Transient analysis of a viscoelastic torsion pendulum

The transient torsion pendulum of arbitrary cross section is analyzed as a device for obtaining physical properties of a viscoelastic material. The damped sinusoidal motion yields a damping factor and frequency from which the complex modulus is computed. The particular cases of circular and rectangular cross section are considered with tables and approximations simplifying the practical application of the method.     

Comparison between 3-point bending and torsion methods for determining the viscoelastic properties of fiber-reinforced epoxy

Dynamic mechanical analysis is a technique used to determine the viscoelastic properties of polymers and their composites. The storage modulus, loss modulus and loss factor in correlation with the glass transition temperature can be detected by several means. In this study, these properties are determined using a dynamic mechanical analyzer in 3-point bending mode, as well as a rheometer in torsion mode. The materials under consideration are a unidirectional glass fiber-reinforced epoxy, a quasi-isotropic carbon fiber-reinforced epoxy and a quasi-isotropic glass fiber-reinforced epoxy. The results of each method and material are presented and the advantages and limitations of each method are discussed. 3-point bending proved to be more suitable to detect the effect of fiber orientation for unidirectional fiber-reinforced epoxy but requires careful control of sample dimensions for accuracy. Torsion, on the other hand, gave consistent measurements for samples of varying lengths, proving to be a suitable method if materials are scarce and limited.     

A five-parameter fractional derivative temperature spectrum model for polymeric damping materials

To capture viscoelastic behavior of polymeric damping materials based on limited dynamic mechanical analysis tests, a simple fractional temperature spectrum model representing the viscoelastic materials is proposed in this paper and experimental tests aims at stressing the validity of the model. The storage modulus, the loss modulus, and the loss factor, are established based on the five-parameter fractional derivative model and the time–temperature superposition principle. The dynamic mechanical tests of two polymeric materials are carried out to verify this temperature spectrum model. Results indicate a good agreement between the temperature spectrum model and experimental tests at various temperature conditions. Furthermore, thermodynamic coupling of the viscoelastic material is investigated by temperature rise calculation and vibration experiment test. Comparison analysis shows that the temperature rise model can simulate the temperature rise process for the shear vibration of the constrained damping, which provide references for the damping capability, thermal damage and failure of viscoelastic material.     

Effect of microstructure uncertainty and testing frequency on storage and loss moduli of injection molded MWCNT reinforced polyamide 66 nanocomposites

The viscoelastic behavior of multiwall carbon nanotube (MWCNT) reinforced polyamide 66 (PA 66) was evaluated to investigate the effect of CNT content and loading frequency on dynamic moduli (i.e. storage modulus E′ and loss modulus E″) and damping factor tan$\delta$. PA 66/CNT disk samples with five different CNT contents ranging from 3 wt % to 15 wt % were manufactured by injection molding. Testing was performed over the frequency range of 0.1–100 Hz at room temperature. Dynamic mechanical analysis results show that the mechanical properties are highly functions of tested frequency and the improvement on loss and storage modulus of nanocomposites with the addition of CNT is highly dependent on tested frequencies. The variability in loss modulus is significantly higher than the variability in the storage modulus indicating the correlation of loss modulus with uncertainties present in nanocomposite microstructure while storage modulus is essentially independent of microstructure for a given reinforcement content.     

Dynamic mechanical response of plasticizer-laden acoustic polyurethanes extrapolated to higher frequencies using time–temperature superposition technique

Acoustically transparent elastomers are the windows through which the US Navy views the ocean. For acoustic clarity and sensitivity, it is important that these elastomers operate well outside damping conditions as dictated by the temperatures and frequencies of interest. Damping behavior is characterized by a peak in the loss tangent and is associated with transitions in molecular mobility, such as the primary glass–rubber or alpha transition. However, the temperature and frequency location of this peak can shift in response to absorbed plasticizing fluids. This material characteristic is under investigation using dynamic mechanical analysis to assess its dependence on the plasticizer and polyurethane component chemistry. In this second stage of the research, the time–temperature superposition technique was employed to extrapolate storage modulus and loss factor to frequencies beyond the limits of the equipment. The technique appears to be valid for plasticized primary transition behavior but becomes circumspect when applied to secondary transition behavior.     

Crosslinked oligoethylene glycols: Correlation between their structure and some rheological properties

Six oligoethylene glycols were crosslinked with triphenylmethane triisocyanate, and polymers with systematically changing network chain lengths were obtained and investigated. The 10-sec. torsion moduli versus temperature, glass transition temperatures, and cohesive energy densities of the polymers were determined and studied. The 10-sec. torsion modulus versus temperature plots show that all six polymers have a glassy transition and rubbery region of rheological behavior. The front factor calculated from the equation for the torsion modulus in the rubbery region when measured values of the modulus were used was compared with the front factor computed from equations that take into consideration molecular structures of the rubbery networks. With the exception of the case of crosslinked diethylene glycol the agreement in all the other cases between the values obtained for the front factor in both ways was good. In the investigated range of temperatures the polymers have below the glass transition temperature another transition point. The solubility parameters of the polymers, calculated from swelling experiments, were with the exception of the first member in the series almost identical.     

Phase behavior actuating morphology and rheological response of polybutadiene/polyisoprene blends under small amplitude oscillatory shear

The morphology evolution and the corresponding linear viscoelastic behavior of the phase-separating polybutadiene （PB）/low vinyl content polyisoprene （LPI） blend have been investigated by phase contrast optical microscopy （PCOM）, small-angle light scattering （SALS） and rheometxy. Two kinds of structure evolutions and rheological responses have been observed. It is found that the co-continuous structure generally gives a power law behavior of the dynamic storage modulus versus frequency and the coarsening of co-continuous structure leads to a decrease of the storage modulus. For the droplet-matrix structure, a platform modulus is observed at the mediate frequencies, followed by the typical terminal relaxation behavior of storage modulus at the extremely low frequencies. The decreasing platform modulus and increasing terminal modulus with the growth of droplets are observed and can be well interpreted by the simplified Palieme model. The platform modulus and terminal modulus at a given frequency are found to be scalable with the phase separation time. Besides, the characteristic relaxation time and domain size of the droplets have been obtained by theology. And it seems that the theologically determined droplet dimensions are consistent with the ones determined by PCOM and SALS.     

High damping and mechanical properties of hydrogen-bonded polyethylene materials with variable contents of hydroxyls: Effect of hydrogen bonding density

Hydrogen bonding is considered to have significant effect on the interaction between polymeric chains and on the viscoelasticity of the polymeric materials. In this paper, we attempt to discuss the relationship between hydrogen bonding density and damping behavior and mechanical properties of polyethylene-based polymeric materials. For this reason, a series of pendant chain hydrogen bonding polymers(PCHBP) with different hydrogen bonding density(HBD) were prepared by quantitatively changing the content of pendent hydroxyl groups on the main chain of polyethylene. It was found that PCHBP with low HBD showed similar properties to polyethylene, indicating that the property of the materials was dependent mainly on the structure of the main chain. However, PCHBP with high HBD exhibited two tanδ peaks and a platform of loss modulus as well as a high storage modulus(about 400 MPa) at the second tanδ peak temperature, demonstrating that a polymeric material with high strength and damping properties was obtained. More importantly, the maximum of loss modulus showed a linear increase with the HBD, indicating that a higher HBD greatly improved the damping properties of the polymeric materials.     

Determination of dynamic properties of flax fibres reinforced laminate using vibration measurements

Experimental and numerical methods to identify the linear viscoelastic properties of flax fibre reinforced polymer (FFRP) composite are presented in this study. The method relies on the evolution of storage modulus and loss factor as observed through the frequency response. Free-free symmetrically guided beams were excited in the dynamic range of 10 Hz to 4 kHz with a swept sine excitation focused around their first modes. A fractional derivative Zener model has been identified to predict the complex moduli. A modified ply constitutive law has been then implemented in a classical laminates theory calculation (CLT) routine. Overall, the Zener model fitted the experimental results well. The storage modulus was not frequency dependant, while the loss factor increased with frequency and reached a maximum value for a fibre orientation of 70°. The damping of FFRP was, respectively, 5 and 2 times higher than for equivalent carbon and glass fibres reinforced epoxy composites.     

Fabrication and vibration characterization of electrically triggered shape memory polymer beams

Shape memory polymers (SMP) exhibit temperature, frequency and strain rate dependent properties which may be manipulated by various types of external stimuli to achieve desirable response characteristics. In recent years, the emphasis has been on designing SMPs which do not require external stimuli (such as a heat source) and have a rapid response time with large homogenous and reversible deformation characteristics. In this research, the fabrication process and dynamic vibration testing of an electrically activated SMP are presented. It is shown that conductive SMP beams can be fabricated to achieve tunable stiffness and damping with a reasonable thermal gradient generated by electrical triggering. This can allow the tuning of a range of frequency bandwidth and damping properties of SMPs for vibration control applications. The experimentation yielded modal properties (natural frequencies and damping) of the SMP beams. These parameters were validated against values obtained from the estimated performance of these beams based on the complex modulus parameters obtained using dynamic mechanical analysis (DMA). For a modest 20 °C temperature range in an epoxy based SMP, a resulting shift of approximately 7% in the natural frequency and 100% change in the damping ratio of a rectangular beam was successfully attained. These results recommend SMPs as being tunable materials that can enhance vibrational performance and expand the operational envelope of structures.     

冷冻/解冻制备的聚乙烯醇水凝胶的结构和流变性研究

研究了冷冻/解冻法制备的不同浓度(5wt%～25wt%)聚乙烯醇(PVA)水凝胶的结构和流变行为之间的关系.由XRD确定了凝胶中PVA的结晶度和晶粒尺寸.用应力流变仪研究了凝胶的流变行为,包括动态模量和蠕变等.在频率为1Hz和低应力的条件下,测量了凝胶的储能模量和损耗模量.在该试验条件下,PVA水凝胶的形变是完全可以回复的.低频率区和低应变区的储能模量随浓度增加而变大,但当浓度超过20wt%时,储能模量增加速率明显降低.由PVA水凝胶在1Hz时的储能模量和结晶度的数据,理论分析得到了形成PVA水凝胶的最低PVA浓度和最小结晶度.当PVA浓度低于15wt%时,储能模量主要由PVA的微晶控制,分子链间的氢键影响很小.通过低应变区储能模量的数值计算出了凝胶网孔尺寸的结构参数.同时对不同温度下PVA水凝胶的储能模量数据进行了标度分析.PVA水凝胶的蠕变行为显示,随浓度提高,凝胶的蠕变黏弹性由线性向非线性转变.     

Low-frequency rheology of magnetically controlled elastomers with isotropic structure

The method of torsion oscillations is used to measure the dynamic modulus of elasticity of magnetically controlled elastomers that comprise silicone rubber and carbonyl iron in the low-frequency (up to 100 Hz) range. The samples are synthesized in the absence of a magnetic field; therefore, they have an isotropic structure. In the measurements, a constant magnetic field (up to 24 kA/m) is superimposed along the axis of forced torsion oscillations of the sample. A simple model of the rheological behavior of magnetically controlled elastomers is proposed; the problem of torsion oscillations of a cylindrical sample is solved. From the comparison with the experiment for the materials under study, we determine the coefficients of the theoretical model and the corrections to them, which are made because of variations in the rheology of magnetically controlled elastomers under the influence of a magnetic field. The derived relations make it possible to exclude artifacts and to adequately describe dependences of the storage and loss moduli on the frequency of mechanical loading and the strength of the applied magnetic field.     

Phase behaviour of poly(vinyl methyl ether)-cross-polystyrene semi-interpenetrating networks

Semi-interpenetrating polymer networks of varying composition are prepared by crosslinking polystyrene containing a small number of maleic anhydride groups (4.8 mol% of MA units) with hexamethylene-diamine (HMDA) in the presence of linear poly(vinyl methyl ether) (PVME). Lightly crosslinked samples are homogeneous at room temperature and show a phase behaviour similar to uncrosslinked blends, i.e. lower critical solution temperature (LCST) behaviour. The influence of crosslinking on the phase behaviour has been studied by small angle light scattering (SALS) and turbidity measurements. The cloud point strongly depends on the heating rate. The presence of the network reduces the stable single phase region in agreement to theory. In systems showing spinodal decomposition, it is expected that some concentration fluctuations will grow more rapidly than others resulting in a separated phase system which shows high degree of connectivity with characteristic dimensions. Using temperature jump experiments, SALS can be used to estimate parameters of the phase separation kinetics and the characteristic dimensions of the phases. In temperature jump experiments into the spinodal region a maximum in the scattered light intensity is observed with time at a certain scattering vector. However, the semi-IPN's develop no scattering maximum. This is explained by a damping of the thermodynamical dominant wavelength in spinodal decomposition in the network.     

Torsion angle preference and energetics of small-molecule ligands bound to proteins

Small organic molecules can assume conformations in the protein-bound state that are significantly different from those in solution. We have analyzed the conformations of 21 common torsion motifs of small molecules extracted from crystal structures of protein-ligand complexes and compared them with their torsion potentials calculated by an ab initio DFT method. We find a good correlation between the potential energy of the torsion motifs and their conformational distribution in the protein-bound state: The most probable conformations of the torsion motifs agree well with the calculated global energy minima, and the lowest torsion-energy state becomes increasingly dominant as the torsion barrier height increases. The torsion motifs can be divided into 3 groups based on torsion barrier heights: high (>4 kcal/mol), medium (2-4 kcal/mol), and low (<2 kcal/mol). The calculated torsion energy profiles are predictive for the most preferred bound conformation for the high and medium barrier groups, the latter group common in druglike molecules. In the high-barrier group of druglike ligands, >95% of conformational torsions occur in the energy region <4 kcal/mol. The conformations of the torsion motifs in the protein-bound state can be modeled by a Boltzmann distribution with a temperature factor much higher than room temperature. This high-temperature factor, derived by fitting the theoretical model to the experimentally observed conformation occurrence of torsions, can be interpreted as the perturbation that proteins inflict on the conformation of the bound ligand. Using this model, it is calculated that the average strain energy of a torsion motif in ligands bound to proteins is approximately 0.6 kcal/mol, a result which can be related to the lower binding efficiency of larger ligands with more rotatable bonds. The above results indicate that torsion potentials play an important role in dictating ligand conformations in both the free and the bound states.     

不同色浆质量分数的水性聚氨酯涂料对聚氯乙烯表皮低温爆破性能的影响

本文制备了一系列不同色浆质量分数的水性聚氨酯涂料,并将其喷涂在汽车仪表板聚氯乙烯(PVC)表皮的背面形成复合材料。 用旋转流变仪表征了涂料的粘度以评价其喷涂性能;用差示扫描量热仪表征了材料的玻璃化转变温度(T_g);利用万能材料试验机表征了材料在-30 ℃条件下的拉伸性能及抗撕裂性能;用动态热机械分析仪表征了材料的损耗比随温度的变化。 结果表明:不同色浆质量分数的涂料都能喷涂,含有涂层材料PVC表皮在-30 ℃低温爆破性能与涂层材料的T_g、低温拉伸性能、抗撕裂性能的关系并不大,而与涂层材料的阻尼性能直接相关。 材料的阻尼性能越好,其低温爆破性能越好。     

Instrumented and temperature-controlled charpy impact tester

An imprivement of a Charpy-type impact tester has been made by attaching a force transducer together with damping materials to the striker, thereby reducing the mechanical vibration.Through processing of a time-based force signal a true force-displacement curve, modulus, rupture energy, deflection and failure stress can readily be obtained.Furthermore, an installation controlling the temperature of the samples has been developed. It consists of, amongst other things, thermally insulated sample holders with an internal coolant flow and a collapsible chamber swept with temperature-controlled dry nitrogen. The precision of the sample temperature thus obtained is as close as ±1 °C.     

Sol‐gel transition of biopolymer dispersions

Sol‐gel transition of dispersions of biopolymers, which are used widely in food, cosmetics, biomedical and related industries, is classified by the temperature dependence of storage shear modulus. Sol‐gel transition of gellan gum solution is described well by a criterion of Winter‐Chambon. Too fast gelation of dispersions of konjac glucomannan in the presence of excessive amount of alkaline coagulant and/or at higher temperatures leads to a formation of gels with lower modulus. A solution of xyloglucan from which a certain amount of galactose residues is removed forms a gel on heating and reverts into a solution on further heating. The lower temperature transition of this xyloglucan solution is induced by hydrophobic interaction.     

The rheological behaviour of suspensions of fat particles in oil interpreted in terms of a transient-network model

The transient-network model for concentrated dispersions, described in a previous paper, is used to describe the rheological behaviour of dispersions of glyceryl tristearate crystals in paraffin oil. The model prediction of the storage modulus of this system is compared with corresponding expressions given in literature. Model calculations are carried out to fit the linear viscoelastic behaviour of the system as well as its stress response in large amplitude shear experiments. Information is thus obtained about the stiffness and strength of the interparticle bonds, and the chance of them breaking in a state of rest or as the result of flow. It is concluded that the probability of interparticle bond fracture strongly depends on the measure of bond stretching. The general findings link up with the Lennard-Jones potential which is assumed to describe the potential energy of the bonds between the particles. Accurate measurements of the temperature dependence of the dynamic moduli by making use of a torsion resonator lead to the conclusion that the energy dissipation at a high frequency originates mainly from the flow of liquid around the particles.     

自流平聚氨酯的制备及阻尼甲板的降噪性能

为降低船舶甲板的振动和空气噪声,以支化和线性多元醇,低粘度聚合多异氰酸酯(PMDI)为主要原料制得阻尼聚氨酯,并将其铺设于钢甲板与浮动甲板之间。 探讨了基体结构、阻尼填料等对阻尼层固化时间、流平、阻尼和力学等性能的影响,以及铺设阻尼层前后甲板整体的隔声性能。 结果表明,调节支链和线性多元醇的质量比,可以改变基体的交联程度与结构,支化多元醇提高了聚氨酯的固化速率,硬度,以及力学性能;线性多元醇降低了体系的玻璃化转变温度,使阻尼温域移向低温,损耗因子峰值提高。 铺设于现有浮动甲板结构下2 mm聚氨酯阻尼层,可以有效增加整个甲板平均3 dB的隔声量,且在低频区增加量更大。 制得的聚氨酯阻尼层流动性优越,室温固化时间可控,可方便快捷的一次性自流平施工,对于提高现有浮动甲板的降噪性能具有实际的意义。     

Synthesis and rheological properties of polylactide/poly(ethylene glycol) multiblock copolymers

Ring-opening polymerization of D,L-lactide was carried out in the presence of poly(ethylene glycol), using Zn powder as catalyst. The hydroxyl-capped PLA-PEG-PLA triblock copolymers were coupled with adipoyl chloride at different molar ratios under mild conditions. N-Dimethylaminopyridine (DMAP) was used as catalyst of the coupling reaction. The resulting PLA/PEG multiblock copolymers were characterized by various analytical techniques such as IR, 1H NMR, SEC, and DSC. Sol-gel transition properties of the multiblock copolymers were investigated by mechanical rheology. The data showed that the sol-gel transition temperature and the transition modulus increased with increasing molecular weight and the solution concentration of the multiblock copolymers. [Graph: see text] Variation of storage modulus (G') and loss modulus (G') as a function of temperature for a 20% sample of MB3.