Chemische Zusammensetzung und Mikrostruktur polymerabgeleiteter Gläser und Keramiken im System Si–C–O. Teil 2: Charakterisierung der Gefügeausbildung mittels hochauflösender Durchstrahlungselektronenmikroskopie und Feinbereichsbeugung

Chemical Composition and Microstructure of Polymer‐Derived Glasses and Ceramics in the Si–C–O System. Part 2: Characterization of microstructure formation by means of high‐resolution transmission electron microscopy and selected area diffraction Liquid or solid silicone resins represent the economically most interesting class of organic precursors for the pyrolytic production of glass and ceramics materials on silicon basis. As dense, dimensionally stable components can be cost‐effectively achieved by admixing reactive filler powders, chemical composition and microstructure development of the polymer‐derived residues must be exactly known during thermal decomposition. Thus, in the present work, glasses and ceramics produced by pyrolysis of the model precursor polymethylsiloxane at temperatures from 525 to 1550 °C are investigated. In part 1, by means of analytical electron microscopy, the bonding state of silicon was determined on a nanometre scale and the phase separation of the metastable Si–C–O matrix into SiO₂, C and SiC was proved. The in‐situ crystallization could be considerably accelerated by adding fine‐grained powder of inert fillers, such as Al₂O₃ or SiC, which permits effective process control. In part 2, the microstructure is characterized by high‐resolution transmission electron microscopy and selected area diffraction. Turbostratic carbon and cubic β‐SiC precipitate as crystallization products. Theses phases are embedded in an amorphous matrix. Inert fillers reduce the crystallization temperature by several hundred °C. In this case, the polymer‐derived Si–C–O material acts as a binding agent between the powder particles. Reaction layer formation does not occur. On the investigated pyrolysis conditions, no crystallization of SiO₂ was observed.     

Facile modifications of polyimide via chloromethylation: II. Synthesis and characterization of thermocurable transparent polyimide having methylene acrylate side groups

From chloromethylated polyimide, a useful starting material for modification of aromatic polyimides, a thermocurable transparent polyimide having acrylate side groups was prepared. In the presence of 1,8‐diazabicyclo[5,4,0]undec‐7‐ene, chloromethylated polyimide was esterified with acrylic acid to synthesize poly(imide methylene acrylate). The polymer was soluble in organic solvent, which makes it possible to prepare a planar film by spin coating. The polymer film became insoluble after thermal treatment at 230 °C for 30 min. Optical transparency of the film at 400 nm (for 1 µm thickness) was higher than 98 % and not affected by further heating at 230 °C for 250 min. Adhesion properties measured by the ASTM D3359‐B method ranged from 4B to 5B. Preliminary results of planarization testing showed a high degree of planarization (DOP) value (>0.53). These properties demonstrate that poly(imide methylene acrylate) could be utilized as a thermocurable transparent material in fabricating display devices such as TFT‐LCD. Copyright © 2004 Society of Chemical Industry     

新取代苯基荧光酮试剂的合成及其性质的研究Ⅱ．新型取代苯基荧光酮与金属离子显色反应的研究

研究了３，５－二溴－４－氨基苯基荧光酮、３，５－二溴－４－偶氮变色酸等８种苯基荧光酮在酸性介质中与高价金属离子Ｚｒ（Ⅳ）、Ｍｏ（Ⅵ）、Ｗ（Ⅵ）、Ａｌ（Ⅲ）、Ｇａ（Ⅲ）等的显色反应。３，５－位二溴取代的试剂的灵敏度高于未取代的灵敏度，摩尔吸光系数绝大多数在１０５Ｌ·ｍｏｌ－１·ｃｍ－１以上。     

Improvement of levitation characteristics in a magnetic bearing system using HTSC‐permanent magnet hybrid structure

Magnetic bearing using pinning force of a permanent magnet and a high‐temperature superconductor has been developed. Additional permanent magnet is introduced to increase the levitation force of the magnetic bearing. In this hybrid magnetic bearing system, levitation force is mainly given by the repulsive force of the permanent magnets, and stability for the lateral direction is given by pinning force of the superconductor. The experimental device is developed. A ring‐type superconductor and a bulk one are examined. Levitation characteristics of the hybrid magnetic bearing are measured. The bulk superconductor shows better characteristics of both levitation and lateral stability than the ring one. Levitation force of the hybrid system becomes about twice as large as that of the nonhybrid one. Although, the repulsive force of the permanent magnet decreases the lateral stability of the system, its influence becomes small by choosing an adequate position of the permanent magnets and the superconductor. © 2004 Wiley Periodicals, Inc. Electr Eng Jpn, 150(1): 71–77, 2005; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/eej.10350     

Viscoelasticity of oxidized starch/low methoxy pectin mixtures in the presence of glucose syrup

The structural properties of mixtures of pectin, oxidized starch and glucose syrup were investigated using small deformation dynamic oscillation. In the absence of added calcium, preparations of low methoxy pectin with glucose syrup formed viscous solutions, which remained crystal-free at subzero temperatures. Samples of oxidized starch and glucose syrup, on the other hand, exhibited solid-like behaviour because of the crystalline nature of the amylose-like helices. Mixtures of the two polysaccharides with the co-solute clearly showed phase inversion from liquid to solid-like behaviour with increasing amounts of starch in the formulation. The transformation was reflected in the textural properties of samples, which varied from thick solutions to firm gels. The viscoelasticity of the system was modified further by the introduction of high methoxy pectin. Preparations of high methoxy pectin and glucose syrup formed rubbery gels whose amorphous nature underwent a glass transition during cooling.     

Magnetic separations in biotechnology—a review

Magnetic separation technology has a broad range of potential applications in both small and large scale biotechnology. This review considers a selection of magnetic techniques and their possible uses.     

Facile optical resolution of amino acid esters via hydrolysis by an industrial enzyme in organic solvents

Racemic amino acid esters were optically resolved via hydrolysis in organic solvents by the catalysis of an industrial alkaline protease, “Alcalase”. The products which were composed mainly of L-amino acids were insoluble and easily separated by filtration. The activity of the enzyme and enantiomeric excess of the products were significantly dependent on the nature of solvent and the water content in the reaction media. Generally, high values of enantiomeric excess were obtained at low water contents. Many natural and unnatural amino acids were resolved by this method.     

Numerical analyses of high‐beta spherical tokamaks with varied elongation

The effect of plasma elongation on the second‐stable spherical tokamak (ST) was numerically studied using the experimentally measured pressure and current profiles of ultrahigh‐beta STs. The maximum beta of ST over 50% was obtained in the TS‐3 ST/CT experiment by applying an external toroidal field to an FRC. It was found that the marginal beta for the ballooning instability increased with the plasma elongation κ of ST. The elongated STs with κ > 2 have the magnetic shear (S)–pressure gradient (α) profiles located in the second‐stable regime for the ballooning mode and the stability margin increased with κ. The close relation between the absolute minimum‐B profile and the second stability was documented. The effect of elongation on maximum beta was observed to saturate when κ exceed 3, indicating that the optimized elongation for high‐beta STs is located around 2 < κ < 3. © 2006 Wiley Periodicals, Inc. Electr Eng Jpn, 155(4): 1–6, 2006; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/eej.20132     

Effect of pretreatments and freezing rate on the firmness of potato tissue after a freeze–thaw cycle

The texture of potato tissue after a freeze–thaw process using different freezing rates and different pretreatments was analysed, in order to select the best strategy for optimum preservation of the textural characteristics of pre‐frozen potato. Ten blanching conditions were tested and a two‐step blanching process with calcium chloride (0.07 g mL^?1) proved the most effective in protecting the tissue after a freeze–thaw process (maximum load force around 10–55% of the raw tissue, depending on potato batch, for air‐blast freezing and 20–60% for immersion freezing). Vacuum impregnation at 100 and 400 mbar, even when followed by different pre‐drying treatments to remove excess water, was very detrimental to resistance to a freeze–thaw process (maximum load force below 10% of the raw tissue for air‐blast freezing and below 20% for immersion freezing). Microstructure analysis confirmed better tissue integrity retention with ethyleneglycol immersion freezing instead of air‐freezing. Differences were found between batches with a 6‐month difference in storage time, indicating that the fresher batch was more suitable for freezing.     

Flow stress of high density polyethylene and nylon 66 at high rates of strain

Measurement of the flow stress of high density polyethylene (HDPE) and nylon 66 at strain rates of 10³ s^?1 using a split Hopkinson pressure bar technique is discussed. The flow stress at a strain of 10% has been determined for both polymers at 20°C. The intrinsic errors involved in this technique are briefly reviewed. The results indicate that the flow stress of HDPE and nylon 66 were 50MPa and 150MPa, respectively, at strain rates of about 10³s^?1.