钛离子注入类金刚石碳膜的结构与性能的研究

使用金属离子注入的方法制备了 Ti掺杂的DLC膜。采用原子力显微镜观察了薄膜的表面形貌,Ti掺杂后 DLC 膜的表面粗糙度明显减小,表面光洁度增加,颗粒细化。拉曼光谱分析表明实验获得的薄膜是典型的DLC膜,掺杂Ti后的 DLC膜的拉曼光谱存在明显的肩峰,DLC膜化学结构中的sp2 组分增加,sp3 组分减少。透射电子显微镜分析表明Ti注入后有TiC纳米晶形成。掺入Ti的 DLC膜的硬度从 14GPa增加到 20GPa。Ti 掺杂后的 DLC 膜的摩擦系数(0.15)明显低于未掺杂的DLC膜的摩擦系数(0.21),Ti离子注入有助于提高薄膜的抗磨损性。     

AlTiN layer effect on mechanical properties of Ti-doped diamond-like carbon composite coatings

Ti/Ti-doped diamond-like carbon (DLC) and Ti/AlTiN/Ti-DLC composite coatings were deposited by magnetron sputtering on W18Cr4V high speed steel substrates. The effect of the AlTiN support layer on the properties of these composite coatings was investigated through microstructure and mechanical properties characterization, including hardness, elastic modulus, coefficient of friction and wear properties measured by scanning electron microscopy, Raman spectroscopy, scratch and ball-on-disk friction tests. Ti and AlTiN interlayers have a columnar structure with 50-80 nm grains. The hardness and elastic modulus of Ti/Ti-DLC and Ti/AlTiN/Ti-DLC coatings is 25.9 ± 0.4, 222.2 ± 6.3 GPa and 19.3 ± 1, 205.6 ± 6.7 GPa, respectively. Adhesion of Ti-DLC, Ti/AlTiN/Ti-DLC and AlTiN/Ti-DLC coatings expressed as the critical lateral force is 26.5 N, 38.2 N, and 47.8 N, respectively. Substrate coefficient of friction without coatings is 0.44, and it is 0.1 for Ti/Ti-DLC and Ti/AlTiN/Ti-DLC coatings. Wear resistance of Ti/AlTiN/Ti-DLC composite coatings is much higher than Ti/Ti-DLC coatings based on the wear track width of 169.8 and 73.2 μm, respectively, for the same experimental conditions.     

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。     

Evaluation of microstructures and mechanical properties of diamond like carbon films deposited by filtered cathodic arc plasma

Diamond-like carbon (DLC) films were deposited by a cathodic arc plasma evaporation (CAPD) process, using a mechanical shield filter combined with a magnetic filter with enhanced arc structure at substrate-bias voltage ranging from − 50 to − 300 V. The film characteristics were investigated using Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and high-resolution transmission electron microscopy (HRTEM). The mechanical properties were investigated by using a nanoindentation tester, scratch test and ball on disc wear test. The Raman spectra of the films showed that the wavenumber ranging from 900 to 1800 cm^− 1 could be deconvoluted into 1140 cm^− 1, D band and G band. The bias caused a significant effect on the sp³ content which was increased with the decreasing of I_D/I_G ratio. The XPS spectra data of the films which were etched by H⁺ plasma indicated the sp³ content are higher than those of the as-deposited DLC films. This implied that there is a sp²-rich layer present on the surface of the as-deposited DLC films. The nanoindentation hardness increased as the maximum load increased. A 380 nm thick and well adhered DLC film was successfully deposited on WC-Co substrate above a Ti interlayer. The adhesion critical load of the DLC films was about 33 N. The results of the wear tests demonstrated that the friction coefficient of the DLC films was between 0.12 and 0.2.     

Deposition and characterization of TiBCN films by cathodic arc plasma evaporation

TiBCN thin films were deposited on Si(100) substrate by reactive cathodic arc evaporation from a graphite/boron-containing composite target and Ti target in an N₂ atmosphere. Characteristics and microstructures of the films were investigated, deposited under different target currents. Raman spectroscopy and high resolution X-ray photoelectron spectroscopy (HRXPS) were employed to investigate the spectrum and bonding states of films. The film microstructures were evaluated by using an atomic force microscope (AFM), a field emission scanning electron microscopy (FEGSEM), a glancing angle X-ray diffractometry (GAXRD) and a high-resolution transmission electron microscopy (HRTEM). Results demonstrated that the TiBCN films were synthesized successfully and adhered well to the silicon substrate. The Raman spectra showed that wavenumbers ranging from 900 to 1800 cm^− 1 consisted of D and G bands, similar to that of cathodic arc plasma deposited DLC. Raman spectra proved that the intensity of D and G bands decreased by increasing Ti target currents. HRTEM results established that TiBCN films revealed an amorphous structure while the Ti target current was low. As the Ti target current increased, the TiBCN films revealed a nanocomposite structure, an amorphous matrix consisting of nano scale Ti(C,N) and TiB crystalline, which were comparable to GAXRD, Raman and HRXPS results. The HRXPS spectra of B1s, C1s, N1s and Ti2p in the TiBCN films reveal much broader peaks; this indicated that there is more than one category of bonding state surrounding each of Ti, B, C and N atoms. Morphology, characteristics and film concentration as a function of deposition parameters were also investigated in this study.     

非平衡磁控溅射类金刚石碳膜的性能

用非平衡磁控溅射的方法在室温下制备了光滑、均匀、致密的类金刚石(DLC)薄膜,分析和研究了DLC膜的形貌、结构和摩擦特性.结果表明,靶工作电流对DLC膜的沉积有重要的影响.随着工作电流的增大,薄膜的沉积速率增大,薄膜中sp3键的含量增加.薄膜的摩擦系数随着工作电流的增加略有增大,在摩擦的初始阶段,摩擦系数较高,随着摩擦循环次数的增加,摩擦系数逐渐减小,并逐渐趋于稳定.     

基体表面粗糙度对MoS_(2)/Ti薄膜摩擦磨损性能的影响EI北大核心CSCD

为揭示基体表面粗糙度对MoS_(2)/Ti固体润滑薄膜摩擦磨损性能的影响规律,并探究其摩擦磨损机理,采用磁控溅射方法,在不同表面粗糙度的轴承钢基体上沉积MoS_(2)/Ti薄膜。通过划痕测试仪、X射线衍射仪、场发射扫描电子显微镜和粗糙度轮廓仪,分别评价MoS_(2)/Ti薄膜的膜基结合力、物相成分、表面微观形貌以及表面粗糙度,并采用球-盘摩擦磨损实验研究干摩擦、固体-油复合润滑和固体-脂复合润滑条件下,MoS_(2)/Ti薄膜的摩擦磨损性能。结果表明:随着基体表面粗糙度的增加,MoS_(2)/Ti薄膜的表面粗糙度逐渐增加;薄膜中(002)_(MoS_(2))和(100)_(MoS_(2))衍射峰的强度先减弱后增加;薄膜与基体的结合性能降低。当基体表面粗糙度为0.01μm时,干摩擦条件下MoS_(2)/Ti薄膜具有良好的润滑特性,平均摩擦因数为0.101,磨痕浅且小;随基体粗糙度的升高,样品的平均摩擦因数和磨损率均是先增大后减小,薄膜的主要磨损机制由磨粒磨损转变为屑片形成和破碎。当基体粗糙度较大时(R_(a)=0.26μm),分子间相互作用的影响大于机械啮合作用。采用固体-油复合润滑,高基体粗糙度的薄膜磨损表面不再出现片层剥落现象,磨痕较浅,平均摩擦因数最高可减小19%。固体-脂复合润滑条件下,样品摩擦磨损性能较差,基体粗糙度对摩擦因数的影响不显著。     

Analysis on Structure and Properties of Diamondlike Carbon Films from Ion Beam Deposition

Diamondlike carbon (DLC) films from a primary ion beam deposition system, were examined using nanoindentation, SEM, AES, XPS, and Raman Spectroscopy. The films have hardness values ranging from 21 to 29 GPa. The results of SEM and AES show that the films are predominantly carbon without any crystalline features, and that nitrogen is incorporated as nitrogen is used as the ion beam source. XPS, and Raman Spectroscopy confirm that the films are amorphous carbon with a combination of sp³ with sp² bonding. It is concluded that DLC films can be directly deposited on steel using a single ion beam to sputter the solid target, and the structure and properties of DLC largely depend on ion beam source.     

无氢DLC涂层的摩擦学性能

为了探究轮胎模具无氢类金刚石(DLC)涂层的摩擦学特性,增强轮胎模具的易脱模、防粘、自清洁性能以及提高轮胎质量与服役寿命,以轮胎模具常用的35钢为基体,利用电弧离子镀在基体试样上制备无氢DLC涂层,对涂层Raman光谱、表面粗糙度、表面微观形貌、纳米硬度、结合力和摩擦系数进行了分析,着重研究涂层摩擦前后表面微观形貌的变化以及摩擦磨损机理。结果表明:通过改变表面粗糙度可以有效降低涂层的摩擦系数,涂层摩擦系数随粗糙度减小而显著降低;在140℃高温条件下,摩擦系数最小低至0.363 4,且涂层纳米硬度可达32.45 GPa,弹性模量高达348.94 GPa。无氢DLC涂层完全满足轮胎模具减摩耐磨和自清洁性的使用要求,为制造高性能轮胎模具提供了一种可行的工艺选择。     

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.     

Wear behaviour and rolling contact fatigue life of Ti/TiN/DLC multilayer films fabricated on bearing steel by PIIID

In order to improve the friction and wear behaviours and rolling contact fatigue (RCF) life of bearing steel materials, Ti/TiN/DLC (diamond-like carbon) multilayer hard films were fabricated onto AISI52100 bearing steel surface by plasma immersion ion implantation and deposition (PIIID) technique. The micro-Raman spectroscopy analysis confirms that the surface film layer possess the characteristic of diamond-like carbon, and it is composed of a mixture of amorphous and crystalline phases, with a variable ratio of sp²/sp³ carbon bonds. Atomic force microscope (AFM) reveals that the multilayer films have extremely smooth area, excellent adhesion, high uniformity and efficiency of space filling over large areas. The nanohardness (H) and elastic modulus (E) measurement indicates that the H and E of DLC multilayer films is about 32 GPa and 410 GPa, increases by 190.9% and 86.4%. The friction and wear behaviours and RCF life of DLC multilayer films specimen have also been investigated by ball-on-disc and three-ball-rod fatigue testers. Results show that the friction coefficient against AISI52100 steel ball decreases from 0.92 to 0.25, the longest wear life increases nearly by 22 times. In addition, wear tracks of the PIIID samples as well as wear tracks of the sliding steel ball were analyzed with the help of optical microscopy and scanning electron microscopy (SEM). The L₁₀, L₅₀, L_a and mean RCF life L of treated bearing samples, in 90% confidence level, increases by 10.1, 4.2, 3.5 and 3.4 times, respectively. Compared with the bearing steel substrate, the RCF life scatter extent of Ti/TiN/DLC multilayer films sample is improved obviously.     

Investigation of the microstructure, mechanical properties and tribological behaviors of Ti-containing diamond-like carbon films fabricated by a hybrid ion beam method

Diamond-like carbon (DLC) films with various titanium contents were investigated using a hybrid ion beam system comprising an anode-layer linear ion beam source and a DC magnetron sputtering unit. The film composition and microstructure were characterized carefully by X-ray photoelectron spectroscopy, transmission electron microscopy and Raman spectroscopy, revealing that the doped Ti atoms had high solubility in the DLC films. The maximum solubility was found to lie between about 7 and 13 at.%. When the Ti content was lower than this solubility, the doped Ti atoms dissolved in the DLC matrix and the films exhibited the typical features of the amorphous DLC structure and displayed low compressive stresses, friction coefficients and wear rates. However, as the doped content exceeded the solubility, Ti atoms bonded with C atoms, resulting in the formation of carbide nano-particles embedded in the DLC matrix. Although the emergence of the carbide nano-particles promoted graphitizing due to a catalysis effect, the film hardness was enhanced to a great extent. On the other hand, the hard carbides particles caused abrasive wear behavior, inducing a high friction coefficient and wear rate.     

离子束类金刚石膜的摩擦磨损及耐蚀性能

研究了沉积类金刚石膜 (DLC)的 4 0Cr钢的摩擦磨损性质 ,定量分析了DLC膜的耐蚀性。研究表明 :DLC膜能显著降低 4 0Cr钢表面摩擦系数和表面粗糙度 ,在相同载荷条件下DLC膜的磨损速率比 4 0Cr钢低 2个数量级 ;在各种腐蚀介质中 ,DLC膜的腐蚀速率明显低于 4 0Cr的 ,且其电极电位、自然腐蚀电位和点蚀击穿电位均高于 4 0Cr钢的 ,表明DLC膜可提高 4 0Cr钢的耐蚀性能     

用于微机电系统的类金刚石膜制备及表征

采用等离子体源离子注入和电子回旋共振-微波等离子体辅助化学气相沉积技术相结合的方法在Si衬底上制备出了性能良好的类金刚石膜.通过共聚焦Raman光谱验证了薄膜的类金刚石特性,用原子力显微镜、微摩擦计和扫描电镜等对薄膜的表面形貌、摩擦系数和耐磨损性能进行了表征和测量.结果表明,用离子注入法制备过渡层大大提高了DLC膜与衬底的结合强度,薄膜的表面比较光滑,粗糙度大约为0.198 nm,具有较低的摩擦系数(0.1～0.15),具有较好的耐磨损性能.     

Microstructure and tribological performance of CNx–TiNx composite films prepared by pulsed laser deposition

CN_x–TiN_x composite films were prepared on high-speed steel (HSS) substrate by pulsed KrF excimer laser co-deposition process with graphite/Ti combined targets and a substrate temperature of 200 °C. The composition, morphology and microstructure of the films were characterized by energy dispersive X-ray spectrum (EDS), scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and high-resolution transmission electron microscopy (HRTEM). The adhesion and tribological performance of the films were investigated using a conventional scratch tester and a ball-on-disk tribometer, respectively. In the graphite/Ti range of 0.5–2.0 of the target, TiN_x, a-CN_x and metallic Ti phase were found in the composite films. The TiN_x disappeared in the films at a high graphite/Ti ratio of the target. With increasing the graphite/Ti ratio of the target, the adhesion to substrate of the composite films deteriorated from 46 N to 26 N, and the friction coefficient decreased from 0.23 to 0.17. The composite film deposited at the graphite/Ti ratio of 1.0 showed a low friction coefficient, good adhesion and wear rate of 3.2 × 10⁻⁷ mm³/Nm in humid air.     

电弧离子镀CrAlN-DLC硬质复合薄膜的成分、结构与性能

为了改善CrAlN薄膜的摩擦性能, 本研究在增强磁过滤脉冲偏压电弧离子镀设备上, 用分离靶弧流调控技术在硬质合金基体上分别制备了不同成分的CrAlN-DLC硬质复合薄膜, 并采用不同手段表征了薄膜的表面形貌、成分、相结构以及力学和摩擦性能。结果表明, 不同成分薄膜表面均平整致密, 膜厚均在1.05 μm左右。随着靶弧流比I_C/I_CrAl的升高, 薄膜中碳的原子分数由33.1%升至74.6%。薄膜的相结构主要由晶体相和非晶相复合组成, 其晶体相主要为c-(Cr,Al)N相, 且随着碳含量增大晶体相减少、晶粒尺寸减小, 其非晶相主要为DLC, 其中sp²/sp³的比值随碳含量增大而减小。相应地, 薄膜的硬度随着碳含量增大而提高, 当碳的原子分数为74.6%时, 达到最大值(26.2±1.4) GPa, 且该成分点处薄膜摩擦系数也降至最小值0.107, 磨损率仅为3.3×10^-9 mm³/Nm。综合而言, 当非晶DLC相最多时, CrAlN-DLC复合薄膜的综合性能达到最佳, 较之CrAlN薄膜, 摩擦性能显著提高。     

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.     

Coating NiTi archwires with diamond-like carbon films: reducing fluoride-induced corrosion and improving frictional properties

This study aims to coat diamond-like carbon (DLC) films onto nickel–titanium (NiTi) orthodontic archwires. The film protects against fluoride-induced corrosion and will improve orthodontic friction. ‘Mirror-confinement-type electron cyclotron resonance plasma sputtering’ was utilized to deposit DLC films onto NiTi archwires. The influence of a fluoride-containing environment on the surface topography and the friction force between the brackets and archwires were investigated. The results confirmed the superior nature of the DLC coating, with less surface roughness variation for DLC-coated archwires after immersion in a high fluoride ion environment. Friction tests also showed that applying a DLC coating significantly decreased the fretting wear and the coefficient of friction, both in ambient air and artificial saliva. Thus, DLC coatings are recommended to reduce fluoride-induced corrosion and improve orthodontic friction.     

基于RFPECVD方法不锈钢上沉积类金刚石薄膜的机械与摩擦特性

讨论用射频等离子体增强化学气相沉积(RFPECVD)工艺,在室温下实现在1Cr18Ni9Ti不锈钢基底上镀类金刚石(DLC)膜.为提高DLC膜的结合力,首先在不锈钢基底上沉积Ti/TiN/TiC功能梯度膜.借助所设计的界面过渡层,成功地在不锈钢基底上沉积了一定厚度的DLC膜.通过优化沉积参数,所沉积的DLC膜在与100Cr6钢球对磨时摩擦系数低于0.020.在摩擦过程中DLC膜的磨损机制借助SEM、Raman分析进行了研究.     

Analysis of plastic deformation in diamond like carbon films-steel substrate system with tribological tests

The influence of plastic deformation of the substrate on the tribological properties of diamond like carbon (DLC) films was investigated in DLC films-steel substrate system. The tribological properties of DLC films deposited on different hardness steel were evaluated by a ball on disk rotating-type friction tester at room temperature under different environments. In dry nitrogen, DLC films on soft steel exhibited excellent tribological properties, especially obvious under high load (such as 20 N and 50 N). However, DLC films on hard steel were worn out quickly at load of 20 N. Plastic deformation was observed on soft steel after tribological tests. The width and depth of plastic deformation track increased with increase of the experimental load. Super low friction and no measurable wear were kept in good condition even large plastic deformation under high load conditions in DLC films-soft steel system. In open air, DLC films on soft steel exhibited high coefficient of friction and DLC films on ball were worn out quickly. Plastic deformation was not observed on soft steel because the contact area increased and the thick hardened layer on contact surface were formed by DLC films and debris particles together on the steel substrate. The wear track on steel became deep and wide with increase of loads and DLC films were worn out. The experimental results showed that super low friction and high wear resistance of DLC films on soft steel can be attributed to the good adhesion and plastic deformation. Plastic deformation played an active role in the tribological properties of DLC films on soft steel in the present work.