椭偏光散射分析类金刚石薄膜的散射特性

 基于光学薄膜反射椭偏法的测量原理,对光学薄膜散射椭偏特性进行了研究。给出了光学薄膜散射逆问题的解决方法,并对不同脉冲频率下采用脉冲真空电弧离子镀技术沉积的类金刚石薄膜的散射特性进行了研究。分析了光学薄膜界面的相关特性以及膜层中局部缺陷对散射光椭偏特性的影响。结果表明:随着脉冲频率的增加,所沉积的类金刚石薄膜的相关性变差,且薄膜中的局部缺陷引起的体散射越明显。     

衬底温度对类金刚石薄膜力学性能的影响

 采用脉冲激光沉积方法在不同衬底温度下制备了最高硬度与弹性模量分别达45 GPa和290 GPa,且表面十分光滑的类金刚石薄膜。在相对湿度为80%的条件下,薄膜最低的摩擦系数与磨损率分别为0.045与5.74×10^-10 mm³·N^-1·m^-1。实验结果表明,硬度与弹性模量随衬底温度升高而降低,摩擦系数与磨损率随衬底温度升高而增大。拉曼光谱表明:在室温下制备的薄膜为典型类金刚石结构,sp³含量高达76.8%,而随温度升高,薄膜结构逐渐经无定形碳结构向纳米晶石墨结构方向发展,sp³含量也随之降低,力学性能变差。     

Effect of deposition voltage on the field emission properties of electrodeposited diamond-like carbon films

Diamond-like carbon (DLC) films were deposited on Al substrates by electrodeposition technique under various voltages. The surface morphology and compositions of synthesized films were characterized by scanning electron microscopy and Raman spectroscopy. With the increase of deposition voltage, the sp² phase concentration decreased and the surface morphology changed dramatically. The influence of deposition voltage on the field electron emission (FEE) properties of DLC films was not monotonic due to two adverse effects of deposition voltage on the surface morphology and compositions. The DLC film deposited under 1200 V exhibited optimum FEE property, including a lowest threshold field of 13 V/μm and a largest emission current density of 904.8 μA/cm² at 23.5 V/μm.     

Influences of ultraviolet irradiation on structure and tribological properties of diamond-like carbon films

Two types of diamond-like carbon (DLC) films with different bonding configurations were produced by pulse-assisted and DC-assisted plasma chemical vapor deposition. The chemical composition, surface morphology, microstructure, internal stress and tribological properties of the two films before and after the ultraviolet (UV) irradiation were investigated and compared. It was found that the UV irradiation had little effects on the chemical composition and surface morphology of both the films, but greatly influenced their tribological properties in the opposite trends. This result was attributed to the different changing outcomes of the bonding configuration induced by the UV actions of primary photo-dissociation and secondary recombination, wherein the inherent bonding configuration and internal stress played important roles.     

Characterization of diamond-like carbon films by SEM, XRD and Raman spectroscopy

Diamond-like carbon films were deposited by electrolysis of a water-ethanol solution on Cu at low voltages (60-100 V) at 2 mm interelectrode separation. The films were characterized by scanning electron microscopy (SEM), X-ray diffractometer (XRD) and Raman spectroscopy. The films were found to be continuous and compact with uniform grain distribution. Raman spectroscopy analysis revealed two broad bands at ∼1350 and ∼1580 cm⁻¹. The downshift of the G band of graphite is indicative of the presence of DLC. For XRD analysis, the three strong peaks located at 2θ values of 43.2°, 74.06° and 89.9° can be identified with reflections form (1 1 1), (2 2 0) and (3 1 1) plane of diamond.     

Improving the conductivity of diamond-like carbon films with zinc doping and its material properties

Zinc doped diamond-like carbon (DLC) nanocomposite thin films are fabricated by KrF pulsed laser deposition. Carbon targets containing 3.0, 5.0 and 10.0 atomic percentages of zinc are used as the source for the laser system. Investigation of electrical properties by the four-point probe shows that doping zinc into DLC can lower the electrical sheet resistivity. Microstructural analysis by Raman spectroscopy and XPS show a lower sp³ content but a higher SiC content with an increasing amount of zinc incorporation. The increase of SiC leads to an increase in adhesion strength. Surface roughness of the films also increases while the coefficients of friction for the films do not change.     

Influence of sulfidation treatment on the structure and tribological properties of nitrogen-doped diamond-like carbon films

The nitrogen-doped diamond-like carbon (DLC) films were deposited on high speed steel (HSS) substrates in the direct current unbalanced magnetron sputtering system. Sulphurized layer was formed on the surface of DLC films by means of liquid sulfidation in the intermixture of urea and thiourea solution in order to improve the tribological properties of DLC films. The influence of sulfidation treatment on the structure and tribological properties of DLC films was investigated in this work. The structure and wear surface morphology of DLC films were analyzed by Raman spectroscopy, XPS and SEM, respectively. It reveals that the treated films are smooth and uniform; and sulfur atoms are bonded chemically. The treated films have broader distribution of Raman spectra in the range of 1000-1800 cm⁻¹ and higher I_D/I_G ratio than the untreated films as a result of the appearance of the crystalline graphite structure after the sulfidation treatment. It is showed that the sp² relative content increase in the treated films from the XPS measurement. The Raman results are consistent with the XPS results. The tribological properties of DLC films were investigated using a ball-on-disk rotating friction and wear tester under dry friction conditions. It is found that the sulfidation concentration plays an important part in the tribological properties of the treated DLC films. The results showed the treated films with low sulfidation concentration have a lower friction coefficient (0.1) than the treated films with high sulfidation concentration (0.26) and the untreated films (0.27) under the same friction testing conditions, which can be attributed to both the presence of sulfur-containing materials and the forming of the mechanical alloyed layer on the wear surface. Adding the dry nitrogen to the sliding surface in the testing system helps the friction coefficient of the treated films with low sulfidation concentration to decrease to 0.04 further in this work. On the basis of the experimental results, it is indicated that the liquid sulfidation technique, which is low-cost, non-polluting and convenience, would be an appropriate method for the surface treatment of DLC films.     

含氮类金刚石薄膜的紫外辐照研究

 用射频等离子体方法在玻璃基底上制备的类金刚石（DLC）薄膜，采用离子注入法掺氮，并对掺氮DLC薄膜紫外（UV）辐照前后的性能变化进行了研究。研究结果表明：随氮离子注入剂量及UV辐照时间的增加，位于2 930cm^-1附近的SP ³C-H吸收峰明显变小，而位于1 580cm^-1附近的SP2C-H吸收峰则明显增强，薄膜的电阻率明显呈下降趋势；随UV辐照时间的增加，位于1 078cm^-1附近的Si-O-Si键数量及位于786cm^-1附近的Si-C键数量明显增加。即氮离子注入和UV辐照明显改变了DLC薄膜的结构与特性。     

激光功率密度对类金刚石膜结构性能的影响

采用大功率高重复频率准分子激光溅射热解石墨靶制备了类金刚石膜，研究了激光功率密度对膜的结构和性能的影响，分析了膜的紫外可见透过谱及膜的带隙结构、Raman谱和电子衍射图，结果表明随着激光功率密度由10⁸W／cm²提高至10¹⁰ W／cm²，膜的结构也由无定形非晶结构转变为纳米晶金刚石结构，膜 中的sp³键舍量及各项性能均有提高. 关键词： 激光功率密度 类金刚石膜 性能 结构     

等离子体增强化学气相沉积法制备含氢类金刚石膜的紫外Raman光谱和X射线光电子能谱研究

利用脉冲辉光放电的方法,在硅片上采用不同的沉积工艺制备了含氢类金刚石膜层,并采用Raman光谱和X射线光电子能谱(XPS)对膜层进行表征.用Raman光谱仪在波长为325 nm的紫外光源的激励下观察膜层的键结构.紫外Raman光谱对含氢类金刚石膜是非常有用的,它能有效避免可见光Raman光谱测量时的荧光干扰,清晰地得到膜层的D峰和G峰.同时利用XPS分析得到膜层的sp3键含量,并与Raman光谱所得数据进行比较.通过Raman光谱和XPS分析可以发现,在紫外光源的激励下,膜层的G峰峰位向高频移方向移动,G峰峰位、I(D)/I(G),G峰半高宽和sp3键含量之间存在一定的关系.     

Structure and tribological properties of amorphous carbon films deposited by electrochemical method on GCr15 steel substrate

Amorphous carbon films were deposited on GCr15 steel substrates by electrolysis of methanol, dimethylsulfoxide (DMSO) and the methanol-DMSO intermixture electrolytes, respectively, under high voltage and low temperature conditions. The microstructure and wear morphology of the deposited films were analyzed using X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM) combined with energy dispersive X-ray fluorescence spectrometer (EDX), respectively. The tribological properties of the films were evaluated using a ball-on-disk rotating friction tester under dry friction condition. The results show that the films deposited by electrodeposition technique on GCr15 steel substrates are amorphous carbon films. It is also found that the electrolytes have an obvious influence on the tribological properties of the deposited films with the electrodeposition method. The tribological properties of the films deposited with the intermixture electrolyte are better than those of the films deposited by other pure electrolytes. The related growth mechanism of the films in the liquid-phase electrodeposition is discussed as well in this study. Via the reaction of the CH₃ groups with each other to form carbon network and reaction of the CH₃ and SO²⁺ groups to achieve the doping of sulfur atom in the carbon network, respectively, in other words, amorphous carbon films can be obtained on GCr15 steel substrates by electrodeposition technique.     

Correlation of sp and sp fraction of carbon with electrical, optical and nano-mechanical properties of argon-diluted diamond-like carbon films

In the present work the correlation of electrical, optical and nano-mechanical properties of argon-diluted diamond-like carbon (Ar-DLC) thin films with sp³ and sp² fractions of carbon have been explored. These Ar-DLC thin films have been deposited, under varying C₂H₂ gas pressures from 25 to 75 mTorr, by radio frequency-plasma enhanced chemical vapor deposition technique. X-ray photoelectron spectroscopy studies are performed to estimate the sp³ and sp² fractions of carbon by deconvoluting C 1s core level spectra. Various electrical, optical and nano-mechanical parameters such as conductivity, I-V characteristics, optical band gap, stress, hardness, elastic modulus, plastic resistance parameter, elastic recovery and plastic deformation energy have been estimated and then correlated with calculated sp³ and sp² fractions of carbon and sp³/sp² ratios. Observed tremendous electrical, optical and nano-mechanical properties in Ar-DLC films deposited under high base pressure conditions made it a cost effective material for not only hard and protective coating applications but also for electronic and optoelectronic applications.     

沉积温度对钛硅共掺杂类金刚石薄膜生长、结构和力学性能的影响

采用中频磁控溅射Ti80Si20复合靶在单晶硅表面制备了共掺杂的类金刚石薄膜.研究了沉积温度对薄膜生长速率、化学成分、结构、表面性质和力学性能的影响.结果表明:随沉积温度升高,薄膜生长速率降低,薄膜Ti和Si原子浓度增加,C原子浓度降低;在高温下沉积的薄膜具有低sp3C含量、低表面接触角、低内应力和高的硬度与弹性模量.基于亚表层注入生长模型分析了沉积温度对薄膜生长和键合结构的影响,从薄膜生长机制和微观结构解释了表面性质和力学性能的变化.     

类金刚石和碳氮薄膜的电化学沉积及其场发射性能研究

利用电化学方法在室温下成功地沉积了类金刚石(DLC)薄膜和非晶CN_x薄膜，并 对制备条件进行了讨论.通过扫描电子显微镜、傅里叶变换红外光谱技术，分析了薄膜的表面形貌和化学结合状态.场发射测量结果表明：DLC膜和非晶CN_x的开启场分别为88和 10V/μm；并且在23V/μm的电场下，DLC膜和非晶CN_x膜的发射电流密度分别达到10 和037mA/cm². 关键词： 电化学沉积 类金刚石薄膜 x薄膜')" href="#">CN_x薄膜 场致电子发射     

射频功率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、红外光谱和纳米压痕仪考察了射频功率对类金刚石薄膜表面形貌、微观结构、硬度和弹性模量的影响.结果表明，制备的薄膜具有典型的含H类金刚石结构特征，薄膜致密均匀，表面粗糙度很小.随着射频功率的升高，薄膜中成键H的含量逐渐降低，而薄膜的sp3³含量、硬度以及弹性模量先升高， 后降低，并在射频功率为100W时达到最大. 关键词： 等离子增强化学气相沉积 类金刚石薄膜 射频功率 结构和性     

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.     

The effect of nitrogen and oxygen plasma on the wear properties and adhesion strength of the diamond-like carbon film coated on PTFE

Diamond-like carbon (DLC) films were deposited on polytetrafluoroethylene (PTFE) using a radiofrequency plasma chemical vapour deposition method. Prior to DLC coating, the PTFE substrates were modified with O₂ and N₂ plasma to enhance the adhesion strength of the DLC film to the substrate. The effect of the plasma pre-treatment on the chemical composition and the surface energy of the plasma pre-treated PTFE surface was investigated by X-ray photoelectron spectroscopy (XPS) and static water contact angle measurement, respectively. A pull-out test and a ball-on-disc test were carried out to evaluate the adhesion strength and the wear properties of the DLC-coated PTFE.In the N₂ plasma pre-treatment, the XPS result indicated that defluorination and the nitrogen grafting occurred on the plasma pre-treated PTFE surface, and the water contact angle decreased with increasing the plasma pre-treatment time. In the O₂ plasma pre-treatment, no grafting of the oxygen occurred, and the water contact angle slightly increased with the treatment time. In the pull-out test, the adhesion strength of the DLC film to the PTFE substrate was improved with the plasma pre-treatment to the PTFE substrate, and N₂ plasma pre-treatment was more effective than the O₂ plasma pre-treatment. In the ball-on-disc test, the DLC film with the N₂ plasma pre-treatment showed good wear resistance, compared with that with O₂ plasma pre-treatment.     

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.     

Structural, mechanical and hydrophobic properties of fluorine-doped diamond-like carbon films synthesized by plasma immersion ion implantation and deposition (PIII–D)

Fluorine-doped diamond-like carbon (a-C:F) films with different fluorine content were fabricated on Si wafer by plasma immersion ion implantation and deposition (PIII–D). Film composition and structure were characterized by X-ray photoelectron spectroscopy (XPS) and Raman scattering spectroscopy. Surface morphology and roughness were analyzed by atomic force microscopy (AFM). Hardness and scratch resistance were measured by nano-indentation and nano-scratch, respectively. Water contact angles were measured by sessile drop method. With the increase of the CF₄ flux, fluorine content was gradually increased to the film. Raman spectra indicates that these films have a diamond-like structure. The addition of fluorine to diamond-like carbon films had a critical influence on the film properties. The film surface becomes more smoother due to the etching behavior of F⁺. Hardness was significantly reduced, while the scratch resistance results show that these films have a fairly good adhesion to the substrate. Evident improvements of the hydrophobicity have been made to these films, with contact angles of double-stilled water approaching that of polytetrafluoroethylene (PTFE). Our study suggests that broad application regions of the fluorine-doped amorphous carbon films with diamond-like structure, synthesized by PIII–D, can be extended by combining the non-wetting properties and mechanical properties which are far superior to those of PTFE.     

Influence of sputter-etching of substrate on the microstructural and optical properties of ZnO films deposited by RF magnetron sputtering

ZnO films were prepared using radio frequency magnetron sputtering on Si(1 1 1) substrates that were sputter-etched for different times ranging from 10 to 30 min. As the sputter-etching time of the substrate increases, both the size of ZnO grains and the root-mean-square (RMS) roughness decrease while the thickness of the ZnO films shows no obvious change. Meanwhile, the crystallinity and c-axis orientation are improved by increasing the sputter-etching time of the substrate. The major peaks at 99 and 438 cm⁻¹ are observed in Raman spectra of all prepared films and are identified as E₂(low) and E₂(high) modes, respectively. The Raman peak at 583 cm⁻¹ appears only in the films whose substrates were sputter-etched for 20 min and is assigned to E₁(LO) mode. Typical ZnO infrared vibration peak located at 410 cm⁻¹ is found in all FTIR spectra and is attributed to E₁(TO) phonon mode. The shoulder at about 382 cm⁻¹ appearing in the films whose substrates were sputter-etched for shorter time (10-20 min) originates from A₁(TO) phonon mode. The results of photoluminescence (PL) spectra reveal that the optical band gap (Eg) of the ZnO films increases from 3.10 eV to 3.23 eV with the increase of the sputter-etching time of the substrate.