压痕/划痕测试若干理论与基于自制仪器的试验研究
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摘要
材料及其制品的失效源于微小变形损伤和缺陷，近年来针对材料微纳米力学行为的研究受到国内外学者的广泛关注。微纳米压痕/划痕测试由于具有高的载荷和位移分辨率，逐渐发展成为材料微纳米力学性能测试的主流技术，在材料科学、半导体技术、薄膜、生物力学、生物医学工程等领域展现出重要的科学意义和广泛的应用前景。目前，美国、瑞士、英国等国掌握了该项技术，且有商业化的压痕/划痕测试仪器产品，而我国在压痕/划痕测试技术方面起步较晚，尚无自主生产的商业化压痕仪。
一方面，进口国外的压痕/划痕测试仪存在价格昂贵、耗时长、高端技术禁运等问题，另一方面，由于我国未掌握压痕/划痕测试的核心技术，完全依赖于国外的测试仪器，无法对其进行功能扩展，使得国内相关研究一直处于跟踪国外的状态，严重制约了研究的深入。因此，研究压痕/划痕测试的核心技术，研制具有我国自主知识产权的压痕/划痕测试仪具有重要意义。同时，在压痕/划痕测试仪器校准、误差校正等理论方面，还有待深入研究。
本文针对国内外在压痕/划痕测试技术与仪器方面的现存不足，开展压痕/划痕测试理论、仪器设计、制造、装配、检测控制、调试、校准等基础理论与技术的研究，研制了具有自主知识产权的离位和原位压痕/划痕测试仪器。在此基础上，借助自制的仪器开展了典型应用研究。论文主要内容如下：
(1)分析了纳米压痕测试经典数据分析方法—Oliver&Pharr方法。在此基础上，对影响压痕测试结果但目前尚未详细讨论的三个因素—“残余压入深度的确定”、“试件表面处理方法”和“压头与试件之间的倾斜”着重进行了分析。针对压痕测试曲线卸载部分不完整或出现明显拐点的情况，提出了一种利用卸载阶段局部曲线拟合确定残余压入深度hf的方法。通过对比试验，研究了不同试件表面处理方法—机械抛光和横切对非晶合金压痕过程中锯齿流变和蠕变行为的影响规律。提出了两种定量评价压头与试件之间倾斜状态的方法，即残余压痕形貌测量法和三点测量法，并通过试验手段验证了这两种方法的有效性。
(2)开展了离位压痕/划痕测试仪器的设计分析与试验研究，研究了其中涉及的结构设计分析、布局优化、动态模型建立、控制系统搭建、校准与性能测试等理论与技术问题，成功研制了离位压痕/划痕测试仪器。提出了一种新的压痕测试仪器机架柔度测试方法，利用该方法测得压痕测试模块的机架柔度为0.425nm/mN，熔融石英标准样品压痕试验结果验证了该方法的可行性。对压痕测试模块进行了性能测试，试验结果表明：在有隔振台、无恒温措施的实验环境下，压痕测试模块的载荷分辨率优于10μN，噪声小于30μN，位移分辨率为1nm，噪声约2nm。熔融石英标准样品重复压痕试验结果表明，压痕测试模块具有很好的重复性和良好的测试精度。利用工字型弹性体和八片应变片，设计了可对划痕测试中横向力和轴向力进行同步测量的力传感器，提出了横向力与轴向力耦合/解耦算法，并开展了标定试验和解耦分析。
(3)利用自制的离位压痕/划痕测试仪器，针对单晶硅和非晶合金等材料开展了典型应用。利用压痕测试模块，研究了单晶硅压痕卸载突退现象的统计性规律。利用研制的拉应力加载模块，开展了预拉应力下单晶硅压痕响应试验。利用玻氏压头和立方角压头开展非晶合金压痕响应的对比试验，研究了非晶合金粘附、锯齿流变、剪切带分布等现象的压头几何尺寸效应。利用划痕测试模块，开展了非晶合金的划痕力学行为研究，分析了划痕测试过程中横向力和摩擦系数波动的可能原因，并发现了维氏压头非对称划入导致非晶合金残余划痕左右边界出现不一致变形的现象。
(4)采用步进电机与压电叠堆混合驱动方式，设计研制了结构紧凑的原位压痕测试仪器，并就其输出特性、闭环控制、校准等开展了试验研究。针对磷化铟晶片和非晶合金的原位压痕试验表明，研制的原位压痕测试仪器与扫描电子显微镜具有良好的兼容性，可在其真空腔内开展材料微观力学性能的原位压痕测试。
(5)基于弹性体变形产生的寄生运动，提出了一种压电驱动新原理，即寄生运动原理。基于该原理设计研制了大行程划痕运动组件，对其运动过程和输出特性进行了理论分析与试验研究。在自制的原位压痕测试仪器基础上，集成该大行程划痕运动组件，研制了可与扫描电子显微镜兼容的原位压痕/划痕测试仪器，并利用该仪器开展了压头与试件表面间的摩擦和切屑堆积条件下的材料去除机理等研究。
Failure of materials and related products is resulted from micro deformation, damageand defect. In recent years, research on mechanical properties of materials in micro/nanoscales is given increasing attention. With high load and displacement resolutions,micro/nano indentation and scratch testing has been a commonly used method to evaluatemechanical properties of materials in micro/nano scales, expressing important scientificsignificance and broad application prospects in fields of materials science, semiconductors,thin films, biomechanics, biomedical engineering and so on. Up to now, America, Swiss,UK, etc. have mastered this technology and there are commercial indentation and scratchinstruments in these countries. However, research on indentation and scratch testingtechnology in China begins relatively late, and there is no commercial home-grownindentation and scratch instrument.
On the one hand, there are many problems by importing indentation and scratchinstruments from abroad such as high cost, time-consuming, high-end technology embargo,and so on. On the other hand, because we don’t master the key technologies of indentationand scratch testing and completely rely on foreign testing instruments, functions of thecommercial instruments can not be extended according to requirements, which makesrelated research work in China be always in the state of follow-up study and restrictsresearch progress seriously. So, it has important significance to study the key technologiesof indentation and scratch testing and develop indentation and scratch instruments withour own intellectual property rights. Meanwhile, some theoretical problems such ascalibration and error correction of indentation and scratch instruments are still needed tobe further investigated.
Aimed at the current deficiencies in indentation and scratch testing technologies andinstruments at home and abroad, basic theories and technologies of indentation and scratchtesting such as testing theory, structure design, fabrication, assembling, measuring andcontrol, debugging, calibration and so on, are studied in this paper. Ex situ and in situ indentation and scratch instruments with our own intellectual property rights aredeveloped, by which typical applications are carried out. The main contents are listed asfollows:
(1) The classical data analysis method—Oliver&Pharr method is discussed firstly, andthen emphasis is put on three factors, determination of the residual indentation depth, thesample preparation method and the tilt between the indenter and the sample surface, whichaffect indentation testing results but are not studied in detail up to now. For the case thatunloading curves are incomplete or there are obvious elbow phenomena, a method byfitting partial unloading curves to determine residual indentation depth hfis proposed.Influences of two different sample preparation methods, mechanical polishing and plungecutting, on the serrated flow and creep behaviors of a bulk metallic glass duringindentation testing are studied by comparison tests. Two methods, the residual indentationmorphology measuring method and the three-point measuring method, are presented toquantificationally evaluate the tilt between the indenter and sample surface. Byexperiments, feasibility of these two methods are verified respectively.
(2) Design, analysis and experimental investigation of an ex situ indentation andscratch testing system are carried out. Related theoretical and technological issues, such asstructure design and analysis, layout optimization, dynamic modelling, control system setup, calibration, performance testing, and so on, are addressed. After that, an ex situindentation and scratch testing system is developed successfully. A new method isproposed to measure compliance of indentation instruments, by which instrumentcompliance of the indentation testing module is obtained, and it is0.425nm/mN.Indentation testing results of the standard sample—fused quartz verify the feasibility ofthe proposed method. Performances of the indentation testing module are tested byexperiments, and results indicate that for the general experimental environment withvibration isolation platform but without constant temperature treatment, the loadresolution of the indentation testing module is higher than10μN and the noise floor is lessthan30μN. The displacement resolution is1nm and the noise floor is about2nm.Nanoindentation testing results of the standard sample—fused quartz indicate that theindentation testing module has good repeatability and testing accuracy. A two-axis loadsensor is designed by integrating an I-shaped structure and eight strain gauges, which canbe used to measure the lateral load and the normal load simultaneously. A decoupling algorithm is presented to obtain the lateral load and the normal load. Calibrationexperiments and decoupling analysis are carried out to obtain the correspondingdecoupling parameters.
(3) Applications of the self-made ex situ indentation and scratch testing system insingle crystal silicon and the bulk metallic glass are carried out. Via the indentation testingmodule, statistical laws of indentation-induced pop-out in unloading curves of singlecrystal silicon are studied. Indentation response of single crystal silicon under tensionstress is revealed by a self-made tension stress loading unit. Indentation comparison testsare carried out by the Berkovich indenter and the cube-corner indenter respectively tostudy indenter dependent indentation behaviors of the bulk metallic glass, such asadhesion, serrated flows, shear bands, and so on. Mechanical behaviors of the bulkmetallic glass are analyzed via the scratch testing module. Possible reasons leading tofluctuations of the lateral load and the friction coefficient during the scratch testing arediscussed. The phenomenon that unsymmetric scratch induces unsymmetric deformationof the bulk metallic glass around borders of the residual scratch is observed.
(4) By combination of the stepper motor and the piezoelectric stack, an in situindentation instrument is developed. Output performances, closed-loop control, calibrationof the instrument are studied by experiments. In situ indentation experiments of the InP(Indium phosphide, InP) wafer and the bulk metallic glass indicate that the developed insitu indentation instrument has good compatibility with the scanning electron microscope,and it can be used to carry out in situ indentation tests of materials inside the vacuumchamber of the scanning electron microscope.
(5) A novel piezo-driving principle is proposed by means of the parasitic motion of theelastic body. Based on this principle, a scratch module with the large motion range isdeveloped using two piezoelectric stacks. Driving processes and output performences ofthe scratch module are investigated via theoretical analysis and experiments. Based on theprevious in situ indentation instrument, an in situ indentation and scratch instrument isdeveloped by integrating the designed scratch module, which is compatible with thescanning electron microscope. Friction between the indenter and the sample surface aswell as material removal mechanism especially when lots of chips are accumulated on therake face of the indenter is studied.
一方面，进口国外的压痕/划痕测试仪存在价格昂贵、耗时长、高端技术禁运等问题，另一方面，由于我国未掌握压痕/划痕测试的核心技术，完全依赖于国外的测试仪器，无法对其进行功能扩展，使得国内相关研究一直处于跟踪国外的状态，严重制约了研究的深入。因此，研究压痕/划痕测试的核心技术，研制具有我国自主知识产权的压痕/划痕测试仪具有重要意义。同时，在压痕/划痕测试仪器校准、误差校正等理论方面，还有待深入研究。
本文针对国内外在压痕/划痕测试技术与仪器方面的现存不足，开展压痕/划痕测试理论、仪器设计、制造、装配、检测控制、调试、校准等基础理论与技术的研究，研制了具有自主知识产权的离位和原位压痕/划痕测试仪器。在此基础上，借助自制的仪器开展了典型应用研究。论文主要内容如下：
(1)分析了纳米压痕测试经典数据分析方法—Oliver&Pharr方法。在此基础上，对影响压痕测试结果但目前尚未详细讨论的三个因素—“残余压入深度的确定”、“试件表面处理方法”和“压头与试件之间的倾斜”着重进行了分析。针对压痕测试曲线卸载部分不完整或出现明显拐点的情况，提出了一种利用卸载阶段局部曲线拟合确定残余压入深度hf的方法。通过对比试验，研究了不同试件表面处理方法—机械抛光和横切对非晶合金压痕过程中锯齿流变和蠕变行为的影响规律。提出了两种定量评价压头与试件之间倾斜状态的方法，即残余压痕形貌测量法和三点测量法，并通过试验手段验证了这两种方法的有效性。
(2)开展了离位压痕/划痕测试仪器的设计分析与试验研究，研究了其中涉及的结构设计分析、布局优化、动态模型建立、控制系统搭建、校准与性能测试等理论与技术问题，成功研制了离位压痕/划痕测试仪器。提出了一种新的压痕测试仪器机架柔度测试方法，利用该方法测得压痕测试模块的机架柔度为0.425nm/mN，熔融石英标准样品压痕试验结果验证了该方法的可行性。对压痕测试模块进行了性能测试，试验结果表明：在有隔振台、无恒温措施的实验环境下，压痕测试模块的载荷分辨率优于10μN，噪声小于30μN，位移分辨率为1nm，噪声约2nm。熔融石英标准样品重复压痕试验结果表明，压痕测试模块具有很好的重复性和良好的测试精度。利用工字型弹性体和八片应变片，设计了可对划痕测试中横向力和轴向力进行同步测量的力传感器，提出了横向力与轴向力耦合/解耦算法，并开展了标定试验和解耦分析。
(3)利用自制的离位压痕/划痕测试仪器，针对单晶硅和非晶合金等材料开展了典型应用。利用压痕测试模块，研究了单晶硅压痕卸载突退现象的统计性规律。利用研制的拉应力加载模块，开展了预拉应力下单晶硅压痕响应试验。利用玻氏压头和立方角压头开展非晶合金压痕响应的对比试验，研究了非晶合金粘附、锯齿流变、剪切带分布等现象的压头几何尺寸效应。利用划痕测试模块，开展了非晶合金的划痕力学行为研究，分析了划痕测试过程中横向力和摩擦系数波动的可能原因，并发现了维氏压头非对称划入导致非晶合金残余划痕左右边界出现不一致变形的现象。
(4)采用步进电机与压电叠堆混合驱动方式，设计研制了结构紧凑的原位压痕测试仪器，并就其输出特性、闭环控制、校准等开展了试验研究。针对磷化铟晶片和非晶合金的原位压痕试验表明，研制的原位压痕测试仪器与扫描电子显微镜具有良好的兼容性，可在其真空腔内开展材料微观力学性能的原位压痕测试。
(5)基于弹性体变形产生的寄生运动，提出了一种压电驱动新原理，即寄生运动原理。基于该原理设计研制了大行程划痕运动组件，对其运动过程和输出特性进行了理论分析与试验研究。在自制的原位压痕测试仪器基础上，集成该大行程划痕运动组件，研制了可与扫描电子显微镜兼容的原位压痕/划痕测试仪器，并利用该仪器开展了压头与试件表面间的摩擦和切屑堆积条件下的材料去除机理等研究。
Failure of materials and related products is resulted from micro deformation, damageand defect. In recent years, research on mechanical properties of materials in micro/nanoscales is given increasing attention. With high load and displacement resolutions,micro/nano indentation and scratch testing has been a commonly used method to evaluatemechanical properties of materials in micro/nano scales, expressing important scientificsignificance and broad application prospects in fields of materials science, semiconductors,thin films, biomechanics, biomedical engineering and so on. Up to now, America, Swiss,UK, etc. have mastered this technology and there are commercial indentation and scratchinstruments in these countries. However, research on indentation and scratch testingtechnology in China begins relatively late, and there is no commercial home-grownindentation and scratch instrument.
On the one hand, there are many problems by importing indentation and scratchinstruments from abroad such as high cost, time-consuming, high-end technology embargo,and so on. On the other hand, because we don’t master the key technologies of indentationand scratch testing and completely rely on foreign testing instruments, functions of thecommercial instruments can not be extended according to requirements, which makesrelated research work in China be always in the state of follow-up study and restrictsresearch progress seriously. So, it has important significance to study the key technologiesof indentation and scratch testing and develop indentation and scratch instruments withour own intellectual property rights. Meanwhile, some theoretical problems such ascalibration and error correction of indentation and scratch instruments are still needed tobe further investigated.
Aimed at the current deficiencies in indentation and scratch testing technologies andinstruments at home and abroad, basic theories and technologies of indentation and scratchtesting such as testing theory, structure design, fabrication, assembling, measuring andcontrol, debugging, calibration and so on, are studied in this paper. Ex situ and in situ indentation and scratch instruments with our own intellectual property rights aredeveloped, by which typical applications are carried out. The main contents are listed asfollows:
(1) The classical data analysis method—Oliver&Pharr method is discussed firstly, andthen emphasis is put on three factors, determination of the residual indentation depth, thesample preparation method and the tilt between the indenter and the sample surface, whichaffect indentation testing results but are not studied in detail up to now. For the case thatunloading curves are incomplete or there are obvious elbow phenomena, a method byfitting partial unloading curves to determine residual indentation depth hfis proposed.Influences of two different sample preparation methods, mechanical polishing and plungecutting, on the serrated flow and creep behaviors of a bulk metallic glass duringindentation testing are studied by comparison tests. Two methods, the residual indentationmorphology measuring method and the three-point measuring method, are presented toquantificationally evaluate the tilt between the indenter and sample surface. Byexperiments, feasibility of these two methods are verified respectively.
(2) Design, analysis and experimental investigation of an ex situ indentation andscratch testing system are carried out. Related theoretical and technological issues, such asstructure design and analysis, layout optimization, dynamic modelling, control system setup, calibration, performance testing, and so on, are addressed. After that, an ex situindentation and scratch testing system is developed successfully. A new method isproposed to measure compliance of indentation instruments, by which instrumentcompliance of the indentation testing module is obtained, and it is0.425nm/mN.Indentation testing results of the standard sample—fused quartz verify the feasibility ofthe proposed method. Performances of the indentation testing module are tested byexperiments, and results indicate that for the general experimental environment withvibration isolation platform but without constant temperature treatment, the loadresolution of the indentation testing module is higher than10μN and the noise floor is lessthan30μN. The displacement resolution is1nm and the noise floor is about2nm.Nanoindentation testing results of the standard sample—fused quartz indicate that theindentation testing module has good repeatability and testing accuracy. A two-axis loadsensor is designed by integrating an I-shaped structure and eight strain gauges, which canbe used to measure the lateral load and the normal load simultaneously. A decoupling algorithm is presented to obtain the lateral load and the normal load. Calibrationexperiments and decoupling analysis are carried out to obtain the correspondingdecoupling parameters.
(3) Applications of the self-made ex situ indentation and scratch testing system insingle crystal silicon and the bulk metallic glass are carried out. Via the indentation testingmodule, statistical laws of indentation-induced pop-out in unloading curves of singlecrystal silicon are studied. Indentation response of single crystal silicon under tensionstress is revealed by a self-made tension stress loading unit. Indentation comparison testsare carried out by the Berkovich indenter and the cube-corner indenter respectively tostudy indenter dependent indentation behaviors of the bulk metallic glass, such asadhesion, serrated flows, shear bands, and so on. Mechanical behaviors of the bulkmetallic glass are analyzed via the scratch testing module. Possible reasons leading tofluctuations of the lateral load and the friction coefficient during the scratch testing arediscussed. The phenomenon that unsymmetric scratch induces unsymmetric deformationof the bulk metallic glass around borders of the residual scratch is observed.
(4) By combination of the stepper motor and the piezoelectric stack, an in situindentation instrument is developed. Output performances, closed-loop control, calibrationof the instrument are studied by experiments. In situ indentation experiments of the InP(Indium phosphide, InP) wafer and the bulk metallic glass indicate that the developed insitu indentation instrument has good compatibility with the scanning electron microscope,and it can be used to carry out in situ indentation tests of materials inside the vacuumchamber of the scanning electron microscope.
(5) A novel piezo-driving principle is proposed by means of the parasitic motion of theelastic body. Based on this principle, a scratch module with the large motion range isdeveloped using two piezoelectric stacks. Driving processes and output performences ofthe scratch module are investigated via theoretical analysis and experiments. Based on theprevious in situ indentation instrument, an in situ indentation and scratch instrument isdeveloped by integrating the designed scratch module, which is compatible with thescanning electron microscope. Friction between the indenter and the sample surface aswell as material removal mechanism especially when lots of chips are accumulated on therake face of the indenter is studied.
引文
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