New laboratory tests to measure rheological properties of paper coatings in transient and steady-state flows

The paper describes pertinent laboratory tests to characterize the rheological properties of paper coatings with regard to blade coating over a very wide range of shear rates in both transient and steady-state shear flows. Shear rates as high as 10⁶ s^–1 can be reached by means of a gas-driven capillary rheometer. Examples for the evaluation of end effects, wall effects, and coating thixotropy are given. A stiff and fast Couette rheometer is used to determine flow curves and the shear stress overshoot in step shear rate tests. The primary normal stress difference can be measured up to 10⁴ s^–1 by means of a high shear cone-plate rheometer with piezo transducer. A correct evaluation of the measurements has to take into account inertia contributions to the normal force. First results using a sinusoidal modulation of the shear rate are presented.Paper presented at: International Symposium on Pigment Coating Structure and Rheology, Helsinki, Febr. 8–9, 1989     

Strain-rate history effects and microstructural aspects in lithium fluoride and aluminium single crystals after dynamic loading

Single crystals of LiF and Al are deformed in shear at a number of constant strain-rates in the range 10^–4 to 1600 s^–1. These constant rate tests are supplemented by a series of jump tests in which a sharp increment in strain rate is imposed during the quasi-static straining. Dislocation arrangements are observed by etch-pits technique for LiF crystals and by TEM for Al crystals. It is shown that cell sizes vary inversely with flow stress and strain-rate sensitivity.     

Direct measurement of static yield properties of cohesive suspensions

A technique of yield stress investigation based upon the combined use of two devices (an applied stress rheometer and an instrument for measuring the propagation velocity of small amplitude, torsional shear waves) is described. Investigations into the low shear rate rheological properties of illitic suspensions are reported for shear rates, typically, in the range 10^–4— 10^–1 s^–1 under applied stresses in the range 0.01 — 10 Nm^–2 and involving shear strains between 10^–1 and 10^–4. Results are presented which demonstrate that the technique does not invoke the excessive structural disruption of material associated with applied shear rate based methods (direct and otherwise) and the widely encountered problem of wall slip at the surface of rotational measuring devices is avoided using miniature vane geometries. Results are compared with those obtained using smooth-walled cyclindrical measuring devices in both applied stress and applied shear rate instruments.Yield measurements are considered in relation to the structural properties of the undisturbed material state and shear moduli obtained by studying the propagation of small amplitude (10^–5 rad), high frequency (~ 300 Hz) torsional shear waves through the test materials are reported. Experimental techniques and instrument modifications to permit these measurements are described.     

Rheological properties of some biphenyl liquid crystals

Rheological measurements have been carried out using a rotational viscometer with a system of coaxial cylinders on four liquid crystalline substances from the group of cyanobiphenyls. On the basis of results of these investigations it was found that in the investigated range of shear rates the nematic phases exhibited Newtonian flow behaviour, while the smectic phases exhibited non-Newtonian behaviour. For shear rates up to ca. 1000 s^–1 the dependence of the shear stress on shear rate is well described by a power-law model.     

Extensional flow of polystyrene melt

Summary The extensional flow of molten polystyrene was studied in the strain rate range of 7.8×10^–4 sec^–1 to 2.2×10^–2 sec^–1 at a test temperature of 300F (149 C) Extensional viscosity was compared to shear viscosity measured at the same degree of stress and temperature and found to be from 3 to 350 times greater in magnitude but much less stress dependent.     

Effects of deformed volume, volume fraction and particle size on the deformation behaviour of W/Cu composites

Tungsten/copper (W/Cu) particle reinforced composites were used to investigate the scaling effects on the deformation and fracture behaviour. The effects of the volume fraction and the particle size of the reinforcement (tungsten particles) were studied. W/Cu-80/20, 70/30 and 60/40 wt.% each with tungsten particle size of 10 μm and 30 μm were tested under compression and shear loading. Cylindrical compression specimens with different volumes (D_S = H) were investigated with strain rates between 0.001 s⁻¹ and about 5750 s⁻¹ at temperatures from 20 °C to 800 °C. Axis-symmetric hat-shaped shear specimens with different shear zone widths were examined at different strain rates as well. A clear dependence of the flow stress on the deformed volume and the particle size was found under compression and shear loading. Metallographic investigation was carried out to show a relation between the deformation of the tungsten particles and the global deformation of the specimens. The size of the deformed zone under either compression or shear loading has shown a clear size effect on the fracture of the hat-shaped specimens.The quasi-static flow curves were described with the material law from Swift. The parameters of the material law were presented as a function of the temperature and the specimen size. The mechanical behaviour of the composite materials were numerically computed for an idealized axis-symmetric hat-shaped specimen to verify the determined material law.     

A linear viscoelastic model for solid polyethylene

Stress relaxation tests have been carried out on a blue, pipe grade PE 80 medium density polyethylene (BP Chemicals), to provide thermo-viscoelastic rheology for use in calculating thermal stresses in pipe production. Stresses up to 4 MPa were used, with strains up to about 2%, in tests at temperatures from 23° to 90°C. Within this range a linear viscoelastic model was applicable, provided the initial ramp strain rate was less than 7×10^–5 s^–1. The stress relaxation data was fitted directly by a model incorporating an elastic response to volumetric strains, and a generalised linear solid model, consisting of two Maxwell elements and a purely elastic element in parallel, for deviatoric strains. Arrhenius type temperature dependence of relaxation times and shear moduli is found, and within experimental accuracy the temperature dependence of all these model parameters is the same. As a consequence, and provided that the duration of the strain ramp is sufficiently short relative to relaxation times, the model leads to time-temperature superposition of the relaxation moduli, using the same shift factor on both the response magnitude and time axes.     

Partition of plastic work into heat and stored energy in metals

This study investigates heat generation in metals during plastic deformation. Experiments were designed to measure the partition of plastic work into heat and stored energy during dynamic deformations under adiabatic conditions. A servohydraulic load frame was used to measure mechanical properties at lower strain rates, 10^–3 s^–1 to 1 s^–1. A Kolsky pressure bar was used to determine mechanical properties at strain rates between 10³ s^–1 and 10⁴ s^–1. For dynamic loading, in situ temperature changes were measured using a high-speed HgCdTe photoconductive detector. An aluminum 2024-T3 alloy and -titanium were used to determine the dependence of the fraction of plastic work converted to heat on strain and strain rate. The flow stress and for 2024-T3 aluminum alloy were found to be a function of strain but not strain rate, whereas they were found to be strongly dependent on strain rate for -titanium.     

High-temperature pressure-shear plate impact experiments using pure tungsten carbide impactors

The pressure-shear plate impact experiment has been modified to test materials at high temperatures (up to 700°C). Together with the high strain rates characteristic of this experiment (10⁶ s^–1), the high-temperature capability allows the shearing resistance of materials to be measured under conditions unattainable with other testing equipment. The compressive and shear responses of pure tungsten carbide at different temperatures are presented, as well as the results of one test on OFHC copper at a temperature of 691°C and a shear strain rate of 1.4×10⁶ s^–1.     

Nonlinear viscoelasticity of PP/PS/SEBS blends

The nonlinear viscoelastic behavior of polypropylene/polystyrene (PP/PS) blends compatibilized or not with the linear triblock copolymer (styrene-ethylene-/butylene-styrene, SEBS) was investigated. Start-up of steady-shear at rates from 0.1 to 10 s^–1 was carried out using a controlled strain rotational rheometer and a sliding plate rheometer for strain histories involving one or several shear rates. The shear stress and first normal shear stress difference were measured as functions of time, and the morphologies of the samples before and after shearing were determined. For each strain history except that involving a single shear rate of 0.1 s^–1 the blends showed typical non-linear viscoelastic behavior: a shear stress overshoot/undershoot, depending on the history, followed by a steady state for each step. The first normal stress difference increased monotonically to a steady-state value. The values of the stresses increased with the addition of SEBS. The shear stress overshoot and undershoot and the times at which they occurred depended strongly on the strain history, decreasing for a subsequent shear rate step performed in the same direction as the former, and the time at which stress undershoot occurred increased for a subsequent shear rate step performed in the opposite direction, irrespective of the magnitude of the shear rate. This behavior was observed for all the blends studied. The time of overshoot in a single-step shear rate experiment is inversely proportional to the shear rate, and the steady-state value of N₁ scaled linearly with shear rate, whereas the steady-state shear stress did not. The average diameter of the dispersed phase decreased for all strain histories when the blend was not compatibilized. When the blend was compatibilized, the average diameter of the dispersed phase changed only during the stronger flows. Experimental data were compared with the predictions of a model formulated using ideas of Doi and Ohta (1991), Lacroix et al. (1998) and Bousmina et al. (2001). The model correctly predicted the behavior of the uncompatibilized blends for single-step shear rates but not that of the compatibilized blends, nor did it predict morphologies after shearing.     

Computational nanoscale plasticity simulations using embedded atom potentials

In determining structure–property relations for plasticity at different size scales, it is desired to bridge concepts from the continuum to the atom. This raises many questions related to volume averaging, appropriate length scales of focus for an analysis, and postulates in continuum mechanics. In a preliminary effort to evaluate bridging size scales and continuum concepts with descritized phenomena, simple shear molecular dynamics simulations using the Embedded Atom Method (EAM) potentials were performed on single crystals. In order to help evaluate the continuum quantities related to the kinematic and thermodynamic force variables, finite element simulations (with different material models) and macroscale experiments were also performed. In this scoping study, various parametric effects on the stress state and kinematics have been quantified. The parameters included the following: crystal orientation (single slip, double slip, quadruple slip, octal slip), temperature (300 and 500 K), applied strain rate (10⁶–10¹² s⁻¹), specimen size (10 atoms to 2 μm), specimen aspect ratio size (1:8–8:1), deformation path (compression, tension, simple shear, and torsion), and material (nickel, aluminum, and copper). Although many conclusions can be drawn from this work, which has provided fodder for more studies, several major conclusions can be drawn.

• The yield stress is a function of a size scale parameter (volume-per-surface area) that was determined from atomistic simulations coupled with experiments. As the size decreases, the yield stress increases.

• Although the thermodynamic force (stress) varies at different size scales, the kinematics of deformation appears to be very similar based on atomistic simulations, finite element simulations, and physical experiments.

Atomistic simulations, that inherently include extreme strain rates and size scales, give results that agree with the phenomenological attributes of plasticity observed in macroscale experiments. These include strain rate dependence of the flow stress into a rate independent regime; approximate Schmid type behavior; size scale dependence on the flow stress, and kinematic behavior of large deformation plasticity.     

Effect of solids concentration in dense suspensions of silica-iron(III) oxide and water

The rheological properties of dense suspensions, of silica, iron (III) oxide and water, were studied over a range of solids concentrations using a viscometer, which was modified so as to prevent settling of the solid components. Over the conditions studied, the material behaved according to power—law flow relationships. As the concentrations of silica and iron(III) oxide were increased, an entropy term in the flow equation was identified which had a silica dependent and an iron (III) oxide dependent component. This was attributed to a tendency to order into some form of structural regularity. A, A, B, C pre-exponential functions (K Pa^–n s^–1) - C _ox volume fraction iron (III) oxide - Q activation energy (kJ mol^–1) - R gas constant (kJ mol^–1 K^–1) - R _v silica/water volume ratio - T temperature (K) - n power-law index - H enthalpy (kJ mol^–1) - S entropy change (kJ mol^–1 K^–1) - shear strain rate (s^–1) - shear stress (Pa)     

An appraisal of rheological models as applied to polymer melt flow

Summary An attempt is made at giving an appraisal of some representative rheological models of both differential and integral type, using the standard rheological measurements of six polymer melts. Experimental data obtained were the steady shear viscosity and the first normal stress difference by means of aWeissenberg rheogoniometer over the range of shear rates: 10^–2 ~ 10 sec^–1, and by means of aHan slit/capillary rheometer over the range of shear rates: 10 ~ 10³ sec^–1. Also measured by means of theWeissenberg rheogoniometer were the dynamic viscosity and dynamic elastic modulus over the range of frequencies: 0.3 × 10^–2 ~ 3 × 10² sec^–1. Rheological models chosen for an appraisal are theSpriggs 4-constant model, theMeister model, and theBogue model.It is found that the capability of the three models considered is about the same in their prediction of the rheological behavior of polymer melts in simple shearing flow. It is pointed out however that, due to the ensuing mathematical complexities, the usefulness of these models is limited to the study of flow problems associated with simple flow situations. Therefore, in analysing the complex flow situations often encountered with various polymer processings, the authors suggest use of the empirical models of the power-law type for both the viscosity and normal stress functions.With 11 figures, 4 schemas and 1 table     

Dynamic compressive behavior of thick composite materials

The effect of strain rate on the compressive behavior of thick carbon/epoxy composite materials was investigated. Falling weight impact and split Hopkinson pressure bar systems were developed for dynamic characterization of composite materials in compression at strain rates up to 2000 s^–1. Strain rates below 10 s^–1 were generated using a servohydraulic testing machine. Strain rates between 10 s^–1 and 500 s^–1 were generated using the drop tower apparatus. Strain rates above 500 s^–1 were generated using the split Hopkinson pressure bar. Unidirectional carbon/epoxy laminates (IM6G/3501-6) loaded in the longitudinal and transverse directions, and cross-ply laminates were characterized. The 90-deg properties, which are governed by the matrix, show an increase in modulus and strength over the static values but no significant change in ultimate strain. The 0-deg and cross-ply laminates show higher strength and ultimte strain values as the strain rate increases, whereas the modulus increnases only slightly over the static value. The increase in strength and ultimate strain observed may be related to the shear behavior of the composite and the change in failure modes. In all cases, the dynamic stress-strain curves stiffen as the strain rate increases. The stiffening is lowest in the longitudinal direction and highest in the transverse direction.     

Rheometry on magnetorheological (MR) fluids

Test fixtures of a commercial concentric cylinder rheometer (Physica Rheolab MC 20) were modified to enable measurements under magnetic inductions up to 0.5 Tesla in a shear rate range of 0.1 up to 1000 s ^–1 and temperatures 0° to 150°C. In the 2 x90°-cups only two 90° sectors of the stationary part of the double concentric cylinder arrangement are submitted to the magnetic field which is created outside the test tools by an electromagnet. A prototype of a 360°-cup contains the electromagnet within the cup and avoids the correction necessary for the sector geometry. Measurements are shown for a carbonyl iron MR fluid and two nano MR fluids. An encouraging comparison of the viscosity function and MR effect (shear stress changes due to the field) measured by using the various cups is presented. The detailed investigation of the magnetic field distribution in the tools yields a distinct radial field gradient and also stray fields that make the quantification of the effective field in the gap difficult. The change of the field when the gap is filled with MR fluid is addressed. MR effects up to 13 000 Pa have been found, the limited torque range of the rheometer making it necessary to use relatively small gap dimensions which introduce errors due to edge effects. Shear rates up to 40000 s^–1 as typical for the application in dampers were investigated by a piston-driven capillary rheometer making use of a thermostated rectangular slit with superimposed magnetic field. A satisfactory agreement of the magnetorheological data with the concentric cylinder results is found in the overlapping shear rate range.     

Hexagonal Defect Array Formed under Steady Shear Flow in Water-in-Cholesteric Liquid Crystal Emulsions

The relation between the liquid crystalline textures and the steady shear viscosity has been investigated in cholesteric emulsions, composed of water, surfactants, and cholesteric liquid crystals. Both at the substrate surface and at the surfactant-coated droplet surface, a homeotropic anchoring is enforced to the adjacent liquid crystal. Under a steady shear flow with the shear rate below 100 s^–1, we observed that point defects spontaneously appear, and tend to adopt a regular hexagonal arrangement in the low shear-rate range of 1–20 s^–1. In viscosity measurements, the shear-thinning behavior was found, showing a clear correspondence to the texture change. We estimated the height of point defects in the hexagonal array from the viscosity increase in the shear-thinning, assuming that the shear-thinning behavior is caused by the reduction of the effective gap between cone and plate, owing to the presence of the hexagonal array anchored on the plate. The relation between the estimated height and the measured lateral size of point defects agreed with that of the quadrilateral array, which is formed after termination of the shear. This agreement informs that the shape of a point defect is preserved in both defect arrays, independently of shearing conditions.     

Viscosity of some clay-based coating colors at high shear rates

The shear viscosity of clay-based coating colors containing latex and carboxymethyl cellulose (CMC) has been measured over a relatively large shearrate region. In the shear-rate range of 50–1500 s^–1 the measurements were performed using a rotational viscometer and, at higher shear rates extending into the region 10⁵ – 10⁶ s^–1, a high pressure capillary viscometer was employed. The viscosity of the clay colors increased with increasing CMC-concentration, but the influence of the CMC-content was less pronounced at higher shear rates. The apparent shear-thinning behavior of the investigated colors could, in part, be attributed to the shear-thinning of the corresponding polymer (CMC) solution constituting the liquid phase of the color, but the influence of another factor was also indicated. At low shear rates, the interaction between the color components can produce relatively high viscosity levels, but in the high shear rate region these interactions appear to be less important for the viscosity level. It is also of interest to note that the viscosity dependence on the solids content in the high shear-rate region could be described with reasonable accuracy using an empirical equation neglecting interactions between the color components.     

Flow stress behavior of porous FVS0812 aluminum alloy during hot-compression

The hot deformation behavior of porous FVS0812 aluminum alloy prepared by spray deposition was studied by means of compression tests on a Gleeble 1500 machine. The samples were hot compressed at temperatures ranging from 573 K to 773 K under various true strain rates of 10⁻⁴–10⁰ s⁻¹. The deformation behaviors are characterized by a significant strain hardening during hot-compression due to the progressive compaction of the pores with increasing compressive strain. A revised formula describing the relationships of the flow stress, strain rate and temperature of the porous alloy at elevated temperatures is proposed by compensation of strain. The theoretical predictions are compared with experimental results, which show good agreement.     

A comprehensive experimental study of the rheological behaviour of HDPE.

Extensional properties of four high density polyethylenes with different molecular weights and molecular weight distributions are presented. The samples have already been well characterized in shear and non-isothermal extensional flow. The data were collected at 180 °C for elongational rates between 3 · 10^–1 and 10^–4s^–1. Some qualitative and quantitative generalizations of the results are given.     

An experimental investigation into the kinematics of a concentrated hard-sphere colloidal suspension during Hopkinson bar evaluation at high stresses

The behavior of a concentrated, hard-sphere colloidal suspension is evaluated using the split Hopkinson pressure bar (SHPB) experimental technique. The composition of the suspension is measured using thermograviometric analysis before and after loading. This, combined with recorded pressure distributions, result in the conclusion that the suspension undergoes high rate squeezing flow. Experimental results demonstrate that the suspension exhibits shear thickening consistent with that observed in standard rotational rheometry. At sufficiently high stresses the suspension exhibits a second regime of shear thinning behavior that is consistent with elastohydrodynamic theory that incorporates the shear modulus of the particles themselves. Further increases in stress result in irreversible behavior, i.e., rather than fracturing or crushing, the particles form non-reversible agglomerates during testing. This fact is demonstrated through the use of dynamic light scattering and electron microscopy. This behavior occurs within a regime of viscous material response which is seen to occur at normal strain rates and stresses over 10⁴ s^?1 and 40 MPa, respectively.