液相沉积法制备类金刚石膜的研究

探讨了用液相法在钛合金表面沉积制备类金刚石膜的可能性,研究了沉积膜工艺条件对膜的影响,得出了适宜的沉积条件。结果表明,通过液相法可以沉积制备得到DLC膜,但与沉积条件有着密切的关系。当电压为1600~1850V、温度为60~62℃、电极间距为8~10mm、沉积时间大于36h时,才能在钛合金表面得到完整的DLC绝缘膜。     

SiC/DLC过渡层对类金刚石薄膜力学性能的影响

采用等离子体浸没离子注入及沉积技术在钛合金(Ti6Al4V)表面制备了类金刚石薄膜和含有SiC/DLC过渡层的类金刚石薄膜。采用拉曼光谱及扫描电子显微镜分析了薄膜的成分和结构,并利用超显微硬度计、薄膜结合力测试仪和往复式摩擦实验机研究了薄膜的硬度、韧性、膜/基结合力和耐磨性。研究结果表明,SiC/DLC过渡层可以提高钛合金(Ti6Al4V)表面类金刚石薄膜的韧性及膜/基结合力,与未制备过渡层的类金刚石薄膜相比,含有SiC/DLC过渡层的类金刚石薄膜的耐磨性明显提高。     

真空弧源沉积类金刚石薄膜及其性能研究

采用真空弧源沉积技术在钛合金及Si(100)表面合成DLC薄膜．通入不同的氩气．控制DLC薄膜中的SP3／SP2比值。研究表明，薄膜硬度可达96GPa．随着氩气流量的增加，薄膜的硬度先增加．后有明显降低。随着氩气流量的增加，类金刚石薄膜中．SP2键增加，SP3键减少，而血液相容性明显提高。DLC薄膜具有优异的耐磨性，摩擦系数低，与钛合金基体结合牢固。     

磁过滤阴极真空弧法制备类金刚石膜的场致发射特性研究

采用磁过滤阴极真空弧沉积法,在Cu基底表面上制备了以钛(Ti)和碳化碳(TiC)作为过滤层的类金刚石膜层。利用自制的场致发射特性测试设备,研究了类金刚石膜层的场致发射特性。利用拉曼光谱仪(Raman)和扫描电子显微镜(SEM)等分析方法对类金刚石膜的键合结构和微观形貌进行了表征。研究发现,利用磁过滤阴极真空弧沉积法可以在沉积温度100℃下制备膜基结合力较好的类金刚石膜。沉积速率为15 nm/min。类金刚石膜具有较好的场致发射特性,开启电压约为40 V/μm。Raman分析得到不同基底偏压下的类金刚石膜的I_D/I_G为1.19～1.57;SEM分析显示薄膜的微观结构上具有微米级突起结构。实验表明,应用磁过滤阴极真空弧方法可以制备出高sp~3含量、表面具有微米级突起的类金刚石膜,这种类金刚石膜具有有利于场致发射的特性。     

直流负偏压对类金刚石薄膜结构和性能的影响

利用直流-射频-等离子体增强化学气相沉积技术在单晶硅表面制备了类金刚石薄膜，采用原子力显微镜、Raman光谱、X射线光电子能谱、红外光谱、表面轮廓仪和纳米压痕仪考察了直流负偏压对类金刚石薄膜表面形貌、微观结构、沉积速率和硬度等性能的影响。结果表明：无直流负偏压条件下，薄膜呈现有机类聚合结构，具有较低的SP3含量和硬度；叠加上直流负偏压后，薄膜具有典型的类金刚石结构特征，SP3含量和硬度得到了显著的提高；但随着直流负偏压的升高，薄膜的沉积速率和H含量逐渐降低，而SP3含量和硬度在直流负偏压为200V时出现最大值，此后逐渐降低。     

316不锈钢表面沉积厚类金刚石膜层的性能研究

采用脉冲辉光放电等离子体气相沉积法在316不锈钢表面沉积膜层较厚的类金刚石膜层。利用拉曼光谱仪(Raman)、X射线光电子能谱仪(XPS)、傅里叶变换红外光谱仪(FT-IR)、光学显微镜、显微硬度计和摩擦磨损实验机分别对膜层组成和微观结构及机械性能进行了表征。研究发现,通过脉冲辉光放电等离子体气相沉积法,在316不锈钢表面制备的类金刚石膜层光滑致密;Raman分析得到的ID/IG和IT/IG比值分别为0.72和0.22;FT-IR分析可知膜层含有较多的CHx组成的sp3键;摩擦磨损试验得到膜层的摩擦系数低至0.100,XPS分析膜层sp3含量高达60.7%和光学显微镜测量膜层的厚度达到7mm。由此可知沉积类金刚石膜层后,可以显著地改善316不锈钢表面的机械性能。     

TiNi合金表面沉积类金刚石薄膜的性能评价

类金刚石膜作为新型的生物材料得到了广泛的关注。本实验制备的薄膜为典型的类金刚石膜,膜层比较致密、均匀和光滑。膜层硬度随离子束能量变化,在束电源为750V附近出现峰值,硬度达到了15GPa,该膜的摩擦系数为0.124。在Troyde’s模拟体液中的电化学分析表明,类金刚石膜显著提高了TiNi合金表面抗点蚀能力。     

电化学沉积DLC膜及其表征

采用电化学沉积方法，甲醇有机溶剂作碳源，在直流电源作用下在单晶硅表面沉积得到碳薄膜。薄膜不溶于苯、丙酮等有机溶剂，具有较高的硬度(16GPa左右)，用AFM、Raman和FTIR分析手段对该薄膜表面形貌和结构进行表征，Raman和FTIR结果表明电化学沉积得到的是含氢的类金刚石碳薄膜。通过研究样品薄膜的XPS和XAES谱图特征，进一步证实薄膜是DLC薄膜，并用线性插入法估算出样品薄膜中SP^3的相对含量为60％，同时推测了电化学沉积DLC薄膜的生长机理。     

含钨类金刚石薄膜的制备与性能研究

为了满足制备较厚低摩擦系数类金刚石薄膜（DLC）耐磨镀层的实际需求，对在等离子增强化学气相沉积的类金刚石薄膜（W—DLC）中掺钨进行了系统研究。研究结果表明，类金刚石薄膜掺入钨，在较宽的工艺条件范围内，都可以沉积厚度超过5μm的薄膜而不发生剥落。适当控制工艺条件和膜中钨的含量可以提高薄膜的硬度，降低磨损率，且保持低的摩擦系数和较高的沉积速率。     

掺氮类金刚石薄膜的制备与性能研究

利用空心阴极放电在玻璃基底表面沉积掺氮类金刚石(DLc)薄膜.拉曼光谱(Raman)分析表明,所制备的碳膜具有典型的类金刚石结构.扫描电镜(SEM)和原子力显微镜(AFM)分析了薄膜表面形貌和粗糙度;利用摩擦磨损仪测量膜的摩擦磨损性能.结果表明,氮的掺入使得薄膜中颗粒致密平整,改变了薄膜的表面微观形貌,进而改善了薄膜的摩擦磨损性能.     

TC4钛合金电火花沉积反应合成Ti(CN)涂层

利用自制的电火花沉积充气密闭式保护装置和DZ-1400型电火花沉积机,以石墨为电极,以工业氮气为保护气和反应气,在TC4钛合金基体上制备Ti(CN)强化层.利用SEM分析了沉积层单沉积点表面形貌和组织结构,利用XRD测定了涂层物相组成,利用XPS分析了沉积层表面元素组成,利用SEM和AES分析了沉积层截面形貌、结合状态和元素组成.结果表明,沉积层是反应涂层,强化相由电极元素C、保护气体元素N和基体元素Ti反应生成,沉积层主要由TiC0.51N0.12相、Ti0.80V0.20相和C相组成,沉积层与基体结合致密,呈冶金结合.     

Electrophoretic deposition of hydroxyapatite

Hydroxyapatite powders were prepared by a chemical precipitation method and electrophoretically deposited on Ti6Al4V surgical alloy substrates. The powders were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), particle size distribution and zeta potential measurements. Prior to electrophoretic deposition, anodic films were obtained on Ti6Al4V and studied by the Auger method. It was established that experimental conditions of powder preparation, electric field and stirring have a significant influence on suspension stability and deposit morphology. The deposition yield was studied at various deposition durations and applied voltages. Sintered coatings were studied by SEM and XRD.     

Growth of polycrystalline and nanocrystalline diamond films on pure titanium by microwave plasma assisted CVD process

Well-faceted polycrystalline diamond (PCD) films were deposited along with nanocrystalline diamond (NCD) films on the pure titanium substrate by a microwave plasma assisted chemical vapor deposition (MWPCVD) system in the environment of CH₄ and H₂ gases at a moderate temperature. Diamond film deposition on pure titanium and Ti alloys is always extremely hard due to the high diffusion coefficient of carbon in Ti, the big mismatch in their thermal expansion coefficients, the complex nature of the interlayer formed during diamond deposition, and the difficulty of attaining very high nucleation density. A well-faceted PCD film and a smooth NCD film were successfully deposited on pure Ti substrate by using a simple two-step deposition technique. Both films adhered well. Detailed experimental results on the preparation, characterization and successful deposition of the diamond coatings on pure Ti are discussed. Lastly, it is shown that smooth NCD film can be deposited at moderate temperature with sufficient diamond quality for mechanical and tribological applications.     

Preparation of Diamond-like Carbon Films on the Surface of Ti Alloy by Electro-deposition

In this paper, diamond-like carbon (DLC) films were deposited on Ti alloy by electro-deposition. DLC films were brown andcomposed of the compact grains whose diameter was about 400 nm. Examined by XPS, the main composition of the filmswas carbon. In the Raman spectrum, there were a broad peak at 1350 cm~(-1) and a broad peak at 1600 cm~(-1), which indicatedthat the films were DLC films.     

Precursor gas effect on the mechanical and optical properties of ion beam deposited diamond-like carbon films

The effect of precursor gases on the diamond-like carbon (DLC) film deposition was investigated by the direct ion beam deposition method. DLC films were deposited using methane and benzene as the precursor gases. Ion energies for the deposition range from 100 to 700 eV were achieved by adjusting the beam voltage. The residual stresses, refractive indices and optical band gaps were compared at the same ion energy. We observed significant differences in residual stress and optical properties between these films. As in r.f. plasma-assisted CVD, the residual stresses of the films deposited from benzene show a characteristic behaviour of lower ion energy deposition than those deposited from methane. The present observations are discussed in terms of the difference in ion energy per carbon atom at the growth surface. We also observed that the Ar addition effect on the residual stress is strongly dependent on the precursor gases.     

TiO2 coating of high surface area silica gel by chemical vapor deposition of TiCl4 in a fluidized-bed reactor

TiO2 was deposited on high surface area porous silica gel (400 m2g(-1)) in a fluidized bed reactor. Chemical vapor deposition was employed for the coating under vacuum conditions with TiCl4 as precursor. Nitrogen physisorption, X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy and UV-vis spectroscopy were applied to characterize the obtained TiO2-SiO2 composites with different Ti loadings up to 5 wt%. Only a slight decrease in the specific surface area was detected at low Ti loadings. At a Ti loading of 2 wt%, TiO2 was found to be highly dispersed on the SiO2 surface likely in form of a thin film. At higher Ti loadings, two weak reflections corresponding to anatase TiO2 were observed in the diffraction patterns indicating the presence of crystalline bulk TiO2. High resolution XPS clearly distinguished two types of Ti species, i.e., Ti-O-Si at the interface and Ti-O-Ti in bulk TiO2. The presence of polymeric TiOx species at low Ti loadings was confirmed by a blue shift in the UV-vis spectra as compared to bulk TiO2. All these results point to a strong interaction between the TiO2 deposit and the porous SiO2 substrate especially at low Ti loadings.     

PZT薄膜反提拉生长的PbO挥发与退火条件研究

通过一新的溶胶-凝胶工艺:反提拉涂膜方法,在Si(100)和Pt(111)/Ti/SiO2/Si(100)基片上制备了PZT(Zr/Ti=52/48)铁电薄膜,并研究了退火工艺及其PbO的挥发对薄膜微结构、表面形貌、取向、及铁电性能的影响.本文首次提出并应用反提拉涂膜技术制备了PZT薄膜,此技术相对于传统的溶胶-凝胶工艺具有以下几方面的优点:操作控制简单方便、成本低、原料利用率高、无污染等.研究发现PZT薄膜通过增加PT晶种层后可以抑制PbO的挥发,同时薄膜呈现较强的(110)取向;在薄膜的退火处理过程中还发现氧气氛有助于降低PbO的挥发、促进晶粒的长大和降低钙钛矿的晶化温度,在氧气氛中退火的PZT薄膜显示了很好的铁电性能,其剩余极化强度明显增大而矫顽场只有极小的增加.     

Synthesis and characterization of nano-crystalline CVD diamond film on pure titanium using Ar/CH4/H2 gas mixture

Titanium and Ti alloys have poor tribological properties and deposition of a well adherent diamond coating is a promising way to solve this problem. But diamond film deposition on pure titanium and Ti alloys is always difficult due to the high diffusion coefficient of carbon in Ti, the large mismatch in their thermal expansion coefficients, the complex nature of the interlayer formed during diamond deposition, and the difficulty of achieving very high nucleation density. A nano-crystalline diamond (NCD) film can resolve Ti and Ti alloys weak tribological performance due to its smooth surface. A well-adhered NCD film was successfully deposited on pure Ti substrate by using a microwave plasma assisted chemical vapor deposition (MWPCVD) system in the environment of Ar, CH₄ and H₂ gases at a moderate temperature. Detailed experimental results on the preparation, characterization and successful deposition of the NCD film on pure Ti are discussed.     

Investigation of anti-corrosion properties of Ti:C gradient layers manufactured in hybrid deposition system

Excellent properties of hard carbon layers and especially, the unique combination of tribological, chemical and physical properties make them a popular coating material for use on surgical prosthesis, biomedical implants, and machine tools. However, their well-known poor adhesion and high internal stress disqualifies them in many possibilities of industrial applications. These drawbacks were improved by deposition of Ti buffer layer. By a combination of Radio Frequency Plasma Assisted Chemical Vapor Deposition (RFPACVD) and DC magnetron sputtering methods, thick carbon films were manufactured on Rex 734 steel. Structure and chemical composition of deposited layers was determined by scanning electron microscope and energy dispersive spectrometer analysis. The main purpose of this work was to determine the corrosion properties of Rex 734 alloy in a typical 0.5 M NaCl solution and to find the influence of Ti:C gradient layers on these properties. Anti-corrosion behavior was measured by the detection of corrosion potential in open circuit and the registration of potentiodynamic characteristics according to Stern–Geary and Tafel methods. Five different types of samples were studied: for full analysis the investigation was conducted for every structural component of the layer: for pure Ti deposited on Rex 734 as well as for Ti containing carbon layer and carbon layer deposited subsequently, and finally the corrosion resistance of Rex 734 steel was measured for comparison. As a result of the investigation it was noticed that the Ti–C interlayer enables to maximize the thickness of DLC films and Ti:C gradient layers have the good influence on the corrosion features of Rex 734 alloy. International Conference on Surfaces Coatings and Nanostructured Materials NanoSMat 2007 Organized by Society of Nanoscience and Nanotechnology.