On the Measurement of two Independent Viscoelastic Functions with Instrumented Indentation Tests

In the present paper, a methodology for complete characterization of linear isotropic viscoelastic material with spherical instrumented indentation test is proposed. The developed method allows for measuring two independent viscoelastic functions, shear relaxation modulus and time-dependent Poisson’s ratio, from the indentation test data obtained at non-decreasing loading, but otherwise arbitrary. Finite element modelling (FEM) is relied upon for validating the proposed methodology and for quantifying the influence of experimental variables on the measurements accuracy. Spherical indentation experiments are performed on several viscoelastic materials: polyoxymethylene, bitumen and bitumen-filler mastics. The viscoelastic material functions obtained with the indentation tests are compared with the corresponding results from the standard mechanical tests. Numerical and experimental results presented indicate that the methodology proposed allows mitigating the machine compliance and loading rate effects on the accuracy of the viscoelastic indentation tests.     

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.     

Nonlinearly Viscoelastic Nanoindentation of PMMA Under a Spherical Tip

The Oliver-Pharr method has been well established to measure Young’s modulus and hardness of materials without time-dependent behavior in nanoindentation. The method, however, is not appropriate for measuring the viscoelastic properties of materials with pronounced viscoelastic effects. One well-known phenomenon is the formation of unloading “nose” or negative stiffness during unloading that often occurs during slow loading-unloading in nanoindentation on a viscoelastic material. Most methods in literature have only considered the loading curve for analysis of viscoelastic nanoindentation data while the unloading portion is not analyzed adequately to determine the nonlinearly viscoelastic properties. In this paper, nonlinearly viscoelastic effects are considered and modeled using the nonlinear Burgers model. Nanoindentation was conducted on poly-methylmethacrylate (PMMA) using a spherical indenter tip. An inverse problem solving approach is used to allow the finite element simulation results to agree with the nanoindentation load–displacement curve during the entire loading and unloading stage. This approach has allowed the determination of the nonlinearly viscoelastic behavior of PMMA at submicron scale. In addition, the nanoindentation unloading “nose” has been captured by simulation, indicating that the negative stiffness in the viscoelastic material is the result of memory effect in time-dependent materials.     

Methods of interconversion between linear viscoelastic material functions. Part I—a numerical method based on Prony series

An efficient and accurate numerical method of interconversion between linear viscoelastic material functions based on a Prony series representation is presented and tested using experimental data from selected polymeric materials. The method is straightforward and applicable to interconversion between modulus and compliance functions in time, frequency, and Laplace transform domains. Good agreement is shown between solutions obtained from the method in different domains. A detailed computational procedure and selection of values for parameters involved in the method are presented and illustrated. In particular, the effects of different choices of relaxation and retardation times on the accuracy of the method are discussed. The mathematical efficiency associated with Prony series representations of both source and target transient material functions is fully utilized. The method is general enough to cover both viscoelastic solids and liquids. The tensile relaxation data from polymethyl methacrylate (PMMA) and the shear storage compliance data from polyisobutylene are used in illustrating the method. In a companion paper (Schapery and Park, 1998) , an extended approximate analytical interconversion method is presented.     

Modelling viscoelastic materials whose storage modulus is constant with frequency

This paper presents a relaxation function characterising viscoelastic materials whose storage modulus is constant with frequency, and whose loss factor shows the representative peak of damping materials. This behaviour is typical of some composite materials, where the elastic constituents give the constant modulus, and the polymeric components provide the variable loss factor. The new model gives a way to provide comparative data for different materials in a form which can easily be incorporated into simulations. The physical meaning of the model parameters is defined from the analysis of the complex modulus in frequency domain. The presented relaxation function is validated by curve fitting to experimental measurements carried out on polymer concrete specimens, made of epoxy resin matrix with mineral aggregates.     

Characterization of viscoelastic properties of polymeric materials through nanoindentation

Nanoindentation testing was used to determine the dynamic viscoelastic properties of eight polymer materials, which include three high-performance polymers and five densities of high-density polyethylene. It was determined that varying the harmonic frequency of nanoindentation does not have a significant effect on the measured storage and loss moduli of the polymers. Agreement was found between these nanoindentation results and data from bulk dynamic mechanical testing of the same materials. Varying the harmonic amplitude of the nanoindentation had a limited effect on the measured viscoelastic properties of the resins. However, storage and loss moduli from nanoindentation were shown to be sensitive to changes in the density of the polyethylene.     

关于黏弹性材料的广义Maxwell模型

采用流变力学分析黏弹性材料的流变特性时，常要用到广义Maxwell模型 表达的应力松弛模量. 而从试验中获得的应力松弛模量，其表达式常为 Kohlrausch-William-Watts function(KWW函数)形式. 通过把KWW函数和广义Maxwell模型的拟合问题转化为两 矩阵相等的求解问题后，又把两矩阵的相等等价于两矩阵差值向量的一阶范数为无穷小的问 题，并通过引入广义逆矩阵，求得两矩阵差值向量的一阶范数的最小值，最后以一阶范数的 最小值为目标函数，松弛时间为约束条件，利用单纯形法对两矩阵差值向量的一阶范数的最 小值优化，从而提出了一种针对黏弹材料的KWW函数与广义Maxwell模型转换的计算方法. 借助于MATLAB软件，实现了对黏弹材料的广义Maxwell模型的拟合.     

Non-linear viscoelastic behavior of polymer melts interpreted by fractional viscoelastic model

Very recently, researchers dealing with constitutive law pertinent viscoelastic materials put forward the successful idea to introduce viscoelastic laws embedded with fractional calculus, relating the stress function to a real order derivative of the strain function. The latter consideration leads to represent both, relaxation and creep functions, through a power law function. In literature there are many papers in which the best fitting of the peculiar viscoelastic functions using a fractional model is performed. However there are not present studies about best fitting of relaxation function and/or creep function of materials that exhibit a non-linear viscoelastic behavior, as polymer melts, using a fractional model. In this paper the authors propose an advanced model for capturing the non-linear trend of the shear viscosity of polymer melts as function of the shear rate. Results obtained with the fractional model are compared with those obtained using a classical model which involves classical Maxwell elements. The comparison between experimental data and the theoretical model shows a good agreement, emphasizing that fractional model is proper for studying viscoelasticity, even if the material exhibits a non-linear behavior.     

The total creep of viscoelastic composites under hydrostatic or antiplane loading

The problem of bounding the total creep (or total stress relaxation) of a composite made of two linear viscoelastic materials and subjected to a constant hydrostatic or antiplane loading is considered. It is done by coupling the immediate and the relaxed responses of the composite, which are pure elastic. The coupled bounds provide the possible range of the total deformation at infinite time as a function of the initial deformation of the composite. For antiplane shear existing bounds for coupled two-dimensional conductivity yield the required coupled bounds, and these are attained by doubly coated cylinder assemblages. The translation method is used to couple the effective bulk moduli of a viscoelastic composite at zero and infinite time. A number of microgeometries are found to attain the bulk modulus bounds. It is shown that the Hashin's composite sphere assemblage does not necessarily correspond to the maximum or minimum overall creep, although it necessarily attains the bounds for effective bulk moduli. For instance, there are cases when the doubly coated sphere microstructure or some special polycrystal arrangements attain the bounds on the total creep.     

From dynamic modulus via different relaxation spectra to relaxation and creep functions

The main goal of the paper is to compare predictive power of relaxation spectra found by different methods of calculations. The experimental data were obtained for a new family of propylene random copolymers with 1-pentene as a comonomer. The results of measurements include flow curves, viscoelastic properties, creep curves and rubbery elasticity of copolymer melts. Different relaxation spectra were calculated using independent methods based on different ideas. It lead to various distributions of relaxation times and their “weights”. However, all of them correctly describe the frequency dependencies of dynamic modulus. Besides, calculated spectra were used for finding integral characteristics of viscoelastic behaviour of a material (Newtonian viscosity, the normal stress coefficient, steady-state compliance). In this sense all approaches are equivalent, though it appears impossible to estimate instantaneous modulus. The most crucial arguments in estimating the results of different approaches is calculating the other viscoelastic function and predicting behaviour of a material in various deformation modes. It is the relaxation and creep functions. The results of relaxation curve calculations show that all methods used give rather similar results in the central part of the curves, but the relaxation curves begin to diverge when approaching the high-time (low-frequency) boundary of the relaxation curves. The distributions of retardation times calculated through different approaches also appear very different. Meanwhile, predictions of the creep curves based on these different retardation spectra are rather close to each other and coincide with the experimental points in the wide time range. Relatively slight divergences are observed close to the upper boundary of the experimental window. All these results support the conclusion about a rather free choice of the relaxation time spectrum in fitting experimental data and predicting viscoelastic behaviour of a material in different deformation modes. Received: 15 March 2000 Accepted: 18 September 2000     

Numerical interconversion between linear viscoelastic material functions with regularization

In this paper, interconversion between linear viscoelastic material functions is studied emphasizing materials with relatively fast rate of relaxation. The aim of this paper is to study the whole material function determination process from a linear viscoelastic experiment to interconversion by taking into account non-ideal loading and noisiness of the data in such an experiment. No assumptions are made concerning the form of the relaxation modulus or the creep compliance. Interconversion is carried out by evaluating numerically the convolution integral. Three different yet similar approaches are studied. In numerical interconversion, the resulting matrix equation is ill-posed. Due to this, Tikhonov regularization is applied to solve the related matrix system. Numerical simulations indicate that reliable results can be obtained with proposed numerical procedures.     

Waterhammer modelling of viscoelastic pipes with a time-dependent Poisson's ratio

Poisson's ratio in viscoelastic materials is a function of time. However, recently developed waterhammer models of viscoelastic pipes consider it constant. This simplifying assumption avoids cumbersome calculations of double convolution integrals which appear if Poisson's ratio is time-dependent. The present research develops a mathematical model taking the time dependency of Poisson's ratio into account for linear viscoelastic pipes. Poisson's ratio is written in terms of relaxation function and bulk modulus which is assumed to be constant. The relaxation function is obtained from creep function given as the viscoelastic property data of pipe material. The results obtained from the present waterhammer model are compared with the experimental data for two different flow rates. The comparison reveals that with the application of the time-dependent Poisson's ratio and unsteady friction, the viscoelastic data of mechanical tests can directly be used for waterhammer analysis with less need for the calibration of the flow configuration. It was also shown that the creep curve calibrated based on the present model is closer to the actual creep curve than that calibrated based on previous models.     

Development of a micro-indentation device for measuring the mechanical properties of soft materials

Indentation is a simple and nondestructive method to measure the mechanical properties of soft materials, such as hydrogels, elastomers and soft tissues. In this work, we have developed a micro-indentation system with high-precision to measure the mechanical properties of soft materials, where the shear modulus and Poisson's ratio of the materials can be obtained by analyzing the load–relaxation curve. We have validated the accuracy and stability of the system by comparing the measured mechanical properties of a polyethylene glycol sample with that obtained from a commercial instrument. The mechanical properties of another typical polydimethylsiloxane sample submerged in heptane are measured by using conical and spherical indenters, respectively. The measured values of shear modulus and Poisson's ratio are within a reasonable range.     

Measurement of Temperature-Dependent Young’s Modulus at a Strain Rate for a Molding Compound by Nanoindentation

The mechanical properties of a molding compound on a packaged integrated circuit (IC) were measured by spherical nanoindentation using a 50 μm radius diamond tip. The molding compound is a heterogeneous material, consisting of assorted diameters of glass beads embedded in an epoxy. Statistical analysis was conducted to determine the representative volume element (RVE) size for a nanoindentation grid. Nanoindentation was made on the RVE to determine the effective viscoelastic properties. The relaxation functions were converted to temperature-dependent Young’s modulus at a given strain rate at several elevated temperatures. The Young’s modulus values at a given strain rate from nanoindentation were found to be in a good agreement with the corresponding data obtained from tensile samples at or below 90 °C. However, the values from nanoindentation were significantly lower than the data obtained from tensile samples when the temperature was near or higher than 110 °C, which is near the glass transition. The spatial distribution of the Young’s modulus at a given strain rate was determined using nanoindentation with a Berkovich tip. The spatial variation of the Young’s modulus at a given strain rate is due to the difference in nanoindentation sites (glass beads, epoxy or the interphase region). A graphical map made from an optical micrograph agrees reasonably well with the nanoindentation results.     

Linear viscoelastic models: Part I. Relaxation modulus and melt calibration

Constitutive models for the linear viscoelasticity of polymers are presented for the relation between the relaxation modulus and the molecular weight distribution (MWD). We also compute the MWD from a simulated relaxation modulus curve by first obtaining the rheologically effective distribution (RED) as a function of time, and converting this into the MWD by melt calibration; that is, the relation between timescale and the molecular weight. This procedure has similarities with the widely used universal calibration with solved polymers. The main principles of our technique are applied here to familiar relaxation modulus data, for which we present two models: (1) an analytical model derived from control theory, which is known capable of modelling partially observed system and (2) a practical characteristic model for obtaining usable results. No relaxation time or spectrum procedures are used to model the process of linear viscoelastic relaxation. The use of relative calculations and melt calibration dispenses with the need to know the real chain structures such as branching and entangled chain dynamics, and the model remains useful for future investigations of polymer chain structures and dynamics, such as using tube theory.     

Relations Between Relaxation Modulus and Creep Compliance in Anisotropic Linear Viscoelasticity

The results obtained previously for scalar and class P completely monotone relaxation moduli are extended to arbitrary anisotropy. It is shown for general anisotropic viscoelastic media that, if the relaxation modulus is a locally integrable completely monotone function, then the creep compliance is a Bernstein function and conversely. The elastic and equilibrium limits of the two material functions are related to each other. The relaxation modulus or its derivative can be singular at 0. A rigorous general formulation of the relaxation spectrum in an anisotropic viscoelastic medium is given. The effect of Newtonian viscosity on creep compliance is examined. Put some makeup on him and lay him to rest. Anonymous     

Influence of excitation amplitude on the characteristics of nonlinear butyl rubber isolators

The purpose of this study is to explore the advantages and characteristics of nonlinear butyl rubber (type IIR) isolators in vibratory shear by comparison with linear isolators. It is known that the mechanical properties of viscoelastic materials exhibit significant frequency and temperature dependence, and in some cases, nonlinear dynamic behavior as well. Nonlinear characteristics in shear deformation are reflected in mechanical properties such as stiffness and damping. Furthermore, even when the excitation amplitude is small the response amplitude may often be large enough that nonlinearities cannot be ignored. The treatment involves developing phenomenological models of the effective storage modulus and effective loss factor of a rubber isolator material as a function of excitation amplitude. The transmissibility of a nonlinear viscoelastic isolator is compared with that of a linear isolator using an equivalent linear damping coefficient. Forced resonance vibration and impedance tests are used to characterize nonlinear parameters and to measure the normalized transmissibility. It is found that as the excitation amplitude of the nonlinear viscoelastic isolator increases, the response amplitude decreases and the transmissibility is improved over that of the linear isolator for excitation frequency that exceeds a particular value governed by the temperature and excitation amplitude. The method of multiple scales and numerical simulations are used to predict the response characteristics of the isolator based on the phenomenological modeling under different values of system parameters.     

Relationship between single and bulk mechanical properties for zeolite ZSM5 spray-dried particles

In this work typical mechanical properties for a catalyst support material, ZSM5 （a spray-dried granular zeolite）, have been measured in order to relate the bulk behaviour of the powder material to the single particle mechanical properties. Particle shape and size distribution of the powders, determined by laser diffraction and scanning electron microscopy （SEM）, confirmed the spherical shape of the spray-dried particles. The excellent flowability of the material was assessed by typical methods such as the Hausner ratio and the Cart index, This was confirmed by bulk measurements of the particle-particle internal friction parameter and flow function using a Schulze shear cell, which also illustrated the low compressibility of the material. Single particle compression was used to characterize single particle mechanical properties such as reduced elastic modulus and strength from Hertz contact mechanics theory. Comparison with surface properties obtained from nanoindentation suggests heterogeneity, the surface being harder than the core. In order to evaluate the relationship between single particle mechanical properties and bulk compression behaviour, uniaxial confined compression was carried out. It was determined that the Adams model was suitable for describing the bulk compression and furthermore that the Adams model parameter, apparent strength of single particles, was in good agreement with the single particle strength determined from single particle compression test.     

Photoviscoelastic behavior and residual thermal birefringence in optical-grade polycarbonates

The stress-optical coefficient functions of two optical-grade polycarbonates (PCs) have been obtained by simultaneous measurements of the relaxation modulus and strain-optical coefficient functions. Nonlinear behavior of the relaxation modulus and strain-optical coefficient was observed at small strains at room temperature. Comparison of these functions in the linear region with those of a commercial grade PC was made. These functions have been incorporated to linear viscoelastic and photoviscoelastic constitutive equations to calculate residual thermal birefringence in freely quenched PC plates. The numerical results have been compared with the measurements indicating a fair agreement between them.