Carbon nanofibers: Synthesis, characterization, and electrochemical properties

Carbon nanofibers (CNFs) have been synthesized by co-catalyst deoxidization process by a reaction between C₂H₅OC₂H₅, Zn and Fe powder at 650 °C for 10 h. These nanofibers exhibit diameters of ∼80 nm and lengths ranging from several micrometers to tens of micrometers. X-ray diffraction, Raman spectroscopy, and high-resolution transmission electron microscopy indicate that as-prepared CNFs possess low graphitic crystallinity. The resultant CNFs as electrode shows capacity of ∼220 mAh/g and high reversibility with little hysteresis in the insertion/deintercalation reactions of lithium-ion. In addition, the possible growth of CNFs is discussed.     

Thermal degradation behaviors of polypropylene with novel silicon‐containing intumescent flame retardant

The N‐[3‐(dimethoxy‐methyl‐silanyl)‐propyl]‐N′‐ (9‐methyl‐3,9‐dioxo‐2,4,8,10‐tetraoxa‐3,9‐diphospha‐spiro[5.5]undec‐3‐yl)‐ethane‐1,2‐diamine/dimethoxy dimethyl silane copolymer (PSiN II), which simultaneously contains silicon, phosphorus, and nitrogen, is synthesized and incorporated into polypropylene (PP). The flame retardancy is evaluated by the limiting oxygen index value, which is enhanced to 29.5 from 17.4 with 20% total loading of PSiN II. The thermal degradation behavior of PP/PSiN II is investigated by thermogravimetric analysis under N₂ and air. The PP/PSiN II sample degrades at 400°C for different amounts of time, and the process of degradation is studied by Fourier transform IR. The morphology of the char formed at 400°C for 10 min is investigated by scanning electron microscopy. The swollen inner structure, close, and smooth outer surface provide a much better barrier for the transfer of heat and mass during fire and good flame retardancy. The thermal stability of PP is improved by incorporation of PSiN II. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 2487–2492, 2005     

Structural features of inclusion complexes of γ-cyclodextrin with various polymers

The crystalline structures of inclusion complexes of γ-cyclodextrin (γ-CD) with poly(ethylene glycol), poly(ethylene adipate), poly(propylene glycol) and poly(isobutylene) were studied by electron microscopy, in combination with X-ray diffraction works and measurements of thermal properties by DSC and TGA. The crystalline structure of as-prepared complexes was tetragonal and its cell dimensions were a = b = 2.380 nm and c = 1.48 nm. When an as-prepared sample was dried in a vacuum at room temperature, the tetragonal modification was transformed into the monoclinic one with the projected cell dimensions of a = 1.75, b = 1.36 nm and γ = 110°. The transformation occurred by progressive ‘shifting’ of rows of polymer necklaces in the [110] direction along the (110) plane in an original tetragonal lamellar crystal. Complexes lost weight by 10-15% in the process of heating up to 140 °C. The tetragonal crystalline modification was transformed into the hexagonal one, and concurrently, the X-ray diffraction profiles of annealed complexes were broadened. When a sample was dried in a vacuum at room temperature or annealed at high temperatures, followed by exposure to water vapor, the original tetragonal crystalline structure was recovered, restoring the original degree of orientation of crystallites in the sample. When water molecules were removed, the lateral stacking order of γ-CD-polymer complexes was destroyed, but the basic necklace structure in which polymer chains threaded through the cavity of γ-CD rings' structure could be retained.     

Microstructure and morphology of amine-cured epoxy coatings before and after outdoor exposures—An AFM study

Atomic force microscopy (AFM) has been used to study the morphology and microstructure of an amine-cured epoxy before and after outdoor exposure. Measurements were made from samples prepared in an essentially CO₂-free, H₂O-free glove box and from samples prepared in ambient conditions. For those prepared in a CO₂-free glove box, AFM imaging was conducted on (1) an unexposed air/coating surface, (2) an unexposed coating bulk, (3) an unexposed coating/substrate interface, and (4) a field exposed air/coating surface. For samples prepared in ambient conditions, only the unexposed air/coating surface was investigated. The same regions of the exposed samples were scanned periodically by the AFM to monitor changes in the surface morphology of the coating as UV exposure progressed. Small angle neutron scattering and Fourier transform infrared spectroscopy (FTIR) studies were performed to verify the microstructure and to follow chemical changes during outdoor exposure, respectively. The results have shown that amine blushing, which occurs only under ambient conditions, had a significant effect on the surface morphology and microstructure of the epoxy. The surface morphology of the samples prepared under CO₂-free, dry conditions was generally smooth and homogeneous. However, the interface and the bulk samples clearly revealed a two-phase structure consisting of bright nodular domains and dark interstitial regions, indicating an inhomogeneous microstructure. Such heterogeneous structure of the bulk was in good agreement with results obtained by small angle neutron scattering of unexposed samples and by AFM phase imaging of the degraded sample surface. The relationship between submicrometer physical changes and molecular chemical degradation is discussed. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004, in Chicago, IL.     

Direct Observation of Internal Structure in Spray-Dried Alumina Granules

The internal structure of spray-dried alumina granules was characterized by optical microscopy by immersing them in a liquid having a refractive index close to that of alumina. This method provides a unique technique for the detailed analysis of the internal structure of spray-dried granules.     

流行性出血热病毒在地鼠肾细胞中增殖动态的形态学及形态发生学研究

用普通电镜及免疫电镜对流行性出血热病毒(EHFV)不同毒株感染地鼠肾细胞(GHKC)的形态及形态发生学特点、其特征性包含体的形态及感染细胞超微结构的改变,以及感染后不同天数的病毒增殖动态进行了观察。     

Use of laser scanning confocal microscopy for characterizing changes in film thickness and local surface morphology of UV-exposed polymer coatings

Laser scanning confocal microscopy (LSCM) has been used to characterize the changes in film thickness and local surface morphology of polymer coatings during the UV degradation process. With the noninvasive feature of LSCM, one can obtain thickness information directly and nondestructively at various exposure times without destroying the specimens or deriving the thickness values from IR measurement by assuming uniform film ablation. Two acrylic polymer coatings were chosen for the study, and the physical and chemical changes of the two systems at various exposure times were measured and analyzed. Those measurable physical changes caused by UV exposure include film ablation, formation of pits and other surface defects, and increases in surface roughness. It was found in both coatings that changes in measured film thickness by LSCM were not correlated linearly to the predicted thickness loss using the changes in the CH band obtained by the Fourier Transform Infrared (FTIR) spectroscopy measurements in the later degradation stages. This result suggested it was not a uniform film ablation process during the UV degradation. At later stages, where surface deformation became severe, surface roughness and profile information using LSCM were also proven to be useful for analyzing the surface degradation process Presented at the 81st Annual Meeting of the Federation of Societies for Coatings Technology, November 13–14, 2004 in Philadelphia, PA.     

Synthesis of polymer materials for use as cell culture substrates

Up to today, several techniques have been used to maintain cells in culture for studying many aspects of cell biology and physiology. More often, cell culture is dependent on proper anchorage of cells to the growth surface. Thus, poly-l-lysine, fibronectin or laminin are the most commonly used substrates. In this study, electrosynthesized biocompatible polymer films are proposed as an alternative to these standard substrates. The electrosynthesized polymers tested were polyethylenimine, polypropylenimine and polypyrrole. Then, the adhesion, proliferation and morphology of rat neuronal cell lines were investigated on these polymer substrates in an attempt to develop new and efficient polymer materials for cell culture. During their growth on the polymers, the evolution of the cell morphology was monitored using both confocal microscopy and immunohistochemistry, leading to the conclusion of a normal development. An estimation of the adhesion and proliferation rates of rat neuronal cell cultures indicated that polyethylenimine and polypropylenimine were the best substrates for culturing olfactory neuronal cells. A method to favour the differentiation of the neuronal cells was also developed since the final aim of this work is to develop a biosensor for odour detection using differentiated neuronal cells as transducers. Consequently, a biosensor was microfabricated using silicon technology. This microsystem allowed us to culture the cells on a silicon wafer and to position the cells on certain parts of the silicon wafer.     

Processing and morphology of molecularly imprinted nylon thin films

The characterization of thin, selectively imprinted films of nylon‐6 was performed. Amino acids were used as template molecules. Spin‐cast films were prepared with sizes ranging from 2 μm to 300 nm, depending on the nylon and template concentration in the casting solution. The morphological characteristics of the film surface were examined by atomic force microscopy, and the structure within the films was observed by freeze‐fracture scanning electron microscopy. The film activity was clearly coordinated with the appearance of nanometer‐sized pores both on the surface and within the film. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2919–2926, 2006     

Carbon nanotubes prepared from three-layered copolymer microspheres of acrylonitrile and methylmethacrylate

Carbon nanotubes (CNTs) were synthesized from fine three-layered copolymer microspheres using the polymer blend technique. Diameter of PMMA core/Poly(AN-co-MMA) shell-1/PMMA shell-2 microspheres, prepared by a radical soap-free emulsion polymerization of methylmethacrylate (MMA) and acrylonitrile (AN), was between 400 nm and 500 nm. Microspheres were subjected to melt-spinning at 305 °C, stabilizing in oxygen at 220 °C for 4 h, and finally carbonizing at 1000 °C for 30 min. FE-SEM study of carbonized sample revealed the presence of CNTs arrays on carbon blocks. Similar arrays were observed in a comparative CNTs sample prepared from three-layered microspheres with the pure PAN shells-1 layers. HRTEM showed that the CNTs derived from copolymer microspheres had different structure when compared to the control sample, i.e. CNTs often adhered to each other and contained the internal compartments. The insufficient PMMA shell-2 coating of copolymer microspheres is believed to be a reason for CNTs adhesion. The possible mechanisms of the carbon block formation and the adhesion of CNTs are introduced.