纳米压痕硬度计测方法的研究进展

针对纳米尺度下的材料硬度测量,利用纳米硬度计得到压痕的载荷-压深曲线,并用原子力显微镜得到压痕的三维形貌图.通过载荷-压深曲线和压痕形貌图,以及相应的计算方法,可以得到纳米压痕硬度.纳米压痕硬度计测方法不同,得到的材料硬度值也不同.分析现有的几种纳米压痕硬度计测方法,找出它们的优缺点,并对未来发展方向做了展望.     

Li_2O-Al_2O_3-SiO_2微晶玻璃超光滑表面纳米硬度实验研究

介绍了纳米压痕技术的原理和方法.采用三角锥形Berkovich金刚石压头对Li2O-Al2O3-SiO2微晶玻璃的超光滑表面(Ra=0.079 nm)进行了纳米压痕实验.结果表明,当载荷低于300 mN时,微晶玻璃表现出延性特性.此外,在不同的载荷条件(20 mN~300 mN)下微晶玻璃的硬度和弹性模量存在较大的差异,分析其原因分别是纳米压痕的尺寸效应和材料发生了塑形变形.通过将实验得到的微晶玻璃的纳米硬度值与传统计算方法得到的硬度值进行比较,发现传统方法得到的硬度值较大,其原因是传统硬度计算方法忽略了材料的弹性恢复.     

残余应力对固体氧化物燃料电池弹塑性性能的影响

半电池结构NiO-YSZ/YSZ由于弹性模量不同和热膨胀系数不匹配,导致烧结过程中产生残余应力. 残余应力对于燃料电池的性能和使用带来一定的影响, 本文把残余应力引入到计算薄膜性能的逆向分析模型中, 建立了考虑残余应力影响的薄膜的纳米压痕分析模型. 利用纳米压痕方法测试了离双层材料界面不同距离处的载荷-位移曲线和相应的材料性能, 用本文建立的模型计算了不同点的性能的变化, 发现离界面越远, 电解质YSZ薄膜的硬度越大. 将热力分析得到的残余应力场作为压痕模拟的初始应力场, 计算三棱锥压头下压痕载荷-位移曲线, 结果显示考虑残余应力时的载荷-位移曲线更接近实验曲线, 并给出了残余应力下压痕形貌图, 发现有残余应力时的压痕形貌更深更大.     

单晶铝纳米级硬度试验研究

使用纳米硬度计对单晶铝进行了纳米压痕试验,利用原子力显微镜对压痕形貌进行扫描并计算硬度值,重点观察和分析了纳米级条件下单晶铝的硬度性质,结果表明,当压痕深度小于2000nm时,单晶铝纳米硬度存在尺寸效应现象;从材料性质的角度分析了纳米硬度尺寸效应现象;探讨了纳米硬度和传统硬度本质上的区别,指出其根本原因在于不同尺度下人们对材料性质的关注点不同。     

维氏压痕对常压固相烧结碳化硅陶瓷材料力学性能的影响

为了研究维氏压痕裂纹对常压固相烧结碳化硅陶瓷(SSiC)材料力学性能的影响, 通过扫描电镜观察了0.1~100 N的压痕载荷下产生的表面裂纹及裂纹剖面的状况, 并测试了相应载荷下的力学性质, 探讨了压痕法测量SSiC材料硬度、韧性等力学性质的适当压力载荷. 结果表明, SSiC材料压痕裂纹起始的临界压力载荷介于0.1~0.2 N; 当压痕载荷小于0.5 N时, 裂纹尺寸小于5 μm, SSiC材料的平均弯曲强度受影响程度较小. 此外, 当压痕载荷为10 N以上时, 压痕法测得的维氏硬度值趋近定值, 且所得到的裂纹是半圆形裂纹, 因此, 10 N为采用压痕法准确测量SSiC材料硬度及韧性的最低压痕载荷值.     

基于AFM纳米硬度测量系统的实验

为了解决用AFM自身压痕软件进行纳米硬度测量时无法直接获得载荷-压深曲线和由于受到扫描陶管扫描范围的限制而进行多点压痕实验范围有限的问题,建立了三维微动工作台和原子力显微镜相结合的纳米压痕硬度测量系统.基于该系统,对单晶薄膜材料进行了单点压痕实验,得出该系统适合进行纳米硬度测量的结论;并对薄膜材料的纳米硬度和弹性模量进行了分析,讨论了尺寸效应对两者的影响.另外,进行了40×40的点阵压痕实验,得到了材料整个压痕面的三维形貌图和三维硬度图.     

一种钠钙硅酸盐玻璃的纳米压痕测试分析

采用纳米压痕测试技术对一种钠钙硅酸盐玻璃进行微观力学性能的测试分析.测得加载-卸载过程载荷与压入深度曲线,发现被测玻璃的最大压深、残余深度和弹性回复量随最大加载力的增加而增大,但其相对弹性回复率系数基本稳定,平均值为58.2%.通过电子显微镜观察了不同最大载荷下的压痕形貌,发现压痕区域出现了边界沉陷现象.当最大加载力为1 000 mN左右时,三棱锥工具头测试的压痕区域出现了较明显的微裂纹;采用四棱锥工具头时出现微裂纹的最大加载力要小于该值,且裂纹取向均与金刚石工具头的棱角取向一致.利用非线性有限元软件MSC.Marc对纳米压痕过程进行了仿真分析,得到载荷与压入深度的仿真曲线,该曲线与试验结果基本相符;分析了载荷作用下材料内部的应力分布.利用Oliver-Pharr模型得到不同压入深度下被测玻璃的接触刚度值,该值随压入深度的增加而增大.     

纳米压痕法测量残余应力的研究现状

概述了纳米压痕技术测量构件残余应力方面的理论知识,回顾了纳米压痕技术的测量原理,包括硬度、接触面积、接触刚度及弹性模量的计算。将纳米压痕测试计算残余应力的模型分为两大类,并重点对以载荷-位移曲线为依据推导出的残余应力计算模型(如Suresh、Lee、Swadener等模型)的分析过程以及它们在实际应用上的优缺点进行了介绍,同时展望了纳米压痕法测量残余应力未来的发展方向。     

压痕尺寸效应的理论分析

针对微纳米尺度下材料硬度测试中出现的压痕尺寸效应(ISE),指出目前用于解释压痕尺寸效应较为常用理论方法;介绍了应变梯度塑性理论的发展过程,引入了几何必需位错密度的概念,详细地描述了Nix-Gao模型及其修正模型的产生,对于预测硬度随压痕深度的变化趋势提供了很好的预测;介绍了能量平衡方法的形成过程,通过描述Meyer方程、Hays-Kendall方法和比例试样阻力模型,推导出能量平衡方程,为分析试验结果提供了理论模型;通过理论公式推导,分析两种理论分析方法对于压痕尺寸效应分析的一致性.     

定向凝固多晶硅在微纳尺度下的力学性能研究

采用纳米压痕测试系统测试了定向凝固多晶硅沿晶体生长方向横/纵截面的硬度与弹性模量,分析了其受组织各向异性影响的变化规律。使用连续刚度方法借助玻氏压头采集压痕开裂前的硬度与弹性模量,并测量压痕开裂后裂纹尖端到压痕中心点的距离,一次性计算出材料的断裂韧性,避免了开裂对硬度以及弹性模量的影响。结果表明:横截面(110)面的硬度与弹性模量均低于纵截面(111)面,但断裂韧性呈现相反趋势。借助3D原位扫描功能扫描压痕裂纹的三维形貌,发现裂纹主要由剪切滑移台阶所形成。拟合不同载荷下的裂纹长度以及压痕尺寸得出临界压痕尺寸,该值与运用理论推导得出的临界压痕尺寸的结果一致。     

Zero‐Point Correction Method for Nanoindentation Tests to Accurately Quantify Hardness and Indentation Size Effect

Abstract: An original treatment method is proposed to accurately determine by nanoindentation, the macrohardness and the indentation size effect (ISE). This method is applied to stainless steel specimens having different rough surfaces. It uses load versus indentation depth curves and is based on two main original features. The first one concerns the correction of the zero point (i.e. depth equals to 0) to minimise the scattering between experimental curves. The latter are all described by usual hardness equations and are shifted by minimising the distance from a leading curve chosen in a random way among the experimental curves. The second feature is the simultaneous treatment of all the nanoindentation curves to compute the macrohardness and evaluate the ISE. The standard deviation for the estimated macrohardness is small, which indicates the robustness of the approach. It is shown that using a single nanoindentation curve can alter macrohardness estimation because of a bad consideration of the ISE. To prevent this misinterpretation, the curves should be treated simultaneously instead of averaging results of separately treated curves. A correlation is identified between the standard deviations of both surface roughness and correction of zero point, which highlights the effect of surface roughness on the scattering of the indentation curves.     

Indentation size effect of hardness of metallic glasses

It has been found that the hardness measured from different metallic glassy samples using the Oliver and Pharr scheme [Oliver WC, Pharr GM. An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J Mater Res 1992;7:1564–83] [1] shows an apparent indentation size effect (ISE), i.e., the hardness decreases as indentation depth increases. A similar ISE of the pile-up ratio has also been found. A ribbon glassy sample fabricated at a larger cooling rate shows larger pile-up and lower hardness value than a bulk glassy sample under the same conditions. The ISE of hardness can be effectively eliminated by taking into account the different pile-up ratios at different indentation depths.     

Indentation toughness of ceramics: A modified approach

The indentation toughness equation proposed by Anstis et al. was re-examined with a particular emphasis on the definition of the hardness parameter used. It was shown that, because of the existence of the well-known indentation size effect (ISE), the apparent hardness defined as the ratio of the applied load to the projected area of the resultant indentation usually varies with the applied load and seems not to be suitable for use in indentation toughness determination. A new equation for determining indentation toughness, in which a load-independent hardness number was incorporated, was proposed.     

Determination of dislocation density from hardness measurements in metals

For the first time the Nix-Gao model for indentation size effect (ISE) is used to estimate the dislocation density in a metal. The estimate of dislocation density obtained by this method, using Ni as a case study, is compared with the values obtained from direct observation by transmission electron microscopy. It is shown that the estimate of dislocation density from indentation hardness measurements, adjusted by the Nix-Gao model, gives values consistent with those obtained by TEM, provided that the proper procedures to minimize errors are adopted. Although the direct observation of dislocations by TEM gives additional structural information, the indirect method to estimate dislocation density based on hardness measurements is more efficient, since the sample preparation method, measurement procedure and analysis of results are easier and faster.     

The effect of work-hardening and pile-up on nanoindentation measurements

Nanoindentation is performed on the cross-section of copper samples subjected to surface mechanical attrition treatment (SMAT). The cross-section of the SMAT samples provides a unique microstructure with varying amounts of work-hardening depending on the distance from the SMAT surface. Results show that for a given indentation load the pile-up height decreases and the indentation depth increases as the distance from the SMAT surface increases, both following a power law relationship. Based on image analysis of the indented surface this increase in the pile-up height and decrease in indentation depth is attributed to the localization of plastic strain due to the increased resistance to dislocation motion in the work-hardened region. For a given amount of work-hardening (in terms of distance from SMAT surface), the indentation depth increased with the indentation load obeying a power law relationship with the exponent ranging from 0.58 to 0.68. However, the pile-up height increased linearly with the load, with the rate (slope) increasing with the amount of work-hardening. The observed linear increase in pile-up height with indentation load would naturally introduce an indentation size effect (ISE) if the hardness is corrected for the pile-up. Interestingly, this ISE associated with pile-up increased with an increase in indentation depth, in contradiction to the ISE associated with strain gradient. Deviation of the hardness values corrected for pile-up from the bulk behavior due to surface effect is highlighted and a method to obtain a bulk-equivalent hardness quantity representing the bulk behavior is proposed.     

Determination of local stress–strain properties of resistance spot-welded joints of advanced high-strength steels using the instrumented indentation test

For spot-welded joints, the resistance to mechanical stress depends on the local strength properties and gradients in the weld area. The commonly used methods for investigating the stress–strain behaviour across the weld area are connected with a high level of sample preparation and with considerable limitations in local resolution. A promising method for determining locally resolved stress–strain curves is the instrumented indentation test in connection with the method of representative stress and strain (RS) and the method of artificial neural networks (NNs). The stress–strain properties of the weld nugget and the base metal determined by these two methods are compared and discussed, additionally in relation to the stress–strain curves obtained from the tensile test. The measured Vickers hardness across the weld area is compared with the evaluated local stress–strain properties. Three steels used in automobile manufacturing are investigated: mild steel DC04 and two advanced high-strength steels (TRIP steel HCT690T and martensitic steel HDT 1200M). The results of the two methods (RS and NN) show good correspondence for the base metal area but some significant differences for the weld nugget. Comparing the data across the weld area, no evidence of the presence of residual stress (which would influence the results) was found.     

The influence of the composition on (the load-dependence of) the microhardness of Y–;Si–;Al–;O–;N glasses as measured by Vickers indentation

The hardness of multiple glasses in the Y–;Si–;Al–;O–;N system has been determined as a function of the indentation load. The measured hardness significantly depends on the load, which implies a substantial influence of the indentation size effect (ISE). The measured hardness has been deconvoluted in a load-dependent part and a load-independent hardness using the method of Bull et al. The influence of the overall composition on the hardness of these glasses has been investigated. It is shown that, by increasing the nitrogen content, a load-independent hardness of over 9 GPa can be achieved, which is far higher than most common glass systems.     

试样倾斜对熔融石英硅三棱锥纳米压痕测试的影响

使用三棱锥压头对不同倾斜角下的熔融石英硅进行纳米压痕实验。结果表明,试样倾斜会影响加载曲线的形状。在相同的载荷下,随着试样倾斜角的增加,压痕最大深度、残余深度及接触深度逐渐减小,但卸载曲线不受影响,彼此保持平行,卸载曲线的拟合参数m及接触刚度值保持恒定。另外,试样倾斜将导致测量的压痕接触面积偏小,从而使得测量的硬度和弹性模量偏大。