A comparison of liquid–liquid porosimetry equations for evaluation of pore size distribution

This paper reviews and numerically tests many of the methods for the determination of pore size distribution of liquid membranes by liquid–liquid porosimetry. The flux through membranes was defined for flow of two immiscible liquids when drops or a liquid jet is formed, as well as the case when the interface is forced out by sufficient pressure. Several methods from literature for the determination of pore size distribution, some variations of these, and one new method are presented with a consistent theoretical basis. Using numerical tests it was found that all methods were very sensitive to measurement noise as low as ±0.1%, and that some form of data smoothing, such as a smoothing spline, was required to obtain a satisfactory distribution. The effects of elastic and permanent membrane compression were tested and a method was proposed to reduce the resulting error. A method based on the ratio of flux liquids with and without a liquid–liquid interface was recommended as it was less sensitive to the effects of compression in some cases and it provides a check when compression is not repeatable.     

Sub-micrometre dielectric and metallic yablonovite structures fabricated from resist templates

This paper reports the optical characterisation and numerical simulations of sub-micrometre yablonovite templates fabricated in poly-methyl methacrylate (PMMA) resist along with the pattern transfer to metals and other dielectrics. The fabrication is based on three consecutive exposures to an X-ray beam through a triangular lattice of holes. Up to seven (111) crystal periods are repeatedly obtained in thick PMMA layers. Optical characterisations of 1.3 m period templates show well-defined stop-bands in the mid-infrared, in good agreement with the numerical simulations. Two simple and low-cost methods are used to replicate the yablonovite structures in other materials. The pattern transfers to a metal (copper) and a high-refractive-index dielectric (titanium dioxide) are obtained by electrodeposition and a sol–gel technique, respectively. Very regular yablonovite-type metallic structures of 2 m lattice constant and 4.3 m height are fabricated with metallic wires of 500 nm diameter over a surface of 150 × 150 m².     

[60]富勒烯及其衍生物结构表征的有力工具－^3He 核磁共振谱

对[60]富勒烯衍生物的结构表征手段,特别是近年来兴起的^3He@C~n(n=60,70,78,84…)的合成及^3He核磁共振谱在结构表征中的应用进行了综述。     

Large deformation extensional rheology of bread dough

The stress–strain curves of bread dough were derived under uniaxial compression, uniaxial tension and equi-biaxial tension loading conditions. In uniaxial compression, a lubricant was used to eliminate frictional effects between the loading platens and the sample. In uniaxial tension, cylindrical samples with thin flat discs at both ends (‘I’ samples) were tested. The discs at both ends were allowed to air-dry and were subsequently glued onto the loading platens. In equi-biaxial tension, a thin disc of dough was inflated into a bubble using pressurised air. The thickness at the top of the bubble was measured by shining a light through the walls of the bubble and recording the change in light intensity as the wall becomes thinner. All methods ensured that uniform deformation was obtained. Stress and strain were accurately evaluated using image analysis techniques. The tests were performed at various strain rates and speeds that defined the time dependence of the material. A non-linear viscoelastic model based on the Prony series and Van der Waals hyperelasticity was used to predict all test data. The model had a total of five material parameters and two time constants, which were set to represent the actual time scales of the experiments. A reasonable agreement between the experimental data and the chosen material model was observed.     

Surface orientation characterisation of rough mc‐silicon surfaces by confocal microscopy and EBSD

For many semiconductor and photovoltaic applications the quality of substrate surfaces is an important requirement for the development of new devices. Therefore, methods are needed to analyse the surface structure in detail. In the following a new method is described that allows a fast analysis of as‐cut or artificially modified and textured surfaces. It uses laser confocal microscopy images. Therefrom the orientation of small surface elements are detected and depicted in an orientation distribution function of surface normals. The method is applied to as‐sawn mc‐silicon surfaces. It will be shown that it is also possible to determine the grain orientation for grains near 〈111〉 crystal direction by this method. The combination of electron backscatter diffraction and orientation distribution function analysis enables the detailed investigation of surface elements of an anisotropic etched silicon wafer. Inhomogeneity of surface textures can easily and rapidly be visualised by this method. Copyright © 2012 John Wiley & Sons, Ltd.     

Emulation of petroleum well-logging D-T2 correlations on a standard benchtop spectrometer

An experimental protocol is described that allows two-dimensional (2D) nuclear magnetic resonance (NMR) correlations of apparent diffusion coefficient D_app and effective transverse relaxation time T_2,eff to be acquired on a bench-top spectrometer using pulsed field gradients (PFG) in such a manner as to emulate D_app − T_2,eff correlations acquired using a well-logging tool with a fixed field gradient (FFG). This technique allows laboratory-scale NMR measurements of liquid-saturated cored rock to be compared directly to logging data obtained from the well by virtue of providing a comparable acquisition protocol and data format, and hence consistent data processing. This direct comparison supports the interpretation of the well-logging data, including a quantitative determination of the oil/brine saturation. The D − T₂ pulse sequence described here uses two spin echoes (2SE) with a variable echo time to encode for diffusion. The diffusion and relaxation contributions to the signal decay are then deconvolved using a 2D numerical inversion. This measurement allows shorter relaxation time components to be probed than in conventional diffusion measurements. A brief discussion of the numerical inversion algorithms available for inverting these non-rectangular data is included. The PFG-2SE sequence described is well suited to laboratory-scale studies of porous media and short T₂ samples in general.     

Synthesis of dipotassium dimethylsilanediolate monohydrate

Dipotassium dimethylsilanediolate monohydrate has been synthesised for the first time. The compound has been extensively characterised. The utilization of this new compound as an initiator or monomer in the interfacial polymerisation of silicones is discussed.     

Characterisation of commercial Perna canaliculus samples and development of extemporaneous oral veterinary paste formulations containing Perna

Perna canaliculus is a nutritional supplement recently studied and highly recommended for its anti-inflammatory effects in both animals and humans. In this study, the physicochemical properties, the microbiological quality, the total lipid content and fatty acids composition of three commercial samples of Perna powder were determined. Subsequently, three simple formulations of extemporaneous oral pastes containing Perna were prepared and designed for veterinary use. Their microbiological stability was assessed after 1-month storage at either room temperature or 35 °C. The results demonstrated that commercial Perna samples lack homogeneity, in regard to some technological properties and fatty acid composition; therefore, a preliminary characterisation of commercial Perna samples is recommended to assure the quality of formulations containing this nutritional supplement. Oral paste formulations are easy and simple to prepare and show good physical and microbiological stability, suggesting their large-scale production.     

Effect of complexing agent (1,10-phenanthroline) on ADP and KDP crystals

1,10-Phenanthroline (Phen) as a new additive was added into the solutions of KH₂PO₄ (KDP) and NH₄H₂PO₄ (ADP) in a small amount (∼2.5·10⁻³ M L⁻¹). The crystals were grown from the aqueous solutions of pH ∼4.5 at constant temperature by solvent evaporation technique. It leads to an increase in metastable zone width and assists the bulk growth process. The growth rate of crystals in the presence of Phen decreases considerably with an increase in impurity concentration (∼2.5·10⁻² M L⁻¹). Not much variation is observed in FTIR and XRD of pure and doped ADP/KDP. It appears that the growth promoting effect (GPE) of Phen is caused by the adsorption of the organic additive on the prism faces of ADP/KDP crystals. Higher optical transmittance is observed in the presence of the dopant. Detailed microhardness studies of ADP crystals reveal the anisotropy in the hardness behaviour. Scanning electron microscope (SEM) photographs exhibit the effectiveness of the impurity in changing the surface morphology of ADP/KDP crystals. Contrary to expectations, Phen depresses the NLO efficiency of ADP/KDP, suggesting that the molecular alignments in the presence of Phen results in cancellation effects disturbing the non-linearity.     

Sorption and diffusion of water vapour on edible films

Two types of films consisting of sodium salt of carboxymethyl cellulose (NaCMC) and hydroxypropyl cellulose (HPC) as film forming materials and glycerin as plasticizer were prepared, characterized and their water vapour sorption properties were determined. The water sorption isotherms of the films were measured using a magnetic suspension balance. Results show that diffusion of water vapour in NaCMC based film is faster than that in HPC based films, due to the heterogeneous structure and larger pore dimensions of the NaCMC films.