TiN/CrN多层薄膜的微观结构与力学性能（英文）

为了研究TiN/CrN多层薄膜微观结构与力学性能的关系,采用磁控溅射技术制备了TiN、CrN单层薄膜和3种不同调制周期的TiN/CrN多层薄膜。通过原子力显微镜和X射线衍射仪分析了膜的表面形貌和相结构。使用纳米压痕仪测试薄膜的硬度和压入塑性,用曲率法测定薄膜的残余应力。结果表明,TiN/CrN的多层薄膜是由TiN和Cr_2N两相组成,随着调制周期的增大,TiN层与CrN层之间的界面区域变小,界面平滑且明显。力学性能方面,多层薄膜的硬度和压入塑性比单层膜好,并且多层薄膜随调制周期的减小,硬度和压入塑性增大,残余应力随周期的增加而逐渐增大。综上可见,TiN/CrN多层薄膜的力学性能的改善取决于界面区域的大小和形貌,即调制周期。该结论与Hall-Petch理论相吻合。     

晶粒尺寸与保载载荷对Cu膜纳米压入蠕变性能的影响

利用纳米压入仪对Si片上的多晶Cu膜进行压入蠕变研究．实验结果显示晶粒尺寸大于200nm时，应力指数对晶粒尺寸不敏感．当晶粒尺寸小于200nm时，因压头底部更多的晶粒参与变形，应力指数随晶粒尺寸的降低而增大．认为薄膜材料存在一个对应力指数不敏感的最小If缶界晶粒尺寸ιc，Cu膜的应力指数随保载载荷增大而增大，其主要原因在于高载荷下位错强化机制使蠕变率降低。     

纳米压痕法分析ECAP变形工业纯钛的力学性能

采用等径弯曲通道变形(Equal Channel Angular Pressing,ECAP)技术制备了不同晶粒尺寸的超细晶工业纯钛,通过纳米压痕测试技术对ECAP变形工业纯钛的力学性能进行研究,讨论了加载应变速率和晶粒尺寸对工业纯钛硬度测试结果的影响,进一步分析了ECAP变形工业纯钛的应变硬化能力和残余应力。结果表明:随着加载应变速率的增大和晶粒尺寸的减小,工业纯钛的硬度值增加。硬度-位移曲线表现出具有硬化效应的压痕尺寸效应(Indentation Size Effect,ISE)。纳米压痕形貌表明:ECAP变形工业纯钛的应变硬化能力降低,存在残余压应力。     

不同基底温度对Ti薄膜表面形貌及残余应力的影响（英文）

采用纳米压痕法中的Suresh模型和Lee模型研究不同基底温度对直流磁控溅射制备的Ti薄膜中残余应力大小及分布的影响。将压痕法计算结果与曲率法结果进行比较研究,同时采用原子力显微镜和X射线衍射仪对Ti薄膜的表面形貌及相结构进行分析。结果表明:Suresh模型计算得到的Ti薄膜残余应力值与曲率法结果最为接近,因此Suresh模型更适合测量Ti薄膜中的残余应力。结合纳米压痕和显微结构的分析发现,随着Ti薄膜基底温度的升高,Ti薄膜的晶粒尺寸先增大后变小,残余应力则从压应力转变为拉应力。     

TiN/CrN多层薄膜微观结构与力学性能的研究

近些年来,TiN/CrN多层薄膜由于其优良的力学性能被广泛应用于表面防护,提高零部件性能和使用寿命等方面。为了研究TiN/CrN多层薄膜微观结构与力学性能的关系,本文采用磁控溅射技术制备了TiN、CrN单层薄膜和三种不同调制周期的TiN/CrN多层薄膜。通过原子力显微镜和X射线衍射分析了膜的表面形貌和相结构。使用纳米压痕仪测试薄膜的硬度和压入塑性,曲率法测定薄膜的残余应力。结果表明,TiN/CrN的多层薄膜是由TiN和Cr2N两相组成,随着调制周期的增大TiN层与CrN层之间的界面区域变小,界面平滑且明显。力学性能方面,多层薄膜的硬度和压入塑性比单层膜好,并且多层薄膜随调制周期的减小硬度和压入塑性越大,残余应力随周期性的增加而逐渐增大。综上可见,TiN/CrN多层薄膜的力学性能的改善取决于界面区域的大小和形貌,即调制周期,该结论与Hall–Petch理论相吻合。     

基于原子力显微镜的薄膜原位压痕力学性能研究

基于原子力显微镜(AFM)和扫描电子显微镜(SEM)建立了一套原位纳米压痕测试系统。该系统可以实现控制带有金刚石(Cube corner)压头的AFM微悬臂梁对样品进行压入实验,并得到载荷-位移曲线,同时可以对压痕过程进行原位SEM实时观察。发展了一种基于AFM微悬臂梁加载和原位SEM压痕图像分析的力学性能测试方法,通过测量压入最大载荷和原位SEM测量压痕残余面积得到塑性薄膜的硬度和弹性模量。利用此方法对磁控溅射硅衬底上纳米晶银薄膜进行了压痕实验,并与Nanoindenter G200型纳米压痕仪实验进行对比研究。结果表明,原位AFM压痕方法具有高的载荷和位移分辨率,可以实现纳牛至微牛级的压痕实验,通过测量压痕面积得到塑性薄膜的硬度值,减小了使用Oliver-pharr方法中软膜硬基底上凸起(Pile-up)效应的影响,计算结果也具有好的测试精度和可靠性。     

对几种薄膜硬度测试方法的评定

用传统的显微硬度计直接测量薄膜硬度难以避免基体的影响且小载荷压入时产生的较小的压痕不易被准确测量。纳米压入仪是一种可以精确控制及测量压入深度的高精度仪器。这种通过测压入深度测硬度值的技术可以减少基体硬度对薄膜测量硬度的影响同时产生的误差较直接测压痕对角线的误差小。但是，纳米压入仪对试样表面光洁度要求高，仪器价格昂贵。这些都限制其在实际工业中的应用。较好的一种硬度测试方法是通过传统显微硬度计在不同的大载荷下测得膜基复合硬度，同时建立适当的模型计算出薄膜的本征硬度值。此方法可能更适合于常规应用。     

表面残余应力对玻璃压痕参数的影响

通过研究化学钢化前、钢化后钠钙玻璃的压痕形貌、几何尺寸和表面力学性能，分析和探讨了表面残余应力对玻璃压痕参数以及表面力学性能变化的影响机理。结果表明，普通玻璃的压痕与钢化玻璃的压痕有明显的差别，钢化玻璃的压痕周围呈圆形放射状光斑，压痕裂纹很小，其硬度值比相同载荷下钢化前玻璃硬度值增加了约15．8％，压痕断裂韧性有明显的提高，是钢化前玻璃断裂韧性的2．75倍，显示了钢化后表面残余压应力对玻璃的压痕参数和力学性能的影响。     

磁控溅射Cu膜屈服强度的有限元计算

采用离子辅助轰击共溅射设备，在Si基体的(111)晶面上制得了所需的铜膜。采用纳米压入实验，获得不同退火温度下Cu膜的弹性模量和硬度。再在纳米压入实验的基础上，结合有限元模型计算不同退火温度下磁控溅射得到的Cu膜屈服强度。发现Cu膜的屈服强度远高于整体Cu材料的屈服强度，并且退火温度对薄膜的屈服强度影响很大。通过XRD测量发现其主要原因是退火改变了晶粒尺寸和多晶Cu膜的晶粒取向分布，而导致Cu膜屈服强度的降低。     

靶基距对Cu/Si(100)薄膜结构和残余应力的影响

采用高功率调制脉冲磁控溅射(MPPMS)技术在 Si(100)基体上沉积 Cu 薄膜,SEM 观察薄膜厚度及生长特征、XRD 分析薄膜晶体结构、nanoindentor 测量薄膜纳米硬度和弹性模量、Stoney 公式计算薄膜残余应力,研究沉积过程靶基距对 Cu / Si(100)薄膜沉积速率、微结构及残余应力的影响。 随着靶基距的增大,薄膜沉积速率降低,薄膜的生长结构由致密 T 区向 I 区转变,Cu(111)择优生长的晶粒逐渐减小,薄膜纳米硬度和弹性模量也相应降低,残余拉应力约为 400 MPa。 较小靶基距时增加的沉积离子通量和能量,决定了薄膜晶粒合并长大体积收缩过程的主要生长形式,导致了 Cu / Si(100)薄膜具有的残余拉应力状态。 MPPMS 工艺的高沉积通量和粒子能量可实现对 Cu / Si(100)薄膜残余应力的调控。     

基体脉冲偏压对TiN/Cu纳米复合薄膜组织结构、力学及耐磨性能的影响

本文采用轴向磁场增强电弧离子镀在高速钢基体上沉积了TiN/Cu纳米复合薄膜,研究了基体脉冲偏压幅值对薄膜成分、结构、力学性能及耐磨性能的影响。结果表明,薄膜中铜含量随着脉冲偏压幅值的增加先增加而后降低,在一个较低的范围内(1.3-2.1at.%)。X射线衍射结果表明所有的薄膜均出现TiN相,并未观察到Cu相。薄膜的择优取向随着脉冲偏压幅值的增加而改变。薄膜的最高硬度为36GPa,是在脉冲偏压幅值为-200V时得到的,对应了1.6at.%的Cu含量。与纯的TiN薄膜相比,Cu的添加明显增强了薄膜的耐磨性能。     

Effect of substrate bias voltage on the texture and microstructure of Cu thin films deposited by ion beam deposition

Cu thin films deposited by non-mass separated ion beam deposition under various substrate bias voltages were investigated. The film textures and microstructure were analyzed by X-ray diffraction and field emission scanning electron microscopy, and the resistivity of the film was measured with the Van der Pauw method. It was found that the optimum negative substrate bias voltage for Cu films was −50 V. The Cu films deposited without substrate bias voltage showed a columnar grain structure with small grains and random orientation. However, when a substrate bias voltage of −50 V was applied, the Cu films had a non-columnar structure with a strong (111) texture and large grains. The electrical resistivity of the Cu films decreased remarkably with increasing negative substrate bias voltage, and reaching a minimum value of 1.8±0.13 μΩ cm at the substrate bias voltage of −50V.     

多弧离子镀负偏压对氮化钛薄膜的影响

目的确定适当的负偏压,提高多弧离子镀氮化钛薄膜的综合性能。方法采用不同的负偏压,在4Cr13不锈钢表面制备Ti N薄膜,探讨偏压对薄膜表面质量、结构、硬度、结合力和摩擦系数的影响。结果负偏压对薄膜表面质量的影响较大:负偏压为0 V时,Ti N薄膜表面凹凸不平,液滴较多;随着负偏压升高,薄膜表面变得光滑,液滴减少并变小,薄膜致密性也得到提高。在不同负偏压下,Ti N薄膜均呈现出在(111)晶面的择优取向,但随着负偏压的增大,这种择优取向逐渐减弱,当负偏压达到400 V时,薄膜在(220)晶面的峰值逐渐增强。随着负偏压从0增至400 V,薄膜的硬度、结合力和耐磨性均先提高,后降低。当负偏压为300 V时,薄膜的硬度和结合力达到最大,分别为2650HV和58 N;摩擦系数和磨损量最小,分别为0.48和0.1065 mm3。结论施加适当的负偏压可以提高薄膜的硬度、结合力、耐磨性等性能,当负偏压为300 V时,薄膜的各项性能达到最佳。     

脉冲偏压对复合离子镀(Ti,Cu)N 薄膜结构与性能的影响

目的 (Ti,Cu)N薄膜是一种新型的硬质涂层材料,关于其结构和性能的研究报道还较少。研究脉冲偏压对(Ti,Cu)N薄膜结构与性能的影响规律,以丰富该研究领域的成果。方法将多弧离子镀和磁控溅射离子镀相结合构成复合离子镀技术,采用该技术在不同脉冲偏压下于高速钢基体表面制备(Ti,Cu)N薄膜。分析薄膜的微观结构,测定沉积速率及薄膜显微硬度,通过摩擦磨损实验测定薄膜的摩擦系数。结果在不同偏压下获得的(Ti,Cu)N薄膜均呈晶态,具有(200)晶面择优取向,当脉冲偏压为-300 V时,薄膜的择优程度最明显。随着脉冲偏压的增加,薄膜表面大颗粒数量减少且尺寸变小,表面质量提高;沉积速率呈现先增大、后减小的趋势,在脉冲偏压为-400 V时最大,达到25.04 nm/min;薄膜硬度也呈现先增大、后减小的趋势,在脉冲偏压为-300 V时达到最大值1571.4HV。结论脉冲偏压对复合离子镀(Ti,Cu)N薄膜的表面形貌、择优取向、沉积速率和硬度均有影响。     

Hexagonal diamond formation on steel substrates by negative bias microwave plasma enhanced chemical vapor deposition

This paper reports for the first time the synthesis of hexagonal diamond thin films on high-speed steel substrates by multi-mode microwave plasma enhanced chemical vapor deposition. Before deposition of the films, the substrate surface was treated by scratching with diamond powder. The deposited films were characterized by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy. The XRD patterns of (100) and (101) planes and the Raman peaks at ~ 1317-1322 cm^− 1 were observed, confirming the formation of hexagonal diamond phase in the prepared films. The effects of voltage bias on the phase formation, microstructure and hardness of the films were also studied by setting the voltage to 0, − 70, − 150 and − 190 V. The highest hardness of 23.8 GPa was found in the film having clusters of size about 550 nm deposited under a bias voltage of − 150 V. These clusters were built up of grains of size about 14 nm.     

Effect of applied dc bias voltage on composition, chemical bonding and mechanical properties of carbon nitride films prepared by PECVD

Carbon nitride films were deposited on Si (100) substrates using plasma-enhanced chemical vapor deposition (PECVD) technique from CH4 and N2 at different applied dc bias voltage. The microstructure, composition and chemical bonding of the resulting films were characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The mechanical properties such as hardness and elastic modulus of the films were evaluated using nano-indentation. As the results, the Raman spectra, showing the G and D bands, indicate the amorphous structure of the films. XPS and FTIR measurements demonstrate the existence of various carbon-nitride bonds in the films and the hydrogenation of carbon nitride phase. The composition ratio of N to C, the nano-hardness and the elastic modulus of the carbon nitride films increase with increasing dc bias voltage and reach the maximums at a dc bias voltage of 300 V, then they decrease with further increase of the dc bias voltage. Moreover, the XRD analyses indicate that the carbon nitride film contains some polycrystalline C3N4 phase embedded in the amorphous matrix at optimized deposition condition of dc bias voltage of 300 V.     

偏压对离子源辅助HiPIMS制备纳米TiN薄膜力学性能和耐蚀性能的影响

为提高磁控溅射制备薄膜的致密度,减少结构缺陷,研究薄膜显微结构对硬度、韧性及耐蚀性能的影响,尝试在改变离子源和基材偏压的条件下,采用离子源辅助HiPMIS技术在304不锈钢和P型（100）晶向硅片上制备TiN纳米薄膜。采用扫描电子显微镜、小角X射线衍射仪对薄膜的形貌和晶体结构进行分析;采用纳米压痕仪和维氏硬度计分别测量计算薄膜的硬度和韧性,并通过电化学工作站对薄膜的耐蚀性能进行检测。结果表明：随着偏压的增加以及离子源的引入,离子的轰击效应增强,薄膜的沉积速率下降,致密度增加。偏压为-200 V时,薄膜的硬度达到最大值16.2 GPa,且对应的晶粒尺寸最小,（111）晶面衍射峰的强度最高。离子源的加入使所制备薄膜的硬度略有下降。此外,随着偏压的增加,薄膜的韧性和耐腐蚀性能也有一定提高。     

负偏压在电弧离子镀沉积TiN／TiCN多层薄膜中的作用

用电弧离子镀方法在高速钢、不锈钢与铜基体上沉积合成Ti/TiCN多层薄膜,在其他参数不变的情况下只改变负偏压,着重考察不同负偏压下薄膜的沉积深度、膜基结合强度、显微硬度以及表面形貌等,研究基体负偏压在沉积多层薄膜中所起的作用。结果表明,负偏压影响沉积温度,负偏压值越大,温度越高;负偏压值增大,表面形貌中的大颗粒数量减少,薄膜质量得到改善;负偏压在－300V左右时,膜基结合强度与硬度出现对应最佳性能点的峰值。     

Effect of bias voltage on microstructure and properties of Ti-doped graphite-like carbon films synthesized by magnetron sputtering

Ti-doped graphite-like carbon (GLC) films with different microstructures and compositions were fabricated using magnetron sputtering technique. The influence of bias voltages on microstructure, hardness, internal stress, adhesion strength and tribological properties of the as-deposited GLC films were systemically investigated. The results showed that with increasing bias voltage, the graphite-like structure component (sp² bond) in the GLC films increased, and the films gradually became much smoother and denser. The nanohardness and compressive internal stress increased significantly with the increase of bias voltage up to −300 V and were constant after −400 V. GLC films deposited with bias voltages in the range of -300--400 V exhibited optimum adhesion strength with the substrates. Both the friction coefficients and the wear rates of GLC films in ambient air and water decreased with increasing voltages in the lower bias range (0--300 V), however, they were constant for higher bias values (beyond −300 V) . In addition, the wear rate of GLC films under water-lubricated condition was significantly higher for voltages below −300 V but lower at high voltage than that under dry friction condition. The excellent tribological performance of Ti-doped GLC films prepared at higher bias voltages of −300--400 V are attributed to their high hardness, tribo-induced lubricating top-layers and planar (2D) graphite-like structure.     

负偏压对电弧离子镀复合TiAlN 薄膜的影响

采用电弧离子镀技术,以W18Cr4V高速钢为基体,调整基体负偏压,制得多个复合TiAlN薄膜试样,研究了基体负偏压对薄膜微观组织形貌、物相组成、晶格位向、硬度、厚度和沉积速率的影响。结果表明,过高或过低的负偏压会使得膜层表面不平整,显微硬度下降。当负偏压为200 V时,膜层的沉积速率最大;负偏压为150 V时,有利于薄膜(111)晶面的择优取向生长,且TiAlN膜的硬度最高。