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571.
High‐temperature tensile cell for in situ real‐time investigation of carbon fibre carbonization and graphitization processes 下载免费PDF全文
Michael Behr James Rix Brian Landes Bryan Barton Gerry Billovits Eric Hukkanen Jasson Patton Weijun Wang Denis Keane Steven Weigand 《Journal of synchrotron radiation》2016,23(6):1379-1389
A new high‐temperature fibre tensile cell is described, developed for use at the Advanced Photon Source at Argonne National Laboratory to enable the investigation of the carbonization and graphitization processes during carbon fibre production. This cell is used to heat precursor fibre bundles to temperatures up to ~2300°C in a controlled inert atmosphere, while applying tensile stress to facilitate formation of highly oriented graphitic microstructure; evolution of the microstructure as a function of temperature and time during the carbonization and higher‐temperature graphitization processes can then be monitored by collecting real‐time wide‐angle X‐ray diffraction (WAXD) patterns. As an example, the carbonization and graphitization behaviour of an oxidized polyacrylonitrile fibre was studied up to a temperature of ~1750°C. Real‐time WAXD revealed the gradual increase in microstructure alignment with the fibre axis with increasing temperature over the temperature range 600–1100°C. Above 1100°C, no further changes in orientation were observed. The overall magnitude of change increased with increasing applied tensile stress during carbonization. As a second example, the high‐temperature graphitizability of PAN‐ and pitch‐derived commercial carbon fibres was studied. Here, the magnitude of graphitic microstructure evolution of the pitch‐derived fibre far exceeded that of the PAN‐derived fibres at temperatures up to ~2300°C, indicating its facile graphitizability. 相似文献
572.
Shaofang Sun Weijun Chen Wei Cao Fenyan Zhang Jirong Song Chengrui Tian 《Journal of Molecular Structure》2008,860(1-3):40-44
In order to locate the exact chelation site, the chelation between quercetin and Cr(III) ion is studied using the theoretical methods. Many different potential complexes, formed with natural and deprotonated quercetin chelating bare and hydrated Cr(III) ion, respectively, are studied by using Density Functional Theory method. Both total and binding energies are calculated. The results from the studies indicate that Cr(III) ion is affine in forming a complex with quercetin at the 5-hydroxy-4-keto site and that deprotonated quercetin has stronger chelating power than natural quercetin. Apart from the theoretical studies, the experiments are performed to modify the theoretical conclusions. Meanwhile, quercetin–Cr(III) complex has been synthesized, and the chelation site is analyzed using IR spectroscopy and UV/vis spectrum. The experimental results are found to have the same conclusions as those by theoretical studies. 相似文献
573.
Liu J Bu W Zhang S Chen F Xing H Pan L Zhou L Peng W Shi J 《Chemistry (Weinheim an der Bergstrasse, Germany)》2012,18(8):2335-2341
Here we report the design and controlled synthesis of monodisperse and precisely size-controllable UCNP@mSiO(2) nanocomposites smaller than 50?nm by directly coating a mesoporous silica shell (mSiO(2)) on upconversion nanocrystals NaYF(4):Tm/Yb/Gd (UCNPs), which can be used as near-infrared fluorescence and magnetic resonance imaging (MRI) agents and a platform for drug delivery as well. Some key steps such as transferring hydrophobic UCNPs to the water phase by using cetyltrimethylammonium bromide (CTAB), removal of the excess amount of CTAB, and temperature-controlled ultrasonication treatment should be adopted and carefully monitored to obtain uniform upconversion core/mesoporous silica shell nanocomposites. The excellent performance of the core-shell-structured nanocomposite in near-infrared fluorescence and magnetic resonance imaging was also demonstrated. 相似文献
574.
The first highly enantioselective decarboxylative addition of β-ketoacids to isatins mediated by a bifunctional tertiary amine-thiourea catalyst has been developed, allowing facile synthesis of biologically important 3-hydroxy oxindoles in good yields and excellent enantioselectivities. The method reported represents a valuable approach of utilizing β-ketoacids as synthetic equivalents of aryl/alkyl methyl ketone enolates. 相似文献
575.
576.
She S Xu C Yin X Tong W Gao C 《Langmuir : the ACS journal of surfaces and colloids》2012,28(11):5010-5016
The deformation and recovery behaviors of multilayer microcapsules were investigated after being forced to flow through a microchannel. The microchannel device with a constriction (5.7 μm in depth) in the middle was designed, and the multilayer microcapsules with different size and layer thickness (and thereby different mechanical strength) were used. Deformation in the microchannel was observed for all the capsules with a size larger than the constriction height, and its extent was mainly governed by the difference between capsule size and constriction height. The squeezed microcapsules could recover their original spherical shape when the deformation extent was smaller than 16%, whereas permanent physical deformation took place when the deformation extent was larger than 34%. The capsules filled with polyelectrolytes could greatly enhance their shape recovery ability due to the higher osmotic pressure in the capsule interior and could well maintain the preloaded low-molecular-weight dyes regardless of the squeezing. 相似文献
577.
A new solid‐phase extraction (SPE) pretreatment method using a home‐made polyvinylpolypyrrolidone‐florisil (PVPP‐F) column was developed for the analysis of patulin in apple and hawthorn products in China. Fifty samples (25 apple juices, 12 apple jams, and 13 hawthorn juices) were prepared using the new method and then analyzed by high performance liquid chromatography with diode array detection (HPLC‐DAD) on an Agela Venusil MP C18 reversed‐phase column (4.6 mm × 250 mm, 5 μm). The cleanup results for all samples using home‐made PVPP‐F column were compared with those obtained using a MycoSep®228 AflaPat column. The correlation coefficient R (0.9998) fulfilled the requirement of linearity for patulin in the concentration range of 2.5–250 μg/kg. The limits of detection (LODs) and quantification (LOQs) of patulin were 3.99 and 9.64 μg/kg for PVPP‐F column, and 3.56 and 8.07 μg/kg for MycoSep®228 AflaPat column, respectively. Samples were spiked with patulin at levels ranging from 25 to 250 μg/kg, and recoveries using PVPP‐F and MycoSep®228 AflaPat columns were in the range of 81.9–100.9% and 86.4–103.9%, respectively. Naturally occurring patulin was found in 2 of 25 apple juice samples (8.0%) and 1 of 13 hawthorn juice samples (7.7%) at concentrations ranging from 12.26 to 36.81 μg/kg. The positive results were further confirmed by liquid chromatography electrospray ionization mass spectrometry (LC‐ESI‐MS). 相似文献
578.
Xingfeng Li Cheng Jin Wei Liu Jian Zhou Weijun Kong Bing Dai Jiabo Wang Dan Yan Yanling Zhao Yun Luo Xiaohe Xiao 《Journal of Thermal Analysis and Calorimetry》2012,108(3):1293-1301
Using microcalorimetry, the characteristic metabolic heat flow power-time curves of S. aureus growth affected by Ursodesoxycholic acid and Hyodeoxycholic acid were measured at 37?°C. The thermal-kinetic parameters such as, growth rate constant k, the maximum power output (P m), the time corresponding to the maximum power output (t p), total heat-production Q t , half inhibitory concentration of the drugs (IC 50) were calculated from the growth curves. For both HDCA and UDCA, with the increasing of concentration, k, P m, and Q t decreased, meanwhile, k?Cc fit a linear equation, t p was prolonged correspondingly. Principle component analysis, the results indicated t p might be the main parameter in evaluating the antibacterial activity of HDCA and UDCA in microcalorimetric method. Combining with t p and IC 50, the results revealed that the differences and trends of antibacterial activity of these bile acid derivatives were: HDCA?>?UDCA. Structure-activity relationship (SAR) analysis showed that the ??-OH at C-3 and C-6 position at equal pace on the steroid nucleus enhanced the hydrophilicity of HDCA, which led to a stronger antibacterial effect than UDCA. In this study, a useful tool was provided to accurately evaluate the antibacterial effects of bile acid derivatives. The thermolysis curve recorded by microcalorimetry could provide a lot of kinetic and thermodynamic information for the study of growth process of living microbial, which could be helpful in the screening of high efficacy antibacterial agents. 相似文献
579.
Xiaoyan Xing Yanling Zhao Weijun Kong Yanwei Zhong Dan Yan Ping Zhang Yumei Han Lei Jia Cheng Jin Xiaohe Xiao 《Journal of Thermal Analysis and Calorimetry》2012,109(1):381-385
In this study, microcalorimetry combined with chemometric analysis was used to investigate the effects of angle and nail animal valuable drugs on Bacillus subtilis (B. subtilis) growth. The power?Ctime curves of the growth metabolism of B. subtilis affected by Cornu Cervi Pantotrichum, Cornu Cervi Elaphi, Cornu Saigae Tataricae, cornu caprae hircus, Cornu Bubali, Squama Manis, and Carapax Trionycis were determined using a thermal activity monitor (TAM) air isothermal microcalorimeter, ampoule mode, at 37?°C. By analyzing these curves and some quantitative parameters using principal component analysis, the effects of the seven animal drugs on B. subtilis could be quickly evaluated from the change of the two main parameters, the maximum heat-flow power P m 2 and total heat output Q t: Cornu Saigae Tataricae, cornu caprae hircus, Cornu Bubali, Squama Manis, and Carapax Trionycis inhibited the growth of B. subtilis, while Cornu Cervi Pantotrichum and Cornu Cervi Elaphi promoted the growth of B. subtilis. Further, the result of hierarchical clustering analysis showed that the drugs which promoted the growth of B. subtilis gathered in one cluster, the other drugs which inhibited the growth of B. subtilis gathered in the other cluster. All these illustrated that the internal characteristics of the seven animal drugs were different though they had similar resources and these drugs could be well clustered according the effects of them on B. subtilis growth with the help of chemometric methods. This study provided an useful idea of the combination of microcalorimetry and chemometric analysis for studying the effects of drugs on organisms. 相似文献
580.
Zhen Jiang Lingjuan Zhang Chaonan Dong Baode Ma Weijun Tang Lijin Xu Qinghua Fan Jianliang Xiao 《Tetrahedron》2012,68(24):4919-4926
A palladium-catalyzed, highly efficient Heck arylation of electron-rich N,N-diprotected allylamine derivatives with a wide range of aryl bromides under ligand-free conditions has been developed. In the presence of Pd(OAc)2 and an appropriate additive, the reaction proceeds with excellent regioselectivity and stereoselectivity, leading exclusively to the γ-arylated (E)-allylamine products in good to excellent yields. It was found that the choice of solvent, olefin, additive and temperature has an important influence on the reaction. Worthy of note is that good results were observed only when using N,N-diprotected allylamines containing carbamate moiety, and the steric properties of allylamines also have important impacts on the regiocontrol. The use of TEMPO (2,2,6,6-tetramethyl-1-piperidinyloxy) or HQ (hydroquinone) as the additive is also crucial for securing a faster reaction rate. This method provides a straightforward approach for the efficient synthesis of various γ-arylated, linear (E)-allylamines. 相似文献