Electrochemical synthesis and characterization of chloride doped polyaniline

Chloride doped polyaniline conducting polymer films have been prepared in a protic acid medium (HCl) by potentiodynamic method in an electrochemical cell and studied by cyclic voltammetry and FTIR techniques. The FTIR spectra confirmed Cl^- ion doping in the polymers. The polymerization rate was found to increase with increasing concentration of aniline monomer. But the films obtained at high monomer concentration were rough having a nonuniform flaky polyaniline distribution. Results showed that the polymerization rate did not increase beyond a critical HCl concentration. Cyclic voltammetry suggested that, the oxidation-reduction current increased with an increase in scan rate and that the undoped polyaniline films were not hygroscopic whereas chloride doped polyaniline films were found to be highly hygroscopic.     

Hybrid gas-to-particle conversion and chemical vapor deposition for the production of porous alumina films

Porous alumina films can be found in a wide variety of materials, including filters, thermal insulation components, dielectrics, biomedical and catalyst supports, coatings and adsorbents. Production methods for these films are as equally diverse as their applications. In this work, a hybrid process based upon chemical vapor deposition and gas-to-particle conversion is presented as an alternative technique for producing porous alumina films, with the main advantages of solvent-free, low substrate-temperature operation. In this process, nanoparticles were produced in the vapor phase by reaction of aluminum acetylacetonate in the presence of oxygen. Downstream of this reaction zone, these nanoparticles were collected via thermophoresis onto a cooled substrate, forming a porous film. Some deposited films were subjected to post-processing in the form of annealing in air. Fourier-transform infrared spectra and X-ray energy-dispersive spectroscopy analysis confirmed the production of alumina at processing temperatures above 973 K. X-Ray diffraction revealed that the films were amorphous. Film thickness, ranging from 30 to 250 μm, and the average deposition rate were determined from scanning electron microscopy results. From transmission electron microscopy, the average primary particle size was determined to be approximately 18 nm and the formation of nanoparticle aggregates was evident. Annealing of the films at temperatures ranging from 523 to 1173 K in the presence of air did not have an effect on particle size. The specific surface area of the powder composing the films ranged from 10 to 185 m² g⁻¹, as determined from nitrogen gas adsorption by the Brunauer–Emmett–Teller method.     

A novel fuzzy clustering algorithm for the analysis of axillary lymph node tissue sections

Recently Fourier Transform Infrared (FTIR) spectroscopic imaging has been used as a tool to detect the changes in cellular composition that may reflect the onset of a disease. This approach has been investigated as a mean of monitoring the change of the biochemical composition of cells and providing a diagnostic tool for various human cancers and other diseases. The discrimination between different types of tissue based upon spectroscopic data is often achieved using various multivariate clustering techniques. However, the number of clusters is a common unknown feature for the clustering methods, such as hierarchical cluster analysis, k-means and fuzzy c-means. In this study, we apply a FCM based clustering algorithm to obtain the best number of clusters as given by the minimum validity index value. This often results in an excessive number of clusters being created due to the complexity of this biochemical system. A novel method to automatically merge clusters was developed to try to address this problem. Three lymph node tissue sections were examined to evaluate our new method. These results showed that this approach can merge the clusters which have similar biochemistry. Consequently, the overall algorithm automatically identifies clusters that accurately match the main tissue types that are independently determined by the clinician.     

Development of nano indium tin oxide (ITO) grains by alkaline hydrolysis of In(III) and Sn(IV) salts

Indium tin oxide (ITO) nano powders of different compositions (In: Sn = 90: 10, 70: 30 and 50: 50) were prepared by heat treatment (300-450°C) of mixed hydroxides of In(III) and Sn(IV). The hydroxides were obtained by the reaction of aq. NH₃ with mixed aq. solutions of In(NO₃)₃ and SnCl₄. FTIR and TG/DTA studies revealed that powders existed as In(OH)₃H₂O—SnO₃H₂H₂O in the solid state and then they transformed to In₂O₃—SnO₂ via some metastable intermediates after 300°C. Cubic phase of In₂O₃ was identified by XRD for the oxides up to 30% of Sn. Particle size measurements of the solid dispersed in acetone and SEM study for microstructure showed that the oxides were in the nano range (55-75 nm) whereas the size range determined from Debye-Scherrer equation were 11–24 nm.     

铜互连中SiCOF/a-C∶F双层低介电常数薄膜的制备和表征(英文)

用等离子体化学气相淀积系统制备了一种新颖的SiCOF/a-C∶F双层低介电常数介质薄膜,并用红外光谱表征了该薄膜的化学结构.通过测量介质的折射率发现该薄膜长时间暴露在空气中,其光频介电常数几乎不变.然而,随退火温度的增加,其光频介电常数则会减小.基于实验结果讨论了几种可能的机理.二次离子质谱分析表明在Al/a-C∶F/Si结构中F和C很容易扩散到Al中,但在Al/SiCOF/a-C∶F/Si结构中,则没有发现C的扩散,说明SiCOF充当了C扩散的阻挡层.分析还发现在SiCOF和a-C∶F之间没有明显的界面层.     

Preparation of an anion‐exchange adsorbent by the radiation‐induced grafting of vinylbenzyltrimethylammonium chloride onto cotton cellulose and its application for protein adsorption

Poly(vinylbenzyltrimethylammonium chloride)‐graft‐cotton cellulose, an anion‐exchange matrix, was synthesized by a mutual radiation‐induced grafting technique with a ⁶⁰Co γ‐radiation source. The grafted matrix was characterized by grafting yield estimation, elemental analysis, Fourier transform infrared spectroscopy, and scanning electron microscopy. The grafting yield decreased with the increase in the dose rate. However, the grafting yield and nitrogen content of grafted samples increased almost linearly with an increase in the total irradiation dose. To evaluate the performance of the grafted anion‐exchange matrix, the protein adsorption and elution behavior were investigated in a continuous column process under various experimental conditions, with bovine serum albumin used as a model protein. The binding and elution behavior of the anion‐exchange matrix depended on different experimental parameters, such as the grafting yield, ionic strength, pH of the medium, and amount of protein loaded. From a breakthrough curve, the equilibrium binding capacity and elution percentage of the grafted anion‐exchange matrix were estimated to be 40 mg/g and 94%, respectively. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5512–5521, 2006     

Development of calibration models for quality control in the production of ethylene/propylene copolymers by FTIR spectroscopy,multivariate statistical tools,and artificial neural networks

Principal component regression (PCR), partial least squares (PLS), StepWise ordinary least squares regression (OLS), and back‐propagation artificial neural network (BP‐ANN) are applied here for the determination of the propylene concentration of a set of 83 production samples of ethylene–propylene copolymers from their infrared spectra. The set of available samples was split into (a) a training set, for models calculation; (b) a test set, for selecting the correct number of latent variables in PCR and PLS and the end point of the training phase of BP‐ANN; (c) a production set, for evaluating the predictive ability of the models. The predictive ability of the models is thus evaluated by genuine predictions. The model obtained by StepWise OLS turned out to be the best one, both in fitting and prediction. The study of the breakdown number of samples to be included in the training set showed that at least 52 experiments are necessary to build a reliable and predictive calibration model. It can be concluded that FTIR spectroscopy and OLS can be properly employed for monitoring the synthesis or the final product of ethylene–propylene copolymers, by predicting the concentration of propylene directly along the process line. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis and structural characterization of methacrylic acid/octadecyl acrylate‐graft‐poly(methylhydrosiloxane) by hydrosilylation

Methylmethacrylate (MMA) and octadecyl acrylate (OA) were grafted to poly(methylhydrosiloxane) (PMHS) by hydrosilylation, respectively, with hexachloroplatinic acid as catalyst, and the former was further hydrolyzed to prepare methacrylic acid (MAA)‐graft‐PMHS under the alkaline condition. Through orthogonal experiment, main factors affecting the graft reaction between OA and PMHS were discussed and arranged in a decreasing order according to their abilities of the effect on the hydrosilylation of OA with PMHS: catalyst dosage, reaction temperature, reaction time, material ratio, and solvent dosage. It was found that the hydrosilylation of OA with PMHS was easier to that of MMA with PMHS. Under optimal conditions, the grafting ratios of MMA with PMHS and OA with PMHS reached about 90 and 95%, respectively. FTIR and ¹H NMR spectra indicated that the hydrosilylation reactions followed the Markovnikov's rule and played a strong preference toward β‐1,2‐addition. The test of contact angle indicated that surface energy of a system was mainly dependent on the polar groups. The surface energy of OA‐graft‐PMHS (35.07 mN/m) was similar to those of PMHS (35.62 mN/m) and polyoctadecyl acrylate (36.57 mN/m), and lower than that of MAA‐graft‐PMHS (43.50 mN/m). © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Antimicrobial finishing of regular and modified polyethylene terephthalate fabrics

An effective two-stage method has been developed for imparting antimicrobial properties to regular polyethylene terephthalate (R-PET), polyethylene glycol modified polyethylene terephthalate (PEG-M-PET), R-PET/Cotton blend (R-PET/C) and PEG-M-PET/Cotton blend (PEG-M-PET/C) fabrics. The method consists of partial hydrolysis of the fabrics to create carboxylic groups in PET macromolecules followed by subsequent reaction with dimethylalkylbenzyl ammonium chloride (DMABAC) under alkaline conditions. The reaction conditions such as pH, reaction temperature and time, carboxylic content, and DMABAC concentration were studied. Characterization of the finished fabrics was carried out through scanning electron microscopy (SEM) and Fourier transform infrared spectra (FTIR). All the modified PET fabrics showed excellent antibacterial activity towards Gram-positive (Bacillus mycoides), Gram-negative (Escherichia coli), and nonfilamentous fungus (Candida albicans). The achieved antimicrobial functions on the PET fabrics are durable in repeated laundering processes. Even after laundering 10 times the fabrics could still provide more than 85% of its antimicrobial activity against B. mycoides, E. coli, and C. albicans. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008