Cr/CrN/CrNC/CrC/Cr-DLC梯度膜层的研究

采用中频磁控溅射结合离子源技术沉积Cr／CrN／CrNC／CrC／Cr-DLC膜层。利用扫描电镜（SEM）、电子能谱（EDS）、Raman光谱和俄歇深层剥层分别对膜层微观形貌、成分组成、键结构及梯度成分深层分布进行分析；采用努氏显微硬度计、摩擦磨损试验机、划痕仪及洛氏硬度计测评膜层机械性能。结果表明：采用中频磁控溅射可沉积出大面积Cr／CrN／CrNC／CrC／Cr-DLC梯度膜层；Cr溅射功率对C键结构影响不大，但表层DLC中Cr的含量和膜层厚度随中频功率增大而增大；随DLC中掺Cr量增多，膜层硬度及摩擦因数略有上升；采用梯度过渡层及掺入金属Cr提高了膜层附着力，但过高的中频功率使沉积离子能量偏高，膜层压应力增加反而降低了膜层附着性能。     

离子源对中频反应磁控溅射AlN薄膜结构和性能的影响

采用离子源辅助中频反应磁控溅射技术在单晶硅及硬质合金基体上沉积AlN薄膜,利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、显微硬度计、薄膜结合强度划痕试验仪等对薄膜结构及性能进行表征,着重研究了离子源对中频反应磁控溅射AlN薄膜结构和性能的影响.结果表明:离子源的辅助沉积有利于AlN相的合成,当离子源功率大于0.7 kW时,AlN沿(100)晶面择优取向明显,当离子源功率为1.3 kW时,所沉积膜层有向非晶化转变的趋势.同时,随着离子源功率的增加,所沉积的AlN薄膜致密度和膜、基结合力均显著提高,而膜层沉积速率和硬度则呈先上升后降低的规律.     

CrTiAlCN多元多层梯度膜的制备及其结构

采用中频反应磁控溅射、离子束辅助方法沉积CrTiAlCN多元硬质薄膜,利用扫描电镜、俄歇电子谱、透射电镜及X射线衍射等技术对膜层的过渡层、界面及微观结构进行研究.结果表明:沉积制备的膜层为多层梯度过渡结构,成分深度分布及相结构分析证实,所制备的多元多层梯度膜与所设计的基体/Cr/CrN/CrTiAlN/ CrTiAlCN结构相吻合;在梯度过渡中,不同层之间界面体现为渐变过渡过程;沉积制备的多元多层梯度膜硬度高达26.31 GPa,膜/基结合力大于80 N,摩擦因数低至0.113,力学性能优良.     

射频辅助磁控溅射制备梯度Cr/CrC膜的性能

目的 改善CrC薄膜的制备工艺,提高薄膜的结合强度。方法 采用射频偏压辅助磁控溅射技术,以Cr和石墨为靶材,C2H2为反应气体,在M42高速钢表面制备梯度Cr/CrC膜。利用扫描电子显微镜（SEM）、能谱仪（EDS）、Raman光谱仪分析薄膜的微观形貌、成分组成、键结构,用纳米压痕仪、洛氏硬度计对薄膜的结合性能进行评价。结果 成功制备了表面致密均匀的梯度Cr/CrC薄膜,薄膜中sp3键含量随石墨靶射频功率的增加而呈现先增大后减小的趋势。薄膜的结合强度随射频功率的增大而先增大后减小,射频功率为250 W时,薄膜中含有最多的sp3键,并且有最高的硬度,硬度值为21 GPa。结论 纯Cr过渡层能有效吸收薄膜中的内应力,改善膜/基结合性能,对Cr/CrC薄膜结合强度有明显增强作用。石墨靶的射频功率大小对梯度Cr/CrC膜的结构和结合强度有显著影响,射频功率为250 W时,制备出的薄膜具有最高的硬度和结合强度。     

925银基底镀覆Ti/DLC薄膜工艺试验

针对925银传统着黑色工艺存在的缺点,采用溅射镀膜与阳极层离子源相结合的镀膜工艺,在925银基底上镀覆Ti/DLC膜,检测了不同工艺参数下膜层的性能。结果表明,通过调整负偏压、工作气体分压及镀膜时间等工艺参数,可以使Ti/DLC膜层获得较纯正、有光泽的暗黑色,并可调节其显微硬度及临界划痕载荷;当负偏压为-120V、Ar气分压为0.40Pa、时间为10min时在925银基底上溅射Ti膜,以及负偏压为-180V,乙炔分压在0.25~0.30Pa、时间为40~45min在Ti膜上沉积DLC膜时,Ti/DLC膜层的外观装饰效果、耐蚀性和力学性能等较好。     

调制周期对Cr/CrN多层膜结构及性能的影响

采用电弧离子镀技术在6Cr13Mo低碳马氏体不锈钢基材表面沉积不同调制周期的Cr/CrN多层膜。利用扫描电镜、显微硬度仪、划痕仪、压痕仪、摩擦磨损试验机、3D轮廓仪研究Cr/CrN多层膜的结构和性能。结果表明:调制周期的变化对Cr/CrN多层膜硬度影响较小;随着调制周期的减小,Cr/CrN多层膜致密性逐渐提高;不同调制周期下,Cr/CrN多层膜与基体结合力均在100 N以上,其中调制周期为321 nm的Cr/CrN多层膜的韧性及与基体结合性能最优;调制周期为569 nm的Cr/CrN多层膜的磨损率最低。     

立方氮化硼薄膜及溅射沉积的研究进展

溅射沉积由于获得的cBN薄膜颗粒尺寸小、立方相含量高,是cBN薄膜制备技术发展的一个重要方向。本文介绍了溅射沉积过程中的基体负偏压、沉积气氛、沉积温度、靶材功率等工艺参数对cBN薄膜中立方相的含量和薄膜性能的影响规律。并从优化沉积工艺参数、采用过渡层及在膜层中引入其它元素方面介绍了在降低膜层应力方面取得的研究进展。分析归纳出溅射沉积cBN薄膜目前存在的主要问题是薄膜应力过大、存在非立方相氮化硼及B、N原子的比例失配。提出了下一步研究工作的重点是通过深入认识溅射沉积cBN薄膜的的形成机理,优化沉积工艺参数及设计合理的过渡层和新型梯度涂层,以提高立方相的含量、保证B、N原子的比例、降低膜层应力。     

基于X射线反射研究溅射工艺对CrAlN/TiAlN周期膜界面结构的影响

为研究X射线反射技术在纳米多层膜界面微结构表征中的应用,采用反应磁控溅射技术在单晶硅基片上制备CrAlN/TiAlN纳米周期膜,利用X射线反射技术系统研究溅射工艺参数对CrAlN/TiAlN纳米周期膜界面微结构的影响规律。结果表明:增加铝靶功率可提高膜层的溅射速率和降低膜层的界面粗糙度,然而较高的铝靶功率会使膜层界面出现严重的弥散;较大和较小的负偏压都不利于形成完整的周期膜调制结构和光滑的界面;提高Ti/Cr靶电流可有效改善周期膜的调制界面结构,但太大的靶电流会导致膜层间扩散加重,形成弥散界面。N2流量与Ar流量对膜层界面粗糙度具有相反的影响作用。试验得到的优化工艺参数为:铝靶功率80W,溅射负偏压-200 V,Ti/Cr靶电流0.2A,N2流量30cm~3/min,Ar流量10cm~3/min。     

铜合金表面过渡层厚度对Cr-DLC薄膜残余应力和结合性能的影响

为提高铜合金表面Cr-DLC薄膜的膜/基结合性能,设计了Cr/CrN/Cr-DLC多层结构薄膜,采用磁控溅射/等离子辅助气相沉积方法在铜合金样品表面制备不同Cr粘结层厚度的Cr掺杂类金刚石（Cr-DLC）薄膜。利用高分辨拉曼光谱仪、薄膜应力仪、纳米压痕仪、划痕仪和连续冲击试验机分别对薄膜的微观结构、残余应力、纳米硬度和弹性模量、薄膜与基体结合性能和耐冲击韧性进行测试。结果表明,随着Cr粘结层厚度的增加,铜合金表面Cr-DLC薄膜的残余应力出现了先升高后降低的趋势,最小残余应力达到-0.47 GPa,降幅高达75.5%。薄膜的膜/基结合力随Cr粘结层厚度的增加而提高,当Cr粘结层厚度为1.01 μm时,Cr-DLC薄膜的膜/基结合力最佳,与无Cr粘结层Cr-DLC薄膜的第1（L_c1）和第2（L_c2）临界载荷相比分别提高69%和67%。经20 000次连续冲击试验,所有薄膜样品冲击坑的冲击深度均没有弹性恢复,薄膜在冲击坑的中心位置均出现一定面积的剥落,其中,Cr粘结层厚度1.01 μm的Cr-DLC薄膜样品的膜层剥落面积最小,表现出了最好的抗连续冲击的能力。一定厚度Cr粘结层能够大幅降低铜合金表面Cr-DLC薄膜的残余应力,提高膜/基结合力和耐冲击性能。     

多弧离子镀制备Cr/CrN多层厚膜的微观结构和力学性能

通过多弧离子镀（MAIP）在室温下将具有不同调制比（1:2、1:3、1:5）的多层Cr/CrN厚涂层沉积在A100钢基底上。腔室温度在沉积过程中由室温逐渐升高到160~170 ℃。设计调制结构是为了使膜/基结合强度和机械性能最大化。调制比为1:2的Cr/CrN多层涂层表现出最高的膜/基结合强度（L_c=63.8 N）,这可能归因于最高的材料硬度(H)/弹性模量(E)和H³/E²数值比（分别为0.083和0.138）。Cr层越厚,多层Cr/CrN厚涂层的塑性和摩擦学性能越好。干摩擦试验表明,与单层CrN相比,Cr/CrN多层涂层的平均摩擦系数和比磨损率分别最高降低了24%和94%。随着Cr层变厚,磨损机理从表面疲劳磨损转变为磨料磨损,这种现象可归因于硬度和塑性的协调变化。     

Microstructural, mechanical and tribological properties of tungsten-gradually doped diamond-like carbon films with functionally graded interlayers

A series of tungsten-gradually doped diamond-like carbon (DLC) films with functionally graded interlayer were prepared using a hybrid technique of vacuum cathodic arc/magnetron sputtering/ion beam deposition. With ‘compositionally graded coating’ concept, the deposition of wear-resistant carbon-based films with excellent adhesion to metallic substrate was realized. In the films, a functionally graded interlayer with layer sequence of Cr/CrN/CrNC/CrC/WC was first deposited onto the substrate, and then, a DLC layer doped with gradually decreasing content of W was coated on. The W concentration gradient along depth of the film was tailored by adjusting the W target current and deposition time. The characterized results indicate that the microstructural, mechanical and tribological properties of these films show a significant dependence on the W concentration gradient. A high fraction of W atom in carbon matrix can promote the formation of sp² sites and WC_1 − x nanoparticles. Applying this coating concept, strongly adherent carbon films with critical load exceeding 100 N in scratch test were obtained, and no fractures or delaminations were observed at the end of the scratched trace. The hardness was found to vary from 13.28 to 32.13 GPa with increasing W concentration. These films also presented excellent tribological properties, especially significantly low wear rate under dry sliding condition against Si₃N₄ ball. The optimum wear performance with friction coefficient of 0.19 and wear rate of 8.36 × 10⁻⁷ mm³/Nm was achieved for the tungsten-gradually doped DLC film with a graded W concentration ranging from 52.5% to 17.8%. This compositionally graded coating system might be a potentially promising candidate for wear-resistant carbon-based films in the demanding tribological applications.     

Adaption of graded Cr/CrN-interlayer thickness to cemented carbide substrates' roughness for improving the adhesion of HPPMS PVD films and the cutting performance

High Power Pulsed Magnetron Sputtering (HPPMS) techniques jointly with the deposition of a graded Cr/CrN-nanointerlayer on cutting inserts can increase the film adhesion and consequently the tool life. These improvements depend on the roughness of the employed cemented carbide substrates. The investigations described in the present paper intend to explain the effect of Cr/CrN-interlayer thickness and substrate roughness on the coating adhesion and cutting performance. To attain various roughnesses, the applied cemented carbide inserts were superficially treated. These treatments were grinding at a medium roughness level, or grinding with subsequent polishing for enhancing the surface integrity and finally, in all cases, micro-blasting by fine Al₂O₃ grains. After Ar-ion etching, graded Cr/CrN adhesive layers with different thicknesses were deposited by HPPMS technology on the variously pretreated substrates. Subsequently, an approximately 3 μm thick (Ti,Al)N film was deposited by HPPMS PVD on all used inserts. Rockwell C indentations and inclined impact tests were performed to assess qualitatively and quantitatively the films' adhesion. The cutting performance of the coated tools was investigated in milling of 42CrMo4 QT. FEM supported calculations of the developed stresses during the material removal process contributed in explaining the obtained tool wear results. In these calculations, the adhesion, dependent on the substrate roughness characteristics and on the adhesive interlayer thickness, was taken into account. The results revealed that the effectiveness of HPPMS adhesive graded Cr/CrN-nanointerlayer strongly depends on the substrate surface integrity and on the interlayer thickness. Thus, the film adhesion and consequently the cutting performance can be significantly improved if the interlayer thickness is adapted to the substrate roughness.     

钼合金磁控溅射镀镍薄膜工艺及后续热处理

目的优化钼表面直流磁控溅射镀镍薄膜的工艺,提出后续热处理方法。方法设计正交实验,探究溅射功率、溅射气压、负偏压和沉积时间对镍薄膜沉积速率和附着力的影响,从而优化工艺参数。利用扫描电镜和平整度仪对最佳工艺参数下制备的薄膜的组织结构进行表征,并研究后续热处理对薄膜附着力的影响。结果工艺参数对镀镍薄膜沉积速率影响的主次顺序为:功率溅射气压负偏压;对薄膜附着力的影响主次顺序为:负偏压沉积时间功率溅射气压。随溅射功率增大,沉积速率增大,薄膜附着力先增后减;随溅射气压增大,沉积速率和薄膜附着力均先增后减。负偏压增大对沉积速率影响较小,但有利于提高薄膜附着力。随沉积时间延长,薄膜附着力降低。在氢气气氛下进行850℃×1 h的后续热处理,能够促进扩散层的形成,明显提高镍薄膜的附着力。结论最佳镀镍工艺参数为:溅射功率1.8 k W,溅射气压0.3 Pa,负偏压450 V,沉积时间10 min。在该条件下制备的镍薄膜厚度达到1.15μm左右,与基体结合紧密,表面平整、连续、致密。后续增加热处理工序是提高镍薄膜附着力的有效方法。     

Influence of interlayers on corrosion resistance of diamond-like carbon coating on magnesium alloy

Diamond-like carbon coating (DLC) was deposited on AZ31 magnesium alloy by ion beam deposition technique in this study. A columnar Cr layer with a (110) preferred texture and a columnar CrN layer with a (111) preferred texture were applied as interlayers in the DLC coating/AZ31 substrate systems. The addition of these interlayers improved the adhesion between coating and substrate effectively, but did not enhance the corrosion resistance of the DLC/AZ31 systems due to the formation of galvanic cell between substrate and interlayer in the region of through-thickness defects in 3.5 wt.% NaCl solution. In addition, the effect of bias voltage on the corrosion resistance of CrN/Cr coatings on magnesium alloys was investigated. Although the application of bias voltage induced the coating denser, it was still difficult for CrN/Cr coating to reduce the corrosion current density of AZ31 due to the large difference between coating and substrate in galvanic series.     

电刷镀Ni-W过渡层与离子镀TiN复合涂层的结合力和磨损特性

研究了3Cr2W8V基体电刷镀Ni-W过渡层和离子镀TiN复合涂层的结合力及强化机理.利用XRD、SEM和TEM分析了涂层结构,用划痕法测定了涂层结合力,并测定和分析了涂层的磨损特性.结果表明由于TiN沉积过程中的温度效应,混合晶态的电刷镀Ni-W层发生晶化和析出强化,并形成界面扩散层和双层复合,从而使TiN复合涂层的结合力和硬度明显提高;Ni-W过渡层对TiN涂层起有力的支撑作用.Ni-W与TiN复合涂层的耐磨性优于TiN单层.     

Cr基及其化合物过渡层对TiCN涂层性能的影响

为研究过渡层材料及结构对TiCN涂层性能的影响,设计3种Cr基及其化合物过渡层,利用多弧离子镀技术制备TiCN涂层。膜系分别为Cr/TiCN、Cr/CrN/TiCN和Cr/CrN/CrCN/TiCN。利用SEM、XRD、纳米压痕仪、划痕仪、摩擦磨损试验机和球磨仪对涂层的微观结构和性能进行表征。结果表明:随着过渡层由单层Cr依次加入CrN和CrCN,涂层原有的柱状晶生长被抑制并最终消除。与具有Ti过渡层的TiCN相比,涂层不再具有明显择优取向,(111)峰强度大大减弱而(200)峰发生宽化。具有CrN和CrCN过渡层的样品硬度和附着力明显高于以单层Cr为过渡层的样品,Cr/CrN/CrCN/TiCN膜系硬度和附着力最高,分别为(30.11±0.34)GPa和(37.21±0.46)N。摩擦磨损试验结果表明:CrCN过渡层的引入显著提升了涂层耐磨性,其对应样品摩擦因数最低,达到0.111,并在球磨测试中表现稳定,而其它膜系均出现不同程度的磨损形貌。     

间隙尺寸对结构钢感应加热淬火淬硬层深度的影响

研究了45、40Cr钢感应加热水冷处理后的组织。感应加热频率为15 kHz,功率、工件相对移动速度分别为40 kW、5~11 mm/s和70 kW、6.5~11 mm/s,感应圈与工件之间的间隙尺寸分别为1.5 mm、3 mm。试验结果表明,淬火试样表面至心部由马氏体、马氏体＋铁素体、马氏体＋铁素体＋珠光体组成,中心为珠光体＋铁素体原始组织。40Cr钢试样与感应圈之间的间隙尺寸由3 mm减小到1.5 mm时,淬硬层深度的增加幅度为：宏观测定法为47%,金相测定法为49%;而45钢试样宏观测定法为45%,金相测定法为46%。     

压痕法研究镶嵌结构界面金刚石膜粘附性能

在铜基体上沉积Cu(Cr)-diamond复合过渡层,用热丝CVD法在复合过渡层上沉积出金刚石膜。用压痕法对沉积的金刚石膜/基结合性能进行了研究。结果表明,在Cu-diamond上沉积的金刚石膜,用147 N压痕时压痕边缘出现大面积崩落,并在基体表面留下被拔出的金刚石凹坑;在Cu-diamond中掺入微量Cr,压痕边缘只形成环形裂纹,增大压痕载荷至441 N,环形裂纹区域增大,并出现部分崩落,崩落区域有被切断的金刚石残留。在Cu-diamond复合层中掺入微量Cr能显著提高金刚石膜/基结合力。