Thermal contraction and volume relaxation of amorphous polymers

Two experimental techniques are described for the determination of the change of specific volume of polymers with temperature and aging time, which allow measurements between – 160 °C and + 200 °C. Four technical amorphous polymers, PS, PVC, PMMA and PC have been investigated. Volume-temperature curves under constant rate of cooling are presented and interpreted with respect to relaxation processes known from other physical investigations. The rate dependence of dilatometric glass transition temperatures is compared with the time dependence of rheometric glass transition temperatures from shear creep data. Volume relaxation data at constant aging temperature are presented. Aging is found to proceed until very low temperatures in the glassy state for e.g. PMMA.For polystyrene, a comparison is made between the predictions of a very simple theory of volume relaxation due to Kovacs with experimental data, using additional information from volume temperature curves and the time temperature shift of the shear creep transition. The theory predicts a rate of volume relaxation which is much lower than that found by experiment.     

物理老化对玻璃态高聚物非线性蠕变行为的影响

在不同应力水平下对经历不同老化时间的有机玻璃(PMMA)进行常温蠕变测试,分析物理老化和应力对材料蠕变柔量函数的影响.分析表明,老化时间对PMMA蠕变行为的影响满足流变简单性规律,即不同老化时间的蠕变柔量曲线可以沿对数时间轴平移而叠加到参考曲线上.取最长的老化时间为参考状态,依时间-老化时间等效原理,得到了各应力水平下的蠕变柔量主曲线.老化移位因子与老化时间在双对数坐标图上呈现线性关系,其负斜率就是老化移位率.结果表明,老化移位率随应力的增高而减小.     

Characterization of physical aging by time-resolved rheometry: fundamentals and application to bituminous binders

Physical aging is a ubiquitous phenomenon in glassy materials and it is reflected, for example, in the time evolution of rheological properties under isothermal conditions. In this paper, time-resolved rheometry (TRR) is used to characterize this time-dependent rheological behavior. The fundamentals of TRR are briefly reviewed, and its advantages over the traditional Struik’s physical aging test protocol are discussed. In the experimental section, the TRR technique is applied to study physical aging in bituminous binders. Small-diameter parallel plate (SDPP) rheometry is employed to perform cyclic frequency sweep (CFS) experiments over extended periods of time (from one to 8.6 days). The results verify that the mutation of rheological properties is relatively slow during physical aging (mutation number N′_mu?<<?1), thus allowing rheological measurements on a quasi-stable sample. The effects of temperature, crystallinity, and styrene-butadiene-styrene (SBS) polymer modification on the physical aging of bitumen are evaluated. The time-aging time superposition is found to be valid both for unmodified and for polymer-modified bitumen. Vertical shifts are necessary, in addition to horizontal time-aging time shifts, to generate smooth master curves for highly SBS-modified bitumen.     

Multiscale Creep Compliance of Epoxy Networks at Elevated Temperatures

Epoxy networks are thermoset polymers for which an important structural length scale, molecular weight between crosslinks (M _c), influences physical and mechanical properties. In the present work, creep compliance was measured for three aliphatic epoxy networks of differing M _c using both macroscale torsion and microscale depth-sensing indentation at temperatures of 25 and 55°C. Analytical relations were used to compute creep compliance (J(t)) for each approach; similar results were observed for the two techniques at 25°C, but not at 55°C. Although creep compliance measurement differed at elevated temperatures, there were clear correlations between M _c, glass transition temperature, T _g, and the observed time-dependent mechanical behavior via both techniques at 55°C, but these correlations could not be seen at 25°C. This work demonstrates the capacity of depth-sensing indentation to differentiate among epoxy networks of differing structural configurations via J(t) for small material volumes at elevated temperatures.     

非线性粘弹体的时间-温度-应力等效原理及其应用

考虑粘弹性材料特征时间的应力相关性,认为应力水平与温度、压力、溶剂浓度、损伤及老化等材料特征时间的影响相似,有其等效性。依自由体积理论,推导了温度－应力移位因子的表达式,提出了时间－温度－应力等 效原理。应用此原理,可以将不同温度和应力水平下的儒变曲线移位成某一参考温度和参考应力水平下的主曲线,从而可以通过较高温度和应力水平下的短期蠕变行为来预测较低温度和应力水平下的较长期的蠕变行为。实例分析了高密度聚乙烯（HDPE）非线性蠕变行为的－应力等效性。     

Time-temperature-stress equivalence and its application to nonlinear viscoelastic materials

Stress-dependence of the intrinsic time of viscoelastic materials is investigated. The influence of stress level on the intrinsic time is considered to be similar to that of temperature, pressure, solvent concentration, damage and physical aging. The time-temperature-stress equivalence principle is proposed, by employing which, the creep curves at different temperatures and stress levels can be shifted into a master curve at reference temperature and stress level. Thus the long-term creep behavior of viscoelastic materials at a lower temperature and stress can be predicted from the short-term one at a higher temperature and stress. As an example, the nonlinear creep behavior of high-density polyethylene (HDPE) at room temperature is studied using the time-temperature-stress equivalence principle presented. Project supported by the National Natural Science Foundation of China (No. 19632030, 50003005) and by the Education committee of Human Province (No. 99C122).     

Creep Properties and Recoverability of Double-wall Corrugated Paperboard

This paper deals with the characterization of creep properties and recoverability of double-wall corrugated paperboard with A and B flutes at different combined conditions of the ambient temperature 20°C with four kinds of relative humidities and five kinds of constant compression loads. The main feature of this paper is the evaluation on the creep properties and recoverability of double-wall corrugated paperboard with A and B flutes by a series of experimental studies on creep testing apparatus, the analysis of effects of relative humidities and constant compression loads on creep properties and recoverability, and the establishment of mathematical model of creep and time curves. By using Method of the Least Square and Method of Nonlinear Regression, the piecewise experimental formulas of creep and time curves have been obtained. The work provides basic data and introduces important mathematical relationships relevant to design applications for protective packaging for transportation and storage of goods.     

考虑老化的混凝土粘弹性分数导数模型

混凝土是一种具有分形结构的材料。采用分数微积分模型来研究具有分形结构材料的老化规律目前尚未见到。本文的目的是采用含分数阶导数的类标准线性体来模拟考虑老化的混凝土的蠕变和松弛规律。给出了分数导数与Abel核之间的关系。讨论了类标准线性体的蠕变柔量和松弛模量及其在考虑老化的混凝土中的应用。与传统的混凝土流变模型相比较表明，类标准线性体可以更好地同时拟合混凝土在不同龄期的蠕变和松弛曲线。而且其形式简单、统一，在计算过程中需要调整的参数很少。可以预见，类标准线性体在混凝土的结构设计和计算中将有着广泛的应用前景。     

Deformational behaviour of a polymeric particle layer

Deformational behaviour of viscoelastic particulate materials in uniaxial compression, at constant temperature, has been studied on powdered PVC. It has been shown that both creep deformation and creep recovery of a PVC particle layer at constant temperature can be described by the equationΦ = A e ^BP t^z whereΦ is porosity,P pressure,t time andA, B andz are constants. For a narrow pressure range the relationshipz = CP applies whereC is a constant dependent onB.     

A new method of representation of fiber creep data tensile creep behavior of some acrylic fibers

Summary Fiber creep data are usually represented as plots of extension versus time at constant stress and temperature. Fiber samples, however, exhibit some degree of variability in structure from filament to filament. Consequently, even when initial applied stresses are nominally equivalent (as determined by measurement of cross-sectional area, and load), the creep of individual fibers can differ significantly, and the creep behavior of a sample can only be characterized statistically.Structural parameters such as orientation, which affect fiber properties greatly, and therefore creep, are not considered in the conventional representation of creep data. Orientation, in turn, is associated with stretch or extension. On this basis, creep, i. e. creep rate, can be expected to depend on extension.In the proposed method for representing creep data, the rate of creep is related to the extension at a constant time and temperature. In these so-called isochronal creep rate curves, the use of stress as an independent variable is omitted, and is replaced by extension. This method of representation discloses common creep characteristics in fibers, which, though taken from the same sample, exhibit widely different creep behavior when treated conventionally. In this way, the creep behavior of the whole sample can be conveniently represented. These plots reveal more detail than the ordinary creep curves, and indicate different creep mechanisms within certain extension regions as well as the stretch-relaxation history of the particular fiber sample. In this paper, the aspects and limitations of these two methods of representation of creep data are discussed, and their relative merits are demonstrated using experimental acrylic fibers.     

ANALYSIS OF MECHANICAL CHARACTERISTICS OF FROZEN CLAY AND MODIFIED S-M CREEP MODEL1)

为合理描述人工冻结法施工的矿井土层力学特性,对某矿井土样的重塑土进行单轴抗压强度实验和单轴压缩蠕变实验,得到重塑冻结黏土在不同温度及载荷加载等级下的应力-应变曲线和蠕变曲线。实验结果表明：冻结温度越低,土样的单轴强度越大;相同冻结温度下,土样的蠕变变形随着应力水平的升高而增大。单轴压缩蠕变的等时应力-应变曲线随时间发展向应变轴靠拢;土样经历初始蠕变和等速蠕变两个阶段,在较高应力水平下有进入加速蠕变的趋势;对S-M模型中各参数的意义进行修正并考虑温度的影响,得到人工冻结黏土改进S-M蠕变显式模型,然后采用粒子群算法对人工冻结黏土S-M蠕变模型参数进行优化。改进S-M蠕变显式模型理论计算值与实验值吻合良好,表明改进S-M蠕变显式模型能较好模拟人工冻结黏土的蠕变特性。改进S-M蠕变显式模型为人工冻土蠕变计算提供一种新方法。     

变温粘弹性蠕变型本构方程

文中给出了变温蠕变曲线的概念，给出了由一组恒温蠕变曲线确定沿某一温度历史的变温蠕变曲线的方法，给出了终态温度等效蠕变曲线的概念，最后给出了粘弹性材料在变温下的蠕变型本构方程的一般形式。文中证明了热流变简单材料理论是本文理论的特例，揭示了热流变简单材料理论数学方法的物理意义。     

Characterization of mechanical properties of aluminum cast alloy at elevated temperature

The tensile response, the low cycle fatigue(LCF) resistance, and the creep behavior of an aluminum(Al) cast alloy are studied at ambient and elevated temperatures.A non-contact real-time optical extensometer based on the digital image correlation(DIC)is developed to achieve strain measurements without damage to the specimen. The optical extensometer is validated and used to monitor dynamic strains during the mechanical experiments. Results show that Young's modulus of the cast alloy decreases with the increasing temperature, and the percentage elongation to fracture at 100℃ is the lowest over the temperature range evaluated from 25℃ to 300℃. In the LCF test, the fatigue strength coefficient decreases, whereas the fatigue strength exponent increases with the rising temperature. The fatigue ductility coefficient and exponent reach maximum values at 100℃. As expected, the resistance to creep decreases with the increasing temperature and changes from 200℃ to 300℃.     

人工冻结深部软岩单轴力学性能试验及蠕变模型1）

为了了解深部软岩在冻结条件下的单轴力学性能,以东北地区的原状泥砂岩为试验对象,利用自行研制的WDT-100型人工冻土试验仪器,对其进行不同温度下的人工冻土单轴抗压强度试验和单轴蠕变试验,得到泥砂岩单轴压缩应力-应变关系曲线,各温度下试样的单轴抗压强度以及蠕变曲线.单轴压缩试验结果表明：试样在给定温度和加载速率条件下,单轴压缩应力-应变关系曲线都有较为明显的屈服点,并且都在屈服点后,强度有所提高,出现硬化现象.单轴蠕变试验结果表明：单轴压缩蠕变曲线有非线性特征,单轴压缩蠕变的等时应力-应变曲线向应变轴靠拢;单轴压缩时蠕变模量随时间的增长而降低.最后采用遗传算法优化模型参数,得出泥砂岩蠕变经验方程.与试验结果对比,发现拟合情况较好.     

Elevated-temperature creep and relaxation of torsion-tension members

Based on the assumption that each material satisfies the condition for isotropic hardening for a von Mises material, an incremental solution is developed to predict axial-strain creep curves and maximum shearing-strain creep and relaxation curves for solid circular torsion-tension members subjected to proportionate and nonproportionate stepped loading including creep in tension and relaxation in torsion. Test data are obtained from torsion-tension members made either of annealed OFHC copper at 800°F (427°C) or hot-rolled SAE 1045 steel at 950°F (510°C). The loading histories include either four stepped proportionate load changes, four stepped nonproportionate load changes, or torsion-tension loading in which the axial load remains constant and the torsional load is allowed to relax during two loading periods of the test. Each test duration is about 100 h. Good agreement is indicated between the predicted and measured creep and relaxation curves.     

Development of High Temperature Nanoindentation Methodology and its Application in the Nanoindentation of Polycrystalline Tungsten in Vacuum to 950 °C

The capability for high temperature nanoindentation measurements to 950 °C in high vacuum has been demonstrated on polycrystalline tungsten, a material of great importance for nuclear fusion and spallation applications and as a potential high temperature nanomechanics reference sample. It was possible to produce measurements with minimal thermal drift (typically ~0.05 nm/s at 750–950 °C) and no visible oxidative damage. The temperature dependence of the hardness, elastic modulus, plasticity index, creep, creep strain, and creep recovery were investigated over the temperature range, testing at 25, 750, 800, 850, 900 and 950 °C. The nanoindentation hardness measurements were found to be consistent with previous determinations by hot microhardness. Above 800 °C the hardness changes relatively little but more pronounced time-dependent deformation and plasticity were observed from 850 °C. Plasticity index, indentation creep and creep recovery all increase with temperature. The importance of increased time-dependent deformation and pile-up on the accuracy of the elastic modulus measurements are discussed. Elastic modulus measurements determined from elastic analysis of the unloading curves at 750–800 °C are close to literature bulk values (to within ~11 %). The high temperature modulus measurements deviate more from bulk values determined taking account of the high temperature properties of the indenter material at the point (850 °C) at which more significant time-dependent deformation is observed. This is thought to be due to the dual influence of increased time-dependency and pile-up that are not being accounted for in the elastic unloading analysis. Accounting for this time-dependency by applying a viscoelastic compliance correction developed by G. Feng and A.H.W. Ngan (J. Mater. Res. (2002) 17:660–668) greatly reduces the values of the elastic modulus, so they are agree to within 6 % of literature values at 950 °C.     

岩石蠕变模型的比较和修正

对三种岩石在不同的应力下进行了蠕变实验,对蠕变实验曲线用粘弹模型进行了模型参数的反演,结果认为标准线性体、伯格斯和对数模型都是实验曲线的很好近似.为了进一步了解蠕变实验时间对模型参数的影响,研究了蠕变模型的预测功能.将实验蠕变曲线分成二部分,第一部分用于模型参数的反演,第二部分用于模型预测数据的检验.时间外延所得的模型的预测曲线都明显偏离了实测曲线,伯格斯和对数模型的预测曲线比实测曲线偏高,而标准线性体模型则偏低.根据不同时间的蠕变实验数据的比较和分析,认为实验时间对蠕变模型参数的反演有较为明显的影响,但只要对标准线性体模型作适当修正,引入与时间尺度有关的函数C(t),则该模型的预测能力就有较大的提高.     

Characterization of 10% Ballistic Gelatin to Evaluate Temperature, Aging and Strain Rate Effects

Ballistic gelatin is widely used as a soft tissue simulant in physical surrogates for the human body to evaluate penetrating impacts and, more recently to evaluate blunt impact and blast loading effects on soft tissues. It is known that the properties of gelatin are sensitive to temperature and aging time, but this has not previously been quantified. The mechanical properties of 10% ballistic gelatin were measured using a compression test apparatus with temperature controlled platens to maintain the sample temperature at a fixed level. Penetration testing was undertaken using a standard BB impact test to assess the effect of aging. The gelatin was found to be within calibration after 3?days (72?h of aging), based on the standard penetration test. The material properties were evaluated using the stress at failure, strain at failure and material stiffness as characterized by the Neo-Hookean constitutive model. The stress at failure and material stiffness increased with decreasing temperature and increasing strain rate, as expected, while the strain at failure remained relatively constant for the test conditions considered (1 to 23??C, strain rate from 0.01 to 1.0?s^?1). The study showed that the penetration resistance was consistent after 72?h of aging, while the mechanical study demonstrated increasing failure stress and stiffness with decreasing failure strain at longer aging times, suggesting that these effects offset one another so that the penetration resistance remains relatively constant. The primary contribution of this study was to show the importance of temperature and aging time, through mechanical and penetration testing, to achieve appropriate and consistent response from ballistic gelatin.     

Nanocharacterization of creep behavior of multiwall carbon nanotubes/epoxy nanocomposite

High temperature instrumented indentation testing was used to evaluate the mechanical properties of multiwall carbon nanotubes/epoxy nanocomposite system. Reference neat epoxy samples were also tested and compared with the results obtained for the nanocomposite. The nanoindentation creep tests were utilized to provide the creep strain rate sensitivity parameter, the contact creep compliance and the time-dependent deformation under constant loads. Different thermo-mechanical conditions comprising three temperatures of 25, 40 and 55 °C and three loads of 1, 2 and 3 mN were utilized. The improvements in the properties were not as high as anticipated through the use of mixture rule, indicating insufficient dispersion. However, variations in modulus, hardness and creep strain rate sensitivity parameter obtained using nanoindentation showed quantifiable differences between the MWCNTs nanocomposite and epoxy specimens.The comparison of the creep strain rate sensitivity A/d(0) from short term, 60 s, creep tests and the creep compliance J(t) from the long term, 1800 s, creep tests suggests that former parameter is a more useful comparative creep parameter than the creep compliance. The analysis of the creep strain rate sensitivity clearly revealed that the addition of MWCNTs to a commercial epoxy reduced the creep rate. This reduction of creep rate sensitivity parameter was observed particularly at thermal environments just below the glass transition temperature.