高熵合金AlCrNbSiTiV氮化物薄膜溅镀参数的优化

以AlCrNbSiTiV为靶材,用反应式磁控溅镀系统分别在住友BNX20刀具和硅晶片上沉积高熵合金氮化物(AlCrNbSiTiV)N薄膜。采用田口方法的L9(34)正交表考察了沉积时间、基材偏压、溅射功率和基材温度对沉积速率、薄膜硬度和刀具寿命的影响,通过方差分析(ANOVA)确定了影响各性能的主要因素。对信噪比(S/N)进行灰关联分析以实现多目标优化,得出最佳工艺参数为:沉积时间20min,基材偏压-100V,溅射功率250W,基材温度400°C。在该条件下,沉积速率为17.28nm/min,薄膜硬度达到2814HV,刀具寿命2.50m。     

基板偏压对溅镀AlCrNbSiTiV高熵合金氮化物薄膜性能的影响

用真空电弧熔炼法制备了AlCrNbSiTiV高熵合金,并将其作为靶材,利用直流反应式磁控溅镀法在T1200A金属陶瓷刀具或硅晶片上沉积了高熵合金氮化物薄膜。通过扫描电镜、能谱仪、X射线衍射仪和纳米压痕仪考察了基板偏压对薄膜形貌、元素含量、物相成分和性能的影响。所得氮化物薄膜均匀、致密,所有元素的原子分数与靶材相当。由于再溅射,沉积速率随着基板偏压增大而减小。薄膜的弹性恢复和显微硬度在基板偏压为0~-100 V时随着偏压增大而提高,进一步增大偏压反而减小。相比未溅镀薄膜的刀具,用溅镀了AlCrNbSiTiV氮化物薄膜的刀具干切削S45C中碳钢圆柱工件,工件表面的粗糙度和刀具的侧面磨损显著降低。-100 V偏压溅镀的刀具的切削性能最佳。     

磁控溅射硅氮类保护膜摩擦性能的分析与表征

采用四靶直流非平衡磁控溅射技术在Co–28Cr–6Mo合金表面沉积了硅氮(SiN)薄膜。借助接触角仪、纳米压痕仪以及摩擦磨损试验机考察了基体偏压对硅氮薄膜表面自由能的影响,并评价了它们的机械性能和摩擦学行为。硅氮薄膜是一类具有两性分子特性的功能材料,表现出良好的湿环境摩擦学性能,是极具潜力的水介质润滑生物机械薄膜。随着基体负偏压增加,薄膜在胎牛血清稀释液中的摩擦因数急剧下降。     

磁控溅射ZrSiN薄膜的微观结构表征及其力学与摩擦学性能研究

通过改变硅靶功率,采用非平衡磁控溅射法制备了不同Si含量的ZrSiN薄膜。采用X射线衍射仪、扫描电镜、能谱仪、热重分析仪、纳米压痕仪、摩擦磨损试验机和三维形貌仪研究了薄膜的微观结构、成分、表面形貌、抗氧化性、力学性能,以及室温和高温下的摩擦磨损行为。ZrSiN薄膜为面心立方结构。随着Si含量的增加,薄膜的显微硬度先减小后增大。适量Si元素的加入可以在一定程度上改善ZrN薄膜与304不锈钢基体的结合力,以及提高其抗氧化性。室温(25°C)下,随着Si含量增加,薄膜的摩擦因数稳定在0.8左右,磨损率逐渐降低。当薄膜中Si的原子分数为7.04%时,随着温度从室温上升到200°C,薄膜的摩擦因数大幅下降,然后随着温度继续升高至800°C,薄膜的摩擦因数趋于稳定。在650°C时,Si元素的加入降低了薄膜的摩擦因数和磨损率。与室温时相比,650°C时薄膜的摩擦因数更小,磨损率更大。     

氮氩流量比与基底温度对射频溅射TiN薄膜性能的影响

采用射频磁控溅射技术,以纯钛为靶材,氮气为反应气体,通过改变氮氩流量比与基底温度在304不锈钢及玻璃表面制备了不同的TiN薄膜.利用能谱仪、扫描电镜、台阶仪、四探针仪、划痕仪和纳米压痕仪对制备的所制薄膜的氮钛原子比、表面形貌、沉积速率、方块电阻、膜基结合力和纳米硬度进行表征.结果表明:随着氮氩流量比的增大,TiN的形貌先由四面锥体凸起结构逐渐过渡至柱状晶体堆积结构,然后转变为稀疏的液滴状颗粒结构,直至平整光滑,致密均匀.在氮气和氩气的流量分别为5.0 mL/min和50.0 mL/min的条件下,基底温度25～400°C范围内制备的TiN薄膜的结合力介于135.4 mN与210.2 mN之间.当基底温度为300℃时,薄膜的沉积速率最大,颜色最接近金黄色,氮钛原子比最接近1,结合力和纳米硬度也都最大.     

氧化锌铝镓透明导电薄膜制备工艺的优化

将氧化锌掺杂铝和镓制成的靶材通过射频磁控溅镀的方式沉积在玻璃基板上.用四点探针法测量了薄膜的电阻率,用紫外可见光谱仪测量其透光率.采用田口法和灰关联分析法得到制备电阻率较低且透光率较高的薄膜的最佳工艺参数为:射频功率90 W,基板温度200°C,沉积时间45 min,制程压力1.333 Pa.溅镀后在溅镀腔体里以石英灯管加热至400°C退火,最终薄膜的电阻率可达4.65×10?3Ω·cm,在可见光区内的透光率为90％.     

硬质合金刀具类金刚石涂层的摩擦磨损性能

以等离子体化学气相沉积技术在硬质合金刀具表面制备了类金刚石(DLC)涂层.研究了DLC涂层刀具和无涂层刀具的硬度,不同载荷、不同转速下两种刀具的摩擦磨损性能,以及在水润滑和油润滑条件下DLC涂层刀具的滑动摩擦行为.结果表明,DLC涂层刀具的平均硬度为2 099.9 HV,比无涂层刀具提高了48.3%;DLC涂层刀具的摩擦因数明显低于无涂层刀具,其磨损率随着载荷的增加而增大,随转速的增大而减小;油润滑比水润滑能更有效减缓摩擦作用.     

载重汽车销轴表面改性及其摩擦磨损性能的研究

在载重汽车销轴基材40Cr钢表面制备Ni-WC纳米复合镀层,实现表面改性,以期提高销轴表面的摩擦磨损性能。观察并分析了纳米复合镀层的表面形貌和微观结构,检测了纳米复合镀层的结合强度、硬度及摩擦磨损性能。结果表明:纳米复合镀层表面较平整、结构致密,与基材结合牢固,其硬度平均值为6 081MPa,约为基材的1.3倍;其平均摩擦因数约为0.35,磨损失重约为1.83mg,均比基材的低。低孔隙率、致密结构和高硬度,使纳米复合镀层具有良好的摩擦磨损性能。     

首饰基材表面反应磁控溅射SiO2薄膜工艺

采用反应磁控溅射工艺在S950首饰基材表面沉积防指纹用的SiO2薄膜,研究了氧气流量、氧气体积分数、溅射电流和沉积时间对沉积速率和薄膜化学组成的影响.结果表明,膜层沉积速率随着溅射电流增大而快速增加,随着氧气流量增加而先升后降,随着氧气体积占比增加而先略升后稳定,随着镀膜时间的延长而略降.膜层的氧硅原子比随着氧气流量增加而快速增加,随着氧气体积分数增加而略有增加,随着溅射电流以及沉积时间的增加而降低.     

蓝宝石衬底表面SiO2薄膜的应力分析

采用射频磁控反应溅射法分别在Si和蓝宝石衬底上沉积SiO2薄膜.通过改变沉积薄膜的工艺参数,考察反应气体流量比、沉积温度、射频功率等因素对SiO2薄膜内应力的影响.采用压痕裂纹法分析了镀膜前后蓝宝石的表面应力.结果表明:制备SiO2薄膜时,工艺参数影响SiO2薄膜的成分,当O2/Ar流量比值为1.25,衬底温度为300℃,射频功率为100 W时,可以制备出化学计量比的SiO2薄膜,此时薄膜中的内应力较小;制备的SiO2薄膜呈压应力状态,镀SiO2薄膜可以改变蓝宝石的表面应力,蓝宝石的表面应力已由原来的拉应力变为压应力.     

Micromechanical and microtribological properties of BCN thin films near the B4C composition deposited by r.f. magnetron sputtering

Ternary materials with compositions in the B–C–N system offer properties of great interest. In particular, mechanical and tribological properties are expected to be excellent, as they can combine some of the specific properties of BN, B₄C and C₃N₄. In this paper, BCN thin films deposited by r.f. magnetron sputtering are characterized by their micromechanical and microtribological behavior. BCN coatings with different composition were obtained by varying the N₂/Ar proportion in the sputtering gas. Hardness and elastic modulus of the coatings were measured by nanoindentation. The adhesion and friction coefficient against diamond have been evaluated by microscratch and the coatings have been characterized in their wear behavior at the nanometric scale. These mechanical and tribological properties have been related to film composition and structure, which have been studied in a previous work. It is found that the measured wear resistance at the nanometric scale is directly related to the coating microhardness rather than friction behavior or adhesion of the coating to the substrate, which are the determinant factors in the macroscopic scale wear behavior.     

Effect of bias voltage on microstructure and phase evolution of Cr–Mo–N coatings by an arc bonded sputter system

Cr–Mo–N hard coatings were deposited on SKD11 and silicon wafer substrates at various substrate bias voltages by hybrid PVD consisting of arc ion plating and unbalanced magnetron sputtering. The results showed that the microstructure, phase evolution, and mechanical properties of the coatings were significantly altered at the different substrate bias voltage ranging from 0 to −400 V. The X-ray diffraction analysis results revealed that most of the diffraction peaks originated from the Cr–N phase. These peaks were observed at lower positions with no substrate bias and were shifted to higher positions with increasing substrate bias power. The preferred orientation of the (200) plane became dominant accompanying the (220) plane as the bias voltage was increased. Maximum hardness of approximately 30 GPa was obtained at a bias voltage of −200 V. Additionally, wear test results reveal that the lowest coefficient of friction, between 0.4 and 0.5, was obtained from the Cr–Mo–N film formed at a bias voltage of −200 V.     

Optimization of wear–corrosion properties of a–C:N films using filtered cathodic arc deposition

Applying a 4-factor (negative substrate bias voltage, arc current, Ar flow and N₂/Ar ratio) 3-level (L9) orthogonal array design using the Taguchi method to optimize the wear–corrosion properties of a–C:N in Filtered Cathodic Vacuum Arc (FCVA) deposition was investigated. The influence of N₂/Ar ratio, over the range of 1/6 to 2/3, is shown by the increase in the following: the wear–corrosion current density changes from 36 to 78 nA/cm², and the friction coefficient changes from 0.042 to 0.086. A higher N₂/Ar ratio induces the a–C:N film's structure to reduce the sp³ content (sp² rich) which implies the formation of loose networks due to N₂ incorporation. Based on the analysis, the N₂/Ar ratio is the most significant control factor as its percentage contribution is 69% for wear–corrosion current density and 32% for frictional coefficient, respectively. There is a tendency for a higher friction coefficient by increasing the following three factors; level of negative substrate bias voltage, Ar flow and N₂/Ar ratio. We observed an increase of N content and sp² bonding which correlated to the decrease of hardness and an also rougher a–C:N surface with increasing the factors level. Over the design range of 4 factors, the optimum wear–corrosion properties and friction coefficient obtained from the Taguchi analysis were obtained using a 20 V negative substrate bias, 30 A arc current, 30 sccm Ar flow and 1/6 N₂/Ar ratio respectively. Overall, the results show an optimum design when compared with the current design as it was able to reduce 84% of the wear–corrosion current density (35.7 down to 5.6 nA/cm²) and 58% of the frictional coefficient (0.060 down to 0.025), respectively.     

The effect of a buffer layer on the structure and the performance of cutting-tools for ZrWN films that are deposited using DCMS and HIPIMS

This paper determines the optimal settings for the deposition of ZrWN nitride films using reactive direct current magnetron sputtering (DCMS) and high-power impulse magnetron sputtering (HIPIMS), with pure Zr and W metal targets and Ar plasma and N₂ reactive gases. The materials tested as buffer layers are metal tungsten (W) and tungsten nitride (WN) thin films. Using a Taguchi method, this study determines the effect of deposition parameters for the buffer layer (W DC power, substrate bias, N₂/(N₂+Ar) flow rate and substrate temperature) on the structural and mechanical properties, and the dry machining performance of cutting-tools for multilayer ZrWN/W and ZrWN/WN/substrates. In the confirmation runs using grey Taguchi analysis, there is an improvement of 32.31% and 13.38% in surface roughness and flank wear, respectively. The films are characterized using X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (FEI-TEM) and a nanoindenter. The TEM pattern for the ZrWN films shown corresponds to the (111), (200) and (220) planes of the face-center-cubic phase. Pretreatment of a tungsten carbide tool uses oxygen plasma etching to enhance the adhesion of the multilayer ZrWN/WN coating. Compared with coatings that are deposited using DCMS, the samples that are deposited using HIPIMS exhibit a higher film density and a smoother surface. In the HIPIMS mode, the XRD diffraction peaks of the films are sharper and more intense, which indicates an improvement in crystallinity.     

A study of hard diamond-like carbon films in mid-frequency dual-magnetron sputtering

A series of hydrogen-free diamond-like carbon (DLC) films were deposited by a mid-frequency dual-magnetron sputtering under basic conditions of Cr and C target power density between 6 and 18 W/cm², bias voltage in a range of − 100 V to − 200 V, and a pure argon atmosphere. Microstructure, microhardness, adhesion, friction and wear properties were investigated for the DLC films to be used as protective films on cutting tools and forming dies, etc. The DLC films exhibited some combined superior properties: high hardness of 30–46 GPa, good adhesion of critical load of 50–65 N, and friction coefficient about 0.1 in air condition. Properties of the magnetron-sputtered carbon films showed a strong dependence on flux and energy of ion bombardment during growth of the films.     

TiCN涂层的制备及其微观结构和性能

采用直流磁控溅射法在AZ31镁合金上制备了TiCN涂层.采用X射线荧光光谱仪、扫描电镜和X射线衍射仪表征了涂层的化学成分、表面形貌和物相,并采用电化学阻抗谱、浸泡试验、显微硬度测试和磨损试验考察了基体偏压(-40、-60和-80 V)对涂层性能的影响.结果表明,涂层由TiCN和TiN组成.随着负偏压增大,涂层中Ti、C...     

磁控溅射Ta-C-N薄膜摩擦学性能研究

采用磁控溅射法在Si基片上沉积非晶态Ta-C-N薄膜。利用纳米压痕仪表征其纳米硬度和弹性模量;摩擦磨损实验检测其摩擦学性能;光学轮廓仪和扫描电镜观察磨痕形貌。结果表明:Ta-C-N薄膜具有较高的纳米硬度9.45 GPa和弹性模量225.71 GPa,同时具有较低的摩擦系数0.238,磨损率5.94×10-6 mm3.N-1.m-1,磨面较为平整光滑,体现了优越的摩擦磨损性能。     

Microstructure and properties of the AlCrMoZrTi/(AlCrMoZrTi)N multilayer high-entropy nitride ceramics films deposited by reactive RF sputtering

The AlCrMoZrTi/(AlCrMoZrTi)N multilayer high-entropy nitride ceramic films (HENCFs) fabricated by reactive RF magnetron sputtering presented (200) preferentially oriented FCC crystal structures. With the increase in the modulation period, the nitrogen content and surface roughness of the multilayer films gradually increased, the template effect between the nanocrystalline and amorphous forms was weakened, and the multilayer interface structure decreased. The S4 film with a modulation period of 1500 nm had the highest hardness and modulus (16.6 and 225.7 GPa, respectively) and the highest H/E* and H³/E*² values. The results of friction experiments showed that the S1 film with the smallest modulation period had a stable friction coefficient and small wear rate on both Si and Cu substrates, and it exhibited the best friction and wear performance due to its low surface roughness, high toughness and compressive yield resistance, and dense multilayer structure. The friction mechanisms of the HECNFs on Si and Cu substrates were mainly adhesive wear, abrasive wear, and a small amount of oxidative wear.     

CIGS absorbing layers prepared by RF magnetron sputtering from a single quaternary target

Cu(In_1−xGa_x)Se₂ (CIGS) thin films were prepared by RF magnetron sputtering from a single quaternary target at multiple processing parameters. The structural, compositional, and electrical properties of the as-deposited films were systematically investigated by XRD, Raman, SEM, and Hall effects analysis. The results demonstrate that by adjusting the processing parameters, the CIGS thin films with a preferential orientation along the (112) direction which exhibited single chalcopyrite phase were obtained. The films deposited at relatively higher substrate temperature, sputtering power, and Ar pressure exhibited favorable stoichiometric ratio (Cu/(In+Ga):0.8–0.9 and Ga/(In+Ga):0.25–0.36) with grain size of about 1–1.5 µm, and desirable electrical properties with p-type carrier concentration of 10¹⁶−10¹⁷ cm⁻³ and carrier mobility of 10–60 cm²/Vs. The CIGS layers are expected to fabricate high efficiency thin film solar cells.     

基于真空镀膜技术的薄膜热传感器实验

采用真空蒸发镀膜技术设计制作了以云母为基片的薄膜热传感器,传感器包括一个用于热流测量的热电堆和一个用于温度测量的热电偶。综合测试发现：云母基片薄膜热传感器性能良好。封装后,薄膜热电偶的静态标定拟合直线相关系数均可以达到0.999。薄膜热流计的静态标定拟合直线的相关系数为0.99439,测头系数为8.78886 W/(m²?μV),灵敏度为0.11378 μV/(W/m²)。薄膜热电偶的动态响应时间是0.446 s且具有良好的复现性。随着加载热流的增大,薄膜热流计的动态响应时间变大,阶跃热流值为600 W/m²时响应时间为0.483 s。