磁控溅射WSx/W/DLC/W多层膜的微观结构及摩擦学性能

采用磁控溅射技术在硅基底上交替沉积WS_x、W以及DLC膜层制备WS_x/W/DLC/W多层膜。利用X射线衍射仪、扫描电镜、纳米压痕仪等对多层膜的微观结构和力学性能进行了表征,使用球盘式摩擦磨损试验机测试了多层膜在大气中的摩擦学性能。结果表明:多层膜表面均光滑致密。随着周期中W单层厚度的增加,多层膜中出现α-W、W_2C和β-WC_(1-x)结晶相,多层膜的硬度大幅提高(6 nm时具有极大值17.3 GPa),摩擦因数呈下降趋势,结合力逐渐降低,磨损率先降低后升高。W单层厚度为6 nm的多层膜的耐磨性能最佳,磨损率约为1.4×10~(-14)m~3·N~(-1)·m~(-1)。     

调制比对磁控溅射法生长DLC/WS_x多层膜微结构和力学性能的影响

采用磁控溅射法在200℃Si(100)基体上交替沉积WS_x和类金刚石碳膜(DLC)制备不同调制比的DLC/WS_x多层膜(周期为10 nm)。利用扫描电镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)、X射线光电子谱(XPS)等手段分析调制比对多层膜成分、微观结构及界面的影响。利用薄膜应力测试仪、纳米压痕仪、涂层附着力划痕仪和球盘式摩擦磨损试验机等测试多层膜的力学性能及大气中的摩擦磨损性能。结果表明:DLC/WS_x多层膜结构致密而平整,界面强化效应明显,膜中WS_x均为非晶结构。随着调制比增大,多层膜的n(S)/n(W)由0.77增大至1.08,硬度先降低后升高,膜内压应力逐渐减小,结合力先增大后减小,摩擦因数由0.307降至0.171,磨损率逐渐上升。调制比为1:39的多层膜性能最优,硬度可达11.4 GPa,磨损率低至1.17×10~(-15) m~3·N~(-1)·m~(-1),显著优于纯WS_x薄膜的。     

GLC/成分梯度CNx多层膜的微观结构和摩擦学性能

类金刚石碳膜通常内应力大、结合力低,而多层膜结构可提高结合力。 采用磁控溅射技术在 Si 基体上沉积不同 CNx 层厚度的 GLC/ 成分梯度 CNx 纳米多层膜。 通过扫描电子显微镜(SEM)、X 射线衍射仪(XRD)、X 射线光电子能谱(XPS)、Raman 光谱仪、球盘式摩擦仪、纳米压痕仪等对多层膜的表面形貌、微观结构、力学以及摩擦性能进行分析。 结果表明:多层膜表面平整光滑,CNx 层厚度为 50 nm 的多层膜有明显的层状结构。 多层膜中存在石墨相而 CNx 以微晶或非晶存在。 薄膜的 sp3 键含量、结合力、硬度等均随 CNx 层厚度的增加先增加后减小。 CNx 层厚度对多层膜的大气环境摩擦因数影响很小,但显著降低其真空环境摩擦因数。 多层膜的硬度为( 15 ~ 17. 6) GPa,大气中的磨损率为 (1. 03~ 2. 33)×10^-16 m³N^-1m^-1 ,真空中为(2. 06~ 3. 34)×10^-16 m³N^-1m^-1 。 CNx 层厚度为 20 nm 的多层膜综合性能最佳。     

Cr基过渡层对钛合金表面类金刚石薄膜摩擦学性能的影响

采用磁控溅射技术在钛合金(Ti6Al4V)表面制备Cr、Cr/Cr N和Cr/Cr N/Cr NC过渡层结构的类金刚石(DLC)薄膜。采用扫描电子显微镜、拉曼光谱仪与原子力显微镜分析薄膜的结构和表面形貌,利用纳米压痕仪、薄膜内应力测试仪、划痕测试仪、摩擦试验机和二维轮廓仪研究薄膜的硬度、内应力、结合力和摩擦磨损性能。结果表明:随着Cr基梯度过渡层的引入,DLC薄膜的内应力逐渐下降,结合力逐渐上升。Cr/Cr N/Cr NC/DLC薄膜具有优异减摩抗磨性能,摩擦因数和磨损率低至0.09±0.02和(1.89±0.15)×10-7 mm3/N·m。试验结果对钛合金表面高性能DLC薄膜制备及应用具有一定的参考价值和指导意义。     

类金刚石/碳化钨多层膜的制备及其结构

采用阳极型气体离子源结合非平衡磁控溅射的方法,在单晶硅及Ti6Al4V钛合金基体上制备掺钨类金刚石多层膜(DLC/WC),利用俄歇电子谱(AES)、透射电镜(TEM)、X射线光电子能谱(XPS)及X射线衍射(XRD)等对膜层的过渡层、界面及微观结构进行研究。结果表明:所制备的膜层厚2.7μm,硬度高达3 550HV,摩擦因数为0.139,与Ti6Al4V基体结合力为52 N;W主要以纳米晶WC的形式与非晶DLC形成WC/DLC多层膜,该多层膜仍呈现出类金刚石膜的主要特征。     

不同调制周期WS_x/a-C多层膜的组织结构及摩擦学特性

采用磁控溅射法交替溅射WS2和石墨靶制备周期为4~23 nm的WSx/a-C纳米多层膜。采用扫描电镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)和X射线光电子谱(XPS)等分析薄膜的组织结构和元素的化学价态;采用纳米压痕仪、涂层附着力划痕仪和球盘式摩擦磨损试验机测试薄膜的硬度、结合力和在潮湿大气下(相对湿度70%)的摩擦磨损特性。结果表明:多层膜结构致密,表面平整。a-C的加入改变WS2的结晶状态,多层膜为微晶或非晶结构;随着调制周期的增大,多层膜的硫与钨摩尔比逐渐降低并趋于稳定(约为1.32),其硬度稍有上升,而结合力明显降低,摩擦因数由0.32降至0.26,而磨损率逐渐上升但显著低于纯WSx膜的。调制周期为4 nm的多层膜的耐磨性能最佳,磨损率约为1.03×10-13 m3·N-1·m-1。     

磁控溅射沉积Al/AlN纳米多层膜的摩擦学性能

纳米多层膜因具有优异的力学性能与抗摩擦磨损性能使其在摩擦学领域具有重要的应用价值。采用磁控溅射沉积法制备了Al、AlN单层薄膜与Al/AlN纳米多层膜,探讨了纳米多层化对薄膜的力学性能和摩擦学性能的影响。采用纳米压痕仪和摩擦磨损试验机测量评价薄膜的纳米硬度和摩擦学性能。结果表明:Al/AlN纳米多层膜具有良好的周期调制结构,多层膜中的大量界面能显著提高薄膜的力学性能与摩擦学性能。多层膜的硬度为8.8GPa,高于采用混合法则计算出的硬度值6.6GPa;多层膜具有软质Al层和硬质AlN层的交替结构,在摩擦过程中,硬质AlN层可以起到良好的承载作用,软质层可以起到良好的减摩作用。相对于Al单层薄膜或AlN单层薄膜,Al/AlN纳米多层膜具有较低的摩擦因数(0.15)和优异的抗磨损性能。     

多弧离子镀制备的大厚度Cr/Cr_2N/CrN多层涂层的结构和力学性能（英文）

采用多弧离子镀制备一种厚度为24.4μm的Cr/Cr2N/CrN多层结构涂层。采用场发射扫描电子显微镜(FESEM)、X射线光电子能谱(XPS)、能量散射谱(EDS)、X射线衍射(XRD)和透射电镜(TEM)对涂层进行表征,并用纳米压痕和划痕仪测试其硬度和结合力。用UMT-3MT往复式摩擦磨损试验机对涂层在大气和海水环境中的摩擦性能进行测试。结果表明,该涂层由3种相结构组成,分别是Cr相、Cr2N相和CrN相。相对于单层CrN涂层,多层涂层的结合力明显提高,该涂层的硬度为(21±2)GPa。多层结构涂层在人工海水中的耐蚀性能显著优于单层CrN涂层的耐蚀性能,且在大气和海水中多层结构涂层的摩擦因数均低于单层CrN涂层的摩擦因数。     

Ti/Al过渡层对共掺杂类金刚石薄膜性能的影响

目的研究Ti/Al过渡层对不同溅射电流下的Ti/Al共掺杂DLC薄膜的成分、结构、机械性能和结合力的影响。方法采用线性离子束复合磁控溅射技术在316L基底上沉积含有Ti/Al过渡层的Ti/Al共掺杂DLC薄膜,利用场发射扫描电子显微镜(SEM)、X射线光电子能谱仪(XPS)、高分辨透射电镜(HRTEM)及共聚焦激光拉曼光谱仪分析了薄膜的界面形貌及键态结构。采用辉光放电光谱仪对样品成分进行深度分析,纳米压痕仪测量薄膜硬度及弹性模量,划痕测试系统测量膜基结合力,残余应力仪测量薄膜内应力。结果与未添加过渡层相比,添加Ti/Al过渡层对薄膜的结构和机械性能影响较小,且均在溅射电流为2.5 A时有最优的机械性能;然而,溅射电流为2.5 A时,添加过渡层使结合力从54.5 N提高到了67.2 N,提高了19%,残余应力从1.28 GPa降低到了0.25 GPa,降低了80%。结论 Ti/Al过渡层可缓解因DLC薄膜和基体的晶格匹配差异和膨胀系数不同而导致的高界面应力。在薄膜与基底界面,过渡层呈现典型柱状晶结构,可促进膜基界面间的机械互锁,显著改善薄膜与基体之间的结合力而不损伤其机械性能。     

AISI 316L表面氮化复合类金刚石涂层的相结构及摩擦学性能

为提高类金刚石涂层与奥氏体不锈钢之间的结合强度,利用等离子体增强化学气相沉积技术分别在未处理和氮化处理的AISI 316L表面沉积类金刚石（DLC）涂层,研究不同沉积温度下DLC及氮化复合DLC涂层的相结构与摩擦学性能。采用X射线衍射仪（XRD）、拉曼光谱仪（Raman）表征涂层的相结构;采用扫描电子显微镜（SEM）观察截面形貌,并用EDS测量氮、碳元素的深度分布;采用纳米压痕仪、摩擦磨损试验机、超景深显微镜、划痕仪检测DLC涂层的摩擦学性能。结果表明：氮化复合DLC涂层的结合力和耐磨性优于DLC涂层;其中100 ℃时,硬度和结合力分别提高25%和175%,综合性能最好。沉积DLC涂层的过程中,氮化层中氮原子因扩散而重新分布,使氮化层的厚度增加,硬度梯度减缓,更有利于基体与DLC涂层间的过渡。     

Influence of deposition conditions on mechanical and tribological properties of nanostructured TiN/CNx multilayer films

Nanostructured TiN/CN_x multilayer films were deposited onto Si (100) wafers and M42 high-speed-steel substrates using closed-filed unbalanced magnetron sputtering in which the deposition process was controlled by a closed loop optical emission monitor (OEM) to regulate the flow of N₂ gas. Multilayers with different carbon nitride (CN_x) layer thickness could be attained by varying the C target current (0.5 A to 2.0 A) during the deposition. It was found that the different bilayer thickness periods (i.e. the TiN layer thickness Λ_TiN was fixed at 3.0 nm while the CN_x layer thickness Λ_CNx was varied from 0.3 to 1.2 nm) significantly affected the mechanical and tribological properties of TiN/CN_x multilayer films. These multilayer films were characterized and analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), atomic force microscopy (AFM), Rockwell-C adhesion test, scratch test, pin-on-disc tribometer, and nanoindentation measurements. XPS analyses revealed that the chemical states, such as TiN, TiC, TiN_xO_y and TiO_2, existed in a TiN layer. Nanoindentation results showed that the hardness was highly dependent on the bilayer thickness. A maximum hardness of ~ 41.0 GPa was observed in a multilayer film at bilayer thickness Λ_TiN = 3.0 nm and Λ_CNx = 0.9 nm. All multilayer films exhibited extreme elasticity with elastic recoveries as high as 80% at 5 mN maximum load. The compressive stresses in the films (in a range of 1.5-3.0 GPa) were strongly related to their microstructure, which depended mainly on the incorporation of nitrogen in the films. By scratch and Rockwell-C adhesion tests, the multilayer films with smaller bilayer thicknesses (Λ_TiN = 3.0 nm, Λ_CNx = 0.3 and 0.6 nm) exhibited the best adhesion and cohesive strength. The critical load value obtained was as high as ~ 78 N for the films with Λ_TiN = 3.0 nm, Λ_CNx = 0.9 nm. The friction coefficient value for a multilayer at Λ_TiN = 3.0 nm and Λ_CNx = 0.9 nm was found to be low 0.11. These adhesive properties and wear performance are also discussed on the basis of microstructure, mechanical properties and tribochemical wear mechanisms.     

Fabrication, microstructure and tribological behavior of pulsed laser deposited a-CNx/TiN multilayer films

a-CN_x/TiN multilayer films were deposited onto high-speed steel substrates by pulsed laser ablation of graphite and Ti target alternately in nitrogen gas. The composition, morphology and microstructure of the films were characterized by energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Raman spectroscopy. The tribological properties of the films in humid air were investigated using a ball-on-disk tribometer. The multilayer films consist of crystalline TiN, metallic Ti and amorphous CN_x (a-CN_x). With an increase in thickness ratio of CN_x to bilayer, the hardness of multilayer film decreases, friction coefficient decreases from 0.26 to 0.135, and wear rate increases. The film with thickness ratio of CN_x to bilayer of 0.47 exhibits a maximum hardness of 30 GPa and excellent wear rate of 2.5 × 10^− 7 mm³ N^− 1 m^− 1. The formation of tribo-layer was observed at contact area of Si₃N₄ ball. The film undergoes the combined wear mechanism of abrasion wear and adhesion wear.     

Ni-P/Ti/DLC多层膜的摩擦磨损性能

目的研究摩擦速度、载荷及加热温度对Ni-P/Ti/DLC多层膜摩擦磨损性能的影响。方法用化学镀镍磷工艺在模具钢基体表面镀上Ni-P层作切削层,采用过滤阴极真空电弧(FCVA)技术分别沉积Ti过渡层和DLC保护层。通过摩擦磨损实验,评价该多层膜的摩擦磨损性能。利用纳米压痕测试和拉曼光谱检测,研究该多层膜在不同加热温度下的硬度、弹性模量和结构成分。利用扫描电镜及表面轮廓仪分别对该多层膜的磨痕形貌和横截面轮廓进行分析。结果随着摩擦速度的增大,Ni-P/Ti/DLC多层膜的摩擦系数呈下降趋势,磨损率和磨损体积呈先减后增的趋势。不同载荷下的摩擦系数变化幅度较小,磨损率和磨损体积随着载荷的增大呈增加的趋势。随着加热温度的升高,摩擦系数呈下降趋势,磨损率和磨损体积呈先增后减的趋势。此外,随着加热温度的升高,多层膜表层DLC膜中石墨相逐渐增多,硬度和弹性模量随之呈先增后减的趋势。结论较高摩擦速度下,多层膜表层DLC膜石墨化趋势增强,摩擦系数变化幅度较大,且表面磨痕宽度和深度显著增加,磨损加剧。多层膜中软质的Ti金属层和硬质的DLC层,能有效提高多层膜在高载荷下的摩擦磨损性能。随着加热温度的升高,多层膜表层DLC膜中石墨相逐渐增多,摩擦过程更易生成转移膜。     

TiBCN:CNx multilayer coatings deposited by pulsed closed field unbalanced magnetron sputtering

In this study, a combination of nanocomposite and multilayer coating design was investigated in an effort to reduce the coefficient of friction (COF) while maintaining good mechanical properties of the TiBCN coatings. The TiBCN:CN_x coatings consist of TiBCN and CN_x nanolayers which were deposited alternately by reactive sputtering a TiBC composite target (80 mol% TiB₂ + 20 mol% TiC) and a graphite target in an Ar:N₂ mixture using a pulsed closed field unbalanced magnetron sputtering system. Low angle X-ray diffraction and transmission electron microscopy characterizations confirmed that the coatings consist of different bilayer periods in a range of 3.5 to 7.0 nm. The TiBCN layers exhibited a nanocomposite structure, whereas the CN_x layers were in an amorphous state. The mechanical properties and wear resistance of the TiBCN:CN_x multilayer coatings were investigated using nanoindentation and ball-on-disk wear test. The TiBCN:CN_x coatings exhibited high hardness in a range of 20-30 GPa. The highest hardness of 30 GPa was achieved in the coating with a bilayer period of 4.5 nm. A low COF of 0.17 sliding against a WC-Co ball was obtained at a bilayer period of 4.5 nm, which is much lower than those of the single layer TiBCN and TiBC nanocomposite coatings (0.55-0.7).     

NbMoWTa/Ag自润滑纳米多层膜的力学性能及摩擦学行为∗

为提高高熵合金薄膜 NbMoWTa 的耐磨减摩性能,采用磁控溅射技术在 Si 基体上制备具有不同调制波长的 NbMoWTa / Ag 纳米多层膜,利用 XRD、SEM 和 TEM 等对纳米多层膜进行表征,分析其硬度和摩擦学性能。 结果表明不同调制周期结构的纳米多层膜结晶性良好。 多层膜硬度随着单层膜厚度 (100~ 5 nm)的降低而增加(5. 62 ~ 8. 39 GPa),在单层膜厚度减小到 20 nm 时,其塑性变形机制由位错在界面处的堆积机制转变为位错穿越界面运动机制;在尺寸小于 10 nm 时,多层膜的硬度接近于高熵合金 NbMoWTa 单质膜 (10. 93 GPa),这可能由随着单层厚度的降低引起 NbMoWTa 膜与 Ag 膜之间界面由半共格向共格转变所引起。 同时,通过摩擦磨损试验获得纯 NbMoWTa 薄膜的摩擦因数为 0. 49,磨损率为 1. 75×10^-5 mm³N^-1m^-1 ;单层膜厚度为 5 nm 的多层膜的摩擦因数为 0. 23,磨损率为 2. 19×10^-5 mm³N^-1m^-1 。 在 NbMoWTa 中添加 50%的 Ag 制备而成的纳米多层膜有共格强化效应,保证了其高硬度高强度的同时,由多层设计实现了耐磨和自润滑的协同控制。     

不同过渡层对DLC薄膜力学性能和摩擦学性能的影响

薄膜与基体间的界面结合性能是决定薄膜性能发挥的关键要素。针对类金刚石薄膜(DLC)在硬质合金上结合力差的问题,采用线性阳极离子束复合磁控溅射技术在硬质合金YG8基体上设计制备了单层W过渡层、WC过渡层、双层W过渡层和三层W过渡层4种不同W过渡层的DLC薄膜,探讨了不同过渡层对DLC薄膜力学和摩擦学性能的影响。结果表明:不同过渡层结构的DLC薄膜结构致密,界面柱状生长随着层数增加及过渡层厚度的降低而打断,有利于改善薄膜的韧性。当为三层W过渡层时,DLC薄膜的断裂韧性达到最大值6.44 MPa·m1/2;与单层W过渡层相比,薄膜硬度有小幅下降,但薄膜内应力降低了55%,且膜/基匹配性更佳,结合强度高达85N,此时薄膜具有较低的摩擦因数和磨损率,表现出比较优异的抗磨减摩性能。     

DLC基纳米多层膜摩擦学性能的研究进展与展望

类金刚石（DLC）薄膜是一种良好的固体润滑剂,能够有效延长机械零件、工具的使用寿命。DLC基纳米多层薄膜的设计是耐磨薄膜领域的一项研究热点,薄膜中不同组分层具备不同的物理化学性能组合,能从多个角度（如高温、硬度、润滑）进行设计来提升薄膜力学性能、摩擦学性能以及耐腐蚀性能等。综述了DLC多层薄膜的设计目的与研究进展,以金属/DLC基纳米多层膜、金属氮化物/DLC基纳米多层膜、金属硫化物/DLC基纳米多层膜以及其他DLC基纳米多层膜为主,对早期研究成果及现在的研究方向进行了概述。介绍了以上几种DLC基纳米多层膜的现有设计思路（形成纳米晶/非晶复合结构、软/硬交替沉积,诱导转移膜形成,实现非公度接触）。随后对摩擦机理进行了分析总结：1）层与层间形成特殊过渡层,提高了结合力;2）软/硬的多层交替设计,可以抵抗应力松弛和裂纹偏转;3）高接触应力和催化作用下诱导DLC中的sp3向sp2转化,形成高度有序的转移膜,从而实现非公度接触。最后对DLC基纳米多层膜的未来发展进行了展望。     

Indentation and scratch tests on sputtered amorphous CN X films deposited on plasma-nitrided Ti-6Al-4V

Sputtered carbon nitride (CN _X ) films were deposited on both untreated and plasma-nitrided Ti-6Al-4V substrates. Surface and cross-section morphology of the deposited CN _X films was studied by scanning electron microscopy (SEM). Modified Vickers hardness tests showed that the intrinsic hardness of the CN _X film was about HV 2000 to 3000. Both the indentation and scratch tests showed that, compared with the CN _X film deposited on Ti-6Al-4V substrate, the load-bearing capacity of CN _X film deposited on a plasma-nitrided layer was improved dramatically. From the results of scratch tests, the duplex-treated system was effective in maintaining a favorable low and stable coefficient of friction and improving the wear resistance of Ti-6Al-4V substrate.     

Structure and mechanical properties of δ-NbN/SiNx and δ′-NbN/SiNx nano-multilayer films deposited by reactive magnetron sputtering

We deposit cubic δ-NbN/SiN_x and hexagonal δ′-NbN/SiN_x nano-multilayer films using reactive magnetron sputtering in discharge of a mixture of Ar and N₂ gas, and explore the effects of SiN_x layer thickness on the microstructure and mechanical properties for both cubic δ-NbN/SiN_x and hexagonal δ′-NbN/SiN_x multilayer films by virtue of X-ray diffraction, electron diffraction, high-resolution transmission electron microscope, and nanoindentation measurements. We find that the structure for NbN layers is a critical factor in determining the hardness of NbN/SiN_x multilayer films. For cubic δ-NbN/SiN_x nano-multilayer films, as SiN_x layer thickness is smaller than or equal to 0.4 nm, the cubic δ-NbN layers force SiN_x layers to crystallize, accompanied with a remarkable increase in hardness with maximum hardness of 32 GPa. With an increase in thickness, SiN_x layers become amorphous, and correspondingly the hardness decreases. For hexagonal δ′-NbN/SiN_x nano-multilayer films, both the stress and hardness decrease with increasing the SiN_x layer thickness and the nano-multilayer films do not show any enhancement in hardness, compared to δ′-NbN single layer film.