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1.
V. Balek T. Mitsuhashi I.M. Bountseva H. Haneda Z. Malek J. Šubrt 《Journal of Sol-Gel Science and Technology》2003,26(1-3):185-189
The diffusion structural analysis (DSA) was used to characterize microstructure changes of hydrous titania gel films under in situ conditions of heating. TG and DTA were used in order to elucidate the processes controlling the formation of anatase film during heating of hydrous titania gel film. The annealing of porosity and near surface structure defects of the dehydrated titania films was indicated by DSA in the temperature range 255–700°C as the decrease of radon release rate. It was demonstrated that the annealing was enhanced on heating in oxygen in comparison with heating in argon. The DSA experimental results were compared with model curves describing the radon diffusion mobility and the annealing of radon diffusion paths. 相似文献
2.
Takayuki Yaegashi Shinya Yodoya Masahiko Nakamura Hiroki Takeshita Katsuhiko Takenaka Tomoo Shiomi 《Journal of polymer science. Part A, Polymer chemistry》2004,42(4):999-1007
Free‐radical homo‐ and copolymerization behavior of N,N‐diethyl‐2‐methylene‐3‐butenamide (DEA) was investigated. When the monomer was heated in bulk at 60 °C for 25 h without initiator, rubbery, solid gel was formed by the thermal polymerization. No such reaction was observed when the polymerization was carried out in 2 mol/L of benzene solution with with 1 mol % of azobisisobutyronitrile (AIBN) as an initiator. The polymerization rate (Rp) equation was Rp ∝ [DEA]1.1[AIBN]0.51, and the overall activation energy of polymerization was calculated 84.1 kJ/mol. The microstructure of the resulting polymer was exclusively a 1,4‐structure where both 1,4‐E and 1,4‐Z structures were included. From the product analysis of the telomerization with tert‐butylmercaptan as a telogen, the modes of monomer addition were estimated to be both 1,4‐ and 4,1‐addition. The copolymerizations of this monomer with styrene and/or chloroprene as comonomers were also carried out in benzene solution at 60 °C. In the copolymerization with styrene, the monomer reactivity ratios obtained were r1 = 5.83 and r2 = 0.05, and the Q and e values were Q = 8.4 and e = 0.33, respectively. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 999–1007, 2004 相似文献
3.
P. Kavouras Th. Kehagias K. Chrissafis Ph. Komninou Th. Karakostas 《Journal of Thermal Analysis and Calorimetry》2006,86(3):715-719
Three batch compositions of pure oxides (SiO2,
Fe2O3, PbO, Na2O)
with equivalent SiO2, Fe2O3
and PbO contents and a gradually increased Na2O content
were vitrified through heating in a high temperature electric furnace and
subsequent quenching. The resulting vitreous products were thermally treated
in order to study the devitrification behaviour, under conditions designated
from differential thermal analysis experiments. Depending on the Na2O
content, crystal phase separation gave rise to the growth of acmite and hematite
or maghemite. A uniformly phase separated glass-ceramic material, with crystallites
of similar size and population density, was produced from devitrification
of the vitreous product with the higher Na2O content. 相似文献
4.
采用光学显微镜和扫描电子显微镜等手段,对某轻型汽车40Cr后桥半轴断裂件的组织及断口特征进行了分析结果表明:半轴在调质处理时的淬火温度不够高,使其表层和心部组织中存在较多的铁素体相,造成了工件最终的硬度和疲劳强度不足,导致半轴在使用中发生扭转疲劳断裂. 相似文献
5.
用射频磁控共溅射法制备了Cu体积分数分别为 10 % ,15 % ,2 0 %和 3 0 %的Cu MgF2 复合金属陶瓷薄膜 .用x射线衍射、x射线光电子能谱和变温四引线技术对薄膜的微结构、组分及电导特性进行了测试分析 .微结构分析表明 :制备的Cu MgF2 复合薄膜由fcc Cu晶态纳米微粒镶嵌于主要为非晶态的MgF2 陶瓷基体中构成 ,Cu晶粒的平均晶粒尺寸随组分增加从 11 9nm增至 17 8nm .5 0— 3 0 0K温度范围内的电导测试结果表明 :当Cu体积分数qM 由 15 %增加到 2 0 %时 ,Cu MgF2 复合薄膜的电阻减小了 8个量级 ,得出制备的复合薄膜渗透阈qCM 应处于 15 %和 2 0 %之间 .qM 在 10 %和 15 %之间的薄膜呈介质导电状态 ,而在 2 0 %和 3 0 %之间的薄膜则呈金属导电状态 .从理论上讨论了复合薄膜中杂质电导和本征电导的激活能及其对电导的贡献 ,并讨论了Cu MgF2 复合纳米金属陶瓷薄膜的渗透阈 ,得到了和实验一致的结果 相似文献
6.
In this article a new technique was developed to fabricate scaffolds with a unique microstructure by solid–liquid separation in combination with particulate-leaching. Firstly, the effects of polymer concentration, quenching temperature on the porous morphology and the mechanical property of obtained scaffolds during solid–liquid separation have been investigated. Then, salt granules as porogen were introduced into the solid–liquid phase separation to produce the unique pore structure of the scaffold. The pore diameter of the scaffold could be controlled with the particulate size and the wall of pores possessed special microstructure, which enhanced the pore interconnectivity. The cell culture results confirmed that a good interconnectivity of the scaffold prepared by the improved solid–liquid separation was useful for nutrition transportation and cell proliferation. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
7.
G. Martínez J. Milln J. Contreras 《Journal of polymer science. Part A, Polymer chemistry》2003,41(4):508-519
A poly(vinyl chloride) (PVC) sample was chlorinated in solution in the presence of 2,2′‐azobisisobutyronitrile and by the fluid‐bed method. The aim was to evaluate the scope of the stereoselectivity of the chlorination reaction. The quantitative microstructural analysis of the residual PVC with a degree of chlorination was followed by 13C NMR spectroscopy. From the evolution of the content of isotactic (mm), heterotactic (mr), and syndiotactic (rr) triads and of mmmm, mmmr, and rmmr isotactic pentads in the unchlorinated parts of the polymer, it was unambiguously inferred that the chlorination reaction proceeds by a stereoselective mechanism in that the mr heterotactic triads are the most reactive structures followed by the isotactic triad at mmmr and rmmr pentads. This conclusion was confirmed on the basis of the Fourier transform infrared results. The results provide valuable information regarding the effect of tacticity and related local conformations in the chemical reactions of PVC. © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 508–519, 2003 相似文献
8.
Rodrigo París Jos Luis de la Fuente 《Journal of polymer science. Part A, Polymer chemistry》2006,44(18):5304-5315
Functional spontaneous gradient copolymers of allyl methacrylate (A) and butyl acrylate (B) were synthesized via atom transfer radical polymerization. The copolymerization reactions were carried out in toluene solutions at 100 °C with methyl 2‐bromopropionate as the initiator and copper bromide with N,N,N′,N″,N″‐pentamethyldiethylenetriamine as the catalyst system. Different aspects of the statistical reaction copolymerizations, such as the kinetic behavior, crosslinking density, and gel fraction, were studied. The gel data were compared with Flory's gelation theory, and the sol fractions of the synthesized copolymers were characterized by size exclusion chromatography and nuclear magnetic resonance spectroscopy. The copolymer composition, demonstrating the gradient character of the copolymers, and the microstructure were analyzed. The experimental data agreed well with data calculated with the Mayo–Lewis terminal model and Bernoullian statistics, with monomer reactivity ratios of 2.58 ± 0.37 and 0.51 ± 0.05 for A and B, respectively, an isotacticity parameter for A of 0.24, and a coisotacticity parameter of 0.33. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 5304–5315, 2006 相似文献
9.
Piotr Dobrzynski Janusz Kasperczyk 《Journal of polymer science. Part A, Polymer chemistry》2006,44(10):3184-3201
Using zirconium(IV) acetylacetonate as an initiator of lactide/trimethylene carbonate copolymerization allowed us to obtain high‐molecular‐weight copolymers with high efficiency. The reactivity ratios of the comonomers were 13.0 for lactide and 0.53 for trimethylene carbonate. Despite the large differences between the values of the reactivity ratios, copolymers with randomized chain structures were obtained. This phenomenon occurred as a result of an intensive intermolecular transesterification process proceeding along with the reaction of copolymer chain growth and modifying its final structure. Conducting the copolymerization at the relatively low temperature of about 110 °C, which minimized the influence of intermolecular transesterification, made it possible to obtain semicrystalline copolymers with multiblock structures. Increasing the temperature of copolymerization up to 180 °C was associated with strong intensification of the transesterification reactions. At this temperature, amorphous copolymers were obtained with identical compositions but highly randomized chain structures. An analysis of the chain microstructures of the obtained copolymers, determining the average length of the blocks, the intermolecular transesterification ratio, and the degree of chain randomization, was conducted by means of NMR spectroscopy. For this purpose, very specific signal assignment in the carbonyl and methylene carbon regions of the 13C NMR spectra to appropriate comonomer sequences of polymeric chains was performed. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 3184–3201, 2006 相似文献
10.
Piotr Dobrzynski Janusz Kasperczyk 《Journal of polymer science. Part A, Polymer chemistry》2006,44(1):98-114
The results of the copolymerization of glycolide with cyclic trimethylene carbonate and 2,2‐dimethyltrimethylene carbonate are described. The copolymerization was conducted in the presence of low‐toxicity zirconium(IV) acetylacetonate as an initiator. With this kind of initiator, the composition of the comonomer units in the copolymer chains was assumed to be obtained with high efficiency. Despite significant differences in the comonomer reactivity, in copolymers containing comparable amounts of glycolidyl and carbonate sequences, highly randomized chain structures were observed. This effect resulted from strong intermolecular transesterification that proceeded during the studied copolymerization and caused glycolidyl microblock randomization. The assignment of the spectral NMR lines to appropriate comonomer sequences of polymeric chains was performed in the region of methylene protons of glycolidyl units in 1H NMR spectra of the copolymers and in the carbonyl region of carbon spectra. The equations were formulated for a detailed characterization of the obtained copolymer chains, the average lengths of the blocks, and the transesterification and randomization coefficients. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 98–114, 2006 相似文献