Modulation of residual stress in diamond like carbon films with incorporation of nanocrystalline gold

Residual stress modulation in the diamond-like carbon coatings with incorporation of gold nanoparticles was studied critically. The films were deposited on glass and Si (1 0 0) substrates by using capacitatively coupled plasma chemical vapor deposition. Stresses in the films were determined from the broadening of the optical absorption tail and were found to decrease from 2.3 GPa to 0.48 GPa with increasing gold content (2-7 at.% Au) in the DLC matrix. Gold incorporation also made the films harder than the corresponding DLC coatings. Modulation of stress with nanocrystalline gold content in the DLC matrix was related to the relative amount of sp²/sp³ content in the DLC films.     

富勒烯作为过渡层生长金刚石薄膜研究

采用微波等离子体化学气相淀积法，以Ｃ６０膜过渡层，在光滑的单晶Ｓｉ衬底（１００）表面的研磨的石英衬底表面等光学衬底上，首次在无衬底负偏压条件下生长出多晶金刚石薄膜，通过扫描电镜观察到生长膜晶粒呈莱花状，生长表面为金刚石（１００）界面。     

Diamond-like carbon coatings for the protection of metallic artefacts: effect on the aesthetic appearance

Plasma-enhanced chemical vapour deposition (PECVD) is an environmentally friendly process used to deposit a variety of nano-structured coatings for the protection or the surface modification of metallic artefacts like the SiO₂-like films that have been successfully tested on ancient silver, bronze and iron artefacts as barriers against aggressive agents. This paper deals with the preliminary results of a wider investigation aimed to the development of eco-sustainable coatings for the protection of Cu and Ag-based artefacts of archaeological and historic interest. Diamond-like carbon (DLC) coatings have been deposited by PECVD in different experimental conditions, in a capacitively coupled asymmetric plasma reactor, placing the substrates either on electrically powered electrode (cathodic mode) or grounded electrode (anodic mode) with and without hydrogen addition in the gas mixture. The final goal is to develop a coating with good protective effectiveness against aggressive atmospheres and contemporarily with negligible effects on the aesthetic appearance of the artefacts. The evaluation of possible colour changes of the surface patinas, due to coating process, was performed by optical microscopy and colorimetric measurements. Furthermore, to evaluate the reversibility of the thin DLC layer, an etching treatment in oxygen plasma has been successfully carried out and optimized. The chemical-physical characterization of the deposited DLC coatings was performed by means of the combined use of micro-Raman and XPS spectroscopies. The results show that the DLC films obtained in the anodic mode, may be proposed as a viable alternative to polymeric coatings for the protection of metallic ancient objects.     

金刚石镶嵌非晶碳膜表面形貌对场致电子发射的影响

用微波等离子体化学气相沉积设备，在经过不同研磨预处理的金属钼衬底上沉积出了表面形貌有较大差异的金刚石镶嵌非晶碳膜，分别用扫描电子显微镜（ＳＥＭ）、金相显微镜和Ｘ射线衍射谱（ＸＲＤ）以及Ｒａｍａｎ光谱对样品进行了分析测试．研究了各样品的场致电子发射特性，结果发现薄膜表面由大量镶嵌有金刚石小晶粒的非晶碳球组成，在我们的实验范围内，薄膜表面非晶碳球尺寸越小，场致电子发射效果越好     

Low energy repetitive miniature plasma focus device as high deposition rate facility for synthesis of DLC thin films

Diamond-like carbon (DLC) films were deposited on Si (1 0 0) substrate using a low energy (219 J) repetitive (1 Hz) miniature plasma focus device. DLC thin film samples were deposited using 10, 20, 50, 100 and 200 focus shots with hydrogen as filling gas at 0.25 mbar. The deposited samples were analyzed by XRD, Raman Spectroscopy, SEM and XPS. XRD results exhibited the diffraction peaks related to SiO₂, carbon and SiC. Raman studies verified the formation amorphous carbon with D and G peaks. Corresponding variation in the line width (FWHM) of the D and G positions along with change in intensity ratio (I_D/I_G) in DLC films was investigated as a function of number of deposition shots. XPS confirmed the formation sp² (graphite like) and sp³ (diamond like) carbon. The cross-sectional SEM images establish the 220 W repetitive miniature plasma focus device as the high deposition rate facility for DLC with average deposition rate of about 250 nm/min.     

Effect of titanium incorporation on the structural, mechanical and biocompatible properties of DLC thin films prepared by reactive-biased target ion beam deposition method

Amorphous diamond like carbon (DLC) and titanium incorporated diamond like carbon (Ti-DLC) thin films were deposited by using reactive-biased target ion beam deposition method. The effects of Ti incorporation and target bias voltage on the microstructure and mechanical properties of the as-deposited films were investigated by means of X-ray photoelectron spectroscopy, Raman spectroscopy, transmission electron microscopy and nano-indentation. It was found that the Ti content in Ti-DLC films gets increased with increasing target bias voltage. At about 4.2 at.% of Ti, uniform sized well dispersed nanocrystals were seen in the DLC matrix. Using FFT analysis, a facility available in the TEM, it was found that the nanocrystals are in cubic TiC phase. Though at the core, the incorporated Ti atoms react with carbon to form cubic TiC; most of the surface exposed Ti atoms were found to react with the atmospheric oxygen to form weakly bonded Ti-O. The presence of TiC nanocrystals greatly modified the sp³/sp² hybridized bonding ratio and is reflected in mechanical hardness of Ti-DLC films. These films were then tested for their biocompatibility by an invitro cell culturing test. Morphological observation and the cell proliferation test have demonstrated that the human osteoblast cells well attach and proliferate on the surface of Ti incorporated DLC films, suggesting possible applications in bone related implant coatings.     

沉积工艺条件对金刚石薄膜红外椭偏光学性质的影响

采用红外椭圆偏振光谱仪对不同工艺条件下制备的CVD金刚石薄膜在红外波长范围内的光学参量进行了测量，分析了工艺条件对金刚石薄膜红外光学性质的影响.获得了最佳的沉积工艺参数，优化了薄膜的制备工艺.结果表明薄膜的折射率和消光系数与薄膜质量密切相关，当温度为750℃，碳源浓度为0.9%和压强为4.0 kPa时，金刚石薄膜的红外椭偏光学性质最佳，折射率平均值为2.385，消光系数在10^-4范围内，在红外波段具有良好的透过性. 关键词： 薄膜光学 红外光学性质 工艺条件 金刚石薄膜     

Substrate bias effects during diamond like carbon film deposition by microwave ECR plasma CVD

Diamond like carbon (DLC) coatings were deposited on silicon(1 1 1) substrates by microwave electron cyclotron resonance (ECR) plasma CVD process using a plasma of Ar and CH₄ gases under the influence of DC self bias generated on the substrates by application of RF (13.56 MHz) power. DLC coatings were deposited under the varying influence of DC bias (−60 V to −150 V) on the Si substrates. Deposited films were analyzed by different techniques like: X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), atomic force microscopy (AFM), Hardness and elastic modulus determination technique, Raman spectroscopy, scanning electron microscopy (SEM) and contact angle measurement. The results indicate that the film grown at −100 V bias has optimised properties like high sp³/sp² ratio of carbon bonding, high refractive index (2.26–2.17) over wide spectral range 400–1200 nm, low roughness of 0.8 nm, high contact angle (80°) compared to the films deposited at other bias voltages (−60 V and −150 V). The results are consistent with each other and find august explanation under the subplantation model for DLC growth.     

Precursors for CVD growth of nanocrystalline diamond

Various routes to grow nanocrystalline diamond films by the chemical vapor deposition technique are reviewed. Among the various routes, NCD films deposited on mirror-polished silicon substrates by biased enhanced growth by microwave plasma chemical vapor deposition are described in detail. The qualitative concentration of NCD was assessed by Raman spectroscopy and x-ray diffraction patterns of the films. The hardness of the films approaches that of natural diamond at optimized conditions while still having a low amount of stress (<1 GPa).     

Characterization of the bonding structure of nanocrystalline diamond and amorphous carbon films prepared by plasma assisted techniques

Thin nanocrystalline diamond/amorphous carbon (NCD/a-C) composite films and amorphous diamond-like carbon (DLC) films were prepared by three methods: microwave plasma chemical vapour deposition (MWCVD) from methane/nitrogen mixtures (NCD/a-C), RF magnetron sputtering of a pure graphite target in argon/methane ambients, and pulsed laser deposition (PLD) in vacuum or argon atmosphere (DLC). The films prepared by the three techniques were comprehensively characterized with respect to their bonding structure by Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). PACS 81.05.Uw; 82.80.Pv     

Wettability and antibacterial activity of modified diamond-like carbon films

Diamond-like carbon (DLC) films can be used in a numerous industrial applications, including biomedical coatings with bactericidal properties. It has been demonstrated that DLC surface can be modified with oxygen plasma treatment. The purpose of this paper is to study the wettability and bactericidal activity of oxygen plasma-treated DLC films produced by plasma enhanced chemical vapor deposition technique. The sp³/sp² ratio increased after the treatment due to the increase in the generation of the unstable carbon bonds caused by the energetic ions, especially O-H group. The treated DLC surface becomes superhydrophilic and rougher, although the roughness values are still lower. DLC antibacterial activity did not increased with plasma treatment. Therefore, oxygen plasma treatment can be used to make superhydrophilic DLC but not to increase its bactericidal properties.     

Growth and Characteristics of Freestanding Hemispherical Diamond Films by Microwave Plasma Chemical Vapor Deposition

Freestanding hemispherical diamond films have been fabricated by microwave plasma chemical vapor deposition using graphite and molybdenum （Mo） as substrates. Characterized by Raman spectroscopy and scanning electron microscopy, the crystalline quality of the films deposited on Mo is higher than that on graphite, which is attributed to the difference in intrinsic properties of the two substrates. By decreasing the methane concentration, the diamond films grown on the Mo substrate vary from black to white, and the optical transparency is enhanced. After polishing the growth side, the diamond films show an infrared transmittance of 35-60% in the range 400-4000 cm^- 1.     

Study on tribological behavior and cutting performance of CVD diamond and DLC films on Co-cemented tungsten carbide substrates

The tribological behaviors of diamond and diamond-like carbon (DLC) films play a major role on their machining and mechanical applications. In this study, diamond and diamond-like carbon (DLC) films are deposited on the cobalt cemented tungsten carbide (WC-Co) substrate respectively adopting the hot filament chemical vapor deposition (HFCVD) technique and the vacuum arc discharge with a graphite cathode, and their friction properties are evaluated on a reciprocating ball-on-plate tribometer with counterfaces of silicon nitride (Si₃N₄) ceramic, cemented tungsten carbide (WC) and ball-bearing steel materials, under the ambient air without lubricating condition. Moreover, to evaluate their cutting performance, comparative turning tests are conducted using the uncoated WC-Co and as-fabricated CVD diamond and DLC coated inserts, with glass fiber reinforced plastics (GFRP) composite materials as the workpiece. The as-deposited HFCVD diamond and DLC films are characterized with energy-dispersive X-ray spectroscopy (EDX), scanning electron microscope (SEM), X-ray diffraction spectroscopy (XRD), Raman spectroscopy and 3D surface topography based on white-light interferometry. Furthermore, Rocwell C indentation tests are conducted to evaluate the adhesion of HFCVD diamond and DLC films grown onto WC-Co substrates. SEM and 3D surface topography based on white-light interferometry are also used to investigate the worn region on the surfaces of diamond and DLC films. The friction tests suggest that the obtained friction coefficient curves that of various contacts exhibit similar evolution tendency. For a given counterface, DLC films present lower stable friction coefficients than HFCVD diamond films under the same sliding conditions. The cutting tests results indicate that flank wear of the HFCVD diamond coated insert is lower than that of DLC coated insert before diamond films peeling off.     

Preparation and Thermal Characterization of Diamond-Like Carbon Films

Diamond-like carbon （DLC） films are prepared on silicon substrates by microwave electron cyclotron resonance plasma enhanced chemical vapor deposition. Raman spectroscopy indicates that the films have an amorphous structure and typical characteristics. The topographies of the films are presented by AFM images. Effective thermal conductivities of the films are measured using a nanosecond pulsed photothermal reflectance method. The results show that thermal conductivity is dominated by the microstructure of the films.     

Diamond-like phase formation in an amorphous carbon films prepared by periodic pulsed laser deposition and laser irradiation method

Diamond-like carbon (DLC) films were fabricated by pulsed laser ablation of a liquid target. During deposition process the growing films were exited by a laser beam irradiation. The films were deposited onto the fused silica using 248 nm KrF eximer laser at room temperature and 10⁻³ mbar pressure. Film irradiation was carried out by the same KrF laser operating periodically between the deposition and excitation regimes. Deposited DLC films were characterized by Raman scattering spectroscopy. The results obtained suggested that laser irradiation intensity has noticeable influence on the structure and hybridization of carbon atoms deposited. For materials deposited at moderate irradiation intensities a very high and sharp peak appeared at 1332 cm⁻¹, characteristic of diamond crystals. At higher irradiation intensities the graphitization of the amorphous films was observed. Thus, at optimal energy density the individual sp³-hybridized carbon phase was deposited inside the amorphous carbon structure. Surface morphology for DLC has been analyzed using atomic force microscopy (AFM) indicating that more regular diamond cluster formation at optimal additional laser illumination conditions (∼20 mJ per impulse) is possible.     

射频等离子体法制备类金刚石薄膜

利用射频等离子体化学气相沉积法，以丁烷、氢气和氩气的混合气体为原料，在Ф200mm锗基片上沉积出均匀的类金刚石薄膜。研究类金刚石薄膜的特性及工艺参数对其性能的影响规律，给出应用于红外装置中的类金刚石薄膜镀膜元件光谱性能。     

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...     

多腔耦合微波表面波PECVD法沉积 DLC薄膜研究

报道了利用多腔耦合微波表面波等离子体增强化学气相沉积(PECVD)的方法制备类金刚石(DLC)薄膜。通过发射光谱(OES)测量,对Ar等离子体中的各种放电参数以及全部四个腔室内放电的均匀性作出评估。采用表面轮廓仪测量了薄膜的厚度;薄膜的表面形貌、组成结构通过原子力显微镜(AFM)、激光拉曼光谱和X射线衍射光谱(XPS)进行了表征。在12.5μm厚度的有机薄膜聚酯(PET)表面沉积一定厚度DLC后,通过测量水蒸气透过率(WVTR)对DLC薄膜的阻隔性能进行了研究。结果表明,这种多腔耦合微波表面波等离子体装置,不仅能够实现四个腔室同时相对均匀的放电,也能够实现单个腔室的轴向均匀放电。制备的DLC薄膜结构致密、成分均匀,可以使PET薄膜阻隔性能提高约20倍。     

Mo离子注入对金刚石涂层附着性能的影响

采用Mo离子注入工艺对YG6硬质合金基体表面进行处理,用微波等离子体CVD(MPCVD)法沉积金刚石涂层,研究了Mo离子注入工艺对金刚石涂层附着性能的影响.结果表明,Mo离子注入后,硬质合金基体表面的化学成分发生了明显变化;采用适当剂量的Mo离子注入基体,可使CVD金刚石涂层的附着性能显著提高. 关键词： 金刚石涂层 Mo离子注入 硬质合金基体 附着性能     

微波ECR全方位离子注入制备类金刚石碳膜的结构及摩擦学性能研究

利用微波ECR全方位离子注入技术，在单晶硅（100）衬底上制备类金刚石薄膜.分析结果表明，所制备的类金刚石碳膜具有典型的类金刚石结构特征，薄膜均匀、致密，表面粗糙度小，摩擦系数小.其中，薄膜的结构和性能与氢流量比关系密切，随氢流量比的增加，薄膜的沉积速率减小，表面粗糙度降低，且生成sp³键更加趋向于金刚石结构，表面能 更低，从而使摩擦系数大幅降低. 关键词： 全方位离子注入 类金刚石碳膜 拉曼光谱 摩擦磨损