Reversible addition–fragmentation chain transfer polymerization has been successfully applied to polymerize acrylonitrile with dibenzyl trithiocarbonate as the chain‐transfer agent. The key to success is ascribed to the improvement of the interchange frequency between dormant and active species through the reduction of the activation energy for the fragmentation of the intermediate. The influence of several experimental parameters, such as the molar ratio of the chain‐transfer agent to the initiator [azobis(isobutyronitrile)], the molar ratio of the monomer to the chain‐transfer agent, and the monomer concentration, on the polymerization kinetics and the molecular weight as well as the polydispersity has been investigated in detail. Matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry and 1H NMR analyses have confirmed the chain‐end functionality of the resultant polymer. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 490–498, 2006
A new method for syntheses of hyperbranched poly(ester-amide)s from commercially available A2 and CB x type monomers has been developed on the basis of a series of model reactions. The aliphatic and semiaromatic hyperbranched poly(ester-amide)s with multihydroxyl end groups are prepared by in situ thermal polycondensation of intermediates obtained from dicarboxylic acids (A2) and multihydroxyl primary amines (CB x ) in N,N-dimethylformamide. Analyses of FTIR, 1H NMR, and 13C NMR spectra revealed the structures of the polymers obtained. The MALDI-TOF MS of the polymers indicated that cyclization side reactions occurred during polymerization. The hyperbranched poly(ester-amide)s contain configurational isomers observed by 13C and DEPT 13C NMR spectroscopy. The DBs of the polymers were determined to be 0.38−0.62 by 1H NMR or quantitive 13C NMR and DEPT 135 spectra. These polymers exhibit moderate molecular weights, with broad distributions determined by size exclusion chromatography (SEC), and possess excellent solubility in a variety of solvents such as N,N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, and ethanol, and display glass-transition temperatures (T gs) between −2.3 and 53.2 °C, determined by DSC measurements. The thermogravimetric analytic measurement revealed that the decomposition temperature of the polymers at 10% weight-loss temperature (T d 10) ranged from 333 to 397 °C in nitrogen.
Chinese Space Station has planned a high-temperature material science experiment rack, equipped with an X-ray projection imaging module, to support the development of material experiments and research in space. BiFeO3 has been selected as the first batch of experimental materials for Chinese Space Station. The melting and solidification process of BiFeO3, an opaque, high-temperature material, is observed by X-ray observation module in situ. X-ray is the dominant way to observe opaque materials due to its penetrability. In-situ observation of materials is the top priority of this study, so we have strict requirements on image quality, and high-quality images can better analyze the properties and properties of materials. Limited by narrow size and high temperature conditions, the X-ray images collected have low contrast, serious noise pollution, and poor imaging quality. To enhance the contrast and improve the edge details of such images, a grayscale weighted histogram equalization combined with high-frequency enhancement (GWHE-HFE) algorithm is proposed. First, we add a mask to the input image to obtain the region of interest (ROI), and then filter out the low-frequency components of the image by Gaussian high-pass filter to preserve high-frequency details. Second, the image obtained in the previous and the X-ray image of ROI are respectively multiplied by a coefficient and added to obtain the edge-emphasized X-ray image. And then, we use grayscale weighted histogram equalization (GWHE) to process the image obtained in the second step to obtain the contrast enhanced X-ray image. The enhanced image shows the crystal grains and the thin bands where the solid and the melt intersect, and it is helpful to accurately locate the solid solution interface. Experiments on X-ray images of BiFeO3 growth demonstrate that this combined method outperforms existing ones both qualitatively and quantitatively, providing an in-depth and effective analysis method for in high-temperature material-science experiments.
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