Rheology stress relaxation test

A variety of rheological tests can be used to evaluate the nature and properties of different network structures in foods. The strength of bonds in a fat crystal network can be evaluated by stress relaxation and by the decrease in elastic recovery in creep tests as a function of loading time (deMan et al. 1985). Van Kleef et al. (1978) have reported on the determination of the number of crosslinks in a protein gel from its mechanical and swelling properties. Oakenfull (1984) used shear modulus measurements to estimate the size and thermodynamic stability of junction zones in noncovalently cross-linked gels. 

The rheological behavior of these materials is still far from being fully understood but relationships between their rheology and the degree of exfoliation of the nanoparticles have been reported [73]. An increase in the steady shear flow viscosity with the clay content has been reported for most systems [62, 74], while in some cases, viscosity decreases with low clay loading [46, 75]. Another important characteristic of exfoliated nanocomposites is the loss of the complex viscosity Newtonian plateau in oscillatory shear flow [76-80]. Transient experiments have also been used to study the rheological response of polymer nanocomposites. The degree of exfoliation is associated with the amplitude of stress overshoots in start-up experiment [81]. Two main modes of relaxation have been observed in the stress relaxation (step shear) test, namely, a fast mode associated with the polymer matrix and a slow mode associated with the polymer-clay network [60]. The presence of a clay-polymer network has also been evidenced by Cole-Cole plots [82]. 

McKinley, G. H., and O. Hassager. 1999. The Considere condition and rapid stretching of linear and branched polymer melts. Journal of Rheology 43 1195-1212. Safari-Ardi, M., and N. Phan-Thien. 1998. Stress relaxation and oscillatory tests to distinguish between doughs prepared from wheat flours of different varietal origin. Cereal Chemistry 75 80-84. 

In Section 24.1 we have defined ways of prediction of long-term behavior from short-term tests. Let us now provide more examples of application of these concepts. Creep and stress relaxation have been determined for PET/ 0.6PHB, where PET is the poly(ethylene terephthalate), PHB, the p-hydroxybenzoic acid, and 0.6 is the mole fraction of the latter in the copolymer [58]. PET/0.6PHB is a polymer liquid crystal, see chapter 41 on PECs in this Handbook. In temperature ranges of interest it forms 4 coexisting phases [60]. Conventional wisdom said that prediction methods work only for so-called rheologically simple materials, practically for one-phase polymers. Therefore, we have decided to apply as severe a test as possible to our prediction methods and a multiphase PLC is a good choice. 

Rheological measurements on the slurry have been performed by Bohlin rheometer model VOR and constant stress rheometer C.. These two units combined are powerful enough to analyze slurries completely in viscometry, oscillatory and relaxation tests. Injection molding compound is fully characterized rheologically using capillary rheometer. 

Finally, it is worth mentioning another approach used to describe nonlinear viscoelastic solids nonlinear differential viscoelasticity [49, 178, 179]. This theory has been successfully applied to model finite amplitude waves propagation [180-182]. It is the generalization to the three-dimensional nonlinear case of the rheological element composed by a dashpot in series with a spring. Thus in the simplest case, the stress depends upon the current values of strain and strain rate rally. In this sense, it can account for the nonlinear short-term response and the creep behavior, but it fails to reproduce the long-term material response (e.g., relaxation tests). The so-called Mooney-Rivlin viscoelastic material [183] and the incompressible version of the model proposed by Landau and Lifshitz [184] belraig to this class. 

Macroscopic properties, alternatively referred to as bulk properties or simply performance , are of the utmost importance in material selection. For any application it is essential that the material provides the properties desired, under the conditions of use. In addition, it is wise to characterise the material more fully in order to understand what the effect might be, for example, of changing the temperature. Consideration should also be given to time-related phenomena, such as creep or stress relaxation. What are the consequences of dimensional instability Techniques that can provide this type of information directly include mechanical testing, rheology and thermal analysis. In cases where knowledge of the relationship between structure and properties is desirable, then obviously the techniques described here must be used in combination with those which follow. 

Most rheological measurements measure quantities associated with simple shear shear viscosity, primary and secondary normal stress differences. There are several test geometries and deformation modes, e.g. parallel-plate simple shear, torsion between parallel plates, torsion between a cone and a plate, rotation between two coaxial cylinders (Couette flow), and axial flow through a capillary (Poiseuille flow). The viscosity can be obtained by simultaneous measurement of the angular velocity of the plate (cylinder, cone) and the torque. The measurements can be carried out at different shear rates under steady-state conditions. A transient experiment is another option from which both y q and ]° can be obtained from creep data (constant stress) or stress relaxation experiment which is often measured after cessation of the steady-state flow (Fig. 6.10). 

Besides the sinusoidal oscillations, transient tests such as stress relaxation, start-up of steady shear flow, and cessation of steady shear flow are also important in the rheological characterization of polymeric liquids. The instrument limitations and features, and their effect on the data obtained in some types of transient tests, are examined in this section. Also, we shall illustrate the use of linear viscoelastic transformation to obtain, for example, stress relaxation data from tests such as start-up of steady shear flow and sinusoidal oscillations. 

For the evaluation of the rheology of the silica dispersions, different test methods were applied (a) a shear rate-controlled relaxation experiment at = 0.5 s (conditioning), 500 s (shear thinning), and 0.5 s (relaxation) to evaluate the apparent viscosity, the relaxation behavior, and thixotropy (b) shear yield-stress measurements using a vane technique introduced by Nguyen and Boger [5] (c) low deformation dynamic tests at a constant frequency of 1.6 s in a stress range of ca. 0.5 - 100 Pa. All samples contained 3 wt% of fumed silica. 

In the rheological structure of most food systems there is a viscous element present, and the deformation curves are often highly influenced by the rate of the imposed strain. This is due to the fact that the material relaxes (or flows) while tested under compression and the resultant deformation of this flow is dependent on the nature of the viscous element (Szczesniak, 1963 Peleg and Bagley, 1983). In the viscoelastic food systems, where during processing it is caused to oscillate sinusoidally, the strain curve may or may not be a sine wave. In cases when a periodic oscillatory strain is applied on a food system like fluid material, oscillating stress can be observed. The ideal elastic solid produces a shear stress wave in phase with... 

The second dependence in Eq. (2.32) is valid when all fractions are either entangled or not. In consequence, the relaxation spectrum of a miscible polymer blend is a linear combination of the component relaxation spectra and their weight fractions, W(. A strong deviation from linearity in plots of log Hq versus Mw/Afn and log Wmax versus log r]o indicates immiscibility [87, 88]. The principle that in miscible blends polydispersity can be calculated and used to test for system miscibility was extended to other rheological functions sensitive to polydispersity, namely, the power-law exponent (n), the cross-point coordinates (G, o) ), the free volume gradient of viscosity, the initial slope of stress growth function, and so on [3]. 

K. Osaki, S. Kimura, and M. Kurata, Relaxation of Shear and Normal Stresses in Double-Step Shear Deformations. A Test of the Doi-Edwards Theory for Polymer Rheology tZ Rheol. 25, 549-562 (1981). 

The raison d itre of this book is that rheological properties of the melt are very sensitive to the molecular structure of a polymer. Rheological properties describe how stress develops in a sample undergoing a prescribed deformation. They also describe the deformation that is caused by a prescribed stress. The most fundamental rheological experiment for a viscoelastic material is a step-strain test, and for melts this nearly always means a step shear strain. In a step shear-strain test, a sample is subjected to a sudden shear strain of magnitude, % at time t=0. The shear stress is measured as a fimction of time, and the ratio of the stress to the applied strain defines the relaxation modulus, G t). 

Extensional flows yield information about rheological behavior that cannot be inferred from shear flow data. The test most widely used is start-up of steady, uniaxial extension. It is common practice to compare the transient tensile stress with the response predicted by the Boltzmann superposition principle using the linear relaxation spectrum a nonlinear response should approach this curve at short times or low strain rates. A transient response that rises significantly above this curve is said to reflect strain-hardening behavior, while a material whose stress falls... 

We have carried out standard rheometric tests as done many times in the literature for entangled polymer solutions. These experiments include startup shear, large amplitude oscillatory shear (LAOS) and large step strain. In terms of the rheological features, we observed the same as others. For example, there is a stress overshoot in startup shear in the stress plateau region the apparent G can drop below G" at frequencies of the elastic plateau and amplitudes around and above 100% and relaxation modulus decreases in time after large step strains. 

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