不同技术制备DLC膜的激光损伤特性研究

随着高能量大功率激光器的发展和激光元件的广泛应用,用于红外窗口表面增透保护的类金刚石薄膜(DLC)的抗激光损伤特性成为评价薄膜质量优劣的一个重要指标。然而,不同的制备方法和技术沉积的DLC薄膜具有各异的微观结构,从而具有不同的抗激光损伤特性。本文采用脉冲真空电弧(PVAD)和非平衡磁控溅射(UBMS)技术沉积了DLC膜,对两种DLC膜抗激光损伤特性进行了研究,测试结果表明,两种技术沉积的DLC薄膜激光损伤阈值分别0.6 J/cm2和0.3 J/cm2,PVAD技术比UBMS技术沉积的DLC薄膜具有更高的抗激光损伤阈值。基于实验研究了薄膜光学常数和表面形态,分析了两种技术制备DLC膜激光损伤特性差异的主要原因。结果表明,采用UBMS技术沉积的DLC膜具有较小的折射率和较大的消光系数,薄膜表面存在较多的疵病和缺陷,这些是其激光损伤阈值较低的主要原因。     

激光辐照对类金刚石薄膜改性及损伤研究

介绍了激光损伤的检测及损伤阈值的测量方法.讨论激光辐照对类金刚石结构和性质的影响规律.并论述不同工作参数的激光对类金刚石薄膜的激光破坏行为及其损伤阈值.在此基础上分析类金刚石薄膜激光损伤的机理.还从物理特性及制备技术方面着手,比较分析金刚石及类金刚石薄膜各自的优缺点和实际应用状况,并提出类金刚石薄膜的应用前景和有待进一步研究的问题.     

非平衡磁控溅射类金刚石薄膜的激光损伤过程研究

类金刚石薄膜是一种很好的红外窗口表面增透保护材料,随着对其抗激光损伤特性研究的不断深入,越来越多的研究者都将研究的重点放在了如何提高其激光损伤阈值上。然而,不同沉积方法制备的薄膜由于其微观结构存在的差异,必然会导致破坏的过程有所不同。本文采用非平衡磁控溅射技术沉积的薄膜,对其损伤过程进行了深入的研究。结果表明：在不同的激光能量下,DLC薄膜出现不同的损伤形态,而这些与薄膜的缺陷、内应力以及薄膜与衬底的结合力密切相关。     

类金刚石薄膜的激光损伤特性及工艺优化

采用脉冲真空电弧沉积(PVAD)技术制备了类金刚石(DLC)薄膜,并对其抗激光损伤特性进行了研究,优化了制备工艺.对DLC薄膜激光损伤阈值(LIDT)的测试结果表明,随着厚度的增加,薄膜的LIDT开始呈下降趋势,当厚度达到100nm以上时,则趋于一个稳定值.正交实验结果的处理和分析表明,在所给定的工艺参数范围内,主回路电压是影响DLC膜抗激光损伤性能的最主要因素,基片温度、清洗时间和脉冲频率则影响较小.为得到较好的抗激光损伤能力,采用PVAD技术制备DLC薄膜的最佳工艺参数为:清洗时间20 min、基片温度150℃、脉冲频率5 Hz、主回路电压150 V.退火处理会使DLC薄膜的激光损伤阈值明显提高.     

外加偏置电场对类金刚石薄膜激光损伤形貌影响研究

研究了使用非平衡测控溅射技术沉积的类金刚石(DLC)薄膜其抗激光损伤能力;通过对比施加偏置电场前后薄膜的损伤情况,发现:DLC薄膜施加偏置电场后,薄膜的激光损伤区域内有大量丝状薄膜,损伤形貌存在明显不同,损伤面积减小;薄膜的激光损伤情况得到改善。实验结果显示,外加偏置电场对DLC薄膜的损伤有影响。认为:激光在DLC薄膜中激励产生的光生电子在电场的作用下产生快速漂移,间接降低了激光辐照区域内的局部能量密度,减缓了薄膜的石墨化,提高了DLC薄膜的抗激光损伤能力。     

液相电沉积金刚石薄膜的研究进展

评述了液相沉积(类)金刚石薄膜的研究现状,介绍了液相合成(类)金刚石薄膜的装置、液态源及薄膜的性能,分析了如何更好地提高(类)金刚石薄膜质量,并在此基础上提出了一种可能制备出高质量金刚石薄膜的脉冲电弧放电沉积装置.     

增强型脉冲离子源镀制DLC薄膜拉曼光谱研究

本文利用增强型脉冲电弧离子源在硅基底上沉积类金刚石薄膜，拉曼光谱分析表明DLC薄膜中sp^3键含量比不加磁过滤装置时脉冲离子源所镀的类金刚石薄膜高，折射率更接近金刚石折射率2．4并且光学带隙也增大，证明用增强型脉冲离子源镀制的类金刚石薄膜sp^3键含量提高，性能得到了很大改善。     

沉积参数对化学气相沉积纳米金刚石薄膜的影响

用强电流直流伸展电弧化学气相沉积金刚石薄膜装置,在CH4-Ar和CH4-H2-Ar气氛中沉积了纳米金刚石薄膜,研究了沉积气氛中H2加入量和沉积压力对金刚石薄膜显微组织和生长机制的影响.沉积气氛中H2含量对金刚石薄膜的表面形貌、晶粒尺寸和生长速度有显著影响,随着H2含量增加,金刚石晶粒尺寸增大,薄膜生长速度提高.在1%CH4-Ar气氛中沉积的纳米金刚石薄膜,晶粒尺寸细小,薄膜表面形貌光滑平整.在1%CH4-少量H2-Ar气氛中沉积的金刚石薄膜,晶粒尺寸小于100nm,薄膜表面形貌较平整.随着沉积压力提高,金刚石薄膜的生长速度增大.用激光Ram an对金刚石薄膜进行了表征.     

激光热处理对类金刚石薄膜结构的影响

用真空阴极过滤电弧法沉积了厚度为2 nm的类金刚石(DLC)薄膜,研究了激光加热退火时薄膜结构和表面粗糙度的变化,分析了激光加热功率对薄膜结构的影响。结果表明,当激光功率小于200 mW时,DLC薄膜的结构基本保持不变;激光功率增大到300 mW,薄膜中少量的sp3键转变为sp2键,但薄膜的表面形貌基本保持不变。随着激光功率增大到400mW,薄膜中sp3键向sp2键的转变量增大;当激光功率达到500 mW时,薄膜中大量的sp3键转变为sp2键,sp2六原子环含量迅速增大,薄膜表面粗糙度开始明显增大,出现凹凸不平的表面形貌。     

类金刚石薄膜作为HgCdTe红外器件增透膜和钝化膜的研究

采用高频等离子体化学气相色沉积法（ＲＦＣＶＤ）在ＨｇＣｄＴｅ红外器件上沉积类金刚石薄膜，俄歇电子能谱对ＤＬＣ／ＨｇＣｄＴｅ界面分析结果表明类金刚石薄膜中的碳原子对衬底材料影响较小，７０ｎｍ的类金刚石薄膜抑制衬底组份的外扩散，而且具有纯度较高的类金刚石薄膜外表面层，是一种理想的钝化膜材料，红外透射光谱测试结果表明类金刚石薄膜在较宽的波长范围内（４－１２μｍ）具有明显的增透效应。     

Adhesion studies of diamond-like carbon films deposited on Ti6Al4V substrate with a silicon interlayer

Diamond-like carbon (DLC) films have proven quite advantageous in many tribological applications due to their low friction coefficient, their extreme hardness, and more recently their high adherence on different substrate materials. However, for many applications, DLC films as thick as 2 μm are required, which cause high residual stress. In order to overcome this problem, this study observed the behavior of different thicknesses of silicon interlayer between DLC films and Ti6Al4V substrates. The study also analyzed the relation of growth parameters to the mechanical properties of DLC films. Silicon and DLC films were grown by using a rf-PECVD at 13.56 MHz with silane and methane atmospheres, respectively. The contribution of an interlayer thickness to the adhesion between the DLC films and Ti6Al4V substrate was evaluated by using a micro-scratch technique. The hardness and friction coefficient were evaluated by using microindentation and lateral force microscopy (LFM), respectively. Raman scattering spectroscopy was used to characterize the film quality. A correlation was found between the intrinsic stress and adhesion of DLC film and the parameters of the silicon interlayer growth. The addition of a silicon interlayer successfully reduced intrinsic stress of the films, even as measured by using a perfilometry technique.     

等离子体源离子注入法制备类金刚石薄膜

用等离子体源注入(PSII)在Si(100)上制备类金刚石膜，放电气体采用CH4，用微波电子回旋共振(ECR)产生等离子体。将-20～-30kV的高压加在衬底上，来提高离子的能量。通过Raman光谱和FT-IR光谱检测了类金刚石膜的化学组成及状态，并对其机械性能和表面形貌进行了检测。结果显示，硅片硬度和摩擦因数得到了改善，用PSII能够制备出性能优良的膜，可以将其应用到微电子器件(MEMS)上去。     

Stress and strain in DLC films induced by electron bombardment

Radiation induced stress and strain have been investigated in amorphous hydrogenated DLC films after their exposure to high-energy (12 MeV) electrons, produced in the medical linear accelerator. DLC structures of different hydrogen contents and thickness, deposited from acetylene gas onto Si<111> wafers in the two-chamber plasmotron system were used in this investigation.Optically levered laser technique was used to measure the radius of curvature of the investigated DLC films and residual stress in the film was determined. Surface morphology of DLC films was defined by AFM “Nanotop-206”. Microhardness measurements were performed using MTS Nanoindenter G200. Bonding structure of the DLC films was analysed using the Raman scattering spectroscopy.It was found that the bombardment of DLC films with high-energy electrons introduced additional residual stress in all investigated samples. However, stress saturation tendency was observed after some fractions of the irradiation. Radiation induced stress was lower in the samples with well-organized networking structure, depending on technological conditions of the film growth. Significant deterioration of the mechanical properties of DLC films after their bombardment with high-energy electrons was not observed. Radiation induced changes in irradiated DLC films are discussed on the basis of the results of measurements.     

Metal-doped diamond-like carbon films synthesized by filter-arc deposition

Diamond-like carbon (DLC) thin films are extensively utilized in the semiconductor, electric and cutting machine industries owing to their high hardness, high elastic modulus, low friction coefficients and high chemical stability. DLC films are prepared by ion beam-assisted deposition (BAD), sputter deposition, plasma-enhanced chemical vapor deposition (PECVD), cathodic arc evaporation (CAE), and filter arc deposition (FAD). The major drawbacks of these methods are the degraded hardness associated with the low sp³/sp² bonding ratio, the rough surface and poor adhesion caused by the presence of particles. In this study, a self-developed filter arc deposition (FAD) system was employed to prepare metal-containing DLC films with a low particle density. The relationships between the DLC film properties, such as film structure, surface morphology and mechanical behavior, with variation of substrate bias and target current, are examined. Experimental results demonstrate that FAD-DLC films have a lower ratio, suggesting that FAD-DLC films have a greater sp³ bonding than the CAE-DLC films. FAD-DLC films also exhibit a low friction coefficient of 0.14 and half of the number of surface particles as in the CAE-DLC films. Introducing a CrN interfacial layer between the substrate and the DLC films enables the magnetic field strength of the filter to be controlled to improve the adhesion and effectively eliminate the contaminating particles. Accordingly, the FAD system improves the tribological properties of the DLC films.     

Chemical diagnosis of DLC by ESR spectral analysis

Diamond-like carbon (DLC) films were deposited utilizing plasma enhanced chemical vapor deposition (PECVD) with four precursor gases such as methane, ethylene, acetylene and benzene in gas phase. Electron spin resonance (ESR) spectra showed that dangling-bond sites (DBSs) observed in all films were characterized by an isotropic broad single line. The DLC film with unsaturated precursor gases had the higher film growth rate and the higher DBS accumulative rate. Although the DBS in DLC films were quite stable at room temperature under anaerobic conditions, the DBS decayed rapidly to level off toward a limiting value when exposed to air. The stability and reactivity of the DBS in DLC film were assumed to depend on chemical structure of organic gas used as precursor. The detailed-ESR study on DBS of the DLC films could be one of the powerful tools for diagnosing the micro-structural properties and the quality of films.     

非平衡磁控溅射技术制备用于红外减反射的无氢碳膜

红外减反射保护膜具有特定的厚度要求,如能进一步减小无氢类金刚石膜(DLC)的光学吸收,就能使其在较大厚度时不过分损失光通量而得以广泛应用.从这点来讲,无氢类金刚石膜是一种极具开发潜力的材料.本文采用非平衡磁控溅射技术(UBMS)制备了无氢类金刚石膜,并研究了其厚度均匀性.研究结果表明:该非平衡磁控溅射装置有能力获得大于φ150 mm的均匀性范围.对DLC膜红外透射谱的分析表明,分别在Si和Ge基底表面单面制备的DLC薄膜,其峰值透射率在波数2983/cm时分别为68.83%和63.05%,这一结果接近无吸收碳材料理论上所能达到的值.同时,在5000到800/cm范围内,未发现明显的吸收峰.这些优良的光学特性表明,采用非平衡磁控溅射技术制备的无氢DLC膜可以作为窗口的红外增透保护膜使用.     

CVD of hard DLC films in a radio frequency inductively coupled plasma source

Chemical vapor deposition (CVD) of hard diamond-like carbon (DLC) films on silicon (100) substrates from methane was successfully carried out using a radio frequency (r.f.) inductively coupled plasma source (ICPS). Different deposition parameters such as bias voltage, r.f. power, gas flow and pressure were involved. The structures of the films were characterized by Fourier transform infrared (FTIR) spectroscopy and Raman spectroscopy. The hardness of the DLC films was measured by a Knoop microhardness tester. The surface morphology of the films was characterized by atomic force microscope (AFM) and the surface roughness (R_a) was derived from the AFM data. The films are smooth with roughness less than 1.007 nm. Raman spectra shows that the films have typical diamond-like characteristics with a D line peak at 1331 cm⁻¹ and a G line peak at 1544 cm⁻¹, and the low intensity ratio of I_D/I_G indicate that the DLC films have a high ratio of sp³ to sp² bonding, which is also in accordance with the results of FTIR spectra. The films hardness can reach approximately 42 GPa at a comparatively low substrate bias voltage, which is much greater than that of DLC films deposited in a conventional r.f. capacitively coupled parallel-plate system. It is suggested that the high plasma density and the suitable deposition environment (such as the amount and ratio of hydrocarbon radicals to atomic or ionic hydrogen) obtained in the ICPS are important for depositing hard and high quality DLC films.