures show excellent optical transmittance and high resistivity. Over the same temperature regime an increase of the spa bonded C content is observed using visible Raman spectroscopy, which is responsible for the enhanced transparency and resistivity properties.