XPS and TEM study of W-DLC/DLC double-layered film

A double-layered film of tungsten-containing diamond-like carbon (W-DLC) and DLC, (W-DLC)/DLC, was investigated. A film of 1.6 µm in thickness was deposited onto silicon substrate. The investigate double-layered coating was deposited by using the combination of PECVD and co-sputtering of tungsten metal target. Structure, interface and chemical bonding state of the investigated film were analyzed by Transmission electron microscope (TEM) and X-ray photoelectron spectroscopy (XPS). From the results of the analyses, the structure of double-layered film is that amorphous phase of carbon is continued from DLC to W-DLC and tungsten metal clusters are dispersed in W-DLC layer.     

Single layer and multilayered films of plasma polymers analyzed by nanoindentation and spectroscopic ellipsometry

Well-defined single layer and multilayered a-SiC:H films, deposited from tetravinylsilane at different powers by plasma-enhanced chemical vapor deposition on silicon, were intensively studied by in situ spectroscopic ellipsometry, nanoindentation, and atomic force microscopy. A realistic model of the sample structure was used to analyze ellipsometric data and distinguish individual layers in the multilayered film, evaluate their thickness and optical constants. Dispersion dependences for the refractive index were well separated for each type of individual layer, if the thickness was decreased from 315 to 25 nm, and corresponded to those of the single layer. A beveled section of the multilayered film revealed the individual layers that were investigated by atomic force microscopy and nanoindentation to confirm that mechanical properties in multilayered and single layer films are similar.     

Investigation of corrosion behavior of nitrogen doped and platinum/ruthenium doped diamond-like carbon thin films in Hank's solution

Undoped (DLC), nitrogen-doped (N-DLC) and platinum/ruthenium doped diamond-like carbon (PtRu-DLC) thin films were deposited on p-Si (100) substrates using a DC magnetron sputtering deposition system. The chemical composition, bonding structure, surface morphology and adhesion strength of the films were characterized using X-ray photoelectron spectroscopy (XPS), micro-Raman spectroscopy, atomic force microscopy (AFM) and micro-scratch test, respectively. The corrosion behavior of the films in a Hank's solution was investigated using potentiodynamic polarization test. The corrosion results revealed that the PtRu-DLC film had the highest corrosion potential among the films used in this study.     

Microstructure and property evolution of Cr-DLC films with different Cr content deposited by a hybrid beam technique

Cr-containing diamond-like carbon (Cr-DLC) films was deposited on silicon wafers by a hybrid beams system, which consists of a DC magnetron sputtering and a linear ion source. The chromium content in the films was adjusted by varying the fraction of Ar in the Ar and CH₄ gas mixture. The composition, microstructure, surface morphology, mechanical properties and tribological behavior of the films were investigated by XPS, TEM, AFM, SEM, nano-indentation and tribological tester as a function of Cr content. It is shown that, as the Cr content increased from 1.49 to 40.11 at.%, the Cr-DLC films transfer from amorphous DLC with dispersed metallic-like Cr to composite DLC with carbide phases embedding in the DLC matrix, and the film surface morphology also evolve from flat surface into rough surface with larger hillocks. The amorphous Cr-DLC films exhibit a low friction coefficient and wear rate as pure DLC, while the composite Cr-DLC films show a higher friction coefficient and wear rate, although they possess a relatively high hardness.     

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。     

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.     

PECVD法制备类金刚石薄膜的结构和摩擦学性能研究

采用射频一直流等离子体增强化学气相沉积技术在单晶硅衬底上沉积了类金刚石薄膜。用激光拉曼光谱仪和原子力显微镜对薄膜的结构和表面形貌进行了表征，并用纳米压痕仪测定了薄膜的硬度。用UMT微摩擦磨损试验机考察了薄膜在不同的滑行速度下薄膜的摩擦学性能。结果表明：所沉积的薄膜具有典型类金刚石薄膜的结构特征，薄膜表面光滑致密，硬度较高；薄膜与氧化铝陶瓷球对磨显示出良好的摩擦学性能，随着滑行速度的增加，薄膜的摩擦系数单调降低，但磨损寿命先增加后降低。     

H13钢离子渗氮(PN)与类金刚石(DLC)复合处理的摩擦磨损性能研究

采用阳极层流离子源与非平衡磁控溅射结合的沉积方法在H13钢基体表面沉积出类金刚石膜(DLC),并对H13钢经不同表面预处理对后沉积的DLC膜的摩擦学性能进行了对比研究.结果表明:DLC膜结构致密,且DLC膜与梯度过渡层及基体三者之间结合牢固;H13钢经离子氮化后,梯度过渡层与氮化层间结合紧密,提高了膜与基体的承载能力;在保持相同摩擦速率的条件下,摩擦系数随着载荷的增加先增大后减小;H13钢离子渗氮处理后沉积的DLC膜其摩擦系数远小于未采用离子渗氮处理沉积的DLC薄膜.     

An examination of trace surface on diamond-like carbon film after ball-on disk measurement

Hydrogenated diamond-like carbon (DLC) films were prepared by the radio frequency plasma-enhanced chemical vapor deposition method on silicon substrates using methane (CH₄) and hydrogen (H₂) gas. The wear track on DLC films was examined after the ball-on disk (BOD) measurement with a Raman mapping method. The BOD measurement of DLC films was performed for 1 to 3 h with a 1-hour step time. The sliding traces on the hydrogenated DLC film after the BOD measurement were also observed using an optical microscope. The films synthesized in this work had a very low friction coefficient (about 0.06) and were adhered very well without peeling off during the BOD measurement even with very thin thickness. Energy dispersive X-ray spectra show the decrease of C atomic % and the increase of O atomic % according to the sliding time. The novel Raman mapping method effectively showed the graphitization of DLC films according to the sliding time.     

The study of adhesion and nanomechanical properties of DLC films deposited on tool steels

In this study, thin diamond-like carbon (DLC) films were deposited onto a steel substrate. By using the plasma immersion ion implantation (PIII) technique, a nitrogen layer was formed on the steel surface before depositing the DLC films. This PIII formed nitrogen layer, which acts as the buffer layer, has apparently increased the adhesion between the DLC film and the steel substrate. The microstructures, the nanomechanical properties, and the adhesion of the DLC were investigated by the techniques of X-ray diffraction (XRD), transmission electron microscopy (TEM), nanoindentation, and nanoscratch. Results show that the hardness and Young's modulus were significantly improved, up to 2 to 9 times; while the implantation depth and the microstructure of the nitrogen layers vary with nitrogen/hydrogen ratio (N:H = 1:0, 1:1, 1:3). Raman analyses indicate that the I(D)/I(G) ratio increases with the thickness of DLC film. By using the PIII technique in the steel substrate, the adhesion of the DLC film onto the substrate is greatly enhanced, and wear resistance is elevated if the DLC film is sufficiently thick.     

Friction force microscopy study of annealed diamond-like carbon film

In this paper we introduce mechanical and structural characteristics of diamond-like carbon (DLC) films which were prepared on silicon substrates by radio frequency (RF) plasma enhanced chemical vapor deposition (PECVD) method using methane (CH₄) and hydrogen (H₂) gas. The films were annealed at various temperatures ranging from 300 to 900 °C in steps of 200 °C using rapid thermal processor (RTP) in nitrogen ambient. Tribological properties of the DLC films were investigated by atomic force microscopy (AFM) in friction force microscopy (FFM) mode. The structural properties of the films were obtained by high resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The wettability of the films was obtained using contact angle measurement. XPS analysis showed that the sp³ content is decreased from 75.2% to 24.1% while the sp² content is increased from 24.8% to 75.9% when the temperature is changed from 300 to 900 °C. The contact angles of DLC films were higher than 70°. The FFM measurement results show that the highest friction coefficient value was achieved at 900 °C annealing temperature.     

Structure and tribological properties of reactively sputtered Zr-Si-N films

Zr-Si-N films were deposited on silicon and steel substrates by magnetron sputtering of a Zr-Si composite target in Ar-N₂ reactive mixtures. The silicon concentration in the films was adjusted in the 0-7.6 at.% range by varying the surface of Si chips located on the erosion zone of the target. The films were characterised by X-ray diffraction, electron probe microanalysis, atomic force microscopy and wear tests. The structure and the tribological properties of Zr-Si-N films were compared to those of ZrN coatings. Depending on the silicon concentration, the films were either nanocomposites (nc-ZrN/a-SiN_x) or amorphous. Introduction of silicon into the zirconium nitride coatings induced a change in the preferential orientation of the ZrN grains: [111] for ZrN films and [100] for Zr-Si-N ones. This texture modification was also observed for a ZrN film deposited on an amorphous SiN_x layer. Thus, within our deposition conditions, the occurrence of a-SiN_x enhanced the [100] preferred orientation. Friction and wear behaviour of the films were carried out against spheres of alumina or 100 Cr6 steel by using a ball-on-disc tribometer. The results showed that addition of silicon into ZrN-based coating induced a strong decrease in the friction coefficient and in the wear rate compared to those of ZrN films. These results were discussed as a function of the films structure and composition.     

医用TiNi合金表面等离子体沉积梯度DLC膜及抗腐蚀性能

采用双放电腔MW-ECR等离子体源增强磁控溅射和沉积技术,在TiNi合金表面成功地镀制了梯度DLC膜.拉曼光谱分析表明实验获得的薄膜是典型的DLC膜,其结构受梯度层工艺影响.采用原子力显微镜(AFM)观察了薄膜的表面形貌,结果显示其表面较为平整.在Troyde's模拟体液中的电化学腐蚀实验结果说明,梯度DLC膜显著地增强了TiNi合金基体的抗腐蚀能力.从示差扫描量热仪(DSC)结果看到表面改性没有明显影响TiNi合金基体的使用性能.     

脉冲真空电弧离子镀在不锈钢上沉积类金刚石薄膜的研究

利用脉冲真空电弧离子镀技术在3Cr13不锈钢上制备了类金刚石(DLC)薄膜,通过Raman光谱分析了膜的结构特征,采用摩擦磨损试验机测试了薄膜在不同载荷下的摩擦系数,运用划痕仪研究了膜基的结合强度.结果表明:所镀制的薄膜具有典型类金刚石结构特征,膜中ID/IG为1.33;摩擦系数随着载荷的增大而减小,载荷为5 N,转速120 r/min时的摩擦系数为0.12;Ti过渡层的引入显著地提高了膜基结合力.     

低温化学气相沉积两种DLC膜的摩擦性能研究

低温条件下在单晶硅表面沉积DLC膜和Si-DLC膜层,采用UMT-2微摩擦磨损实验机研究了两种膜层的摩擦磨损特性,借助拉曼光谱、X射线衍射仪及立体三维形貌仪分析了两种膜层的表面形貌和组成。使用扫描电子显微镜检测了两种膜层磨损后的表面形貌。结果表明两种膜层表面都非常平滑,属于纳米硬膜;两种膜层都具有良好的减摩托磨作用,其...     

Nanoindentation and AFM studies of PECVD DLC and reactively sputtered Ti containing carbon films

Amorphous carbon film, bdalso known as DLC film, bdis a promising material for tribological application. It is noted that properties relevant to tribological application change significantly depending on the method of preparation of these films. These properties are also altered by the composition of the films. In view of this, bdthe objective of the present work is to compare the nanoindentation and atomic force microscopy (AFM) study of diamond like carbon (DLC) film obtained by plasma enhanced chemical vapour deposition (bdPECVD with the Ti containing amorphous carbon (Ti/a- C : H) film obtained by unbalanced magnetron sputter deposition (UMSD). Towards that purpose, DLC and Ti/a- C : H films are deposited on silicon substrate by PECVD and UMSD processes, respectively. The microstructural features and the mechanical properties of these films are evaluated by scanning electron microscopy (SEM), bdtransmission electron microscopy (TEM), nanoindentation and by AFM. The results show that the PECVD DLC film has a higher elastic modulus, hardness and roughness than the UMSD Ti/a- C : H film. It also has a lower pull off force than Ti containing amorphous carbon film.     

介质阻挡放电化学气相沉积法制备DLC薄膜研究

采用介质阻挡化学气相沉积法(DBD CVD)在Si及石英衬底上、室温下成功的沉积出光滑、致密、均匀、膜基结合较好的类金刚石(DLC)薄膜,并考察了电源电压对类金刚石薄膜结构及性能的影响。拉曼光谱(Raman)、扫描电子显微镜(SEM)、原子力显微镜(AFM)、紫外可见光谱(UV Vis)、高阻仪等测试及分析结果显示DBD CVD 法适于制备高质量硬质DLC薄膜。对DBD放电做了理论分析,结果与工艺研究的结论相符合。     

TiO2缓冲层对掺钨氧化钒热敏智能玻璃的制备及性能影响

用直流磁控溅射法在玻璃基片上先沉积TiO2缓冲层,再用直流/射频反应磁控共溅射法制备掺钨VOx薄膜,然后在氮气中退火.用X射线衍射、原子力显微镜、紫外可见光分光光度计、红外光谱仪等对薄膜的结构、表面形貌、光透过率等进行测试分析.结果表明:在溅射气压为1Pa,氧氩气体比例为1:4,Ti靶采用100 W直流电源时,所制备的TiO2缓冲层上的掺钨VOx薄膜致密,晶粒大小均匀.掺钨VOx薄膜样品的相变温度降低至35℃,可见光透过率较高,对红外光的屏蔽效果明显.     

Direct ion beam deposited carbon films and clusters

Carbon films and clusters have been formed by direct ion beam deposition. In all experiments crystalline n-Si 〈1 0 0〉 wafers with the 300 nm thermal SiO₂ film have been used as substrates. Effects of thermally microstructured Ni and substrate temperature were studied. Chemical structure of the carbon films was investigated using Raman spectroscopy. Surface morphology was studied by atomic force microscopy (AFM). Supplemental research on sheet resistance of the films has been performed. Rough diamond-like carbon film was grown onto the catalytic layer at 400 K temperature, and surface of the diamond-like carbon film deposited directly onto the SiO₂ layer at 400 K temperature was very smooth. At 750 K growth of the array of cylindrically shaped clusters was observed by AFM in the case of catalytically assisted deposition. Raman spectra of deposited films were typical for glassy carbon and/or carbon nanotubes with the carbonaceous deposits. Catalyticless deposition at 750 K temperature resulted in the formation of the conductive polymer-like carbon film with the graphite clusters in it.     

Spectroscopic studies on DLC/TM (Cr,Ag, Ti,Ni) multilayers

The hydrogen-free diamond-like carbon (DLC) films with transition metal (TM = Cr, Ag, Ti, Ni) interlayer (bilayer and multilayer) were deposited on to stainless steel and silicon substrates using pulsed laser deposition technique. Secondary ion mass spectroscopy (SIMS) confirmed that the films were hydrogen free. Incorporation of chromium inter layer reduced the stress value by about 3 GPa as determined by micro Raman spectroscopy. Incorporation of the TM inter layer enhanced the photoluminescence (PL) intensity as compared to the monolithic DLC films. The optical band gap determined by spectroscopic ellipsometry for DLC/TM films was found to be in the range of 1.56–1.67 eV.