Control of polymerization processes of 10,12-pentacosadiynoic acid LB films

Studies have been carried out on KrF excimer laser light (EX), X-ray or electron beam (EB) induced polymerization of 10,12-pentacosadiynoic acid (PDA) Langmuir-Blodgett (LB) films in relation to molecular density or molecular arrangement of the films using X-ray diffraction analysis, infrared (IR) spectroscopy and Raman spectroscopy. The molecular arrangement or density of the PDA LB films was controlled by subphase conditions when the films were built up, such as pH, temperature of a subphase or salt concentration in the subphase. Polymerization sensitivity of the PDA LB film was affected by the arrangement or molecular density. On low density (A type) films the polymerization occurred by irradiation with EX, X-ray or EB, but on high density (B type) films the polymerization occurred only when the irradiation was carried out by high energy beams such as X-ray or EB. Decomposition of polymerized films was observed further by excessive irradiation of EX or X-ray, but not on the B type films. It was revealed by X-ray diffraction analysis that in the A type film, the PDA molecules bent to a larger extent than those in the B type film and the polymerization proceeded topochemically, that is, the thickness decreased little after EB irradiation in a helium atmosphere. On the other hand, in the B type film, the thickness decreased by about 10% as a result of EB irradiation. By IR reflection-absorption (RA) and Raman measurements, it was confirmed that conjugated diacetylenic bonds disappeared and conjugated double and new conjugated triple bonds appeared after high energy beam irradiations. These results support the supposition that 1,4-polymerization, i.e. polydiacetylene type polymerization, occurs easily in the A type film and 1,2- or 3,4-polymerization, i.e. polyacetylene type polymerization, occurs in the B type film, and that the polymerized A type film was decomposed at the polydiacetylenic bond when the irradiation continued further. It was also shown that the polyacetylene type polymer was obtained only when the B type film was irradiated with the high energy beam.     

Thermogravimetry and wide angle X-ray diffraction study on the structure of irradiated and thermally treated kodar film

The degradation behaviour of Kodar [poly(1,4-cyclohexylene dimethyl-eneterephthalate)] was investigated in air using thermogravimetry, differential thermal analysis and wide angle X-ray diffraction studies. The rates of crystallization and degradation were influenced by thermal exposure and polychromatic irradiation (Λ > 290 nm) for different time intervals. The crystallinity changes (X_c%) and activation energies (ΔE) for the systems have been determined.     

Micro-computerized tomographic observation of the spinning apparatus in Bombyx mori silkworms

Silkworms and spiders have evolved complex spinning apparatus thought to use highly controlled conditions to optimize protein folding and crystallization to provide a tough fiber. Accordingly, the structure and function of the natural spinning apparatus has been studied with great attention as an interesting piece of biological engineering with potential for mimicry in an industrial process. However it is still not well understood. Here we used Micro-Computerized Tomographic equipment (mCT) to visualize the three-dimensional structure of the spinning apparatus in Bombyx mori silkworms. Multidirectional tomograms obtained by X-ray radioscopy provided valuable information on the detailed arrangement of each muscle of the silk press. It is suggested that the duct in the silk press part plays a part as an extrusion die whose cross-sectional area can be controlled by muscles to optimize applied stresses in the partially gelled silk within its lumen.     

Characterization of supported Pd-Pt catalysts by chemical probes

The temperature programmed (palladium) hydride decomposition appeared very effective method for diagnosing the extent of alloying in Pd-Pt/SiO₂ catalysts. Introduction of Pt to Pd catalysts moves the TPHD peak gradually towards lower temperatures and the shift in hydride decomposition peak is accompanied by a decrease in the amount of released hydrogen. The catalysts prepared the direct redox method showed much better alloy homogeneity than the samples prepared by coimpregnation. The results of probing with other techniques, i.e. catalytic probing with hydrodechlorination of CCl₂F₂ and XRD, were in line with TPHD data. The catalytic probing showed the presence of synergistic effect, a clear indication of Pd-Pt mixing. XRD data of post-reaction samples showed carbon incorporation into Pd-rich phase, whereas separate Pt-rich phase did not experience any bulk carbiding.     

化学镀Ni—P镀层的X射线衍射研究

根据X射线衍射分析结果,对化学镀高P(含P>11wt％或19at％)Ni-P镀层加热时效时,镀层成分和加热温度对结构转变的影响作了研究,结果表明,高P共晶、过共晶(含P>11wt％或19at％)合金的结构转变有如下特征:(1)相同加热时效条件下,Ni-P合金的结构转变与成分有密切关系:(2)对同一成分的过共晶合金,Ni-P合金的结构转变与时效温度密切相关;(3)过共晶合金在290～360℃温度范围内时效处理,出现Ni_xP_y介稳相,X射线衍射分析认为Ni_xP_y为Ni_(12)P_5。     

双能X射线骨密度仪测定技术研究

以Ｌｕｎａｒ公司ＤＰＸ－Ｌ型双能Ｘ射线骨密度仪为例，研究引起测量误差的主要因素并提出质控措施。用自检模块、腰椎体膜评定仪器的体外测量精度好于１％。对１０位志愿者重复２次测量，体内精度对腰椎，ＭＰＤ（平均百分差）为０．４６，ＣＶ（变异系数）为０．７５；对股骨颈，ＭＰＤ为１．２６、ＣＶ为０．４７；Ｗａｒｄ’ｓ三角区ＭＰＤ为２．０１、ＣＶ为１．１４；大转子ＭＰＤ为１．６６、ＣＶ为０．７２。扫描图像由２位     

基于微机的X射线分析自动测量系统

本文介绍了一个基于微机的X射线分析自动测量系统。该系统有三个基本功能:自动获取数据、自动换样和处理谱数据。     

Synthesis and characterization of mechanical-alloyed Ti–xMg alloys

The synthesis and characterization of Ti–xMg (x=4, 9, 12, 15, 21, 24 at%) alloys using mechanical alloying was investigated. A nanometer-sized Ti–24Mg alloy was produced. During mechanical alloying, the height of the XRD peaks of the Mg in the Ti–9Mg alloy decreased, and then disappeared, whereas the Ti XRD peaks broadened, and the grain size decreased with increasing milling time. The Mg firstly dissolved in the grain boundaries of the Ti, and then diffused into the Ti grain interiors. The grain boundaries played an important role in enhancing the solid solubility of Mg in Ti. With increasing Mg content the volume fraction of grain boundaries increased, and a decrease in grain size occurred after mechanical alloying for 48 h.