Characterisation and analysis of micro-contaminants in industrial polymers

Analysis of very small particles can present problems. This paper describes the application of temperature programmed solid insertion probe mass spectrometry (TP-SIP-MS), scanning electron microscopy and SEM X-ray microanalysis to the identification of foreign particles present in an industrial product. The relative advantages and limitations of the techniques are discussed. It is shown that TP-SIP-MS is a powerful tool for such work and complements the use of more conventional microanalytical methods.     

Thin‐Layer Cyclic Voltammetric and Scanning Electrochemical Microscopic Study of Antioxidant Activity of Ascorbic Acid at Liquid/Liquid Interface

An electron transfer reaction between ascorbic acid (H₂A) in an aqueous solution and oxidizing agent in an organic solution immiscible with water has been studied by thin‐layer cyclic voltammetry (TLCV) for charge transfer at the interface between two immiscible electrolyte solutions (ITIES). As an antioxidant, H₂A provide electrons through the aqueous/organic interface to reduce Fc⁺ and the procedure has been proved to be a one electron process again. In this work, the first combination of TLCV and scanning electrochemical microscopy (SECM) was achieved and showed a reasonable agreement between the results from the two different approaches. Otherwise, lower concentration ratios Kr of aqueous to organic reactants was adopted, which is given as evidence to the proposed procedure of Barker.     

Cellulose Synthesized by Acetobacter Xylinum in the Presence of Acetyl Glucomannan

Acetobacter xylinum was cultured in Hestrin-Schramm medium (control medium) and Hestrin-Schramm medium containing acetyl glucomannan (mannan medium). Loose bundles of the cellulose microfibrils are formed in the mannan medium in contrast to the normal ribbons being produced in the control medium. Rapid-freeze and substitution method followed by metal-shadowing revealed the droplet-like structures around the microfibril synthesized in the mannan medium. The cellulose synthesized in the mannan medium was stained heavily by the periodic acid-thiocarbohydrazide-silver proteinate (PATAg) method, while the cellulose synthesized in the control medium was not stained. X-ray diffractometry and FT-IR spectroscopy indicated that the addition of mannan induced a change in the crystal structure from the algal-bacterial type to the cotton-ramie type. Thus the presence of acetyl glucomannan in the medium prevents the assembly of cellulose microfibrils and changes the crystal structure of cellulose.     

Structure inhomogeneities of medium-range order in fluorozirconate glasses

Images of cleaved surfaces were obtained for 53ZrF₄-20BaF₂-4LaF₃-3AlF₃-20NaF (ZBLAN) glasses and fused quartz using an NTMDT atomic force microscope. It is shown that the scatter of particle size depends on the cooling rate and is 21–48.5 Å for the cleaved surface of ZBLAN glass obtained by very fast cooling and 68–172 Å for the cleaved surface of ZBLAN after slow cooling. For cleaved fused quartz, the range is 25-18 Å.     

四苯基卟啉铜分子的扫描隧道显微镜成像

本文首次以ＬＢ技术将四苯基卟啉铜（ＣｕＴＰＰ）分子沉积到高定向热解石墨上，并用ＳＴＭ研究其表面形貌，得到了原子级分辨的ＣｕＴＰＰ分子的表面形貌图，结果表明，ＣｕＴＰＰ分子具有近似圆状平面结构，分子直径为１．０ｎｍ，与理论结果十分吻合，结合ＳＴＭ原理，讨论了有机大分子ＳＴＭ成像的条件。     

电子显微技术应用于生物纳米材料表征与测试的研究进展

该文简述了电子显微技术的发展历程,并介绍了现代电子显微镜的新功能。针对生物纳米材料理化性能与功能应用的特殊性,结合研究实例,重点阐述运用电子显微结构表征与原位分析测试技术指导构建新颖纳米结构、揭示材料与细胞/组织相互作用并发挥功能的机制。并在此基础上,展望了电子显微技术在生物纳米材料研究领域的发展方向(大尺寸图像拼接、三维重构、动态原位实时成像)。     

加氢脱氮催化剂中硫化钼结构的表征

众所周知,重油加氢脱氮(HDN)所用Mo-Ni/Al2O3催化剂需经预硫化后始有显著的活性,关于硫化的条件工业上已较成熟,但在持续反应过程中硫化催化剂的结构与活性间的关系则很复杂,如硫化钼的价态和结构、金属组分和担体间的相互作用、反应条件及原料对催化剂组分的影响,以及硫化态催化剂中MoS2结晶的形貌等都可以引起催化剂活性本质的变化.     

PEO-LiClO_4-ZSM5 composite polymer electrolyte (IV): Polarized optical microscopy study

All solid-state lithium polymer batteries may be one of the best choices for the future electrochemical power source, characterized by high energy densities, good cyclability, reliability and safety[1,2]. Owing to its potential capability to replace the t…     

Investigation of polymer-protected noble metal nanoparticles by transmission electron microscopy: control of particle morphology and shape

 Noble metal nanoparticles were prepared by the in situ reduction of the respective metal salt precursors in the presence of various protective polymers. Transmission electron microscopy (TEM) has been used to determine the particle shapes and morphologies. These are strongly influenced by the reduction methods and conditions chosen, but the choice of the protective polymer is equally important for controlling the particle morphologies and for the stabilization of the colloids. A whole spectrum of nanoparticle morphologies and shapes was obtained, ranging from nanoagglomerates which are nevertheless well-defined and well-stabilized to nanosized single crystals with triangular shape. Received: 2 February 1998 Accepted: 29 May 1998     

Chemical Liquid Phase Deposition of Thin Aluminum Oxide Films

Introduction Inorganic oxide films have attracted a lot of interest in the last several decades. Among them, silicon dioxide films are widely used in modern microelectronics, optics and mechanics. This material has been grown by various methods including thermal oxidation, chemical vapor phase deposition, plasma-enhanced chemical vapor phase deposition, and so on.1,2 Recently, Nagayama et al.3 have reported that SiO2 thin films could be produced by a new chemical method of liquid phase depos…