摘要
随着环境污染、能源危机与资源短缺等问题的日益突出,世界各国越来越高度重视高效、清洁、可再生能源以及电动汽车、电动自行车、便携式电动工具等相关技术的发展。目前,电动交通工具用的动力电源主要为铅酸电池和镍氢电池。现在人们已认识到铅的毒害问题,铅酸电池的使用开始受到限制;而镍氢电池的能量密度不能满足快速发展的市场需求。因此,人们必须重新选择与开发新型能源存储器件。
新兴的绿色动力型储能器件已成为全球高科技产业关注的热点,动力电源作为新型绿色能源受到国内外的广泛关注。动力电源的外壳材料是动力电源的关键组成部分之一,其性能的好坏直接决定着动力电源性能的优劣。由本课题组提出并长期研究的镀镍钢带是一种将电沉积镍薄膜与低碳钢基底紧密结合、具有较好同步延伸率和耐腐蚀性能的新型预镀镍动力电源外壳材料。但是,随着镀镍钢带的产业化进程,许多基础问题也不断呈现出来,这是平时的经验所不能解决的,而基础理论又比较薄弱,鉴于这些因素,给生产过程增加了成本和风险。为了解决这些问题,必须从基础理论入手,找到这些生产过程中出现的问题的本质。有关这些重要问题始终没有得到解决,其主要原因有两个:(1)薄膜的尺度本身比较小,不易操作,而且冲压成型过程中的变形非常复杂,建立相关理论比较复杂;(2)小尺度下的力学性能受多种因素的影响,比如尺度效应、基底效应等,如何正确剔除这些影响因素,得到真实薄膜材料的力学性能是非常困难的。
基于以上原因,本文旨在通过反推法研究金属薄膜材料的力学性能,取得的主要创新性研究结果如下:
1、用纳米压痕法研究了金属薄膜材料的应力应变关系,在这一过程中主要考虑了三个方面的问题:①针对反推过程中出现的硬度、弹性模量和屈服强度等出现的尺度效应问题进行了研究;②通过引入塑性区半径成功解决了唯一性问题;③为了得到可靠的压痕实验数据对压痕过程中出现的蠕变问题进行了系统研究。具体结果主要有以下五个部分:
(1)通过Π定理对纳米压痕问题进行了量纲分析,导出了金属材料基本力学性能同压痕的加卸载参量间的无量纲函数关系,为利用数值方法建立两者之间的具体关系提供了理论指导。
(2)通过有限元数值模拟的方法,选取合适的指数形式的拟合函数,确定了三种压头的无量纲函数关系的具体表达式,即Berkovich、Conical和Cube corner三种压头。针对这三种压头的载荷位移曲线,分析了压头的几何形状以及摩擦效应对无量纲函数的影响,结果表明,对于大角度的Berkovich的压头,其摩擦效应几乎对无量纲函数没有什么影响;但对于小角度的Conical和Cube corner压头,摩擦效应的影响十分显著,是一个必须考虑的因素。反推结果敏感性的研究表明,我们建立的模型对于不考虑尺度效应的块体材料是非常可靠的。
(3)将建立的反推模型应用在镍薄膜材料上,将反推结果与拉伸实验结果进行对比,发现存在强烈的尺度效应。通过对压痕实验数据进行深入分析,得到弹性模量也存在尺度效应的结论,将弹性模量的尺度效应与硬度的尺度效应结合起来,得到了镍薄膜材料的真实屈服强度。
(4)对压痕法表征材料应力应变关系的唯一性问题进行了研究,并找到其根源。通过引入压痕塑性区半径rp来解决这一问题,得到新的反分析模型。通过数值法对上述反推模型的有效性进行了研究,发现得到的反推结果非常可靠,从而证实了该模型的可行性。
(5)基于Maxwell粘弹性理论模型,讨论了研究压痕蠕变的理论方法,并根据此方法探讨了压痕蠕变对纳米压痕响应测试的影响。为了修正测试弹性模量过程中出现的误差,我们详细讨论了“Nose”(鼻子)效应对压痕响应的干扰。通过修正刚度和接触深度,有效剔除了压痕蠕变带来的误差,得到了材料的真实弹性模量,并找到了压痕过程中“Nose”效应出现的判据,这对实际工程应用具有重要的指导意义。另外,研究了压痕蠕变的尺度效应问题,通过对不同载荷下压痕蠕变实验数据的分析发现,保载阶段的蠕变位移、速率、应变率甚至应力指数等都存在尺度效应,其物理机制可以通过位错攀爬、晶界滑移和晶粒旋转进行解释。
2、对金属膜/基体系的硬度进行了表征,从压痕复合硬度(综合考虑基底效应和尺度效应的双重贡献)得到了薄膜材料的本征硬度。我们考虑这两种效应对测试硬度的影响,建立了新的理论模型,成功提取出了薄膜和基底的真实硬度。其详细结果如下:
(1)为了表征金属膜/基体系的硬度,我们综合考虑了基底效应和尺度效应对复合硬度的影响,建立了新的理论模型。我们对于其物理机制进行了探讨,结果表明,在压痕深度比较浅的时候,由于尺度效应不同体系复合硬度变化的物理机制相同,都是随着压痕深度的减小硬度增加;随着压痕深度逐渐增加,基底效应不能忽略,这时不同体系复合硬度变化的物理机制完全不同,对于硬(软)膜/软(硬)基底,其复合硬度随压痕深度的增加而减小(增加)。
(2)在实验方面,对硬膜/软基底和软膜/硬基底两种体系进行了研究。结果表明,我们建立的模型能够同时刻画这两种体系的实验数据,可以得到薄膜和基底的真实硬度。
(3)基于低阶应变梯度塑性理论(the Conventional theory of Mechanism-based Strain Gradient plasticity,简称为CMSG理论),用有限元数值模拟对两种膜/基体系进行了压痕研究,并用我们建立的模型对计算的数据进行拟合,证实了模型中确实包含尺度效应。
3、通过前面建立的反推法理论模型,研究了拉伸应变对镍薄膜力学性能的影响,主要包括弹性模量、屈服强度、硬度和硬化指数等。结果表明,弹性模量和硬化指数与材料的变形程度无关,但是屈服强度的变化在塑性变形阶段遵循指数硬化趋势,在弹性变形阶段没有发生变化(依然为未变形材料的屈服强度)。
(1)考虑到微纳米测试系统的载物台比较狭小,为了研究拉伸状态下镍薄膜的力学性能,我们设计了一个微小拉伸加载装置,不仅可以方便地对样品进行拉伸加载,还可以将其放入纳米压痕仪直接进行实验。为了排除挠度的干扰,要求试样厚度最少要达到3.7mm。
(2)通过对压痕过程中出现的堆积效应进行修正,发现反推法得到的弹性模量和硬化指数与拉伸应变无关。
(3)借助金属材料的应力应变关系,可以推导出加工过程中镍薄膜的屈服强度与拉伸应变的关系。从这一关系可以知道,屈服强度在弹性变形阶段不发生变化;而发生塑性变形以后,材料的屈服强度遵循指数硬化趋势。
(4)从有限元数值模拟得到的硬度与屈服强度的关系出发,得到了硬度与拉伸应变之间的关系。结果发现,此关系与屈服强度不同,并不遵循硬化指数的趋势。
With environmental pollution, energy crisis and shortage of resources and other issues becoming prominent increasingly, countries around the world attach more importance to efficient, clean, renewable energy and electric cars, electric bicycles, portable power tools and other related technology. The current power supply used in electrical vehicles is mainly lead-acid battery and nickel-metal hydride battery. Now the use of lead-acid battery begin to be restricted due to people’s awareness of lead poisoning; while the energy density of nickel-metal hydride battery can not meet market demand of rapid development, so people must re-select and develop new energy storage device.
The shell material whose property determines that of the power supply is a key component. Proposed and long-term studied by our group , nickel-plated steel which integrate nickel thin film electrodeposited on the low carbon steel substrate closely is a kind of new pre-shell material of nickel-plated power supply,with good synchronization elongation and corrosion resistance. However, with the industrialization of nickel-plated steel strip, many basic problems arose, not solved by the experience. Production costs and risks increased for the lack of basic theory. To solve these problems, we must start from the basic theory, and find the nature of these problems in the production process. These important issues have not been resolved is due to the two main reasons: (1) film itself is relatively small scale and hard to operate, and the deformation of metal forming process is very complicated to build more complex theories; (2) The mechanical property are influenced by the multi-effects in small-scale, such as the scale effect, substrate effect, etc.. If these negative factors cannot be removed effectively, it will be difficult to obtain the true mechanical properties of thin films.
For these reasons, this paper aims to study mechanical properties of metallic thin films by anti-analysis, and the achieved main contents and results are as follows:
1. The stress-strain relationship of metallic thin films was studied by nanoindentation method; and many problems are considered arising in the reverse analysis:①the scale effect problems of the hardness, elastic modulus and yield strength were studied;②the uniqueness issue was solved by introducing the plastic zone radius; and③the creep problem in the process of the indentation and was studied in order to obtain the accurate experimental data. The five main contents are as follows:
(1) Dimensional analysis were done byΠTheorem for nanoindentation issues, and the dimensionless functions between the same basic mechanical properties of metallic materials and load-displacement curves were obtained, offering theoretical guidance to establish the specific relationship between these two parameters with numerical methods.
(2) The specific expression of these three dimensionless functions Berkovich, Conical and Cube corner tips were determined by numerical simulation by finite element method and selection of the appropriate fitting function. For the load-displacement curves of the three indenters, the impacts of the indenter geometry and friction effects on nondimensional functions were analysized. The results show that for the wild-angle Berkovich indenter, the friction effect is almost nothing on the dimensionless function; but for small-angle Conical and Cube corner indenters, the friction effect is very significant and is a factor that should be considered. Based on the results of the sensitivity of inverse analysis, it is kown that the model for the non-scale effects of bulk materials is very reliable.
(3) It was found that there is a strong scale effect when the inversing model used for the Ni thin film material, through comparation between the inverse results and the results of tension tests. There was scale effect for elastic modulus through the experimental data. We combined the scale effects of elastic modulus and hardness together to obtain the real yield strength of Ni thin films.
(4) The uniqueness problem through the stress-strain relationship characterized by indentation was studied and its root was found. Through introducing the plastic radius rp of indentation, a new reversing model was obtained. The validity of the inverse model was veryfied by the numerical method, and it is found that the reverse results were very reliable, thereby confirmed the feasibility of the model.
(5) Based on Maxwell visco-elastic model, the theory method of indentation creep was discussed. According to the method, the impact of the indentation creep on nano-indentation response was studied. In order to correct elastic modulus error during the tests, we discussed the "Nose" effect of the indentation response. Through modifying the stiffness and contacting the depth of indentation creep, the error was removed effectively, and the real modulus of the material can be obtained. The real mechanical properties criterion of nickel film was found by the indentation test which has important guiding significance on the practical engineering application. In addition, the scale effect of the indentation creep was studied and its physical mechanism was also discussed. The creep displacement, velocity, strain rate and stress exponent all shown scale effect by analyzing the experimental data of the indentation creep under different load.
2. The metal film/substrate system hardness was characterized; and from the composite indentation hardness (considering the double contribution of the scale effect and the substrate effect), the intrinsic hardness of thin films has been extracted.
(1) To characterize the metallic film/substrate system hardness, we took the influence of substrate effect and scale effect on the composite hardness into account, and established a new theoretical model. In order to verify the reliability of the model, we verified the effectiveness by both experiment and simulation.
(2) The two systems of the hard film/soft substrate and soft film / hard substrate were studied by the experiments. The results show that the model can describe the experimental data of the two systems. In addition, the physical mechanism of composite hardness of different systems was discussed briefly.
(3) Based on CSMG theory, the indentation responds of the two film/substrate systems were studied by the finite element numerical simulation. The model can fit the calculated data and confirmed that the model does include scale effects.
3. The influence of tensile strain on mechanical properties of Ni films was studied by the previous theoretical models, including elastic modulus, yield strength, hardness and the hardening exponent. The results show that the values of elastic modulus and hardening exponent didn’t change, but the yield strength increased with the increasing tensile strain for the plastic deformation following the hardening exponent law.
(1) Considering the small loading platform of micro and nano test system, in order to study mechanical properties of Ni films under tensile, we designed a smile tensile loading device, not only being easily loaded on the tensile samples but also being directly into the nanoindention experiments. In order to exclude the interference of deflection, the sample thickness was required to achieve at least 3.7mm.
(2) By correcting the accumulation effect appearing in the process of indentation, the elastic modulus and hardening exponent from inverse method were found to be not sensitive to tensile strain.
(3) Using the stress-strain relationship of metallic materials, the relationship of tensile strain and yield strength can be derived in the process of nickel thin films and. From this relationship, it was found that the yield strength in the elastic deformation stage does not change; and the yield strength follows exponential hardening trend after plastic deformation.
(4) From the relationship between the hardness and yield strength by the finite element simulation, the relationship between hardness and tensile strain can be obtained. The results showed that of this relationship was different from the yield strength, not comply with the hardening exponent trend.
引文
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