A shear rheometer for measuring shear stress and both normal stress differences in polymer melts simultaneously: the MTR 25

The MTR 25 is a multitask rheometer (for shear and squeeze flow) with 25 kg of normal force and a partitioned plate. Torque and normal force are measured at both, the inner disk and the outer ring of the plate. The first and second normal stress differences can be determined from a single test. The axial stiffness is high (10⁷ N/m) by using rigid springs and strain gauges for the load cell. Monodisperse polystyrene (M _w = 206 kg/mol, 180°C) has been sheared in the range from 0.05 to 47 s^− 1. The viscosity and first normal stress difference are highly reproducible. The second normal stress difference scatters and mirrors the instability at the rim. A critical comparison is made between the MTR 25 method and the single transducer evaluation method (RMS 800 method, Schweizer, Rheol Acta 41:337–344, 2002): Both yield excellent and coinciding viscosity and first normal stress difference data. The RMS 800 method gives more stable second normal stress difference data, since the normal force from the outer ring, which is influenced by edge fracture, is not used. Data for the RMS 800 method can be acquired on the MTR 25. The high normal force capacity permits larger samples and higher shear rates than on the RMS 800.

Transient shear flow behavior of concentrated long glass fiber suspensions in a sliding plate rheometer

In order to eventually predict the behavior of long fiber suspensions in complex flows commonly found in processing operations, it is necessary to understand their rheology and its connection to the evolution of fiber orientation and configuration in well defined flows. In this paper we report the transient behavior at the startup of shear flow of a polymer melt containing long glass fibers with a length (L) >1 mm, using a sliding plate rheometer (SPR). The operation of the SPR was confirmed by comparing the transient shear viscosity (η⁺) for a polymer melt and a melt containing short glass fibers (L < 1 mm) with measurements obtained from a cone-and-plate device, using a modified sample geometry that was designed to avoid wall effects. For the long fiber systems, measurements could only be obtained in the SPR because these systems would not stay within the gap of the rotational rheometer. Transient stress growth behavior of the long fiber systems was obtained as a function of shear rate and fiber concentration for samples prepared with three different initial orientations. Results showed that, unlike short fiber systems (with a random planar initial orientation) that usually exhibit a single overshoot peak followed by a steady state, η⁺ of the long fiber suspensions often passed through multiple transient regions, depending on the fiber concentration and applied shear rate. Additionally, η⁺ of the long fiber suspensions was found to be highly dependent on the initial orientation of the sheared samples. Finally, the initial and final fiber orientations of the long glass fiber samples were measured and used to initiate an explanation of the viscosity behavior. The results obtained in this research will be useful for future assessment of a quantitative correlation between transient rheology and the evolution of fiber orientation.     

Time dependent flow in equimolar micellar solutions: transient behaviour of the shear stress and first normal stress difference in shear induced structures coupled with flow instabilities

Recently we studied time dependent structural changes that are coupled with flow instabilities (Fischer 1998; Wheeler 1998; Fischer 2000). Within a stability analysis, a classification scheme for the feedback circuit of coupled shear-induced structure and flow instabilities was derived by Schmitt et al. (1995) and applied to our samples. Here, inhomogeneous flow layers of different concentration and viscosity are generated by shear-induced diffusion (spinodal demixing) and, as consequence, one no longer observes a homogeneous solution but a type of shear banding that is seen here for the first time. In this paper we present the behaviour of the first normal stress difference observed in the critical shear-rate regime where transient shear-induced structure is coupled with flow instability. Similar to the oscillations of the shear stresses (strain-controlled rheometer) one observes oscillations in the first normal stress difference. This behaviour indicates that elastic structures are built up and destroyed while the shear-induced structures occur and that the induced phase is more elastic than the initial one. Oscillations of shear stress and first normal stress difference are in phase and indicate that both phenomena are caused by the same mechanism. Received: 30 June 1999/Accepted: 14 December 1999     

On the measurement of normal stress differences in steady shear flow

Summary Compared to the similar pressure-distribution cone-and-plate apparatus of Adams and Lodge (4), the new apparatus' improvements include: temperature control of the cone (as well as the plate); increased stiffening of the frame; four (not three) pressuremeasuring holes in the cone/plate region; inclusion of a pressure-measuring hole on the axis under the cone truncation; exclusive use of a vertical free liquid boundary at the cone rim (without a sea of liquid). Temperature control of the rotating cone and of the fixed plate leads to acceptable temperature uniformity in the test liquid for working temperatures within 10°C or 20°C of ambient; the corresponding interval is about 1°C if the cone temperature control is abandoned. Pressure gradients measured using a Newtonian liquid agree with those calculated using Walters' eq. (3). For a viscoelastic liquid, after subtracting inertial contributions, pressure distributions measured at a given shear rate in the cone/plate region do not change when the gap angle is changed from 2° to 3°, showing that the effects of secondary flow are negligible. Values ofN ₃ =N ₁ + 2N ₂ obtained from the gradients of these distributions are believed to be in error by not more than ±1 Pa, in favorable cases. The present most useful ranges are: 10 to 5000 Pa forN ₃; 0.1 to 200 sec^–1 for shear rate; up to 5 Pa s for viscosity; and 5 to 40°C for temperature. As an application, it is shown that adding 0.1% of a high molecular weight polyisobutylene to a 2% polyisobutylene solution doublesN ₃ and has no detectable effect on the viscosity measured at low shear rates with a Ferranti-Shirley viscometer.

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Zusammenfassung Im Vergleich zu dem ähnlichen Kegel-Platte-Gerät von Adams und Lodge (4) zur Messung der Druckverteilung wurden an dem neuen Gerät die folgenden Verbesserungen vorgenommen: Temperaturregelung an Kegel und Platte, Versteifung des Rahmens, vier (anstatt drei) Druckmeßlöcher im Kegel-Platte-Bereich, ein zusätzliches Druckmeßloch auf der Achse unter der Kegelstumpf-Deckfläche, ausschließliche Verwendung einer vertikalen freien Grenzfläche der Flüssigkeit am Kegelrand (ohne umgebenden Flüssigkeitssee). Die Temperaturregelung des rotierenden Kegels und der festen Platte führt zu einer ausreichenden Temperaturgleichförmigkeit in der Testflüssigkeit für Betriebstemperaturen, die höchstens um 10–20°C von der Umgebungstemperatur abweichen. Dieses Intervall beträgt dagegen nur etwa 1°C, wenn auf die Temperaturregelung am Kegel verzichtet wird. Für newtonsche Flüssigkeiten entsprechen die gemessenen Druckgradienten den mittels der Gleichung von Walters (3) berechneten. Für viskoelastische Flüssigkeiten zeigen sich bei der Änderung des Spaltwinkels von 2° auf 3° nach Abzug der Trägheitsbeiträge keine Änderungen der bei einer bestimmten Schergeschwindigkeit gemessenen Druckverteilung. Dies zeigt, daß Sekundärströmungseffekte vernachlässigbar sind. Es darf angenommen werden, daß die Werte vonN ₃ =N ₁ + 2N ₂, die man aus den Gradienten dieser Verteilungen erhält, unter günstigen Umständen mit einem Fehler von nicht mehr als ±1 Pa behaftet sind. Gegenwärtig liegen die günstigsten Bereiche bei 10 bis 5000 Pa fürN ₃, 0,1 bis 200 s^–1 für die Schergeschwindigkeit, unterhalb von 5 Pa s für die Viskosität und 5 bis 40°C für die Temperatur. Als Anwendung wird gezeigt, daß ein Zusatz von 0,1% hochmolekularen Polyisobutylens zu einer 2%igen Polyisobutylenlösung den Wert vonN ₃ verdoppelt, aber keinen erkennbaren Einfluß auf die (bei geringen Schergeschwindigkeiten mit einem Ferranti-Shirley-Viskosimeter gemessen) Viskosität hat.

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udsf unidirectional shear flow - TCP truncated-cone and plate - N ₁,N ₂ 1st and 2nd normal stress differences in udsf - N ₃ N ₁ + 2N ₂ - : = A is defined by the equationA := B - P ^* hole pressurePw – Pm; Pw, Pm = pressures measured by flush transducer and by hole-mounted transducer - t time - , strain rate, shear rate - (P,t) covariant body metric tensor at particleP and timet - ⁱ , _i covariant and contravariant udsf body base vectors (i = 1, 2, 3) - ^–1 inverse of - R, plate radius, cone/plate gap angle - r ₀,h ₀ radius and height of cone truncation - r,, spherical polar coordinates; cone axis = 0; plate surface = /2 - physical components of stress; for a tensile component - cone angular velocity - p on the plate = /2 - ,T, density, absolute temperature, viscosity - P 0.15 ²(r ² –R ²) (inertial contribution) [2.7] - P _ve contribution [2.8] from flow perturbations of viscoelastic origin - r _i i = 1,2,3,4; values ofr at centers of holes in cone/plate region - P _i () pressure change recorded by transducerTi when cone angular velocity goes from zero to - 1/2 {P _i ()+ P _i (–)} (average for 2 senses of rotation) - rim pressure, from least-squares line through four points - Re Reynolds' number:R ²/ - (P,t)/t With 11 figures and 2 tables     

Comparison of optical and mechanical measurements of second normal stress difference relaxation following step strain

Relaxation of the second normal stress difference (N ₂) following step strain of a concentrated monodisperse polystyrene solution has been studied using mechanical and optical rheometry. Measurements of normal thrust in a parallel plate geometry are corrected for strain inhomogeneity and combined with independent measurements of the first normal stress difference (N ₁) to determine N ₂. Optical experiments were performed using a novel configuration where flow birefringence data collected using multiple light paths within the shear plane are combined with the stress-optical law to determine all three independent stress components for shearing deformations. This technique eliminates end effects, and provides an opportunity to oversample the stress tensor and develop consistency checks of experimental data. N ₂ is found to be nonzero at all accessible times, and relaxes in roughly constant proportion to N ₁. This reflects nonaffine distribution of chain segments, even well within the regime of chain retraction at short times. Data collected with the two techniques are reasonably consistent with each other, and with results of previous studies, generally lying between the predictions of the Doi-Edwards model with and without the independent alignment approximation. The normal stress ratio –N ₂/N ₁ shows pronounced strain thinning in the nonlinear regime.     

The determination of the first normal stress coefficient of an exopolysaccharide solution by rheo-optical measurements

This paper illustrates how rheo-optical techniques may be utilized to determine the first normal stress coefficient for an exopolysaccharide (EPS) produced by the Lactobacillus delbrueckii ssp. bulgaricus LY03, which is widely used in yoghurt production. In this technique both shear stress, optical birefringence and extinction angle are measured simultaneously as a function of shear rate. From the stress optical rule the first normal stress difference can be determined directly without relying on any specific rheological model. Of special interest is the point where the first normal stress difference become comparable in magnitude to the shear stress. Here we expect to find a notable influence of the first normal stress difference on mouthfeel.This paper was presented at the first Annual European Rheology Conference (AERC) held in Guimarães, Portugal, September 11-13, 2003.     

The normal stress behaviour of suspensions with viscoelastic matrix fluids

 We investigate the variations in the shear stress and the first and second normal stress differences of suspensions formulated with viscoelastic fluids as the suspending medium. The test materials comprise two different silicone oils for the matrix fluids and glass spheres of two different mean diameters spanning a range of volume fractions between 5 and 25%. In agreement with previous investigations, the shear stress–shear rate functions of the viscoelastic suspensions were found to be of the same form as the viscometric functions of their matrix fluids, but progressively shifted along the shear rate axis to lower shear rates with increasing solid fraction. The normal stress differences in all of the suspensions examined can be conveniently represented as functions of the shear stress in the fluid. When plotted in this form, the first normal stress difference, as measured with a cone and plate rheometer, is positive in magnitude but strongly decreases with increasing solid fraction. The contributions of the first and the second normal stress differences are separated by using normal force measurements with parallel plate fixtures in conjunction with the cone-and-plate observations. In this way it is possible for the first time to quantify successfully the variations in the second normal stress difference of viscoelastic suspensions for solid fractions of up to 25 vol.%. In contrast to measurements of the first normal stress difference, the second normal stress difference is negative with a magnitude that increases with increasing solid content. The changes in the first and second normal stress differences are also strongly correlated to each other: The relative increase in the second normal stress difference is equal to the relative decrease of the first normal stress difference at the same solid fraction. The variations of the first as well as of the second normal stress difference are represented by power law functions of the shear stress with an unique power law exponent that is independent of the solid fraction. The well known edge effects that arise in cone-and-plate as well as parallel-plate rheometry and limit the accessible measuring range in highly viscoelastic materials to low shear rates could be partially suppressed by utilizing a custom- designed guard-ring arrangement. A procedure to correct the guard-ring influence on torque and normal force measurements is also presented. Received: 20 December 2000 Accepted: 7 May 2001     

Obtaining the steady shear rheological properties and apparent wall slip velocity data of a water-in-oil emulsion from gap-dependent parallel plate viscometry data

A two-stage Tikhonov regularisation procedure has been used to obtain rheological properties for a high internal phase emulsion from gap-dependent steady-state parallel plate shear data. This method is beneficial in that it can convert the steady shear data into rheological property functions. The built-in regularisation parameters of the method are able to keep noise amplification under control. The two-stage method is able to obtain not only the shear stress–shear rate function but also the apparent slip velocity as a function of wall shear stress. The method is such that it obtains the rheological functions over the maximum range of shear rate covered by the data. The results obtained using the new method are compared to those obtained using the vane geometry with good agreement being observed.     

Elastic properties of polyethylene melts at high shear rates with respect to extrusion

At high shear rates a steady state of shear flow with constant shear rate, constant shear stress, and constant recoverable shear strain is observed in the short-time sandwich rheometer after some few shear units already. The melt exhibits rather high elastic shear deformations and the recovery occurs at much higher speed than it is observed in the newtonian range. The ratio of first normal stress difference and twice the shear stress, being equal to the recoverable strain in the second-order fluid limit, significantly underestimates the true elastic shear strains at high shear rates. The observed shear rate dependence of shear stress and first normal stress difference as well as of the (constrained) elastic shear strain is correctly described on the basis of a discrete relaxation time spectrum. In simple shear a stick-slip transition at the metal walls is found. Necessary for the onset of slip is a critical value of shear stress and a certain amount of elastic shear deformation or orientation of the melt.     

Elastic properties of a dilute surfactant solution in the shear induced state

The first normal stress differences N ₁ of a highly dilute cationic surfactant solution are investigated in a cone-and-plate rheometer. In continuation of a previous paper (Nowak 1998), where the buildup of a shear induced structure in such a solution was attained after a reduced deformation, the N ₁ turned out to be in proportion to the square of the shear rate γ˙ reduced by a critical value γ˙ _c in a first range above γ˙ _c . At higher shear rates the N ₁ tend to lower values than predicted by this relation. Relaxation experiments were performed in the same geometry to determine the characteristic time scales of the shear induced state's decay. In the lower range above &γdot; _c the stress decay is a monoexponential process, while a second time constant has to be introduced to describe the relaxation in that range, where the N ₁ deviate from the parabolic dependence of the reduced shear rate. Received: 10 May 1999 Accepted: 15 November 2000     

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对于连续截面直梁平面横力弯曲情形, 分析了剪切变形引起横截面翘曲的影响. 基于位移模式假定, 用材料力学方法得到相应的正应力与切应力表达式, 并以均布力作用的矩形截面简支梁为例说明截面翘曲对于应力的影响. 该分析方法及其结果适用于材料力学教学.     

Rheo-optical measurements of the first and third normal stresses of homopolymer poly(vinyl methyl ether) melt

Normal stresses play a key role in polymer processing, yet accurate measurements are still challenging. Simultaneous rheo-optical measurements are conducted on a poly(vinyl methyl ether) homopolymer melt over a wide range of temperatures and oscillatory shear frequencies, in an effort to measure the normal stresses, by using quantitative flow birefringence measurements. The stress optical rule holds well for this polymer as expected, with the value of the stress optic coefficient of (6.38±0.19)×10⁻¹¹ cm²/dyn at 30°C. The first and third normal stress difference coefficients, calculated using a single memory constitutive equation applied to the stress and birefringence data, are in excellent agreement. The ratio of the measured third and first normal stress difference coefficients, (1−β)=0.71±0.05, agrees well with the result of the Doi–Edwards model with independent alignment approximation (β=0.28). The measurement of normal stress difference coefficients with such small deviations proves the robust nature of the improved rheo-optical instrument and its ability to measure complete stress tensor.     

Thrust and slip of a track determined by the compression–sliding approach

Driving gear of a vehicle (here a track) generates thrust as a reaction to the opposite force taken by the ground. This force causes rearward soil deformation, which is associated with vehicle slippage. The presented compression–sliding (CS) approach, based on field measurements with the original double plate (DP) meter, states that the soil deformation as a consequence to the increasing thrust occurs in two principal stages: (a) primary horizontal soil compression, which steadily increases towards the back of the contact length forming virtual soil segments among neighboring grousers and (b) secondary slide of these sheared off segments referred to as soil blocks, which may collapse under specific conditions. These two stages are separated by a transient situation when both the compression and sliding occur simultaneously.The respective compression–sliding (CS) approach enables to analyze the effect of track arrangement, design and loading on its thrust–slip characteristics. The paper also deals with situation of the existing shear plane theory in view of the CS approach and finally suggests a practical thrust–slip function complying with the CS logic.     

An investigation of squeeze flow as a viable technique for determining the yield stress

A systematic study of squeeze flow (SF) was performed on different concentrations of Carbopol with varying yield stresses. A sample of constant volume was placed between two parallel plates and a series of constant force steps applied, following the plate separation as a function of time. Precise rheological measurements of the model yield stress fluids were performed in addition to the well-controlled SF tests. These rheological measurements were used in conjunction with the SF equations to determine the time-dependent plate separation, allowing a direct comparison of theory and experiment throughout the entire test. The limiting height achieved during constant force SF reveals information about the yield stress of the fluid as predicted by the theory. It appears that by carefully controlling the experimental conditions of the squeeze test one can obtain yield stress values that agree with the rheological measurements within 10%. Additionally, the validity of the lubricational theory was tested; not only for the determination of the yield stress but throughout the flow as well.     

The expression of stress and strain at the tip of notch in reissner plate

In this paper, the eigenequation of notch in Reissner plate is derived by the eigenfunction method. Eigenvalues of different notches with different angles are calculated by Muller iteration method.The expression of stress and strain at the tip of notch in Reissner plate is obtained.     

Simulations of the unsteady separated flow past a normal flat plate

Well-resolved two-dimensional numerical simulations of the unsteady separated flow past a normal flat plate at low Reynolds numbers have been performed using a fractional step procedure with high-order spatial discretization. A fifth-order upwind-biased scheme is used for the convective terms and the diffusive terms are represented by a fourth-order central difference scheme. The pressure Poisson equation is solved using a direct method based on eigenvalue decomposition of the coefficient matrix. A systematic study of the flow has been conducted with high temporal and spatial resolutions for a series of Reynolds numbers. The interactions of the vortices shed form the shear layers in the near-and far-wake regions are studied. For Reynolds numbers less than 250 the vortices are observed to convect parallel to the freestream. However, at higher Reynolds numbers (500 and 1000), complex interactions including vortex pairing, tearing and deformations are seen to occur in the far-wake region. Values of the drag coefficient and the wake closure length are presented and compared with previous experimental and numerical studies.     

Measurements of the first normal-stress difference in a new Rheo-dilatometer for molten polymers: Triple-step-shear-strain tests for all K-BKZ constitutive equations

Following the 3rd of a triple-step-shear-strain sequence, the relaxation of the first normal-stress difference,N ₁ (t), has been measured for a sample (IUPAC A) of low-density polyethylene at 150 °C over a range of shear-strain magnitudes up to 28 shear units. A new cone-plate Rheodilatometer was used, giving sample volume change data as well as thrust and torque data during cone rotation. At 130 °C, prior measurements (described elsewhere) gave an upper limit of 0.001% for the volume change with IUPAC A; this gave an estimated error of only 1.7% in determiningN ₁(t) from time-dependent thrust data. Wagner's network-rupture model (based on a postulated strain-induced irreversible network disentanglement process) gave quantitative agreement withN ₁(t) data for IUPAC A at 150 °C over some of the ranges of time and shear-strain investigated. Wagner's earlier constitutive equation (of K-BKZ type) gave no quantitative agreement. Using a special choice of strain magnitudes in which the 3rd is half that of the 1st and 2nd, it is shown that a critical test of all K-BKZ equations can be made on the basis ofN ₁ (t) data only. This test excludes all K-BKZ equations for IUPAC A under the conditions here used. In all the present investigations, the 1st and 3rd shears had the same sign while the 2nd had the opposite sign.     

Wall shear stress modified by bubbles in a horizontal channel flow of silicone oil in the transition region

We performed laboratory experiments on bubbly channel flows using silicone oil, which has a low surface tension and clean interface to bubbles, as a test fluid to evaluate the wall shear stress modification for different regimes of bubble migration status. The channel Reynolds numbers of the flow ranged from 1000 to 5000, covering laminar, transition and turbulent flow regimes. The bubble deformation and swarms were classified as packing, film, foam, dispersed, and stretched states based on visualization of bubbles as a bulk void fraction changed. In the dispersed and film states, the wall shear stress reduced by 9% from that in the single-phase condition; by contrast, the wall shear stress increased in the stretched, packing, and foam states. We carried out statistical analysis of the time-series of the wall shear stress in the transition and turbulent-flow regimes. Variations of the PDF of the shear stress and the higher order moments in the statistic indicated that the injection of bubbles generated pseudo-turbulence in the transition regime and suppressed drag-inducing events in the turbulent regime. Bubble images and measurements of shear stress revealed a correlated wave with a time lag, for which we discuss associated to the bubble dynamics and effective viscosity of the bubble mixture in wall proximity.