High temperature controlled atmosphere experiments for catalysts in a transmission electron microscope

A new transmission electron microscopy (TEM) specimen preparation procedure for high temperature experiments using a controlled atmosphere specimen holder (HTCASH) has been developed. It is designed for studying the microstructure of catalyst specimens before and after treatments in various gases. The procedure involved (1) finding a new formula for the embedding material, (2) devising a new method of making specimen supports, and (3) developing a method for removing the embedding material after the specimen has been microtomed. These techniques were then brought together to produce the ideal specimens for the HTCASH experiments. As an extra benefit, this procedure is also suitable for preparing specimens for ultrahigh resolution imaging experiments. The application of the new procedure in HTCASH experiments is illustrated through a high temperature reduction of a Co/SiO₂-923 catalyst.     

含氯取代基的聚间苯二甲酰间苯二胺的合成与表征

以 2 ,5 -二氯对苯二甲酰氯作为第三单体 ,将其与间苯二甲酰氯、间苯二胺在N ,N -二甲基乙酰胺中进行低温溶液共缩聚反应 ,合成了含氯取代基的聚间苯二甲酰间苯二胺。研究了单体摩尔浓度、反应初始温度、叔胺添加剂种类、第三单体用量等对共聚物相对分子质量的影响 ,并用红外光谱、热重分析等方法对共聚物进行了表征。     

Poly(butylene terephthalate)–clay nanocomposites prepared by melt intercalation: morphology and thermomechanical properties

Nanocomposites based on poly(butylene terephthalate) (PBT) and an organoclay (Cloisite 30B) were prepared by melt blending using a twin‐screw extruder. Two kinds of PBTs, ie PBT‐A and PBT‐B, with different inherent viscosities (η_inh), were used for this study (η_inh of PBT‐A and PBT‐B were 0.74 and 1.48, respectively). Dispersion of the clay layers in the PBT nanocomposites was characterized by using X‐ray diffraction (XRD) and transmission electron microscopy (TEM). Tensile and dynamic mechanical properties and non‐isothermal crystallization temperatures of the nanocomposites were also examined. Nanocomposites based on the higher‐viscosity PBT (PBT‐B) showed a higher degree of exfoliation of the clay and a higher reinforcing effect when compared to the composites based on the lower‐viscosity PBT (PBT‐A). The clay nanolayers dispersed in PBT matrices lead to increases in the non‐isothermal crystallization temperatures of the PBTs, with such increases being more significant for the PBT‐B nanocomposites than for the PBT‐A nanoocomposites. Copyright © 2004 Society of Chemical Industry     

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     

Precision equipment for symmetrical bending— Part 1. The loading system

The design and performance of precision bending equipment for testing straight beams with constant rectangular section under a pure bending moment is described. Part 1 deals with the loading arrangements and Part 2 with the rig for measuring beam deflection. The methods for recording deflection of strain gauges applied on the beam have been described elsewhere.^1–4
The reactions to the deadweight gravity loads are taken via ball bearings. The total bending moment inaccuracy, i.e. the sum of estimated systematic errors and random errors, the latter expressed as the 2Ga confidence interval about the mean (2G_cim), is about ± 25 x. 10^-4%, for 23 tests with a steel beam with 15 mm × 75 mm cross sectional dimensions, loaded to 1-1.5 mm/m strain.
The measuring rig stands on the beam via hardened and polished spherical segment feet and uses a capacitive transducer system with less than 5nm resolution. Various application tasks are described. The total inaccuracy of the measured deflection, i.e. apart from bending moment inaccuracy, is about ± 35 times 10^4% for about 10 reproduced, not repeated, tests with the same steel beam. The deflection for such a beam is of the order of 2 to 4 mm.     

Generalized difference control of parallel streams temperatures

A furnace with multiple parallel passes and multiple burners is commonly seen in petroleum refineries. In order to maintain the furnace running in a safe, stable, and high-efficiency state it is necessary to control the outlet temperatures of the multiple passes to be the same. Due to the fact that the process of the oil heating in such furnace is nonlinear, multivariable, time varying, has serious coupling among passes, has frequent dynamic changes and a large time delay, traditional control methods have trouble in controlling these temperatures, and some advanced control methods, including predictive control, adaptive control, and robust control, are usually too complex for convenient use. In this paper, a control technique, called differences control technique (DsCT), is proposed to distribute the stream flowrates such that the stream temperatures are as identical as possible. The principle of the proposed technique is explained and demonstrated, and the results of its application to a real-life petroleum refinery furnace are also reported. The DsCT technique has the following advantages: it does not need complicated design procedures, the controller structure is simple, it is easy to apply, and it can be canonically applied to furnaces with different number of passes.     

改性生物质作为型煤黏结剂的研究

探讨了用NaOH改性生物质秸秆作为型煤黏结剂的可行性,考察了NaOH溶液浓度对生物质改性的影响以及生物质添加量、无机物(MgO和MgCl2)添加量对型煤机械强度、防水性能和着火温度的影响。研究结果表明,NaOH改性液的质量分数为1.0%~2.0%时,制得的生物质型煤有较高的机械强度;生物质添加量在2%~20%时,随生物质添加量的增加,机械强度增加,着火温度降低,但防水性较差;而在生物质型煤中加入适量无机黏结剂后,型煤有很高的浸水强度,表现出优越的防水性能。     

微型生化分析仪样品室温度控制系统研究

结合微型生化分析仪样品室的要求,设计了一种基于单片机的微型生化分析仪样品室温度控制系统.它以AT89S51为核心,采用单总线高精度数字温度传感器DS18B20对样品室温度采样,同时利用汇编语言编写温度设定与控制程序,采用半导体制冷的方式,实现了温度在25℃、30℃、32℃和37℃四个温度值的稳定,控制精度达±0.5℃.     

Operation of superconducting fault current limiter using vacuum interrupter driven by electromagnetic repulsion force for commutating switch

Using conventional high‐temperature superconducting wire, a model superconducting fault current limiter (SFCL) is made and tested. Solenoid coil using Bi2223 silver sheath wire is so made that inductance is as small as possible and a vacuum interrupter is connected in series to it. A conventional reactor coil is connected in parallel. When the fault current flows in this equipment, superconducting wire is quenched and current is transferred into the parallel coil because of voltage drop of superconducting wire. This large current in parallel coil actuates magnetic repulsion mechanism of vacuum interrupter. Due to opening of vacuum interrupter, the current in superconducting wire is broken. By using this equipment, current flow time in superconducting wire can be easily minimized. On the other hand, the fault current is also easily limited by large reactance of parallel coil. © 2008 Wiley Periodicals, Inc. Electr Eng Jpn, 164(1): 52–61, 2008; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/eej.20315