A method for determining the spectral relaxation functions of polymers under single stretching of micro samples

A. A. Rybin, D. V. Ruban, A. A. Chervyakov, S. A. Ulyanov
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Abstract

The principles of designing products made of the latest complex-structured polymer composite materials necessitate the need to take into account the large-scale structural effects determined by processes at the supramolecular and molecular levels of the polymer: relaxation, kinetic (breaking and recombination of chemical bonds), recrystallization of supramolecular structures, etc. The development of these processes is described by relaxation functions, which, in turn, can be calculated using the functions of relaxation time spectra. The purpose of the work was to develop a specialized equipment for testing micro-samples with a variable working part for uniaxial stretching along with the experimental technique and computational algorithms for processing the obtained measurement data, and experimental approbation of the developed approach to determining spectral relaxation functions. A method is proposed for estimating relaxation functions not at fixed stress levels within linear elasticity, at secant points of deformation diagrams, at fixed values of the linear elasticity modulus, but within an extended range of the sample deformation up to pre-rupture states. A set of test equipment designed for tensile tests of micro-samples with a thickness of the working part of 0.2 – 1.2 mm has been developed. The tooling can be installed on modern high-precision breaking machines. Tensile tests of polyethylene terephthalate micro-samples with a thickness of 50 and 175 μm were carried out taking into account the scale factor. A tensile test of micro-samples that are technologically stabilized by paper frames of a special shape is described. Diagrams illustrating the kinetics of changes in the spectral relaxation functions of oriented polyethylene terephthalate (PET) are constructed proceeding from the data of testing micro-samples with a constant strain rate. A method for using these diagrams in calculations of empirical relaxation time spectra is described. The results of testing micro-samples of polyethylene terephthalate are presented. Illustrative deformation diagrams of the studied polymer samples and calculated diagrams of functions of relaxation time spectra calculated according to the described method are given.
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一种确定微小样品单次拉伸下聚合物光谱弛豫函数的方法
根据最新的复杂结构聚合物复合材料产品设计原则,必须考虑到聚合物超分子和分子 层面过程所决定的大规模结构效应:弛豫、动力学(化学键的断裂和重组)、超分子结构 的再结晶等。这些过程的发展可以用弛豫函数来描述,而弛豫函数又可以用弛豫时间谱函数来计算。这项工作的目的是开发一种专用设备,用于测试具有可变工作部分的单轴拉伸微型样品,同时开发用于处理所获测量数据的实验技术和计算算法,并通过实验验证所开发的确定光谱弛豫函数的方法。提出了一种估算松弛函数的方法,这种方法不是在线性弹性范围内的固定应力水平、变形图的正割点、线性弹性模量的固定值,而是在样品变形的扩展范围内直至破裂前状态。我们开发了一套测试设备,用于对工作部分厚度为 0.2 - 1.2 毫米的微型样品进行拉伸测试。该工具可安装在现代高精度破壁机上。考虑到比例因素,对厚度为 50 和 175 μm 的聚对苯二甲酸乙二酯微样品进行了拉伸试验。此外,还介绍了通过特殊形状的纸框对微小样品进行技术稳定的拉伸试验。根据以恒定应变速率测试微型样品的数据,绘制了取向聚对苯二甲酸乙二酯(PET)光谱弛豫函数变化动力学图。描述了在计算经验弛豫时间光谱时使用这些图表的方法。介绍了聚对苯二甲酸乙二酯微小样品的测试结果。文中给出了所研究聚合物样品的变形示意图以及根据所述方法计算出的弛豫时间谱函数计算图。
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