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.     

Influence of ethyl methacrylate content on the volume‐phase transition of temperature‐sensitive poly[(N‐isopropylacrylamide)‐co‐(ethyl methacrylate)] microgels

A novel series of temperature‐sensitive poly[(N‐isopropylacrylamide)‐co‐(ethyl methacrylate)] (p(NIPAM‐co‐EMA)) microgels was prepared by the surfactant‐free radical polymerization of N‐isopropylacrylamide (NIPAM) with ethyl methacrylate (EMA). The shape, size dispersity and volume‐phase transition behavior of the microgels were investigated by transmission electron microscopy (TEM), ultraviolet–visible (UV–Vis) spectroscopy, dynamic light scattering (DLS) and differential scanning calorimetry (DSC). The transmission electron micrographs and DLS results showed that microgels with narrow distributions were prepared. It was shown from UV–Vis, DLS and DSC measurements that the volume‐phase transition temperature (VPTT) of the p(NIPAM‐co‐EMA) microgels decreased with increasing incorporation of EMA, but the temperature‐sensitivity was impaired when more EMA was incorporated, causing the volume‐phase transition of the microgels to become more continuous. It is noteworthy that incorporation of moderate amounts of EMA could not only lower the VPTT but also enhance the temperature‐sensitivity of the microgels. The reason for this phenomenon could be attributed to changes in the complicated interactions between the various molecules. Copyright © 2004 Society of Chemical Industry     

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     

High char‐yielding poly[acrylonitrile‐co‐(itaconic acid)‐co‐(methyl acrylate)]: synthesis and properties

Polyacrylonitrile terpolymers of various compositions consisting of acrylonitrile (AN), itaconic acid (IA) and methyl acrylate (MA) were synthesized by solution polymerization in dimethylsulfoxide. Increase in concentration of either IA or MA retarded the overall polymerization rate and the polymer molecular weight. The system consisting of AN + MA and varying IA concentration was more prone to retardation in comparison with the system composed of AN + IA with variable MA concentration. The retardation factors were quantified. Minor quantities of MA boost the reactivity of IA in the terpolymer system. The terpolymer was richer in MA vis‐à‐vis the feed. The thermal characteristics of the terpolymer were examined as a function of its composition. In contrast to the copolymer of AN and IA requiring 1–1.5 mol% IA, the terpolymer required an IA content of approximately 2.5 mol% for optimum thermal stability. The polymer with 90 mol% AN, 2.5 mol% IA and 7.5 mol% MA exhibited reasonably good char‐forming characteristics and thermal stability. The overall crystallinity and crystallite size of the polymers were found to decrease on incorporation of the comonomers. The ‘aromatization index’ of the copolymer increased with the temperature of pyrolysis through re‐organization of the tetrahydropyridine ladder structure. Copyright © 2005 Society of Chemical Industry     

Ozonation of CI Reactive Black 5 using rotating packed bed and stirred tank reactor

This study investigates the ozonation of CI Reactive Black 5 (RB5) by using the rotating packed bed (RPB) and completely stirred tank reactor (CSTR) as ozone contactors. The RPB, which provides high gravitational force by adjusting the rotational speed, was employed as a novel ozone contactor. The same ozone dosage was separately introduced into either the RPB or the CSTR for the investigation, while the experimental solution was continuously circulated within the apparatus consisting of the RPB and CSTR. The decolorization and mineralization efficiencies of RB5 in the course of ozonation are compared for these two methods. Moreover, the dissolved and off‐gas ozone concentrations were simultaneously monitored for the further analysis. As a result, the ozone mass transfer rate per unit volume of the RPB was significantly higher because of its higher mass transfer coefficient and gas–liquid concentration driving force. Furthermore, ozonation kinetics was found to be independent of the gravitational magnitude of an ozone gas–liquid contactor. Therefore, the results suggest employing RPBs as ozone‐contacting devices with the advantage of volume reduction. The experimental results, which can be used for further modeling of the ozonation process in the RPB, also show the requirement of correct design for the RPB. Consequently, the present study is useful for the understanding of practical application of RPBs. 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。     

Analysis of supersaturation and nucleation in a moving solution droplet with flowing supercritical carbon dioxide

A supercritical antisolvent (SAS) process is employed for production of solid nanoparticles from atomized droplets of dilute solution in a flowing supercritical carbon dioxide (SC CO₂) stream by attaining extremely high, very rapid, and uniform supersaturation. This is facilitated by a two‐way mass transfer of CO₂ and solvent, to and from the droplet respectively, rendering rapid reduction in equilibrium solubility of the solid solute in the ternary solution. The present work analyses the degree of supersaturation and nucleation kinetics in a single droplet of cholesterol solution in acetone during its flight in a flowing SC CO₂ stream. Both temperature and composition are assumed to be uniform within the droplet, and their variations with time are calculated by balancing the heat and mass transfer fluxes to and from the droplet. The equilibrium solubility of cholesterol with CO₂ dissolution has been predicted as being directly proportional to the Partial Molar Volume Fraction (PMVF) of acetone in the binary (CO₂–acetone) system. The degree of supersaturation has been simulated up to the time required to attain almost zero cholesterol solubility in the droplet for evaluating the rate of nucleation and the size of the stable critical nuclei formed. The effects of process parameters have been analysed in the pressure range of 7.1–35.0 MPa, temperature range of 313–333 K, SC CO₂ flow rate of 0.1136–1.136 mol s^?1, the ratio of the volumetric flow rates of CO₂‐to‐solution in the range of 100–1000, and the initial mole fraction of cholesterol in acetone solution in the range of 0.0025–0.010. The results confirm an extremely high and rapid increase in degree of supersaturation, very high nucleation rates and stable critical nucleus diameter of the order of a nanometre. Copyright © 2005 Society of Chemical Industry     

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     

建(构)筑物机械拆除方法综述

介绍了几种常用的建(构)筑物机械拆除方法,对其工作原理、特点、应用条件及局限性加以分析和说明。     

窄带中频数字接收机高速信号处理技术

窄带中频数字接收机在雷达对抗侦察中得到了广泛应用，其高速信号处理技术是目前研究的重点。本文详细介绍了数字雷达告警接收机高速信号处理技术的发展现状和关键技术，最后通过对该技术的全面分析指出了值得深入研究的领域。