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.     

High-frequency viscoelasticity of crosslinked actin filament networks measured by diffusing wave spectroscopy

We study the short-time relaxation dynamics of crosslinked and uncrosslinked networks of semi-flexible polymers using diffusing wave spectroscopy (DWS). The networks consist of concentrated solutions of actin filaments, crosslinked with increasing amounts of α-actinin. Actin filaments (F-actin) are long semi-flexible polymers with a contour length 1–100μm and a persistence length of 5–15μm; α-actinin is a small 200kDa homodimer with two actin-binding sites. Using the large bandwidth of DWS, we measure the mean-square-displacement of 0.96μm diameter microspheres imbedded in the polymer network, from which we extract the frequency-dependent viscoelastic moduli via a generalized Langevin equation. DWS measurements yield, in a single measurement, viscoelastic moduli at frequencies up to 10⁵Hz, almost three decades higher in frequency than probed by conventional mechanical rheology. Our measurements show that the magnitude of the small-frequency plateau modulus of F-actin is greatly enhanced in the presence of α-actinin, and that the frequency dependence of the viscoelastic moduli is much stronger at intermediate frequencies. However, the frequency-dependence of loss and storage moduli become similar for both crosslinked and uncrosslinked networks at large frequencies, G′(ω)∝G′′(ω)∝ω^0.75±0.08. This high-frequency behavior is due to the small-amplitude, large-frequency lateral fluctuations of actin filaments between entanglements. Received: 20 January 1998 Accepted: 12 February 1998     

Broadband Identification of Material Properties of an Orthotropic Composite Plate Using the Force Analysis Technique

This work presents an original broadband method able to determine the homogenized mechanical properties of orthotropic composite plates in their main directions. This method is based on a vibratory inverse method and do not need using Eigen mode. This technique is derived from the Force Analysis Technique (FAT), originally designed to identify vibration sources on bars and plates. The main advantage of this method is that it does not require any specific preparation and can be carried out on a real and complex structure. Moreover it is non-destructive and non-invasive method and only requires the excitation by a classical electromagnetic shaker. The main characteristic mechanical parameters (Young’s moduli and damping loss factors) are identified at all measured frequencies and not only at the Eigen frequencies as compared to others measurement techniques. An experimental validation shows a good correlation with the expected values for the Young’s moduli of the test plate. Working on a complex structure shows that the method is applicable for various configurations of operating conditions and leads to a good determination of the mechanical properties of a planar component.     

Dynamic shear and compressional behavior of polydimethylsiloxanes: Ultrasonic and low frequency characterization

The dynamic rheological properties of a series of entangled polydimethylsiloxanes are investigated. Rheometrical shear measurements are first reported for three different molecular weight samples, together with ultrasonic tests, thus allowing to obtain dynamic shear master curves over ten decades. Winter‘s model for slightly polydisperse polymers is used and works well in this case. This provides an example of the applicability of this model. The propagation of longitudinal waves in the MHz range for the same PDMSs is studied next. The results are analyzed and combined with static measurements of the compressibility. They indicate that different relaxation mechanisms have to be considered in shear and compression, and that the ratio between volume and shear viscosity is frequency dependent, with a preponderance for shear effects at higher frequencies. Shear and compressional relaxational mechanisms are also well separated. Moreover, it is verified that the shear and compressional moduli are independent of the molecular weight in the transition region, above a certain frequency. This frequency corresponds to a wavelength comparable to the distance between entanglements, in the case of shear waves. Received: 9 December 1997 Accepted: 30 March 1998     

固体的弹性模量和内耗测量方法研究进展

弹性模量和内耗是固体材料的基本力学性质, 其测量的准确性和便捷性对工业生产和科学研究都很重要. 本文回顾了近一百年来固体材料弹性模量和内耗的测量方法, 主要分为四类: 准静态方法、低频法、共振法和波传播法. 首先对每类方法的测量原理进行了简单介绍及总体评价. 接着对几种共振方法, 包括自由梁共振法、脉冲激励法、超声共振谱方法和压电超声复合振动技术(PUCOT)进行了详细介绍和评价. 然后, 重点介绍了本课题组最新提出的基于机电阻抗的模量内耗测量方法(称之为M-PUCOT或Q-EMI), 它可以同时、准确、快速地测量杨氏/剪切模量及相应内耗. 最后, 对这种新型弹性模量/内耗测量方法的意义和应用前景进行了讨论和展望.      

Generalized Maxwell model for the viscoelastic behavior of a soda-lime-silica glass under low frequency shear loading

The linear viscoelastic behavior of a soda-lime-silica glass under low frequency shear loading is investigated in the glass transition range. Using the time-temperature superposition technique, the master curves of the shear dynamic relaxation moduli are obtained at a reference temperature of 566°C. A method to determine the viscoelastic constants from dynamic relaxation moduli is proposed. However, some viscoelastic constants cannot be directly measured from the experimental curves and others cannot be precisely obtained due to non-linearity effects at very low frequencies. The generalized Maxwell model is investigated from the experimental dynamic moduli without fixing the viscoelastic constants. A set of parameters is shown to be in good agreement with the experimental dynamic relaxation moduli, but does not give the correct values of the viscoelastic constants of the investigated glass. The soda-lime-silica glass exhibits a non-linear viscoelastic behavior at very low stress level which is usually observed for organic glasses. This non-linear behavior is questioned.     

Closed-form solution for horizontal and vertical shiftings of viscoelastic material functions in frequency domain

The closed-form shifting (CFS) algorithm is a simple mathematical methodology which determines the unique solution in the process of constructing master curves at selected reference temperature and pressure conditions. In a previous paper, the CFS algorithm has been fully described for monotonically increasing or monotonically decreasing functions only. This paper presents detailed steps of the generalized CFS methodology for non-monotonic functions, like the loss tangent. Performing shifting on the loss tangent, which does not require vertical shifting, is particularly important for materials which require vertical adjustment of dynamic viscoelastic functions, i.e., loss and storage moduli. Thus, based on horizontal shifting of the loss tangent, the CFS-based procedure of consecutive horizontal-vertical superposition for the storage modulus is proposed and analyzed. The analysis is done on the example of two synthetically generated non-monotonic tan delta segments and corresponding storage modulus segments in respect to different experimental parameters. It has been shown that the error brought by the shifting method into non-monotonic loss tangent and storage modulus master curves is twice smaller than the corresponding experimental noise level.     

基于导波技术的螺柱轴力无损检测

根据弹性动力学理论,采用纵向导波与弯曲导波相结合的方法对螺柱所受轴向应力进行无损检测。计算了M22螺柱中纵向导波和弯曲导波的群速度频散曲线。根据频散曲线,确定了采用导波对螺柱轴向应力进行无损检测的最优检测信号频率范围(50~80 kHz),此频率范围的纵向导波与弯曲导波模态单一,并且频散性较低。分别计算了不同轴向应力σ作用下,多种频率的纵向导波和和弯曲导波在螺柱中传播的群速度值cgσrL和cgσrF。结果表明,随着轴向应力的增大,同频率纵向导波和弯曲导波的群速度皆呈线性递减趋势。利用纵向导波和弯曲导波群速度与轴向应力的线性关系及纵向导波和弯曲导波在轴向应力作用螺柱端面的反射时间tLσ和tσF,可以迅速确定螺柱所受轴向应力值。     

Microstructural effects on the dynamic rheology of a discotic mesophase pitch

The dynamic rheology and accompanying microstructure of a synthetic mesophase pitch (AR-HP) is reported. The loss modulus (G″) was found to be higher than the storage modulus (G′) at all frequencies (∼0.1 to ∼100 rad/s) and temperatures (280–305 °C) tested. The slope of the low-frequency terminal zone for G′ was found to be approximately 0.8, much lower than a value of 2 that is observed for flexible chain polymers. Cross-polarized optical microscopy with full-wave retardation plate confirmed the presence of different textures of mesophase pitch processed under different conditions. While loss moduli remained fairly unchanged, finer textures led to significantly lower storage moduli. Consistent with this trend, coarsening of the microstructure during textural relaxation led to an increase in storage moduli. Therefore, for the discotic mesophase pitch, the viscous component was found to remain unaffected by the microstructure, but the elastic modulus was dependent on the orientation of layer-planes and size of the texture.     

Resonance in Polyurea-Based Multilayer Structures Subjected to Laser-Generated Stress Waves

We report resonance associated with polyurea layers sandwiched between identical acrylic and polycarbonate plates when subjected to laser-generated stress waves of several nanoseconds in duration. Transmitted stress wave amplitudes almost 16 times the incident stress wave amplitudes are observed. An elastodynamics simulation identified the thickness of the polyurea layer as the key parameter controlling the amplitude of the transmitted stress wave. This resonance effect was found absent when the polyurea was sandwiched between the steel and aluminum plates of similar thickness. However, for these samples, a dramatic reduction in the amplitudes of the transmitted stress waves was recorded. A finite element analysis of the wave propagation through the sandwiched polyurea layer in these samples tied the large amplitude reduction to the large acoustic impedance mismatch and the viscoelastic dissipation within the polyurea layer.     

Comparison of Low Impedance Split-Hopkinson Pressure Bar Techniques in the Characterization of Polyurea

The split-Hopkinson pressure bar (SHPB) technique has been widely employed for over fifty years in characterizing the high strain-rate properties of many common engineering materials. Historically, however, this technique has had limited success in characterizing soft materials, since their low mechanical impedances can increase delays in attaining dynamic equilibrium and result in transmission pulses with extremely low signal-to-noise ratios. Due to interest in improving characterization of soft materials at high strain rates, numerous modifications to the traditional SHPB technique have been proposed. These include: using more sensitive piezoelectric gauges, employing hollow transmission bars, utilizing lower impedance polymeric pressure bars, and the use of pulse shaping techniques. To date, there has been no comparative studies or consensus within the SHPB community as to which approach is most advantageous. The goal of this investigation is to compare a number of these techniques, specifically the use of PMMA pressure bars and a hollow aluminum transmission bar (both with and without pulse shaping), alongside more traditional solid aluminum pressure bars in the characterization of polyurea, a common low impedance polymer. The advantages and disadvantages of each technique in generating high strain-rate stress-strain curves are discussed.     

Memory decay rates of viscoelastic solids: not too slow, but not too fast either

Fading memory is a distinguishing characteristic of viscoelastic solids. Its assessment is often achieved by measuring the stress due to harmonic strain histories at different frequencies: from the experimental point of view, the storage and loss moduli are, hence, introduced. On the other side, the mathematical modeling of viscoelastic materials is usually based on the consideration of a kernel function whose decay rate is sufficiently fast. For several different solid materials, we have collated experimental evidence showing an high sensitivity to frequency variations of both the storage and loss moduli. By contrast, we prove that the commonly employed viscoelastic kernels (Prony series, continuous kernel, etc.) cannot reproduce this experimental behavior, as the resulting frequency sensitivity of the storage modulus is always zero when assessed at low frequency. This leads to identification problems of the material parameters which are strongly ill conditioned. However, we identify the specific kernel property which is responsible for this misbehavior: the long-term material memory must not decrease too fast. Some viscoelastic kernels, showing the correct memory??s rate of decay, are introduced and their improved ability to match the experimental data analyzed.     

Extensional and shear rheometry of oriented triblock copolymers

 The effects of extensional flow orientation on the rheological properties of two poly(styrene)-poly(ethylene-co-butylene)-poly (styrene) (PS-PEB-PS) triblock copolymers containing either spherical or cylindrical PS microdomains were studied by oscillatory shear and oscillatory extensional experiments. Extensional measurements revealed that below the PS block glass transition temperature pre-oriented triblocks display highly anisotropic mechanical properties. For both polymers, the storage modulus E ′ is higher along the flow direction. Above the PS glass transition temperature the materials are no longer anisotropic and the same storage moduli are obtained along the flow direction and perpendicular to it. Above the PS glass transition temperature the rheological behaviour parallel and perpendicular to the flow direction was also probed in pre-oriented and non-oriented samples by oscillatory shear rheometry. At high frequencies, the mechanical response of the triblocks was found to be independent of the orientation for both copolymers while at low frequencies a strong effect of the flow orientation could be observed. For both polymers the value of the storage modulus was found to be lower along the flow direction that perpendicular to it. This was explained by the ability of PS blocks to relax more easily along the flow direction. Received: 10 September 1999/Accepted: 1 October 1999     

Oscillating plate viscometer in the Hz to kHz range

A low and audio frequency viscometer with a frequency range 2 Hz to 1 kHz and possibly up to 10 kHz is described, which shears a liquid sample (shear volume < 0.3 ml) between an oscillating glass plate and the wall of a cuvette. Alternating velocity and force exerted on the oscillating plate are measured by a mechanical impedance head, designed for the frequency range 1 Hz to 10 kHz. This device permits the determination of frequency dependent viscous liquid properties. Real and imaginary part of the complex viscosity can be obtained from the complex mechanical impedance. Inertial forces from the oscillating plate are compensated in an adjustable electronic circuit.Significant shear parameters, as the frequency, the exciting wave form and the amplitude, can be set independently. In this way viscous spectral data and also nonlinear properties can be studied, e.g., in aqueous DNA solutions. In addition, processes with time constants >0.1 s in (relaxing) viscoelastic systems, which do not obey the Boltzmann superposition principle, can be monitored by means of the (nonlinear) modulation of an LF sampling signal. Some examples of measurements will be shown. Model calculations for water and for glycerol give typical values for the complex impedances to be obtained with this oscillatory rheometric device.     

Blast Mitigation in a Sandwich Composite Using Graded Core and Polyurea Interlayer

The dynamic behavior of two types of sandwich composites made of E-Glass Vinyl-Ester (EVE) facesheets and Corecell™ A-series foam with a polyurea interlayer was studied using a shock tube apparatus. The materials, as well as the core layer arrangements, were identical, with the only difference arising in the location of the polyurea interlayer. The foam core itself was layered with monotonically increasing wave impedance of the core layers, with the lowest wave impedance facing the shock loading. For configuration 1, the polyurea interlayer was placed behind the front facesheet, in front of the foam core, while in configuration 2 it was placed behind the foam core, in front of the back facesheet. A high-speed side-view camera, along with a high-speed back-view 3-D Digital Image Correlation (DIC) system, was utilized to capture the real time deformation process as well as mechanisms of failure. Post mortem analysis was also carried out to evaluate the overall blast performance of these two configurations. The results indicated that applying polyurea behind the foam core and in front of the back facesheet will reduce the back face deflection, particle velocity, and in-plane strain, thus improving the overall blast performance and maintaining structural integrity.     

High-bandwidth one-and two-particle microrheology in solutions of wormlike micelles

We have developed a large-bandwidth two-particle microrheology technique to measure loss and storage moduli of viscoelastic materials from 0.1 Hz to about 100 kHz using laser trapping and interferometry. We found that quantitative agreement between one- and two-particle microrheology exist in entangled solutions of wormlike micelles chosen as a simple model viscoelastic system. These results validate both experimental method and data interpretation. The consistent results also prove that in a simple system, where the solution length scales are much smaller than the micron probe size, one-particle microrheology can accurately measure bulk viscoelastic parameters.This paper was presented at the AERC 2005     

Plane waves in linear elastic materials with voids

The behavior of plane harmonic waves in a linear elastic material with voids is analyzed. There are two dilational waves in this theory, one is predominantly the dilational wave of classical linear elasticity and the other is predominantly a wave carrying a change in the void volume fraction. Both waves are found to attenuate in their direction of propagation, to be dispersive and dissipative. At large frequencies the predominantly elastic wave propagates with the classical elastic dilational wave speed, but at low frequencies it propagates at a speed less than the classical speed. It makes a smooth but relatively distinct transition between these wave speeds in a relatively narrow range of frequency, the same range of frequency in which the specific loss has a relatively sharp peak. Dispersion curves and graphs of specific loss are given for four particular, but hypothetical, materials, corresponding to four cases of the solution.     

Simulation-based conceptual design of an acoustic metamaterial with full band gap using an air-based 1-3 piezoelectric composite for ultrasonic noise control

This paper aims at proposing a novel type of acoustic metamaterials with complete band gap composed of piezoelectric rods with square array as inclusions embedded in an air background (matrix). A modified plane wave expansion method accompanied with the principles of the Bloch–Floquet method with electromechanical coupling effect and also impedance spectra are used to get a band frequency and to investigate the passband for the selected cut of piezoelectric rods. We investigate both the electromechanical coupling coefficient and mechanical quality factor and their dependency to passband and bandwidth, which depends on both the density and the wave impedance of the matrix and the inclusions (rods). The ratio of the volume of inclusion to the matrix is used to define the fill factor or the so-called inclusion ratio, to introduce the bandwidth as a function of that. Furthermore, the fabrication method is presented in this paper. The results make a suitable foundation for design purposes and may develop an inherently passive ultrasonic noise control. In addition, the results provide the required guidance for a simulation-based design of elastic wave filters or wave guide that might be useful in high-precision mechanical systems operated in certain frequency ranges and switches made of piezoelectric materials; they also propose a novel type of elastic metamaterials, which is independent of the wave direction and has an equal sensitivity in all directions in which it reacts omnidirectionally and mitigates the occupational noise exposure.