Effect of Cloisite and modified Laponite clays on the rheological behavior of TPU–clay nanocomposites

The effect of nanoclays (modified Laponite and Cloisite) on the dynamic modulus, dynamic viscosity, and relaxation time of thermoplastic polyurethane (TPU)-based nanocomposites is studied by using the dynamic mechanical rheometer in strain, temperature, frequency sweeps, and stress relaxation experimental modes. Cloisite 20A preferentially associates to the soft domains and dodecyl amine-modified Laponite RD favors the hard domains of the TPU, whereas cetyl trimethyl ammonium bromide-modified Laponite RD does not show any preference and gets distributed both in the hard and soft domains randomly. Cloisite-based nanocomposites, having longer diskette size, possess greater dynamic modulus and viscosity than Laponite-based ones. The change in modulus and viscosity of the nanocomposites over the range of frequencies registers a completely different behavior at different temperature regimes depending on the size of diskettes of the nanoclays and their distribution (before and after the softening of the hard domains). Addition of clay is found to increase the elastic component of stress relaxation of the TPU at 120°C. This behavior is more prominent in the case of Cloisite-based nanocomposites as compared to their Laponite-based counterparts. The morphology correlates well with the dynamic rheological properties of these nanocomposites.     

Thermal Conductivity of Soils at Very Low Moisture Content and Moderate Temperatures

An analysis of soil thermal conductivity data shows that, at very low moisture content, this property first varies insignificantly and then begins to increase from a certain critical moisture content, whose value tends to depend on clay mass fraction. Two simple models evaluating the critical moisture content were developed; the first one is a fraction of the permanent wilting point; the second one is a simple linear function dependent on clay mass fraction. An insignificant variation of soil thermal conductivity is observed at 20°C, within a water pressure head ranging from 1×10³ to 1×10³m, while for higher temperatures (45–50°C) from 5000 to 100000m. Three extensions of the enhanced thermal conductivity model by Sundberg, namely SUN-1, SUN-2 and SUN-3, were proposed and tested. They produce an average root mean square error of 27%, 24% and 30%, respectively, with respect to experimental data. SUN-1and SUN-2 predictions could be further improved if better estimates of thermal conductivity at the dry state and the permanent wilting point were provided. SUN-3 is a simple model which does not require information about the PWP and critical moisture content. All SUN models have a potential for implementing the latent heat transfer component.     

基于热老化实验的螺杆马达定子橡胶本构模型研究

随着我国油气资源勘探开发向深部地层迈进,螺杆钻具定子橡胶井下高温热老化问题日益凸显,导致螺杆钻具输出性能衰减,严重影响钻进效率,迫切需要揭示热老化对螺杆钻具定子橡胶力学性能的影响,以在设计之初提出可减小螺杆钻具输出性能衰退的综合方案。本文开展了螺杆马达定子橡胶在不同温度下的热老化实验,通过拉伸实验得出应力应变数据并拟合出Mooney-Rivlin模型常数和Yeoh模型常数;再对所得实验数据及所求得的模型常数数据进行分析;最后,使用确定了基本常数的模型开展了数值计算。计算结果表明,随着温度的上升,Mooney-Rivlin模型常数C_1增大、C_2减小,C_1和C_2呈明显相反变化的趋势,Yeoh模型常数C_(10)和C_(20)增大,C_(30)减小;通过模型计算结果与室内实验测定结果的对比,证明了Mooney-Rivlin模型较Yeoh模型更适合于螺杆马达定子橡胶的力学分析。不考虑环境温度热老化和考虑环境温度热老化,螺杆钻具定子衬套的计算结果存在很大差别,研究工作不仅证明了螺杆钻具定子橡胶热老化研究的必要性,更为螺杆钻具定子橡胶的线型设计和过盈量选取提供了参考。     

Photoviscoelastic stress analysis of a plate with a central hole

An epoxy resin containing excessive plasticizer was developed and characterized. The material, which deforms viscously at room temperature, has optical properties that depend on stress and strain. A tensile specimen was prepared from the epoxy resin so that the mechanical and optical properties of the epoxy resin could be characterized. The elastic and plastic behavior was determined at 37°C using tensile stresses between 4 and 26 MPa. The birefringence was also recorded as a function of time and stress. From these results, a photoviscoelastic constitutive equation was constructed to describe the dependence of the birefringence on stress and strain. The constitutive equation was then applied to study the deformation of a tensile specimen containing a central circular hole. By using the isochromatic fringes in combination with the isoclinic, the time-dependent variation of the stress field in the specimen was solved.     

Residual fracture energy of cement paste, mortar and concrete subject to high temperature

Quantifying high temperature damage is an issue that can hardly be dealt with experimentally because of the complexity of the loading control, of temperature and of moisture. The experimental investigation was carried out. The measurement of the mechanical characteristics (fracture energy, tensile strength, elastic modulus and thermal damage parameter) of five cementitious materials, cement paste, mortar, ordinary concrete and two HPC concretes were performed by three-point bending tests after heating/cooling cycles at 120, 250 and 400 °C. The tests showed that the cementitious materials behave almost identical when the fracture energy G_f is considered as a function of maximum temperature. The thermal damage due to heating from 120 to 400 °C increases the fracture energy by 50% with the reference tests at room temperature. A more tortuous crack surface is one reasonable explanation for the significant increase in G_f. It is demonstrated that the temperature exposure makes all cementitious materials tested significantly more ductile and less resistant.     

EXPERIMENTAL STUDY OF MECHANICAL PROPERTIES OF WATER-COOLED GRANITE UNDER HIGH TEMPERATURE1)

通过对高温加热-遇水快速冷却后的花岗岩试样进行单轴和三轴实验,研究了800°C内高温花岗岩遇水快速冷却后的力学性质随温度和围压的变化规律。实验结果表明：(1)400°C为高温加热-遇水快速冷却对花岗岩力学性质影响的阈值;(2)同一温度条件下,峰值偏应力、峰值应变随围压的增大而增大;弹性模量随围压的增大先增大后减小;(3)单轴实验中,温度低于400°C时,岩样表现为复合破坏,随着温度的升高破坏形式转变为拉破坏;三轴实验中,岩样整体上表现为剪切破坏。     

High-temperature deformation measurements using digital-image correlation

The ability of the computer-vision technique of digital-image correlation to measure full-field in-plane surface deformations at elevated temperatures was evaluated by a series of experiments. Samples were subjected to pure translation, free thermal expansion and uniform tensile loads. Results are presented which show that the digital-image-correlation technique remains fully capable of accurate measurement of the displacements and strains on the surface of a planar object at temperatures up to 650°C.     

热障涂层高温失效行为的正射投影-单相机三维数字图像相关实验研究

热障涂层(Thermal Barrier Coating,TBC)作为一种隔热材料,可降低发动机高温部件的表面温度,提高涡轮发动机的整体性能。涂层服役过程中,TBC陶瓷层的失效将导致高温部件中的金属基底直接暴露于恶劣的高温环境中,严重影响发动机的安全性。其高温服役环境下的力学性能研究是备受材料和力学工作者关注的问题。本文结合热障涂层高温检测的需求,实现了涂层-基底异质表面的高对比度高温散斑制作;发展了正射投影-单相机三维数字图像相关方法(正射投影-单相机3DDIC),构建了跨界面形函数,实现了涂层与基底的三维形貌及位移、应变的同时测量;基于涂层结构的高温拉伸实验结果,建立了依据涂层-基底应变方差差值的涂层失效判断方法,得到了热障涂层在室温(27℃)至1000℃的断裂极限应变。实验结果表明,正射投影-单相机3DDIC方法作为一种可靠测试方法,可以应用于涂层结构高温下的力学失效行为研究。     

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.     

Effects of physical aging on yielding kinetics of polycarbonate

The purpose of this work was to investigate the effects of physical aging on the kinetics of yielding in polycarbonate. PC samples were annealed over a wide range of aging times and temperatures. Both tensile and compressive tests were performed over various loading rates and temperatures to analyze the effects of aging time and aging temperature on yielding kinetics. Two grades of polycarbonate, Makrolon, of different molecular weights, PC-2608 (low M_w), and PC-3208 (high M_w), supplied by Bayer were analyzed. In unaged condition, PC is hard and tough, but after aging, it becomes more brittle. In terms of molecular movement, the yielding process is a thermally activated process involving inter- and intra-molecular motions. The time–temperature dependence of yielding behavior can be separated into two regions. Aging does not affect localized molecular motions of the β process during yielding. Physical aging in PC results in a slower jump rate of the main segments of macromolecules between two equilibrium positions. It reduces the flexibility of the macromolecules and thus, makes the polymer more brittle. Heat aging also causes a decrease of the entropy (ΔS) in polycarbonate, and this decrease is more important when the molecular weight is reduced. Increasing the annealing time and temperature results in a continuous reduction of ΔS. The rate of aging decreases with decreasing annealing temperature and below about 30 °C, no aging takes place. Annealing also strongly affects the excess of enthalpy in PC. However the effect of physical aging on yielding differs to that on enthalpy excess. The kinetics of yielding and aging processes in polycarbonate are also different. An increase in the strain rate does not have the same effect on the yield stress as an increase in the aging time by a same factor.     

Creep performance of PVC aged at temperature relatively close to glass transition temperature

In order to predict the mechanical performance of the polyvinyl chloride(PVC) at a high operating temperature,a series of short-term tensile creep tests(onetenth of the physical aging time) of the PVC are carried out at 63 C with a small constant stress by a dynamic mechanical analyzer(DMA).The Struik-Kohlrausch(SK) formula and Struik shifting methods are used to describe these creep data for various physical aging time.A new phenomenological model based on the multiple relaxation mechanisms of an amorphous polymer is developed to quantitatively characterize the SK parameters(the initial creep compliance,the characteristic retardation time,and the shape factor) determined by the aging time.It is shown that the momentary creep compliance curve of the PVC at 63 C can be very well fitted by the SK formula for each aging time.However,the SK parameters for the creep curves are not constant during the aging process at the elevated temperatures,and the evolution of these parameters and the creep rate versus aging time curves at the double logarithmic coordinates have shown a nonlinear phenomenon.Moreover,the creep master curves obtained by the superposition with the Struik shifting methods are unsatisfactory in such a case.Finally,the predicted results calculated from the present model incorporating with the SK formula are in excellent agreement with the creep experimental data for the PVC isothermally aged at the temperature relatively close to the glass transition temperature.     

Mechanical Characterization of Angle-Ply Composite Laminates by Differential Moiré Method: The Influence of Specimens' Length-to-Width Ratio

The influence exerted by the specimen proportions on the measured performance of angle-ply [+45°/–45°]_s composite laminates is studied. Three kinds of specimens are considered, having different length-to-width ratios, made with glass/epoxy unidirectional or fabric laminae. The static tensile characteristics are measured by means of load cells, electric strain gauges and through the Moiré fringes method. The strain fields are analysed and the effects of stress concentration at the laminate-free edges are evaluated, as well as their influence on the strain distribution and the measured strength and stiffness. The results are summarized as diagrams of ultimate load and elastic modulus versus length-to-width ratio of the different specimens investigated. These diagrams allow the designer to evaluate the influence exerted by specimen proportions on the measured performance, as well as to compare characteristics which are heterogeneous, as obtained with different kinds of specimen.     

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.     

高低温加载对大理岩力学特性影响的试验研究

许多工程（如采矿、隧道掘进、地热开采等）都涉及到岩石损伤及破碎问题．传统的岩石损伤破碎技术,如爆破法、水射流法、机械掘进法等均面临着一系列问题,利用岩石的热损伤性质辅助机械破岩有望实现安全、高效破岩的目的．大理岩是一种典型的硬岩,常见许多工程之中,因此本文以大理岩为研究对象,首先将均质性较好的大理岩试样加热至不同温度(20~1000 °C)后放入液氮中进行急速冷处理,然后对其进行了系列的物理力学性质测试．试验结果表明：处理后密度、纵波波速、抗拉强度、单轴抗压强度(UCS)和弹性模量整体上都随温度的上升而下降;当加热温度在100 °C之前,大理岩表现出一定的热硬化现象,即随着温度升高,其UCS、纵波波速以及弹性变形模量均增大;UCS变化的阈值温度为400 °C左右,一旦温度超过400 °C,UCS迅速下降,其速率达到了9 MPa/100 °C,当温度超过500 °C弹性模量迅速下降,其速率达到7.00 GPa/100 °C,表明岩样抵抗变形能力减弱．整体上,热加载降低了大理岩的脆性,使其在单轴作用下的破坏模式由脆性破坏逐渐转化为弹塑性破坏．     

A methodology for thermomechanical fatigue crack growth testing in MMCs

This paper describes the experimental techniques used in an investigation of the crack growth characteristics of a four-ply, unidirectional, silicon carbide fiber reinforced, titanium matrix composite (SCS-6/Ti–6Al–2Sn–4Zr–2Mo) subjected to thermomechanical fatigue. A mechanical test system was assembled which is capable of conducting fully automated, computer-controlled thermomechanical fatigue crack growth tests. The system is able to simultaneously impose operator-defined arbitrary mechanical and thermal histories on the specimen. Crack lengths in single-edge tension [SE(T)] or middle tension [M(T)] specimens are measured by the direct-current electric potential method and optically using a unique telemicroscope system. A series of isothermal, in-phase and out-of-phase crack growth tests was conducted to obtain baseline data for material modeling purposes. The test temperatures ranged from 150°C to 538°C, and the highest thermal frequency was 0.0083 Hz.     

Rheology and microstructure of heat-induced egg yolk gels

The evolution of native egg yolk undergoing a thermal-induced sol-gel transition was studied by using temperature controlled small amplitude oscillatory shear measurements. The critical gel point was determined according to Winters criterion: 1) from the measurements of storage and loss moduli as a function of heating time at different frequencies, and 2) from the exponents of the power law mechanical spectra obtained after cure experiments performed up to a maximum temperature (60–90 °C) followed by a sudden decrease in temperature up to 20 °C. Differential Scanning Calorimetry (DSC) was performed in order to investigate thermal transitions in egg yolk. Microstructure of gels was evaluated by Transmission and Scanning Electron Microscopy. The results obtained were discussed in terms of the processes involved in protein gelation: change in the protein system, aggregation of partially denaturated protein molecules and association of aggregates. As a result, an elastic gel network was always obtained. The influence of frequency, heating rate, solids concentration and maximum temperature of processing, was analysed. Most of the transformations found during thermal processing were found to be basically irreversible, even at the sol state and gel point. However, some reversible phenomena were detected during constant temperature processing depending on the maximum temperature performed.     

Measurement of the concentration diffusion coefficient for He-Ar and Ne-Kr by a two bulb method

Summary A two bulb glass apparatus was used to measure the concentration diffusion coefficient of the binary gas systems He-Ar and Ne-Kr. The coefficients were determined for equimolar mixtures at temperatures between 0°C and 70°C. The diffusion was followed as a function of time by withdrawing samples and analyzing them in a specially designed thermal conductivity analyzer with high accuracy. The diffusion coefficients agree with earlier reported experimental values and with those obtained on the basis of the Chapman-Enskog theory in conjunction with the modified Buckingham exp-six and Lennard-Jones (12-6) intermolecular potentials. The smoothed values were used to predict viscosity and thermal conductivity of these mixtures as a function of composition and temperature.     

Modelling mechanical property recovery of a linepipe steel in annealing process

In this paper a set of mechanism-based unified viscoplastic constitutive equations has been used to model the effect of microstructural evolution on mechanical property recovery in the annealing process of a cold formed linepipe steel. Dislocation density and plasticity-induced damage accumulation during deformation, and recovery and recrystallisation of the deformed material during subsequent annealing have been modelled. The effects of annealing time on microstructural evolution also have been investigated. Tensile tests were performed on the low carbon ferritic linepipe steel before and after annealing at 700 °C with different holding times. The experimental results have been used to characterise the unified constitutive equations, using an Evolutionary Programming (EP)-based optimisation method. Using these equations, the stress–strain relationships for the interrupted constant strain rate tensile tests were predicted and close agreement between the computed and experimental results was obtained, for various annealing times and for the materials with different amounts of pre-deformation.     

水硬性石灰合成及拉破坏特性试验研究

水硬性石灰在欧洲石质文物修复和加固中获得了很大成功。我国的石质文物主要是砂岩,水硬性石灰的修复效果不好。为满足我国石质文物修复和加固的需求,本文以石灰石和黏土为原料,在950℃煅烧不同时间,制备出水硬性石,对试样的成分、微观形貌、收缩率、抗拉强度和拉破坏过程等进行了研究。结果表明:(1)试样中含有水硬性成分2CaO·SiO2(C2S);煅烧8h时,成分与欧洲水硬性石灰NHL5接近;1.5CaO·SiO2·xH2O(C-S-H)和CaCO3的含量随龄期的增加逐渐增加。(2)龄期1~3d,收缩率较小;龄期4~6d,收缩率以线性规律增加;7d以后,收缩率趋于稳定。(3)局部变形区随拉应力的增加而变大,邻近局部变形区逐渐合并,形成面积更大的应变局部化带;载荷超过峰值后,产生微裂隙;随载荷进一步增加,微裂隙扩展,贯穿整个试件,发展成宏观裂隙,使试件破坏。(4)抗拉强度随龄期的增加而增加,水硬性石灰中C-S-H、CaCO3等相互交织,构成空间致密体,使试件力学强度提高。合成的水硬性石灰物理力学性能与欧洲水硬性石灰NHL5相近,并且成分均匀、可控,在石质文物修复和加固工程中具有良好应用前景。     

结晶特性与制造工艺对炸药件力学性能的影响

通过对塑料粘结炸药(PBX)在压制、热老化及贮存中炸药HMX、TATB和粘结剂F的性能变化规律的研究,揭示了加工和贮存条件对炸药件的力学性能的影响。得出如下结论:1)随着老化温度的提高,粘结剂F结晶度增加。TATB基PBX炸药经老化后力学性能没有明显变化,说明粘结剂结晶度和炸药颗粒度的变化对炸药总体性能影响不大。2)钢模压制的TATB基PBX药柱在经历多次温度循环后,TATB与粘结剂F界面的作用有所减弱,药柱内部产生由脱粘引起的缺陷,其力学强度下降。TATB基PBX药柱的力学强度与模量均随着环境温度的升高而呈下降趋势,而等静压成型能明显改善TATB基PBX的力学性能。