On the elastic properties of model suspensions as investigated by creep recovery measurements in shear

 The elastic properties of model suspensions with spherical monodisperse hydrophilic glass spheres that were dispersed in a Newtonian liquid were determined in creep and creep recovery measurements in shear with a magnetic bearing torsional creep rheometer. The creep and creep recovery measurements were performed depending on the applied level of shear stresses ranging from 0.19 Pa to 200 Pa. Since the recoverable creep compliances of the chosen suspending medium (i.e. a low molecular weight polyisobutylene) were far below the lower limit of the resolution of the creep rheometer it can be considered to behave as purely viscous. By applying a large shear stress in the creep tests the investigated suspensions with a volume fraction of Φ _t =0.35 behave as Newtonian liquids, too. For these suspensions no significant recoverable creep compliances could be detected, as well. In contrast to the Newtonian state of suspensions at high shear stresses, where a shear induced ordering of the particles can be expected, a non-Newtonian behaviour arises by applying a very low shear stress in the creep test. In this state large recoverable creep compliances were detected for the suspensions. The magnitude of the recoverable creep compliances of the suspensions exceeded the largest creep compliances of polymer melts that are reported in the literature by more than two decades. From the results obtained by creep recovery measurements with a magnetic bearing torsional creep rheometer it can clearly be concluded that the particle structure present in the chosen model suspension gives rise to a pronounced elasticity. Received: 21 November 2000 Accepted: 12 July 2001     

Large-scale synthesis of hollow titania spheres via flame combustion

A one-step method for continuous large-scale synthesis of well-defined hollow titania spheres was established by feeding titanium tetrachloride mixed with ethanol vapor to a facile diffusion flame. A mixture of TiCl₄ and C₂H₅OH vapor was transported at 100 m/s into a flame reactor and condensed into mesoscale droplets due to Joule–Thomson cooling and the entrainment of cool gases into the expanding high-speed jet. Hollow crystalline TiO₂ spheres with good thermal stability were formed after the hydrolysis of TiCl₄ in the H₂/air flame at about 1500 °C. Structural characterization indicates that the hollow spheres, with uniform diameter of 300 nm and shell thickness of 35 nm, consist of 20–30 nm TiO₂ nanocrystallites. A formation mechanism of the hollow spheres was proposed, involving the competition between chemical reaction and diffusion during the flame process. The present study provides a new pathway for continuous and large-scale engineering of hollow nanomaterials.     

Free oscillatory shear measurements —an interesting application of constant stress rheometers in the creep mode

A constant stress rheometer in the creep mode was used to perform free oscillatory shear measurements on soft solids. The results obtained are in good to excellent agreement compared to forced oscillatory shear measurement data. Depending on the rheologic properties of the sample and the moment of inertia of the rotating device of the measurement system, free oscillations are suited to confirm or supplemented forced oscillatory measurement results.Dedicated to Professor W. Nitsch on the occasion of his 60^th birthday.     

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.     

摩擦信号分形维数与载荷和速度的关系研究

在立式万能摩擦磨损试验机上对GCr15/45#钢摩擦副进行不同接触载荷和滑动速度下的摩擦磨损试验,对初始滑动距离1 000 m内的摩擦系数信号进行数据采集,运用结构函数测度方法对摩擦系数信号进行分形表征,计算不同载荷和速度下的分形维数,研究摩擦信号的分形维数随载荷和速度的变化规律.结果表明,摩擦系数信号具有显著的分形特征,其分形维数随载荷和速度而变化.在相同载荷下,分形维数随滑动速度增加而增大;在相同速度下,分形维数随着接触载荷增加而增大.磨损率与摩擦系数信号的分形维数正相关.     

碳酸钙纳米颗粒复合超分子凝胶润滑剂的摩擦学性能研究

采用碳酸钙纳米颗粒与全氟聚醚型超分子凝胶复合得到了一种新型的纳米颗粒复合超分子凝胶润滑剂. 超分子凝胶具有错综复杂的网络结构,有效地提高了碳酸钙纳米颗粒在全氟聚醚润滑油中的分散稳定性. 此外,碳酸钙纳米颗粒作为添加剂极大地提高了超分子凝胶的润滑性能,使其表现出较好的耐高温性能,以及较高的承载力. 采用差式扫描量热仪、热重分析仪和流变分析仪对该复合润滑剂的热力学性能进行表征,结果显示该复合润滑剂具有很好的热稳定性以及较好的力学性能. 最后,通过X射线光电子能谱(XPS)对其摩擦机理进行表征,结果表明碳酸钙纳米颗粒复合超分子凝胶润滑剂优异的摩擦学性能可归因于碳酸钙纳米颗粒在摩擦副表面形成了易剪切的薄膜,以及小尺寸的纳米粒子在摩擦过程中对摩擦表面进行的自修复效应.      

Measurement of Creep Deformation across Welds in 316H Stainless Steel Using Digital Image Correlation

Spatially resolved measurement of creep deformation across weldments at high temperature cannot be achieved using standard extensometry approaches. In this investigation, a Digital Image Correlation (DIC) based system has been developed for long-term high-temperature creep strain measurement in order to characterise the material deformation behaviour of separate regions of a multi-pass weld. The optical system was sufficiently stable to allow a sequence of photographs to be taken suitable for DIC analysis of creep specimens tested at a temperature of 545 °C for over 2000 h. The images were analysed to produce local creep deformation curves from two cross-weld samples cut from contrasting regions of a multi-pass V-groove weld joining thick-section AISI Type 316H austenitic stainless steel. It is shown that for this weld, the root pass is the weakest region of the structure in creep, most likely due to the large number of thermal cycles it has experienced during the fabrication process. The DIC based measurement method offers improved spatial resolution over conventional methods and greatly reduces the amount of material required for creep characterisation of weldments.     

Linear viscoelastic behavior of asphalt and asphalt based mastic

The rheological properties of an asphalt mastic and its matrix are investigated. For the purpose of comparison a sample of thermal aged asphalt matrix is also considered. Dynamic and creep shear measurements are reported. The reduced shear rate concept proposed by Ohl and Gleissle is used to correlate mechanical properties of the three materials at the same temperature. We found that the concept gives only qualitative trends. A similar conclusion is found concerning the applicability of the time-temperature superposition principle for each sample. Our experimental results show also that the increase in viscosity due to thermal treatment or to the inclusion of solid particles is not uniform with temperature. The differences in the increase of the Vogel temperature from the asphalt to the mastic, or to the thermally aged asphalt, relate to the different mechanisms involved. Sedimentation of steel spheres in asphalt and mastic, is studied next. The Newtonian wall correction factor for the Stokes drag law holds for the three samples. Despite the similar behavior observed in conventional shear tests, Stokes' law gives the correct trend for the two asphalts although it overestimates the experimental settling velocity by a factor of approximately two in the case of the mastic. Received: 8 June 1999/Accepted: 19 October 1999     

A carbon nanotube sensor for wall shear stress measurement

A novel carbon nanotube (CNT) sensor is being developed to measure the mean and fluctuating wall shear stress (WSS) in a turbulent boundary layer. The CNT WSS sensor is based on the thermal principle and featured by high spatial and temporal resolutions (in the order of nm and kHz, respectively), low power consumption (in the order of μW), and a compact fabrication process compared with traditional WSS measurement sensors. The CNT WSS-sensing element was characterized in detail before its calibration. The CNT sensor was operated under a constant temperature (CT) operation mode and an overheat ratio range of −0.15 to −0.19 and calibrated in a fully developed turbulent channel flow. It has been observed for the first time in a macroscopic flow that the sensor output power is approximately proportional to the 1/3 powered WSS, as expected for a thermal-principle-based WSS sensor, and the wall shear stress measurement is demonstrated for a low Reynolds number flow.     

Steady shear rheology of dilute polystyrene particle gels

This paper describes an experimental study on dispersions of monodisperse polystyrene (PS) spheres with a typical radius of 1 μm, dispersed in an electrolyte at high ionic strength, screening the electrostatic repulsion. These suspensions gelate at rest even at low volume fractions of PS particles. The density of the particles is matched with the solvent by using deuterium oxide for volume fractions φ≤0.117. Steady-state flow curves, viscosity as a function of shear rate, are measured and reported for 0.014<φ<0.322. The measured flow curves are analyzed on the basis of two models: 1. In the giant floc model (van Diemen and Stein 1983, 1984; Schreuder et al. 1986, 1987; Laven et al. 1988), at low shear rates, the shear is not distributed homogeneously but is limited to certain shear planes; the energy dissipation during steady flow is due primarily to overcoming the viscous drag on the suspended particles during motion caused by encounters of particles in the shear planes. Though this model was developed for higher solid volume fractions (0.35–0.425), we found that it also describes the rheology of dilute particle gels for 0.15≤φ≤0.3, using the same values for the parameters in the model as in the high solid volume fraction region. For φ<0.15, the model also describes the data if the fraction of distance by which a moving particle entrains its neighbors, is assumed to increase in this φ region. 2. The model of de Rooij (de Rooij et al. 1993, 1994) considers aggregates in shear flow to be monodisperse impermeable spheres with a fractal structure. The permeability is taken into account by considering a hydrodynamic radius smaller than the gyration radius in the Krieger-Dougherty expression for the hydrodynamic contribution to the viscosity. Through the use of a yield criterion the aggregate radius is modeled as a function of shear rate. We found that the model describes our experimental results, with a combination of parameter values used already by de Rooij, but only for φ<0.15. Received: 7 May 1998 Accepted: 22 December 1998     

切应力对牛骨蠕变变形的影响研究

骨尤其是湿骨,在恒定载荷作用下会发生蠕变变形。为了确定切应力是否影响骨的蠕变变形,采用对骨薄板试样分别施加集中载荷和均布载荷的方式,测量试样挠度实时的变化曲线。结果显示,在载荷恒定时,骨试样的挠度随时间不断增加,体现了典型的蠕变特性。集中荷载下骨的蠕变变形远大于均布荷载下骨的蠕变变形,湿骨的蠕变位移比干骨高近7倍。分析认为,对试样粘弹性性质的影响不仅有正应力的作用,也有切应力的作用;切应力产生的蠕变变形约为正应力所产生蠕变变形的0.85倍。     

Evaluation of the Effect of Thermal Oxidation and Moisture on the Interfacial Shear Strength of Unidirectional IM7/BMI Composite by Fiber Push-in Nanoindentation

Fiber push-in nanoindentation is conducted on a unidirectional carbon fiber reinforced bismaleimide resin composite (IM7/BMI) after thermal oxidation to determine the interfacial shear strength. A unidirectional IM7/BMI laminated plate is isothermally oxidized under various conditions: in air for 2 months at 195 °C and 245 °C, and immersed in water for 2 years at room temperature to reach a moisture-saturated state. The water-immersed specimens are subsequently placed in a preheated environment at 260 °C to receive sudden heating, or are gradually heated at a rate of approximately 6 °C/min. A flat punch tip of 3 μm in diameter is used to push the fiber into the matrix while the resulting load-displacement data is recorded. From the load-displacement data, the interfacial shear strength is determined using a shear-lag model, which is verified by finite element method simulations. It is found that thermal oxidation at 245 °C in air leads to a significant reduction in interfacial shear strength of the IM7/BMI unidirectional composite, while thermal oxidation at 195 °C and moisture concentration have a negligible effect on the interfacial shear strength. For moisture-saturated specimens under a slow heating rate, there is no detectable reduction in the interfacial shear strength. In contrast, the moisture-saturated specimens under sudden heating show a significant reduction in interfacial shear strength. Scanning electron micrographs of IM7/BMI composite reveal that both thermal oxidation at 245 °C in air and sudden heating induced microcracks and debonding along the fiber/matrix interface, thereby weakening the interface, which is the origin of failure mechanism.     

Viscoelasticity: Fractal parameters studied on mammalian erythrocytes under shear stress

In this work, experimental determinations are carried out using a home-made device called an erythrodeformeter, which has been developed and constructed for rheological measurements on red blood cells subjected to definite fluid shear stress. A numerical method formulated on the basis of the fractal approximation for ordinary and fractionary Brownian motion¹ is proposed to evaluate the viscoelastic behavior of mammalian erythrocyte membranes. The diffraction pattern, which is circular when the mammalian erythrocyte membranes are at rest, becomes elliptical when the cells undergo shear stress. Photometric readings of light intensity variation along the major axis of the elliptical diffraction pattern are recorded during the creep and recovery process. These data series are used to calculate, fractal rheological parameters of self-affine Brownian motion on the erythrocytes, averaged over several millions of cells. Three different parameters over the time dependent process could be obtained, which are: correlation coefficient <C(t)>, correlation integral, andK ₂-entropy, and very different results were obtained.     

A Measuring System for Bulk and Shear Characterization of Polymers

This paper describes a novel measuring system for investigating the influence of pressure and temperature on the mechanical properties of time-dependent polymer materials. The system can measure the volume and the shear relaxation moduli of solid polymer specimens simultaneously subjected to temperatures from −50 to +120°C with a precision of ±0.01°C, and pressures from atmospheric to 500 MPa with a precision of ±0.1 MPa. The paper demonstrates the measuring capabilities of the apparatus. For poly(vinyl) acetate (PVAc) are presented sample measurements of the shear relaxation modulus as function of time, pressure and temperature; specific volume; the bulk creep compliance; the coefficient of thermal expansion; the bulk modulus; and the pressure drop experiments which simulate conditions to which a material is exposed during the injection molding process. The shear moduli may be measured in the range from 1 to 4,000 MPa with the relative error of 3%.The error of volumetric measurements is 0.05%, which corresponds to 0.00005 cm³/g. In all cases results are shown as measured, no additional smoothing or filtering was employed. This paper is dedicated to Professor Nicholas W. Tschoegl on the occasion of his 87th birthday, for his contributions to the field of time-dependent bulk properties of polymeric materials.     

Effect of tube diameter on Preston tube calibration curves for the measurement of wall shear stress

The effect of tube diameter (d) on Preston tube calibration curves for the measurement of wall shear stress (τ_w) in a zero pressure gradient turbulent boundary layer has been investigated. Five different outside diameter tubes of 1.46, 1.82, 3.23, 4.76 and 5.54 mm, corresponding to (d/δ) of 0.022, 0.027, 0.048, 0.071 and 0.082 were used to measure τ_w at Reynolds numbers based on momentum thickness (R_θ) of 2800–4100. The calibration curves of Patel (V.C. Patel, J. Fluid Mech. 23 (part I) (1965) 185–208) and Bechert (D.W. Bechert, AIAA J. 34 (1) (1995) 205–206) are both dependent on the tube diameter. The maximum difference in the τ_w measurements from the different tubes using Patel's calibration is about 8%, while Bechert's calibration gives a maximum difference of approximately 18%.     

Turbulence structure in a diabatically heated forest canopy composed of fractal Pythagoras trees

We investigate the turbulent flow through a heterogeneous forest canopy by high-resolution numerical modeling. For this purpose, a novel approach to model individual trees is implemented in our large-eddy simulation (LES). A group of sixteen fractal Pythagoras trees is placed in the computational domain and the tree elements are numerically treated as immersed boundaries. Our objective is to resolve the multiscale flow response starting at the diameter of individual tree elements up to the depth of the atmospheric surface layer. A reference run, conducted for the forest flow under neutral thermal stratification, produces physically meaningful turbulence statistics. Our numerical results agree quantitatively with data obtained from former field-scale LESs and wind tunnel experiments. Furthermore, the numerical simulations resolve vortex shedding behind individual branches and trunks as well as the integral response of the turbulent flow through the heterogeneous forest canopy. A focus is the investigation of the turbulence structure of the flow under stable thermal stratification and in response to the heating of the fractal tree crowns. For the stratified flows, statistical quantities, e.g. turbulent kinetic energy and vorticity, are presented and the turbulent exchange processes of momentum and heat are considered in detail. The onset and formation of coherent structures such as elevated shear layers above the diabatically heated forest canopy are analyzed. For the stably stratified flow, temperature ramps above the forest canopy were simulated in agreement with previous observations. Thermally driven vortices with a typical diameter of the canopy height were simulated when the tree crowns were diabatically heated. The impact of the coherent flow structures on the heat flux is investigated.     

Creep simulation of asymmetric effects by use of stress mode dependent weighting functions

The paper presents a framework for creep modeling of materials exhibiting different behaviors in different loading scenarios, such as tension, compression and shear, respectively. To this end an additive decomposition of the flow rule is assumed into a sum of weighted stress mode related quantities. The characterization of the stress modes is obtained in the octahedral plane of the deviatoric stress space in terms of a single scalar variable, such that stress mode dependent scalar weighting functions can be constructed. Furthermore the numerical implementation into a finite element program of the resulting set of constitutive equations and aspects of the sensitivity analysis for parameter identification are addressed. Verification of the constitutive equations is succeeded for an aluminum alloy AK4-1T and a superalloy René 95, respectively. In two finite element examples the proposed model is applied to investigate the relaxation behavior of a square plate with circular hole and the evolution of creep damage in a gasturbine blade subjected to centrifugal and thermal loads.     

单层微通道热沉拓扑结构对芯片中心热点的降温效能研究

通过热流固耦合模拟分析得到了不同微通道结构热沉基底的温度场及微通道内速度场,研究了相同入流功率下不同单层微通道拓扑结构对中心有高热流密度热点芯片的散热能力。结果表明:相同入流功率(0.05W)下,不同结构的散热能力排序由高到低为Y分形、弯曲散射、直散射(双侧出流)、直螺旋、直散射(单侧出流)、圆螺旋、树状分形、直槽结构;采用中心入流可有效降低芯片中心热点附近的温度,对于中心入流的散射结构,采用对称出流结构可提升其流动传热性能;Y分形结构具有良好的流动传热特性,对于热源面和中心热点均具有良好的散热效果。     

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。     

平纹编织陶瓷基复合材料面内剪切细观损伤行为研究

采用约西佩斯库(Iosipescu)纯剪切试件,研究了平纹编织SiC/SiC和C/SiC复合材料的面内剪切应力-应变行为和细观损伤特性.通过试验获得了材料不同方向上的单调和迟滞应力-应变行为,对比分析了两种材料的剪切损伤特性,结果表明材料的剪切损伤演化规律受热残余应力水平影响严重.由试件断口电镜扫描结果发现剪切加载状态下桥连纤维承受显著的弯曲载荷和变形,据此提出了纤维弯曲承载机制,并结合裂纹闭合效应分阶段阐释了材料的剪切迟滞环形状.基于材料的剪切细观损伤机制,通过两个损伤变量表征了材料的剪切损伤演化进程,得到了材料的面内剪切细观损伤演化模型.对比发现2D-C/SiC复合材料45°方向基体裂纹的起裂应力明显小于2D-SiC/SiC复合材料,而两者0°/90°方向裂纹的起裂应力基本相同.