Temperature dependence of the interfacial tension of PS/PMMA, PS/PE, and PMMA/PE blends

The effect of temperature on the interfacial tension for PS/PMMA, PS/PE, and PMMA/PE was measured using the imbedded fiber retraction method. Interfacial tensions for PS/PMMA, PS/PE, and PMMA/PE were measured over temperature ranges of 160–250 °C, 140–220 °C, and 140–220 °C, respectively. The interfacial tension was found to follow a dependence of 3.6–0.013 T dyn/cm, 7.6–0.051 T dyn/cm and 11.8–0.017 T dyn/cm for PS/PMMA, PS/PE, and PMMA/PE, respectively. Comparison of the data with the mean field theory of Helfand and Sapse were made; however, a simple linear fit to the data described the temperature dependence in the experimental window as well as the predictions of the mean field theory. Received: 6 July 1999 Accepted: 23 March 2000     

The imbedded disk retraction method for measurement of interfacial tension between polymer melts

A method for measuring interfacial tension of high viscosity polymer melts at elevated temperatures is described. The method involves the tracking of the shape evolution of a disk of one material imbedded in a second one. This makes it possible to determine the interfacial tension over a relatively short time period. The technique of preparing the samples makes it possible to measure on practically any combination of polymer melts without restrictions on viscosities and melting temperature, as long as one of the materials is transparent in the molten state.The retraction of the disk is observed by using a microscope with a high resolution video camera. The camera is connected to a video frame grabber in a personal computer which is programmed to collect images with preselected time intervals. Data of the retraction is acquired by using an image analysis software, measuring the average radius of the disk.The driving force for the shape evolution is interfacial tension and it is balanced by viscous forces. The analysis of the retraction process is done analytically with a simplified one-dimensional model. The model has been compared to experiments with the system PS/PMMA at 210 °C, covering viscosity ratios over a range of six decades and five different molecular weight values of PS. It is shown that interfacial tension can be determined over the whole range and a value of 1.1±0.2 mN/m was obtained for all samples.     

Droplet retraction in the presence of nanoparticles with different surface modifications

We studied the influence of nanoparticles with different surface modifications on the interfacial tension and relaxation of model polymer blend after cessation of different strains. The droplet retraction experiments were carried out on a model system composed of polydimethylsiloxane (PDMS) as the suspending fluid and polyisobutylene (PIB) as droplet at room temperature in the presence of hydrophobic and hydrophilic nanosilica. Different weight fractions of particles were dispersed in the PIB droplet before forming a dispersed droplet by using a microsyringe in shear cell. We found that applied strain, nanoparticle concentration and their thermodynamically preferred localization affect both nominal interfacial tension and droplet retraction process. By addition of nanoparticles at a concentration as low as 0.2%wt, the nominal interfacial tension decreases from 3.12?±?0.15 mN/m for neat PIB-PDMS interface depending on the surface characteristics of nanosilica. Hydrophilic nanosilica has the most effect on nominal interfacial tension and decreases it as low as 0.2?±?0.21 mN/m at 1 wt.% loading under a strain of 7. The results show that the retraction process in this system is mainly controlled by interfacial phenomena rather than bulk rheological properties. Additionally, the shape evolution of droplets changes and the retraction rate slows down in the presence of nanoparticles.     

Recoverable deformation and morphology after uniaxial elongation of a polystyrene/linear low density polyethylene blend

The transient recoverable deformation ratio after melt elongation at various elongational rates and maximum elongations was investigated for pure polystyrene and for a 85 wt.% polystyrene/15 wt.% linear low density polyethylene (PS/LLDPE 85:15) blend at a temperature of 170 ^oC. The ratio p of the zero shear rate viscosity of LLDPE to that of PS is p = 0.059 ≈ 1:17. Retraction of the elongated LLDPE droplets back to spheres and end-pinching is observed during recovery. A simple additive rule is applied in order to extract the contribution of the recovery of the elongated droplets from the total recovery of the blend. In that way, the recoverable portion of the PS/LLDPE blend induced by the interfacial tension is determined and compared with the results of a theory based on an effective medium approximation. The effective medium approximation reproduces well the time scale of the experimental data. In addition, the trends that the recoverable deformation increases with elongational rate and maximum elongation are captured by the theoretical approach.     

Effect of temperature and molecular weight on the interfacial tension of PS/PDMS blends

The imbedded-fiber retraction (IFR) method was used to study the effect of temperature and PDMS molecular weight on the interfacial tension of PS/PDMS blends. The interfacial tension decreased with increasing temperature and analysis of the temperature dependence using a simple linear fit gave –dγ/dT value of 0.058±0.010 dyn/cm-deg. Reported –dγ/dT values of PS/PDMS blends are highly dependent on the molecular weights of the polymers and can have values that are <0, 0, or >0. Our interfacial tension values were independent of the molecular weight of PDMS and this was attributed to the molecular weights studied here being well above the entanglement values of both polymers. However, analysis of interfacial tension data from this work and the literature showed the following empirical relationship between apparent blend molecular weight, M_b, and interfacial tension of PS/PDMS blends with a correlation of 0.94: γ₁₂=γ₀+k₂M_b ^(–2/3), where γ₀=7.3±0.3 dyn/cm; k₂=–517±41 (dyn/cm)(g/mol)^2/3.     

A New Device for Mechanical Testing of Blood Vessels at Cryogenic Temperatures

As part of an ongoing program to study the thermo-mechanical effects associated with cryopreservation via vitrification (vitreous in Latin means glassy), the current study focuses on the development of a new device for mechanical testing of blood vessels at cryogenic temperatures. This device is demonstrated on a bovine carotid artery model, permeated with the cryoprotectant cocktail VS55 and a reference solution of 7.05M DMSO, below glass transition. Results are also presented for crystallized specimens, in the absence of cryoprotectants. Results indicate that the elastic modulus of a specimen with no cryoprotectant, at about −140°C (8.6 and 15.5°C below the glass transition temperature of 7.05M DMSO and VS55, respectively), is 1038.8 ± 25.2 MPa, which is 8 and 3% higher than that of a vitrified specimen permeated with 7.05M DMSO and VS55, respectively. The elastic modulus of a crystallized material at −50°C is lower by ∼20% lower from that at −140°C.     

Thermoreversible gels in oil/EVA systems

In this work we investigate the gel formation of EVA/recycled motor oil systems as a route to obtain synthetic binders which could be used instead of natural bitumen, as well as mixed with natural bitumen to modify adequately its viscoelastic response. The EVA copolymer studied in this work has a vinyl acetate content of 18 wt% and solutions of EVA/motor oil have been prepared up to a concentration of 50 wt%. Dynamic viscoelastic frequency sweeps between 10⁻² Hz and 10² Hz have shown that above 3 wt%, at 25 °C, EVA/motor oil systems form gels. It has been possible to define an elastic equilibrium modulus, G_e, for each gel. The dependence of G_e on concentration has been compared with that of PVC/DOP and SBS/oil gels on the basis of the De Gennes model. Thermal stability of EVA/motor oil gels has also been analyzed, indicating that for the highest polymer concentrations gel point is above 80 °C. Received: 23 December 1999 Accepted: 13 June 2000     

Rheological behavior of dilute solutions of a side-chain liquid-crystalline polysiloxane in 4,4′-n-octylcyanobiphenyl

The electrorheological (ER) behavior and stress transient response of dilute solutions of a side-chain liquid-crystalline polysiloxane (LCP) in 4,4′-n-octylcyanobiphenyl (8CB) is studied. In the flow-tumbling regime of 8CB, i.e. from T = 34–38 °C, the stress transients of both 8CB and LCP/8CB solutions show oscillatory responses, but with shorter oscillation periodicities for the solution. In the flow-aligning regime of 8CB, i.e. at 39 and 40 °C, a transformation to flow-tumbling is observed in the stress transients of the LCP/8CB solution. In both cases, analysis of the transient responses indicates that the change in Leslie viscosity coefficients on dissolving the LCP are δα₂ < 0 and δα₃ > 0. The amplitude of the ER response, defined as the viscosity difference between the on and off states, Δη = η_on − η_off, is only weakly affected by the dissolution of LCP. These rheological results can be interpreted consistently using a modified version of a hydrodynamic theory by Brochard, provided an additional dissipation mechanism is included, which derives from the presence of an elastic torque between director rotation and LCP orientation. Received: 8 September 1999/Accepted: 13 December 1999     

Experimental Investigation of Strain Rate Dependence of Nanocrystalline Pt Films

A new microscale uniaxial tension experimental method was developed to investigate the strain rate dependent mechanical behavior of freestanding metallic thin films for MEMS. The method allows for highly repeatable mechanical testing of thin films for over eight orders of magnitude of strain rate. Its repeatability stems from the direct and full-field displacement measurements obtained from optical images with at least 25 nm displacement resolution. The method is demonstrated with micron-scale, 400-nm thick, freestanding nanocrystalline Pt specimens, with 25 nm grain size. The experiments were conducted in situ under an optical microscope, equipped with a digital high-speed camera, in the nominal strain rate range 10⁻⁶–10¹ s⁻¹. Full field displacements were computed by digital image correlation using a random speckle pattern generated onto the freestanding specimens. The elastic modulus of Pt, E = 182 ± 8 GPa, derived from uniaxial stress vs. strain curves, was independent of strain rate, while its Poisson’s ratio was v = 0.41 ± 0.01. Although the nanocrystalline Pt films had the elastic properties of bulk Pt, their inelastic property values were much higher than bulk and were rate-sensitive over the range of loading rates. For example, the elastic limit increased by more than 110% with increasing strain rate, and was 2–5 times higher than bulk Pt reaching 1.37 GPa at 10¹ s⁻¹.     

2D temperature measurements in the wake of a heated cylinder using LIF

A technique is described to measure the instantaneous 2D temperature distribution in the wake of a heated cylinder using `laser-induced fluorescence'. Rhodamine B, a fluorescent dye, is used as a temperature indicator. The relation between fluorescence intensity and temperature is determined by means of calibration experiments in the temperature range of 20–35 °C with an accuracy of ±0.1 °C. The temperature distribution behind the heated cylinder is well visible and can be measured with a high spatial resolution. Corrections for variation in laser energy and intensity distribution in the laser sheet have to be made to further improve the accuracy of the measuring method. Received: 3 January 2001/Accepted: 18 May 2001     

Strain-gage stability measurements for three years at 150°C in air

The zero shifts of nickel-chromium foil strain gages (modified Karma) were measured over a period of three years at a constant temperature of 150°C in air. Three gage lengths were included—1.585 mm (1/16 in.), 3.170 mm (1/8 in.), and 6.340 mm (1/4 in.). The strain gages were bonded to constant-stress cantilever beams which were subjected to nomial mechanical strain levels of 0, ±780 μm/m, and ± 1350 μm/m. Each strian gage was connected by threewire leads to a Wheatstone-bridge circuit for the test duration. The data support two general observations: (1) short gage lengths suffer larger zero shifts than longer gage lengths, and (2) gages in compression suffer large zero shifts than gages in tension. On the assumption that the major cause of the zero shifts is a combination of corrosion of the foil and creep of the gage/epoxy/beam system, the author suggests a possible way to correct for the zero shift by experimentally determining the combined corrosion/creep effect and substracting it from the strain-gage readings. Some of the data appear to be consistent with this assumption, but some of the data do not.     

Influence of humidity on the convective heat transfer from small cylinders

 The convective heat transfer from a cylinder to a humid air stream flowing normal to the cylinder was investigated experimentally at atmospheric pressure over a range of variables which is relevant to the use of hot‐wire anemometry: air temperatures between 30 °C and 70 °C and velocities between 12 and 37 m/s. For molar fractions of water vapour up to 0.27, the heat transfer increased with increasing humidity. The ratio of heat transfer rates in humid air and dry air is a unique function of the molar fraction of water vapour, independent of the air temperature and flow velocity. Received: 28 November 1996/Accepted: 5 July 1997     

Ionic strontium fluorescence as a method for flow tagging velocimetry

A flow tagging technique based upon ionic fluorescence in strontium is investigated for applications to velocity measurements in gas flows. The method is based upon a combination of two laser based spectroscopic techniques, i.e. resonantly-enhanced ionisation and laser-induced ionic fluorescence. Strontium is first ionised and then planar laser-induced fluorescence is utilised to give 2D `bright images' of the ionised region of the flow at a given time delay. The results show that this method can be used for velocity measurements. The velocities were measured in two types of air–acetylene flames – a slot burner and a circular burner yielding velocities of 5.1 ± 0.1 m/s and 9.3 ± 0.2 m/s, respectively. The feasibility of the method for the determination of velocities in faster flows than those investigated here is discussed. Received: 5 November 1998/Accepted: 19 January 2000     

Rheological properties of gluten plasticized with glycerol: dependence on temperature, glycerol content and mixing conditions

The rheological behaviour of a gluten plasticized with glycerol has been studied in oscillatory shear. The mixing operation in a Haake batch mixer leads to a maximum torque for a level of specific energy (500–600 kJ/kg) and temperature (50–60 °C) quite independent of mixing conditions (rotor speed, mixing time, filling ratio). The gluten/glycerol dough behaves as a classical gluten/water dough, with a storage modulus higher than the loss modulus over the frequency range under study. A temperature increase induces a decrease of moduli, but the material is not thermorheologically simple. Glycerol has a plasticizing effect, which can be classically described by an exponential dependence. Mixing conditions influence the viscoelastic properties of the material, mainly through the specific mechanical energy input (to 2000 kJ/kg) and temperature increase (to 80 °C). Above 50 °C, specific mechanical energy highly increases the complex modulus. The aggregation of proteins, as evidenced by size-exclusion chromatography measurements, occurs later as the dough temperature reaches 70 °C. The nature of network interactions and the respective influence of hydrophobic and disulphide contribution is discussed. A general expression is proposed for describing the viscous behaviour of a gluten/glycerol mix, which could seem simplistic for such a complex rheological behaviour, but would remain sufficient for modelling the flow behaviour in a twin screw extruder. Received: 24 November 1997 Accepted: 28 April 1999     

Experimental investigation of mixed convection heat transfer in a horizontal and inclined rectangular channel

 Mixed convection heat transfer in rectangular channels has been investigated experimentally under various operating conditions. The lower surface of the channel is subjected to a uniform heat flux, sidewalls are insulated and adiabatic, and the upper surface is exposed to the surrounding fluid. Experiments were conducted for Pr=0.7, aspect ratios AR=5 and 10, inclination angles 0° ≤ θ ≤ 30°, Reynolds numbers 50 ≤ Re ≤ 1000, and modified Grashof numbers Gr*=7.0 × 10⁵ to 4.0 × 10⁷. From the parametric study, local Nusselt number distributions were obtained and effects of channel inclination, surface heat flux and Reynolds number on the onset of instability were investigated. Results related to the buoyancy affected secondary flow and the onset of instability have been discussed. Some of the results obtained from the experimental measurements are also compared with the literature, and a good agreement was observed. The onset of instability was found to move upstream for increasing Grashof number and increasing aspect ratio. On the other hand, onset of instability was delayed for increasing Reynolds number and increasing inclination angle. Received on 19 March 2001 / Published online: 29 November 2001     

Strain Measurements of Silicon Dioxide Microspecimens by Digital Imaging Processing

Silicon dioxide thin film is a common component in electronic devices and in MEMS, but its mechanical properties have rarely been studied. Techniques have been adapted and developed to conduct tensile tests on 1.0 μm thick silicon dioxide specimens that are 100, 150, and 200 μm wide and either 1 or 2 mm long. One end of the specimen remains fastened to the substrate, and the other is glued to a silicon carbide fiber attached to a 30 g load cell mounted on a piezoelectric translation stage. Strain is measured by digital imaging of two gold lines applied to the gage section of the transparent specimen. Twenty-five tests yield a Young’s modulus of 60.1 ± 3.4 GPa and a fracture strength of 364 ± 57 MPa.     

Irradiation-Induced Solute Clustering in a Low Nickel FeMnNi Ferritic Alloy

Understanding the radiation embrittlement of reactor pressure vessel (RPV) steels is required to be able to operate safely a nuclear power plant or to extend its lifetime. The mechanical properties degradation is partly due to the clustering of solute under irradiation. To gain knowledge about the clustering process, a Fe−1.1 Mn−0.7 Ni (at.%) alloy was irradiated in a test reactor at two fluxes of 0.15 and 9 ×10¹⁷ n _E > 1MeV .m^− 2.s^− 1 and at increasing doses from 0.18 to 1.3 ×10²⁴ n _E > 1MeV .m^− 2 at 300°C. Atom probe tomography (APT) experiments revealed that the irradiation promotes the formation in the α iron matrix of Mn/Mn and/or Ni/Ni pair correlations at low dose and Mn–Ni enriched clusters at high dose. These clusters dissolve partially after a thermal treatment at 400°C. Based on a comparison with thermodynamic calculations, we show that the solute clustering under irradiation can just result from an induced mechanism.     

Temperature dependence of the viscosity of highly starch-filled poly(hydroxy ester ether) biodegradable composites

 The temperature dependence of the viscosity of starch-filled poly(hydroxy ester ether) (PHEE) biodegradable composites was analyzed using Arrhenius and WLF equations. Corn starch/PHEE materials were extruded using a twin screw extruder with starch volume fractions from 0.27 to 0.66. Dynamic strain sweep measurements were carried out at 10 rad/s at six different temperatures from 100 °C to 150 °C. Both Arrhenius and WLF equations model equally well the temperature effect on viscosity of PHEE and starch/PHEE composites with starch volume fractions up to 0.36. Arrhenius equation with stress correction describes the stress dependence of viscosity of starch/PHEE composites with higher starch volume fractions. The activation energy using both Arrhenius equation and Arrhenius equation with stress correction is 62.7 kJ/mol for pure PHEE and starch/PHEE composites. Received: 10 September 1999 Accepted: 27 March 2000     

Measurements and model predictions of transient elongational rheology of polymeric nanocomposites

Transient elongational rheology of two commercial-grade polypropylene (PP) and the organoclay thermoplastic nanocomposites is investigated. A specifically designed fixture consisting of two drums (SER Universal Testing Platform) mounted on a TA Instruments ARES rotational rheometer was used to measure the transient uniaxial extensional viscosity of both polypropylene and nanoclay/PP melts. The Hencky strain rate was varied from 0.001 to 2 s^− 1, and the temperature was fixed at 180°C. The measurements show that the steady-state elongational viscosity was reached at the measured Hencky strains for the polymer and for the nanocomposites. The addition of nanoclay particles to the polymer melt was found to increase the elongation viscosity principally at low strain rates. For example, at a deformation rate of 0.3 s^− 1, the steady-state elongation viscosity for polypropylene was 1.4 × 10⁴ Pa s which was raised to 2.8 × 10⁴ and 4.5 × 10⁴ Pa s after addition of 0.5 and 1.5 vol.% nanoclay, respectively. A mesoscopic rheological model originally developed to predict the motion of ellipsoid particles in viscoelastic media was modified based on the recent developments by Eslami and Grmela (Rheol Acta 47:399–415, 2008) to take into account the polymer chain reptation. We show that the orientation states of the particles and the rheological behavior of the layered particles/thermoplastic hybrids can be quantitatively explained by the proposed model.