应用纳米压痕法测试类金刚石薄膜的力学性能

纳米压痕仪被称为材料机械性质微探针,它借助于加载-卸载过程中压痕对载荷和压入深度的敏感关系,使得测试始终在薄膜材料的弹性限度内,克服了维氏法和努氏法等传统方法引起压痕边缘模糊或者碎裂的缺点,从而正确地、可靠地测试出薄膜材料的硬度和弹性模量等纳米力学性能.试验用微波电子回旋共振等离子体增强化学气相沉积技术,在不同偏压条件下制备三种类金刚石薄膜(DLC膜),用纳米压痕仪测试不同载荷下薄膜的硬度和弹性模量值.试验结果表明,材料的纳米硬度和弹性模量随着载荷的增大而逐渐减小.     

摩擦表面膜纳米力学性能评定新方法

介绍了新型纳米压痕技术的基本测量原理，该技术利用加载-卸载过程中压痕对载荷和压入深度的敏感关系，测试材料的硬度和弹性模量等力学性能。由于该技术纳米级的压头位移和纳牛顿级的作用力，使之成为研究摩擦表面膜的有力工具，应用纳米压痕法对纳米铜摩擦表面膜进行了硬度和弹性模量的测试和分析。     

薄膜/基体结构的纳米压痕实验及其有限元分析

利用纳米压痕实验测定了氮化钛薄膜/高速钢基体中薄膜的弹性模量和硬度,并得到了纳米压痕过程的载荷—位移曲线;根据实验所得材料参数建立了纳米压痕实验的DEFORM计算模型,利用该有限元模型分析了不同薄膜厚度的膜/基结合处的切应力分布,研究了膜/基分离的可能性大小及分离位置与薄膜厚度的关系。     

一种新型纳米硬度检测装置的研究

纳米压痕装置是一种具有纳米级压痕深度检测能力，能够完成载荷一位移测量的一种装置，根据所得到的载荷一位移曲线可以用来获得材料的纳米硬度值。文中讨论了一种新型便携的纳米硬度检测装置的研制，并通过对单晶铝进行压痕试验，验证此硬度检测装置的实用性与可靠性。     

两步压入法--薄膜力学性能的可靠测量方法

提出了采用力学探针测量薄膜力学性能的两步压入法.该方法通过大载荷压入展示基体变形对薄膜硬度的影响,从而选择不影响基体变形的小载荷测出薄膜的硬度和弹性模量.对高速钢基片上的TiN硬质薄膜,单晶硅片上的金属Ni薄膜和(Ti,Al)N/VN纳米多层膜的测量表明,两步压入法能够测出各种性质薄膜的力学性能,并且具有准确可靠的特点.此外,两步法对(Ti,Al)N/VN纳米多层膜的力学性能的测量表明,该体系的纳米多层膜存在硬度和弹性模量异常升高的超硬、超模量效应.     

纳米压痕硬度尺寸效应分析及其试验研究

针对材料纳米压痕硬度的压痕尺寸效应(Indentation size effect,ISE),利用纳米压痕技术测得单晶铝和单晶硅的载荷-压深曲线,获得最大载荷和最大压深,并结合原子力显微镜,获得压痕的三维形貌,计算出压痕的真实残余面积。根据最大压深和残余面积提出了一个新的模型——残余面积最大压深模型,此模型能更好地理解和描述材料硬度的压痕尺寸效应,并与其他几种典型的理论和模型进行了比较和分析。     

单晶硅纳米力学性能的测试

对材料纳米力学性能测试手段进行了研究,着重分析了纳米压痕技术的原理和方法.结合纳米压痕技术,采用尖端四面体Vickers型单晶金刚石压头对单晶硅(100)晶面进行了纳米压痕实验测试.实验发现,在载荷为1 000 mN时,晶体硅出现了明显的裂纹和脆性断裂;而在载荷低于80 mN的情况下,晶体硅则表现出延性特性.此外,在不同载荷条件下对晶体硅的硬度进行了实验测试,测试结果发现,不同载荷条件下晶体硅的硬度测量值存在较大的差异,认为导致这种差异的原因在于压痕区域晶体硅所受压力不同,使得晶体硅内部结构发生了改变,较为准确的单晶硅的硬度测量值为15.7 GPa.     

薄膜厚度对Si基SiO2薄膜力学性能的影响

为了研究薄膜厚度对Si基SiO_2薄膜力学性能的影响规律,利用纳米压痕技术及有限元模拟方法对不同厚度的Si基SiO_2薄膜材料进行测试,分析了不同厚度薄膜的硬度及弹性模量等力学性能,讨论了不同压深膜厚比对不同厚度薄膜弹性恢复率的影响,并在试验的基础上,建立了有限元模型,模拟了不同厚度薄膜在相同压深下的载荷位移关系,分析了薄膜的弹性恢复性能。结果表明:SiO_2薄膜越厚其弹性模量越小,而薄膜的硬度在薄膜较薄时压痕的尺寸效应更明显,并利用模拟进一步分析得出薄膜越薄弹性恢复性能越好。     

基于原子力显微镜和分子动力学的纳米压痕技术研究

利用原子力显微镜对真空蒸发镀膜技术制得的单晶铜薄膜试件进行了纳米压痕试验。通过进行各种压痕深度下的试验,获得了压痕深度对试件力学性能的影响关系。试验得到的试件弹性模量为67.0 GPa±6.9 GPa。试件的硬度值随着压痕深度的减小而不断增大,表现出强烈的尺寸效应。在原子力显微镜试验的同时,使用分子动力学仿真方法对单晶铜薄膜的纳米压痕过程进行了研究。仿真结果表明单晶铜薄膜的纳米压痕的力学机理不是位错在晶体中运动产生的塑性变形,而是非晶态产生的变形,从而解释了尺寸效应产生的原因。     

纳米尺度接触过程力学特性实验研究

利用纳米压痕仪进行纳米尺度接触力学特性实验研究,通过金刚石探针与单晶硅试件接触作用,获得不同载荷、不同接触深度条件下的接触压入和脱离接触的位移-载荷曲线,并利用原子力显微镜对接触区域扫描,获得接触区域AFM三维形貌图。研究表明,在不同载荷条件下接触压入,随着载荷的增大,接触深度也随之增大;在不同深度条件下接触压入,随着接触深度的增大,接触作用力也随之增大。脱离接触的时候,接触区有弹性恢复,但有残余变形,接触区域表现出了塑性变形,压痕附近区域没有裂纹情况出现,载荷或接触深度越大,接触塑性变形越明显。此外,在不同载荷、不同接触深度条件下,接触区的压痕硬度和弹性模量相应有不同值,接触压痕硬度值和弹性模量值均有一定变化。     

Study of the effect of imperfect tips on nanoindentation by FEM

In this paper, the imperfect tip effect of the Ti film on Si substrate on nanoindentation with Berkovich probe tip was investigated with the finite element method (FEM). In the literature, we found the effects of tip deformation and tip radius on nanoindentation were investigated frequently, but the imperfect centerline of tip has never been studied. In this work, at first, the Ti film on Si substrate was conducted with a high-resolution nanomechanical test. The Young’s modulus of Ti films can be obtained by using the Oliver and Pharr method while the nanoindentation depth is smaller than 20% of the film thickness for avoiding the substrate effect. Second, the FEM was employed to determine the yield stress of thin films because it cannot be found from nanoindentation. Finally, the load-depth of nanoindentation was compared between the experimental data and numerical results. The results show while choosing the suitable yield stress of films, the load-depth curves of numerical simulation were very close to the experimental curves with the imperfect effect being ignored. Moreover, it is concluded while the imperfect angles of tip were considered that the larger imperfect angles |θ _x | orθ _x , the smaller displacement on nanoindentation.     

Indentation modulus and hardness of viscoelastic thin films by atomic force microscopy: A case study

We propose a nanoindentation technique based on atomic force microscopy (AFM) that allows one to deduce both indentation modulus and hardness of viscoelastic materials from the force versus penetration depth dependence, obtained by recording the AFM cantilever deflection as a function of the sample vertical displacement when the tip is pressed against (loading phase) and then removed from (unloading phase) the surface of the sample. Reliable quantitative measurements of both indentation modulus and hardness of the investigated sample are obtained by calibrating the technique through a set of different polymeric samples, used as reference materials, whose mechanical properties have been previously determined by standard indentation tests. By analyzing the dependence of the cantilever deflection versus time, the proposed technique allows one to evaluate and correct the effect of viscoelastic properties of the investigated materials, by adapting a post-experiment data processing procedure well-established for standard depth sensing indentation tests. The technique is described in the case of the measurement of indentation modulus and hardness of a thin film of poly(3,4-ethylenedioxythiophene) doped with poly(4-styrenesulfonate), deposited by chronoamperometry on an indium tin oxide (ITO) substrate.     

An edge reversal method for precision measurement of cutting edge radius of single point diamond tools

A method, which is referred to as the edge reversal method, is proposed for precision measurement of the cutting edge radius of single point diamond tools. An indentation mark of the cutting edge which replicates the cutting edge geometry is firstly made on a soft metal substrate surface. The cutting edge of the diamond tool and its indentation mark, which is regarded as the reversal cutting edge, are then measured by utilizing an atomic force microscopy (AFM), respectively. The cutting edge radius can be accurately evaluated through removing the influence of the AFM probe tip radius, which is comparable to the cutting edge radius, based on the two measured data without characterization of the AFM probe tip radius. The results of measurement experiments and uncertainty analysis are presented to demonstrate the feasibility of the proposed method.     

MoS2/Ti复合固体润滑膜的力学性能与摩擦特性

采用非平衡磁控溅射法在9Cr18轴承钢基底上制备了厚度约3μm的MoS2/Ti复合固体润滑膜,基于球形压头纳米压痕试验,采用连续刚度法对MoS2/Ti复合固体润滑膜的力学性能进行研究,探究MoS2/Ti复合固体润滑膜力学性能随压痕深度的变化规律;根据压痕试验载荷-位移曲线,采用Hertz接触理论计算MoS2/Ti复合固体润滑膜的弹性模量并与试验结果进行对比;利用CSM摩擦试验机对低速、低载下MoS2/Ti复合固体润滑膜的摩擦特性进行研究;基于压痕试验提出了一种能够更准确计算钢球加载时MoS2/Ti复合固体润滑膜接触应力的方法,并计算了摩擦试验不同载荷下的接触应力。结果表明:MoS2/Ti复合固体润滑膜的力学性能和摩擦特性都会受到表面形貌的影响;除表面初始压入阶段外,MoS2/Ti复合固体润滑膜的弹性模量和接触刚度都随着压痕深度的增大而增大;滑动速度和载荷共同影响MoS2/Ti复合固体润滑膜的摩擦特性。     

Nano-wear of the diamond AFM probing tip under scratching of silicon, studied by AFM

In order to improve such a widely used microtribological testing procedure as surface scratching by an AFM diamond tip, an experimental study has been carried out using single-crystalline silicon as the tested material. Wear of the AFM diamond tip under scratching was observed by a decrease in the scratch depth with increasing wear cycles and by the direct imaging of the diamond tip shape using a Si₃N₄ AFM tip. It was shown that the current widely used experimental method, which assumes the diamond tip to be non-wearable, introduces uncontrollable error into the obtained values for the tested material's wear rate. The harder the tested material, the larger may be the tip wear, and, therefore, the bigger may be its effect on the obtained wear rate values. The specific wear rates for the diamond tip and a silicon wafer were estimated to be 1.4 × 10^-9 and 4.5 × 10^-4 mm³/(N m), respectively.     

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A force-matching method for quantitative hardness measurements by atomic force microscopy with diamond-tipped sapphire cantilevers

We present a new method to improve the accuracy of force application and hardness measurements in hard surfaces by using low-force (<50 μN) nanoindentation technique with a cube-corner diamond tip mounted on an atomic force microscopy (AFM) sapphire cantilever. A force calibration procedure based on the force-matching method, which explicitly includes the tip geometry and the tip-substrate deformation during calibration, is proposed. A computer algorithm to automate this calibration procedure is also made available. The proposed methodology is verified experimentally by conducting AFM nanoindentations on fused quartz, Si(1 0 0) and a 100-nm-thick film of gold deposited on Si(1 0 0). Comparison of experimental results with finite element simulations and literature data yields excellent agreement. In particular, hardness measurements using AFM nanoindentation in fused quartz show a systematic error less than 2% when applying the force-matching method, as opposed to 37% with the standard protocol. Furthermore, the residual impressions left in the different substrates are examined in detail using non-contact AFM imaging with the same diamond probe. The uncertainty of method to measure the projected area of contact at maximum force due to elastic recovery effects is also discussed.     

弹性模量对水润滑轴承的性能影响

从材料的角度,研究弹性模量对水润滑塑料合金轴承的性能影响,包括轴承承载能力、水膜形状曲线、压力曲线和最小水膜厚度等。研究表明:在选择水润滑轴承材料时应根据其承载能力来确定轴承材料的弹性模量范围;在承载能力范围内,从弹性模量这个角度来说,应当尽可能选择弹性模量低并具有良好摩擦磨损性能的材料,因为选择较小弹性模量的材料有利于提高最小水膜厚度,从而改善水润滑轴承摩擦副的摩擦磨损性能。     

A force-matching method for quantitative hardness measurements by atomic force microscopy with diamond-tipped sapphire cantilevers

We present a new method to improve the accuracy of force application and hardness measurements in hard surfaces by using low-force (<50 μN) nanoindentation technique with a cube-corner diamond tip mounted on an atomic force microscopy (AFM) sapphire cantilever. A force calibration procedure based on the force-matching method, which explicitly includes the tip geometry and the tip-substrate deformation during calibration, is proposed. A computer algorithm to automate this calibration procedure is also made available. The proposed methodology is verified experimentally by conducting AFM nanoindentations on fused quartz, Si(1 0 0) and a 100-nm-thick film of gold deposited on Si(1 0 0). Comparison of experimental results with finite element simulations and literature data yields excellent agreement. In particular, hardness measurements using AFM nanoindentation in fused quartz show a systematic error less than 2% when applying the force-matching method, as opposed to 37% with the standard protocol. Furthermore, the residual impressions left in the different substrates are examined in detail using non-contact AFM imaging with the same diamond probe. The uncertainty of method to measure the projected area of contact at maximum force due to elastic recovery effects is also discussed.