Reliable plate–plate MRF magnetorheometry based on validated radial magnetic flux density profile simulations

The apparent shear stress from plate–plate magnetorheometry, using the commercial magnetocell MRD180/1T (Physica/Anton Paar) in standard configuration, is distinctly overestimated. The effect is due to a flux density maximum near the sample rim and radial migration of iron particles towards the rim. Radial magnetic flux density profiles were investigated by finite element simulations using the Maxwell^®2D code and by direct Hall probe measurements. The reliability of the finite element method results, both for the empty magnetocell and with magnetorheological fluid (MRF) in the measuring gap, allows conclusions on the true flux density within the MRF, which cannot be accessed by Hall probe measurements. If the MRF sits on top of the bottom yoke (standard configuration), the flux density maximum reaches twice the plateau value (0.74 T for 3 A coil current and 0.3 mm gap height of the investigated MRF). This yields a higher effective flux density and causes radial iron particle migration, resulting in an additional magnetic flux increase near the rim due to augmented MRF magnetisation. As a result, the rotor torque at constant rotary speed increases with time. Reliable results are achieved by a modification of the magnetocell, such that the MRF sits on a non-magnetic Hall disc of 1.5 mm thickness, allowing an online flux density measurement by a FW Bell Hall probe. In this configuration, the radial flux density profile near the rim remains sufficiently flat and no iron particle migration is detected.     

Measurement of pressure coefficient of melt viscosity: drag flow versus capillary flow

The pressure coefficient of viscosity of poly(α-methylstyrene-co-acrylonitrile) was measured using a high-pressure sliding plate rheometer (HPSPR) and two types of capillary rheometer: a piston-driven device with a throttle at the exit [piston capillary rheometer with throttle (PCRWT)] operated at a fixed flow rate, and a counter-pressure nitrogen capillary rheometer (CPNCR) operated at a fixed pressure drop. In the HPSPR, the pressure, shear rate, density, and viscosity are all uniform throughout the sample, while the analysis of capillary data is complicated by the axial pressure gradient and the radial shear rate gradient. The polymer was found to be piezorheologically simple, and the HPSPR data indicated that the pressure coefficient of viscosity β ≡ dln(a _P)/dP decreased slightly with increasing pressure at high pressure. While β from PCRWT data from different laboratories and instruments agreed fairly well, the β values were on average about 2/3 of that from the HPSPR. The CPNCR yields β about 18% lower than that of the HPSPR.     

Measurement modes of the response time of a magneto-rheological fluid (MRF) for changing magnetic flux density

The response of a magneto-rheological fluid (MRF) to a change of magnetic flux density is investigated by using a commercial plate–plate magneto-rheometer MCR501 (Anton Paar GmbH) at constant shear rate. The instrument was modified to allow an online determination of the transient flux density in the MRF. Both current and voltage imposition to the magneto-cell were applied by using a power operational amplifier to drive the electromagnet. Assuming a Maxwell behavior with switching time λ and a linear increase in shear stress with flux density, analytic relations for the transient shear stress are derived for sinusoidal and single exponential flux densities vs time. True switching times of a few milliseconds are only obtained if the low pass filter in the original MCR501 torque signal is surpassed by a firmware allowing a sampling rate of 0.1 ms. For a sinusoidal flux density, the switching time is derived from the modulation depth of the shear stress. An upper bound of λ < 3 ms for a flux density of 0.8 T was found. For step coil current imposition of 1 T magnitude, switching times of 2.8 ms (start-up) and 1.8 ms (shutdown) allowed to fit the transient torque signal more than 2/3 of the total change. Finally, the effect of a sigmoidal characteristic on the switching time determination is addressed. This paper was presented at Annual European Rheology Conference (AERC) held in Hersonisos, Crete, Greece, April 27-29, 2006.     

Rheometry towards complex flows: Squeeze flow technique

Disk-like samples are submitted to controlled squeezing forces between parallel plates and the time-dependent sample height is measured. Isothermal tests at constant force enable the determination of viscosity functions of melts. Experiments using a constant disk radius and a constant disk volume are compared. Creep and creep recovery tests are made possible by a height-dependent control of the force. The evaluation of a pressure-dependent yield stress is demonstrated for wax powder. The squeeze flow technique is of advantage for systems with a layer structure or matrices containing long fibres or mats. In non-isothermal experiments on solidifying materials, either by crystallization or polymerization, the total deformation and the speed of solidification in processes like stamp moulding can be determined.     

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     

Correlation between the gel time and quiescent/quasi-quiescent crystallization onset time of poly(butene-1) as determined from rheological methods

A comparison between two quantities concerning quiescent crystallization of polymer melts, namely the quiescent crystallization onset time (t _on,q) and gel time (t _gel), is performed using rheological methods. It was found that t _gel as measured from the evolution of loss angle (tan δ) occurs slightly earlier than t _on,q, defined as the time required for the viscosity to reach twice its steady-state value. The change of viscosity with time was measured with Small Amplitude Oscillatory Shear (SAOS) method. Two alternative methods to measure t _on,q are studied: by continuous shear at a very small shear rate and by creep method. A very good agreement from all the three methods was achieved, indicating the robust nature of this quantity. Finally, the gel times for different PB-1 samples are considered. When the difference in crossover angular frequencies (ω _x ) of the samples is taken into account in performing t _gel experiments, it can be shown that the temperature dependence of t _gel for the samples are the same. However, for samples having high molecular weight t _gel measurements are problematic. In this case, t _on,q serves as an easier tool to compare the crystallization behaviour of different samples.     

Model analysis of nonlinear viscoelastic behaviour by use of a single integral constitutive equation: Stresses and birefringence of a polystyrene melt in intermittent shear flows

Summary A single integral constitutive equation with strain dependent and factorized memory function is applied to describe the time dependence of the shear stress, the primary normal-stress difference, and, by using the stress-optical law, also the extinction angle and flow birefringence of a polystyrene melt in intermittent shear flows. The theoretical predictions are compared with measurements. The nonlinearity of the viscoelastic behaviour which is represented by the so called damping function, is approximated by a single exponential function with one parametern. The damping constantn as well as a discrete relaxation time spectrum of the melt can be determined from the frequency dependence of the loss and storage moduli.

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Zusammenfassung Eine Zustandsgleichung vom Integraltyp mit einer deformationsabhängigen und faktorisierten Gedächtnisfunktion wird zur Beschreibung der Zeitabhängigkeit der Schubspannung, der ersten Normalspannungsdifferenz und, unter Verwendung des spannungsoptischen Gesetzes, auch des Auslöschungswinkels und der Strömungsdoppelbrechung einer Polystyrol-Schmelze bei Scherströmungen herangezogen. Die theoretischen Voraussagen werden mit Messungen verglichen. Die Nichtlinearität des viskoelastischen Verhaltens, repräsentiert durch die sogenannte Dämpfungsfunktion, wird durch eine einfache Exponentialfunktion mit nur einem Parametern angenähert. Die Dämpfungskonstanten kann, wie auch ein diskretes Relaxationszeitspektrum der Schmelze, aus der Frequenzabhängigkeit der Speicher- und Verlustmoduln bestimmt werden.

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a _i weight factor of thei-th relaxation time - a _T shift factor - C stress-optical coefficient - n flow birefringence in the shear flow plane - shear relaxation modulus - G() shear storage modulus - () shear loss modulus - H() relaxation time spectrum - h( _t,t ² ) damping function - M _w weight-average molecular weight - M _n number-average molecular weight - n damping constant - p ₁₂ shear stress - p ₁₁ –p ₂₂ primary normal stress difference - t current time - t past time - extinction angle - ( — _i) delta function - time and shear rate dependent viscosity - | ^*| absolute value of the complex viscosity - shear rate - _t,t relative shear strain between the statest andt - memory function - angular frequency - relaxation time - _i i-th relaxation time of the line spectrum - time and shear rate dependent primary normal stress coefficient - s steady-state value - t time dependence - ° linear viscoelastic behaviour With 6 figures and 1 table     

Shear-induced crystallization of PB-1 up to processing-relevant shear rates

Two experimental methods to study shear-induced crystallization of poly(butene-1) (PB-1) in the high shear rate region are presented: one using a concentric cylinder rheometer and the other a capillary rheometer equipped with a cylindrical die. The crystallization onset time (t _on) is used as the parameter to monitor crystallization progress through the output signal from each device. By combining the new data with the results from a previous paper (2005) in which a plate–plate rheometer was used, onset time data covering a shear rate range from 10^-4 to 500 s^-1 at temperatures 99–107°C are obtained. In this range, a decrease in onset time spanning five decades is observed. The onset times obtained from the capillary rheometer are larger compared to those from the other two methods, which can be explained from the different type of flow. The data also confirm the procedure to construct a temperature-invariant curve, which can be extended to high shear rates for three PB-1 samples having different molecular weight distributions. The slope of the fitted curve for all three cases is −1, which suggests that a critical value is required for shear-induced crystallization. The morphology of the formed crystals (spherulitic or rod-like) depends on the molecular weight, but this does not affect the validity of the T-invariant curve. Above the melting point, it is shown that the amount of long chains influences the temperature limit where shear-induced crystallization can still take place.The paper was presented at AERC 2005, Grenoble, with the title “Shear-Induced Crystallization of Polybutene-1 Covering a Wide Shear Rate Range.”An erratum to this article can be found at     

Orientation effects and rheology of short glass fiber-reinforced thermoplastics

The rheology of polyolefines, polyamide 6, and polystyrene-acrylonitrile filled with glass fibers of different concentrations and aspect ratios have been investigated in simple shear flow, capillary rheometry, and uniaxial elongation. A comparison is made with unfilled and glass bead-filled melts. Fiber orientation was investigated by X-ray microradiography.Steady-state viscosities are obtained on fibers aligned parallel to the direction of flow. Entrance pressure losses, the shape of the viscosity function, and the appearance of a yield stress are depending on the fiber aspect ratio. The temperature dependence of the viscosity function is not significantly different from that of the unfilled melt.Transient shear stresses were measured on samples of different initial orientations of the fibers. The change of fiber orientation during shear flow gives rise to a pronounced overshoot of shear stress and normal stress difference. Elastic strains in shear are increased by the fibers but elastic elongational strains are reduced. Mechanisms are proposed to explain the experimental observations.Dedicated to Dr. D. Heinze on the occasion of his 60th birthday.     

Asymmetrical hippocampal connectivity in mesial temporal lobe epilepsy: evidence from resting state fMRI

Background

Recent studies have shown that the human right-hemispheric auditory cortex is particularly sensitive to reduction in sound quality, with an increase in distortion resulting in an amplification of the auditory N1m response measured in the magnetoencephalography (MEG). Here, we examined whether this sensitivity is specific to the processing of acoustic properties of speech or whether it can be observed also in the processing of sounds with a simple spectral structure. We degraded speech stimuli (vowel /a/), complex non-speech stimuli (a composite of five sinusoidals), and sinusoidal tones by decreasing the amplitude resolution of the signal waveform. The amplitude resolution was impoverished by reducing the number of bits to represent the signal samples. Auditory evoked magnetic fields (AEFs) were measured in the left and right hemisphere of sixteen healthy subjects.

Results

We found that the AEF amplitudes increased significantly with stimulus distortion for all stimulus types, which indicates that the right-hemispheric N1m sensitivity is not related exclusively to degradation of acoustic properties of speech. In addition, the P1m and P2m responses were amplified with increasing distortion similarly in both hemispheres. The AEF latencies were not systematically affected by the distortion.

Conclusions

We propose that the increased activity of AEFs reflects cortical processing of acoustic properties common to both speech and non-speech stimuli. More specifically, the enhancement is most likely caused by spectral changes brought about by the decrease of amplitude resolution, in particular the introduction of periodic, signal-dependent distortion to the original sound. Converging evidence suggests that the observed AEF amplification could reflect cortical sensitivity to periodic sounds.