Nano-Hardness Tester and its Application in MEMS

微机电系统(MEMS)技术的迅速崛起,推动了对其所用材料和结构的力学性能研究。简要介绍纳米硬度技术的发展展、理论模型和MTS公司的Nano Indenter XP系统的配置、测量原理及功能。并根据我们的一些研究结果,说明它在微机电系统中的应用。

电磁式纳米压入仪的载荷精度研究

纳米压入仪(Nanoindenter)已成为纳米/微米力学测试的基本工具之一,广泛应用于纳米材料、薄膜、MEMS微结构的力学性能测试。目前商业化仪器有MTS NanoIndenter(incorporated into Agi lent in 2008),Hysitron TriboIndenter,CSM NanoHardness Tester,MML NanoTest,and CSIRO UMIS,其中原MTS Nano Indenter、CSMNano Hardness Tester和MML NanoTest都采用电磁驱动兼载荷计量的原理设计。这类仪器主要优点之一是载荷分辨力高,可以达到50nN甚至更小。然而仪器制造商从未明确给出此类仪器的载荷精度。目前对纳米压痕测试技术的研究也主要集中在压头形状、试样表面粗糙度、毛细力等因素对压痕测试结果的影响,尚未见针对仪器载荷精度的研究报道。国际标准ISO 14577-2:2002虽对仪器施加的试验力的允差进行了规定,但由于电磁式纳米压入仪的结构响应和试样力学行为耦合在一起,试样上的载荷并不完全等同于通过电磁转换原理计量的试验力,因此实际测试时试样上的载荷精度仍是未知。

计算机控制的亚微米硬度计及其应用

本文描述了一台有微机控制的可变温亚微米深度灵敏的硬度计及其应用实例。该硬度计的负荷范围从0.01N到2N负荷测量精度为1mN。为该硬度计配备了各种角度的四棱锥型，三棱锥型和Knoop型金刚压头用来得到各种不同的深度面积比。利用该硬度计研究了测量中的压痕尺寸效应（ISE）马氏体不锈钢辐照和He注入后的硬化脆化效应，连接奥氏体不锈钢焊接材料和碳--金属焊接材料的辐照效应。同时，还研究了在稳定负荷下硬度与加压时间的关系（压痕蠕变）和在循环负荷下硬度与循环次数的关系（压痕疲劳）

Nano-hardness Techniques and Its Applications in Mechanical Property Measurements for Surface Engineering

结合纳米硬度技术测量各类薄膜和块体材料表层的纳米压痕硬度、弹性模量、断裂韧性、膜厚、微结构的弯曲变形,采用纳米划痕硬度技术测量各类薄膜和块体材料的粗糙度、临界附着力、摩擦系数、划痕横剖面.纳米硬度计是检测材料表层微米乃至几十纳米力学性能的先进仪器,可广泛应用于表面工程中的质量检测.

Evaluation of the Effectiveness of Representative Methods for Determining Young's Modulus and Hardness from Instrumented Indentation Data

The effectiveness of Oliver & Pharr's (O&P's) method, Cheng & Cheng's (C&C's) method, and a new method developed by our group for estimating Young's modulus and hardness based on instrumented indentation was evaluated for the case of yield stress to reduced Young's modulus ratio (sigma(y)/E-r) >= 4.55 x 10(-4) and hardening coefficient (n) <= 0.45. Dimensional theorem and finite element simulations were applied to produce reference results for this purpose. Both O&P's and C&C's methods overestimated the Young's modulus under some conditions, whereas the error can be controlled within +/- 16% if the formulation was modified with appropriate correction functions. Similar modification was not introduced to our method for determining Young's modulus, while the maximum error of results was around +/- 13%. The errors of hardness values obtained from all the three methods could be even larger and were irreducible with any correction scheme. It is therefore suggested that when hardness values of different materials are concerned, relative comparison of the data obtained from a single standard measurement technique would be more practically useful. It is noted that the ranges of error derived from the analysis could be different if different ranges of material parameters sigma(y)/E-r and n are considered.

Relationships between hardness, elastic modulus, and the work of indentation

The work done during indentation is examined using dimensional analysis and finite element calculations for conical indentation in elastic-plastic solids with work hardening. An approximate relationship between the ratio of hardness to elastic modulus and the ratio of irreversible work to total work in indentation is found. Consequently, the ratio of hardness to elastic modulus may be obtained directly from measuring the work of indentation. Together with a well-known relationship between elastic modulus, initial unloading slope, and contact area, a new method is then suggested for estimating the hardness and modulus of solids using instrumented indentation with conical or pyramidal indenters.

What is indentation hardness?

Using dimensional analysis and finite element calculations, we derive simple scaling relationships for loading and unloading curve, contact depth, and hardness. The relationship between hardness and the basic mechanical properties of solids, such as Young's modulus, initial yield strength, and work-hardening exponent, is then obtained. The conditions for 'piling-up' and 'sinking-in' of surface profiles during indentation are determined. A method for estimating contact depth from initial unloading slope is examined. The work done during indentation is also studied. A relationship between the ratio of hardness to elastic modulus and the ratio of irreversible work to total work is discovered. This relationship offers a new method for obtaining hardness and elastic modulus. Finally, a scaling theory for indentation in power-law creep solids using self-similar indenters is developed. A connection between creep and 'indentation size effect' is established.

Revelation of a Functional Dependence of the Sum of Two Uniaxial Strengths/Hardness on Elastic Work/Total Work of Indentation

Dimensional and finite element analyses were used to analyze the relationship between the mechanical properties and instrumented indentation response of materials. Results revealed the existence of a functional dependence of (engineering yield strength sigma(E,y) + engineering tensile strength sigma(E,b))/Oliver & Pharr hardness on the ratio of reversible elastic work to total work obtained from an indentation test. The relationship links up the Oliver & Pharr hardness with the material strengths, although the Oliver & Pharr hardness may deviate from the true hardness when sinking in or piling up occurs. The functional relationship can further be used to estimate the SUM sigma(E,y) + sigma(E,b) according to the data of an instrumented indentation test. The sigma(E,y) + sigma(E,b) value better reflects the strength of a material compared to the hardness value alone. The method was shown to be effective when applied to aluminum alloys. The relationship can further be used to estimate the fatigue limits, which are usually obtained from macroscopic fatigue tests in different modes.

The mechanical properties of an aluminum alloy by plasma-based ion implantation and solution-aging treatment

The age-strengthening 2024 aluminum alloy was modified by a combination of plasma-based ion implantation (PBII) and solution-aging treatments. The depth profiles of the implanted layer were investigated by X-ray photoelectron spectroscopy (XPS). The structure was studied by glancing angle X-ray diffraction (GXRD). The variation of microhardness with the indenting depth was measured by a nanoindenter. The wear test was carried on with a pin-on-disk wear tester. The results revealed that when the aluminum alloys were implanted with nitrogen at the solution temperature, then quenched in the vacuum chamber followed by an artificial aging treatment for an appropriate time, the amount of AIN precipitates by the combined treatment were more than that of the specimen implanted at ambient temperature. Optimum surface mechanical properties were obtained. The surface hardness was increased and the weight loss in a wear test decreased too.

Influence of Indenter Tip Roundness on Hardness Behavior in Nanoindentation

In this paper. the effect of indenter tip roundness on hardness behavior for two typical elastic perfectly plastic materials is studied by means of finite element simulation. A rigid conical indenter of semi apex angle 70.3 degrees fitted smoothly with a spherical tip is employed. It is shown that as the indentation depth increases hardness first rises from zero, reaches a maximum and then decreases slowly approaching asymptotically the limiting value equal to that due to a conical indenter of ideally sharp tip. The range within which hardness varies appreciably is comparable to the radius of the indenter tip. The difference between the maximum value and the limiting value depends on the yield stress over the Young's modulus ratio. The smaller this ratio the greater the difference is. Numerical simulation also provides an opportunity for checking the accuracy and limitations of the widely used Oliver-Pharr method.

(Ti,Al)N Film On Normalized T8 Carbon Tool Steel Prepared By Pulsed High Energy Density Plasma Technique

Under optimized operating parameters, a hard and wear resistant ( Ti,Al)N film is prepared on a normalized T8 carbon tool steel substrate by using pulsed high energy density plasma technique. Microstructure and composition of the film are analysed by x-ray diffraction, x-ray photoelectron spectroscopy, Auger electron spectroscopy and scanning electron microscopy. Hardness profile and tribological properties of the film are tested with nano-indenter and ring-on-ring wear tester, respectively. The tested results show that the microstructure of the film is dense and uniform and is mainly composed of ( Ti,Al)N and AlN hard phases. A wide transition interface exists between the film and the normalized T8 carbon tool steel substrate. Thickness of the film is about 1000 nm and mean hardness value of the film is about 26GPa. Under dry sliding wear test conditions, relative wear resistance of the ( Ti,Al)N film is approximately 9 times higher than that of the hardened T8 carbon tool steel reference sample. Meanwhile, the ( Ti,Al)N film has low and stable friction coefficient compared with the hardened T8 carbon tool steel reference sample.

Experimental Verification And Theoretical Analysis Of The Relationships Between Hardness, Elastic Modulus, And The Work Of Indentation

The relationship between hardness (H), reduced modulus (E-r), unloading work (W-u), and total work (W-t) of indentation is examined in detail experimentally and theoretically. Experimental study verifies the approximate linear relationship. Theoretical analysis confirms it. Furthermore, the solutions to the conical indentation in elastic-perfectly plastic solid, including elastic work (W-e), H, W-t, and W-u are obtained using Johnson's expanding cavity model and Lame solution. Consequently, it is found that the W-e should be distinguished from W-u, rather than their equivalence as suggested in ISO14577, and (H/E-r)/(W-u/W-t) depends mainly on the conical angle, which are also verified with numerical simulations. (C) 2008 American Institute of Physics.

Nanoindentation of thin-film-substrate system: Determination of film hardness and Young's modulus

In the present paper, the hardness and Young's modulus of film-substrate systems are determined by means of nanoindentation experiments and modified models. Aluminum film and two kinds of substrates; i.e. glass and silicon, are studied. Nanoindentation XP II and continuous stiffness mode are used during the experiments. In order to avoid the influence of the Oliver and Pharr method used in the experiments, the experiment data are analyzed with the constant Young's modulus assumption and the equal hardness assumption. The volume fraction model (CZ model) proposed by Fabes et al. (1992) is used and modified to analyze the measured hardness. The method proposed by Doerner and Nix (DN formula) (1986) is modified to analyze the measured Young's modulus. Two kinds of modified empirical formula are used to predict the present experiment results and those in the literature, which include the results of two kinds of systems, i.e., a soft film on a hard substrate and a hard film on a soft substrate. In the modified CZ model, the indentation influence angle, phi, is considered as a relevant physical parameter, which embodies the effects of the indenter tip radius, pile-up or sink-in phenomena and deformation of film and substrate.

Characteristics of the interface of a laser-quenched steel substrate and chromium electroplate

The interface of a laser-discrete-quenched steel substrate and as-deposited chromium electroplate was investigated by ion beam etching, dissolving-substrate-away and using a Vickers microhardness tester, in an attempt to reveal the mechanism that the service life of the chromium-coated parts is increased by the duplex technique of laser pre-quenching plus chromium post-depositing. The laser quenching of the steel substrate can reduce the steep hardness gradient at the substrate/chromium interface and improve the load-bearing capacity of chromium electroplate. Moreover, the laser quenching prior to plating has an extremely great effect on the morphologies and microstructure of the substrate/chromium interface: there is a transient interlayer at the original substrate/chromium interface while there is not at the laser-quenchedzone/chromium interface; the near-substrate surface microstructure and morphologies of the free-standing chromium electrodeposits, whose substrate was dissolved away with nital 30% in volume, inherit the periodically gradient characteristics of the laser-discrete-quenched substrate surface. (c) 2006 Elsevier B.V. All rights reserved.