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Nitrogen Atmosphere (nitrogen + atmosphere)
Selected AbstractsEffect of Nitrogen Atmosphere on the Densification of a 3-mol%-Yttria-Doped ZirconiaJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 6 2002Yeong-Kyeun Paek The densification behavior of a 3-mol%-Y2O3 -doped ZrO2 (3Y-ZrO2) has been investigated under N2 and O2 atmospheres. Powder compacts have been sintered at 1550° and 1400°C for various times. The density of the specimen sintered at 1550°C is higher in N2 than in O2, while the contrary result is obtained in the case of the specimen sintered at 1400°C. Such results can be explained in terms of nitrogen solubility and oxygen vacancy in a ZrO2 matrix. Because nitrogen solubility into the ZrO2 increases with an increase in heat-treatment temperature, leading to the formation of oxygen vacancy, the densification rate becomes higher. The present study thus shows evidence of nitrogen solubility into the ZrO2 and its role on the densification behavior of 3Y-ZrO2. [source] Laser plasma plume kinetic spectroscopy of the nitrogen and carbon speciesCONTRIBUTIONS TO PLASMA PHYSICS, Issue 7 2003Z. Zelinger Abstract The formation and decay of carbon and nitrogen atoms, CN radicals and C2 molecules were monitored using spatial- and time-resolved emission spectroscopy in a plasma plume formed during laser ablation of a graphite target in nitrogen atmosphere. A simple exponential model was used to explain the effect of the individual chemical reactions and plasma dynamics on the measured kinetic characteristics. The succession of emissions C , N , CN was observed in the time-resolved spectra, supporting the suggestion that the CN radical is formed mainly by the direct reaction C + N , CN or C2 + N2 , 2CN. The formation of CN radical was enhanced by the additional generation of atomic nitrogen through the RF discharge. (© 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Effect of AlN doping on the growth morphology of SiCCRYSTAL RESEARCH AND TECHNOLOGY, Issue 9 2009N. B. Singh Abstract AlN doped SiC films were deposited on on-axis Si-face 4H-SiC (0001) substrates by the physical vapor transport (PVT) method. Thick film in the range of 20 ,m range was grown and morphology was characterized. Films were grown by physical vapor deposition (PVD) in a vertical geometry in the nitrogen atmosphere. We observed that nucleation occurred in the form of discs and growth occurred in hexagonal geometry. The X-ray studies showed (001) orientation and full width of half maxima (FWHM) was less than 0.1° indicating good crystallinity. We also observed that film deposited on the carbon crucible had long needles with anisotropic growth very similar to that of pure AlN. Some of the needles grew up to sizes of 200 ,m in length and 40 to 50 ,m in width. It is clear that annealing of SiC-AlN powder or high temperature physical vapor deposition produces similar crystal structure for producing AlN-SiC solid solution. SEM studies indicated that facetted hexagons grew on the top of each other and coarsened and merged to form cm size grains on the substrate. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Thermal, phase transition and spectral studies in erythromycin pseudopolymorphs: dihydrate and acetone solvateCRYSTAL RESEARCH AND TECHNOLOGY, Issue 12 2006Zhanzhong Wang Abstract The thermal, phase transition and spectral studies of erythromycin A dihydrate and acetone solvate were performed by Differential Scanning calorimetry (DSC), Thermo Gravimetry (TG-DTA), X-Ray Powder Diffraction (XRPD) and Fourier Transform Infra-Red (FTIR) spectrum. The non-thermal kinetic analysis of erythromycin A dihydrate was carried out by DSC at different heating rates in dynamic nitrogen atmosphere. The result showed that heating rate has substantial influence on the thermal behavior of erythromycin dihydrate. The Arrhenius parameters were estimated according to the Kissinger method. Corresponding to dehydration of dihydrate, melting of dehydrated dihydrate, phase transition from dehydrated dihydrate to anhydrate, and melting of anhydrate, the calculated activation energy were 39.60, 269.85, 261.23, and 582.16 kJmol,1, the pre-exponential factors were 3.46 × 103, 8.06 × 1032, 9.23 × 1030, and 7.29 × 1063 s,1, respectively. Ozawa method was used to compare activation energy values calculated by Kissinger method. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Tartatric Acid and L -Cysteine Synergistic-Assisted Synthesis of Antimony Trisulfide Hierarchical Structures in Aqueous SolutionEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 35 2009Jun Pan Abstract Alveolate amorphous Sb2S3 microspheres about 2 ,m in diameter were hydrothermally synthesized in aqueous solution without the use of a surfactant at 180 °C by using SbCl3, L -cysteine, and tartaric acid as starting materials. After annealing at 250 °C for 3 h under a nitrogen atmosphere, polycrystalline Sb2S3 hollow spheres were obtained. The morphology, structure, and phase composition of alveolate Sb2S3 microspheres were characterized by X-ray diffraction, field-emission scanning electron microscopy, energy dispersive X-ray analysis, and X-ray photoelectron spectroscopy. It was demonstrated that tartaric acid and L -cysteine play a key role in the formation of such hierarchical structures. In addition, the possible aggregation mechanism was proposed to illustrate the formation of Sb2S3 microspheres on the basis of the experimental results and analyses.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Tuning Carbon Materials for Supercapacitors by Direct Pyrolysis of SeaweedsADVANCED FUNCTIONAL MATERIALS, Issue 7 2009Encarnación Raymundo-Piñero Abstract The sea provides a large variety of seaweeds that, because of their chemical composition, are fantastic precursors of nanotextured carbons. The carbons are obtained by the simple pyrolysis of the seaweeds under a nitrogen atmosphere between 600 and 900,°C, followed by rinsing the product in slightly acidic water. Depending on the origin of the seaweed and on the pyrolysis conditions, the synthesis may be oriented to give an oxygen-enriched carbon or to give a tuned micro/mesoporous carbon. The samples with a rich oxygenated surface functionality are excellent as supercapacitor electrodes in an aqueous medium whereas the perfectly tuned porous carbons are directly applicable for organic media. In both cases, the specific surface area of the attained carbons does not exceed 1300 m2 g,1, which results in high-density materials. As a consequence, the volumetric capacitance is very high, making these materials more interesting than activated carbons from the point of view of developing small and compact electric power sources. Such versatile carbons, obtained by a simple, ecological, and cheap process, could be well used for environment remediation such as water and air treatment. [source] Synthesis and Characterization of a Composite Zeolite,Metglas Carbon Dioxide Sensor,ADVANCED FUNCTIONAL MATERIALS, Issue 7 2005G. Giannakopoulos Abstract The synthesis of a faujasite,Metglas composite material that can be used in gas-sensing applications is presented. A continuous faujasite film was synthesized on a Metglas magnetoelastic strip using the secondary growth method. The ability of the new composite to remotely sense carbon dioxide in a nitrogen atmosphere at room temperature over a wide range of concentrations is demonstrated by monitoring the changes in the resonance frequency of the strip. The novel sensor combines the electromagnetic properties of the magnetoelastic material with the adsorption properties of the faujasite crystals. Experiments performed over a period of a few months showed that the composite sensor remained fully operational, thus indicating its long-term stability. Furthermore, the present work demonstrates that a zeolite,Metglas composite can be used as a sensor of an analyte in a mixture as long as it adsorbs selectively larger amounts of the particular analyte than other compounds present in the mixture. [source] Identification of the effective distribution function for determination of the distributed activation energy models using the maximum likelihood method: Isothermal thermogravimetric dataINTERNATIONAL JOURNAL OF CHEMICAL KINETICS, Issue 1 2009Bojan Jankovi The new procedure for identification of the effective distribution function for determination of the distributed activation energy models, which is based on use the maximum likelihood method (MLM), was established. The five different continuous probability functions (exponential, logistic, normal, gamma, and Weibull probability functions (the extended set of distributions)) were used for searching the best reactivity model for two heterogeneous processes: (a) the isothermal reduction process of nickel oxide under hydrogen atmosphere and (b) the isothermal degradation process of bisphenol-A polycarbonate (Lexan) under nitrogen atmosphere. The MLM showed that for both processes, the most suitable reactivity model represents the Weibull distribution model. It was concluded that the values of Arrhenius parameters (ln A and Ea), evaluated from the Weibull distribution model, represent the effective kinetic values for both considered processes. This procedure enables identification the suitable distribution model for considered process only from the experimental data (based on the shapes of obtained integral kinetic curves), and this fact represents the advantage of established analysis. The established mathematical procedure, which is based on the MLM, can be applied as the preliminary analysis for evaluating the distribution of activation energies for complex heterogeneous processes. © 2008 Wiley Periodicals, Inc. Int J Chem Kinet 41: 27,44, 2009 [source] Preparation and characterization of epoxidate poly(1,2-butadiene),toughened diglycidyl ether bisphenol-A epoxy compositesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2009Jie He Abstract By the oxidation of liquid poly(1,2-butadiene) (LPB) with H2O2/HCOOH, epoxidate poly(1,2-butadiene) (ELPB) was obtained as a toughening agent to prepare diglycidyl ether bisphenol-A (DGEBA) epoxy composites by using V115 polyamide(PA) as a cross-linking agent. DGEBA, ELPB, and the composites were effectively cured by PA at 100°C for 2 h followed by postcuring at 170°C for 1 h. Thermal gravimetric analysis results in air and nitrogen atmosphere showed that the thermal stability of composites could be improved by the addition of ELPB. Compared with DGEBA/PA, the composites exhibited a decrease in strength at yield but an increase in strain at break with the increase in ELPB amount. The composite with 10% ELPB exhibited both thermal stability and tenacity superior to those of DGEBA/PA and composites with 5 and 20% ELPB, respectively. The improvements in thermal and mechanical properties of composites depended on the formation of Inter Penetrating Networks (IPN) among DGEBA/PA/ELPB and their distributions in the matrix. At an appropriate ELPB amount, the IPN, mostly made of DGEBA/PA/ELPB, may be distributed more evenly in the matrix; less ELPB resulted in the formation of IPN mainly made of DGEBA/PA; excessive addition of ELPB resulted in the local aggregation of ELPB/PA and phase separations. The toughening mechanism was changed from chemically forming IPN made of DGEBA/PA/ELPB to physically reinforcing DGEBA/PA by ELPB/PA with the increase in ELPB addition. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009 [source] Optimized conditions for the grafting reaction of poly(methyl methacrylate) onto oil-palm empty fruit bunch fibersJOURNAL OF APPLIED POLYMER SCIENCE, Issue 2 2008Aznizam Abu Bakar Abstract This article describes the graft copolymerization of poly(methyl methacrylate) (PMMA) onto oil-palm empty fruit bunches (OPEFBs) with a fiber length of less than 75 ,m. The graft copolymerization was carried out under a nitrogen atmosphere by a free-radical initiation technique in an aqueous medium. Hydrogen peroxide and ferrous ions were used as a redox initiator/cocatalyst system. The PMMA homopolymer that formed during the reaction was removed from the grafted copolymers by Soxhlet extraction. Determining the effects of the reaction period, reaction temperature, and monomer concentration on the grafting percentage was the main objective, and they were investigated systematically. The optimum reaction period, reaction temperature, monomer concentration, and initiator concentration were 60 min, 50°C, 47.15 × 10,3 mol, and 3.92 × 10,3 mol, respectively. The maximum percentage of grafting achieved under these optimum conditions was 173%. The presence of PMMA functional groups on OPEFB and the enormous reduction of the hydroxyl-group absorption band in PMMA- g -OPEFB spectra provided evidence of the successful grafting reaction. The improvement of the thermal stability of PMMA- g -OPEFB also showed the optimal achievement of the grafting reaction of PMMA onto OPEFB. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] Synthesis and comparative physicochemical investigation of partly aromatic cardo copolyestersJOURNAL OF APPLIED POLYMER SCIENCE, Issue 4 2007N. B. Joshi Abstract Copolyesters were synthesized through the condensation of 0.0025 mol of 1,1,-bis(3-methyl-4-hydroxyphenyl)cyclohexane, 0.0025 mol of ethylene glycol/propylene glycol/1,4-butanediol/1,6-hexane diol, and 0.005 mol of terephthaloyl chloride with water/chloroform (4:1 v/v) as an interphase, 0.0125 mol of sodium hydroxide as an acid acceptor, and 50 mg of cetyl trimethyl ammonium bromide as an emulsifier. The reaction time and temperature were 2 h and 0°C, respectively. The yields of the copolyesters were 81,96%. The structures of the copolyesters were supported by Fourier transform infrared and 1H-NMR spectral data and were characterized with the solution viscosity and density by a floatation method (1.1011,1.2697 g/cm3). Both the intrinsic viscosity and density of the copolyesters decreased with the nature and alkyl chain length of the diol. The copolyesters possessed fairly good hydrolytic stability against water and 10% solutions of acids, alkalis, and salts at room temperature. The copolyesters possessed moderate-to-good tensile strength (11,37.5 MPa), good-to-excellent electric strength (19,45.6 kV/mm), excellent volume resistivity (3.8 × 1015 to 2.56 × 1017 , cm), and high glass-transition temperatures (148,195°C) and were thermally stable up to about 408,427°C in a nitrogen atmosphere; they followed single-step degradation kinetics involving 38,58% weight losses and 34,59% residues. The copolyesters followed 2.6,2.9-order degradation kinetics. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] Modification of guar gum through grafting of 4-vinyl pyridine using potassium peroxymonosulphate/ascorbic acid redox pairJOURNAL OF APPLIED POLYMER SCIENCE, Issue 2 2007Abhishek Srivastava Abstract In the present article, the graft copolymerization of 4-vinyl pyridine onto guar gum initiated by potassium peroxymonosulphate/ascorbic acid redox pair in an aqueous medium was studied gravimetrically under a nitrogen atmosphere. Grafting ratio, grafting efficiency, and add on increased on increasing the concentration of potassium peroxymonosulphate from 5.0 × 10,4 to 10 × 10,4 mol/L and ascorbic acid concentration from 0.4 × 10,3 to 2.0 × 10,3 mol/L. On increasing the hydrogen ion concentration from 2.5 × 10,3 to 10.0 × 10,3 mol/L, grafting ratio, efficiency, add on and conversion were increased. Maximum grafting was obtained when guar gum and monomer concentration were 1.0 g/L and 20.0 × 10,2 mol/L, respectively. An increase in temperature from 30 to 35°C increased the grafting ratio, but conversion and homopolymer decreased. The graft copolymers were characterized by IR spectroscopy and thermogravimetric analysis. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] Synthesis, characterization, and electrical properties of diazophenylene bridged Co, Ni, Cu, Ce, and Er phthalocyanine polymersJOURNAL OF APPLIED POLYMER SCIENCE, Issue 1 2007Cemil Alkan Abstract In this research, diazophenylene bridged metal-phthalocyanine (Pc) polymers were produced from diazonium salt of 1,4-diaminophenylene and presynthesized 1,8,15,22-tetraamino metal-Pcs. 1,8,15,22-Tetraamino metal-Pc complexes of Co, Ni, Cu, Ce, and Er were obtained by reducing 1,8,15,22-tetranitro metal-Pc complexes synthesized from 3-nitrophthalic anhydride, urea, metal salt, and ammonium molybdate catalyst. Complexes and polymers were characterized by Fourier transform infrared (FTIR), ultraviolet,visible (UV,vis), and X-ray powder diffraction spectroscopes. X-ray analysis of the polymers showed that there were short-range orientations in the polymers. Thermal analysis of the complexes and the polymers were done by differential scanning calorimeter (DSC) and thermal gravimetric analysis (TGA) at a heating rate of 10°C min,1 under nitrogen atmosphere. Ash analysis was performed to determine the metal content of the polymers. Viscosimetry and ebullioscopy measurements of the soluble part of the polymers were done for molecular weight analysis of the soluble part in tetrahydrofuran (THF) at 25°C. Four-probe conductivity measurements on isothermal conditions revealed that the polymer samples showed 104 fold increases in their electrical conductivities when doped with iodine. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] Radical polymerization of n -butyl methacrylate initiated by stibonium ylideJOURNAL OF APPLIED POLYMER SCIENCE, Issue 4 2007Sumita Srivastava Abstract 1,2,3,4-Tetraphenylcyclopentadiene triphenyl stibonium ylide initiated radical polymerization of n -butyl methacrylate (n -BMA) in dioxane at (60 ± 0.2)°C for 90 min under nitrogen atmosphere has been carried out. The system follows nonideal kinetics, i.e., Rp , [ylide]0.2 [n -BMA]1.8. The value of k/kt and overall energy of activation have been computed as 0.133 × 10,2 L mol,1 s,1, 33 kJ/mol, respectively. The FTIR spectrum shows a band at 1745 cm,1 due to acrylate group of n -BMA. The 1H NMR spectrum shows a peak of two magnetically equivalent protons of methylene group at 2.1 , ppm. The DSC curve shows glass transition temperature (Tg) as 41°C. The presence of six hyperfine lines in ESR spectrum indicates that the system follows free radical polymerization and the initiation is brought about by phenyl radical. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 2457,2463, 2007 [source] Effect of oxygen inhibition on composite repair strength over timeJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 2 2007Susanna Dall'Oca Abstract The study was aimed at examining whether an oxygen inhibition layer is required for bonding a repairing to a pre-existing composite, and to determine the time required for free radicals within a composite substrate to decay to the extent that the composite repair strength drops significantly. Ten slabs of Gradia Direct Anterior (GC Corp.) were divided into (1) control group: an interfacial oxygen inhibition layer was created by applying and light-curing two layers of bonding resin (D/E Resin, Bisco) to the slabs surface in atmospheric air; (2) experimental group: the absence of an interfacial oxygen inhibition layer was obtained by light-curing the second bonding resin layer in a nitrogen atmosphere. After 1 and 2 h, 1, 14, and 30 days of air storage, a composite repair was layered over the bonding resin. Microtensile bond strengths were measured and statistically analyzed. The curing atmosphere was not a significant factor for bond strength (p = 0.82), and time and curing atmosphere-time interaction were significant (p < 0.001). The 30 day-strengths were the lowest (p < 0.05). An oxygen-inhibited layer is not initially required for bonding to resin composite, and it takes more than 14 days before the bond strength between a pre-existing and a fresh composite drops. © 2006 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2006 [source] Evaluation of the Self-Heating Tendency of Vegetable Oils by Differential Scanning CalorimetryJOURNAL OF FORENSIC SCIENCES, Issue 6 2008Amélie Baylon M.S. Abstract:, The evaluation of the self-heating propensity of a vegetable (or animal) oil may be of significant importance during the investigation of a fire. Unfortunately, iodine value and gas chromatographic-mass spectrometric analysis do not lead to meaningful results in this regard. To the contrary, differential scanning calorimetry (DSC), which does not measure the chemical composition of the oil, but rather its thermodynamic behavior, produces valuable results. After a thorough literature review on the autooxidation of vegetable oils, several oils with different self-heating tendencies were analyzed using a Mettler-Toledo differential scanning calorimeter DSC 25 between 40°C and 500°C. Analyses were carried out both under air and nitrogen atmosphere to identify the phenomena due to autooxidation reactions. Using DSC, it was possible to observe the induction period of the oil (when available), the three different exothermic events, and the autoignition temperature (relatively independent of the oil type). [source] Synthesis and electroluminescent properties of polyfluorene-based conjugated polymers containing bipolar groupsJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 22 2009Sheng-Tung Huang Abstract A bipolar dibromo monomer, bis-(4-bromophenyl)[4-(3,5-diphenyl-1,2,4- triazole-4-yl)-phenyl]amine (9), containing electro-rich triphenylamine and electro-deficient 1,2,4-triazole moieties was newly synthesized and characterized. Two fluorescent fluorene-based conjugated copolymers (TPAF, TPABTF) were prepared via facile Suzuki coupling from the dibromo bipolar monomer, 4,7-dibromo-2,1,3-benzothiadiazole (BTDZ), and 9,9-dioctylfluorene. They were characterized by molecular weight determination, IR, NMR, DSC, TGA, solubility, absorption and photoluminescence spectra, and cyclic voltammetry. The polymers showed good solubility in common organic solvents such as dichloromethane, chloroform, tetrahydrofuran, and dichlorobenzene at room temperature. They had glass transition temperatures (Tg) higher than 135 °C and 5% degradation temperatures in nitrogen atmosphere were higher than 428 °C. Single layer polymer light-emitting diodes (PLED) of ITO/PEDOT:PSS/polymer/metal showed a blue emission at 444 nm and Commission Internationale de I'Eclairage (CIE) 1931 color coordinates of (0.16, 0.13) for TPAF. The device using TPABTF as emissive material showed electroluminescence at 542 nm with CIE1931 of (0.345, 0.625), low turn-on voltage of 5 V, a maximum electroluminance of 696 cd/m2, and a peak efficiency of 2.02 cd/A. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 6231,6245, 2009 [source] Optical properties of a novel fluorene-based thermally stable conjugated polymer containing pyridine and unsymmetric carbazole groupsJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 4 2009Der-Jang Liaw Abstract A new diiodo monomer containing heterocyclic pyridine and carbazole groups was synthesized via Chichibabin reaction and used in the preparation of a conjugated polymer via Suzuki coupling approach. The conjugated polymer was highly soluble in common organic solvents such as NMP, THF, dichloromethane, chloroform, toluene, xylene, and benzene at room temperature. The polymer had high glass transition temperature at 191 °C and Td10 at 434 °C in nitrogen atmosphere. The pristine polymer exhibited the UV,vis maximum absorption at 355 nm and shifted to 420 nm after protonation. The emission of the polymer in THF solution changed from the blue region with maximum peak at 400 nm to the yellow region with maximum peak at 540 nm after protonated by HCl, and the intensity of emission depended on the concentration of acid. The polymer also showed electrochromic behavior under applied voltage. The emission color of the polymer film changed from blue (435 nm) to yellow (570 nm) when 2.5 V bias voltage was applied. The polymer also exhibited write-once and read-many-times (WORM) polymer memory effect with tristable states. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 991,1002, 2009 [source] Preparation of polybenzoxazole fibers via electrospinning and postspun thermal cyclization of polyhydroxyamideJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 24 2008Steve Lien-Chung Hsu Abstract Polybenzoxazole (PBO) fibers with a submicron diameter were successfully prepared by electrospinning its precursor, polyhydroxyamide (PHA), solutions to obtain the PHA fibers first, followed by appropriate thermal treatments for cyclization reaction. BisAPAF-IC PHA with two different molecular weights (MWs) were synthesized from a low temperature polymerization of 2,2,-bis(3-amino-4-hydroxyphenyl) hexafluoropropane (BisAPAF) and isophthaloyl chloride (IC). Using dimethylacetamide (DMAc) and tetrahydrofuran (THF), solvent effects on the electrospinnability of PHA solutions were investigated. For balancing the solution properties, it was found that DMAc/THF mixture with a weight ratio of 1/9 was the best cosolvent to prepare smooth PHA fibers; uniform PHA fibers with a diameter of 325,720 nm were obtained by using 20 wt % PHA/(DMAc/THF) solutions. For a fixed PHA concentration, solutions with a lower MW of PHA yielded thinner electrospun fibers under the same electrospinning condition. After obtaining the electrospun BisAPAF-IC PHA fibers, subsequent thermal cyclization up to 350 °C produced the corresponding thermally stable BisAPAF-IC PBO fibers with a diameter of 305,645 nm. The structure of the precursor fibers and the fully cyclized fibers were characterized by FTIR. For the cyclized BisAPAF-IC PBO fibers, thermogravimetric analysis showed a 5% weight loss temperature at 523 °C in nitrogen atmosphere. The interconnected fiber structure in the BisAPAF-IC PBO fiber mats was irrelevant to the curing process, but resulted from the jet merging during the whipping process as revealed by the high speed camera images. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 8159,8169, 2008 [source] Monomer reactivity ratios of the 2-(3-mesityl-3-methylcyclobutyl)-2-hydroxyethyl methacrylate and styrene system from 1H NMRJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 11 2002Ibrahim Erol Abstract 2-(3- Mesityl-3-methylcyclobutyl)-2-hydroxyethyl methacrylate (MCHEMA) was prepared from the reaction of methacrylic acid with the oxirane compound obtained from the chlorhydrin formed in the cyclization of 1-chloro-2,3-epoxy-5-methyl-5-hexene. Copolymers of MCHEMA and styrene were prepared in 1,4-dioxane solution at 60 °C using 2,2,-azobisisobutyronitrile as the initiator. They were characterized by IR, 1H NMR, and 13C NMR spectra. Their compositions were determined by the 1H NMR technique. The monomer reactivity ratios were determined by the Fineman,Ross, Kelen, Tüdös, and Yezrielev,Brokhina,Roskin method. Thermogravimetric analysis of the copolymers was carried out under a nitrogen atmosphere. The glass-transition temperature of the copolymers as determined by differential scanning calorimetry agreed with the Flory,Fox relationship. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 1756,1763, 2002 [source] Simultaneous Synthesis and Densification of Titanium Nitride/ Titanium Diboride Composites by High Nitrogen Pressure CombustionJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 12 2002Masachika Shibuya Composites of TiN/TiB2 were synthesized by a combustion process of BN, Ti in a nitrogen atmosphere. The effect of the BN/Ti ratio and the nitrogen gas pressure on the synthesis of these composites was investigated. Dense TiN/TiB2 composites with relatively high hardness and toughness were fabricated by combustion synthesis from Ti and BN under a nitrogen pressure of 4.0 MPa. The Vickers microhardness of the products obtained from reactants with a BN/Ti mole ratio of 0.11 increased with an increase in nitrogen pressure and had a maximum value of ,25 GPa. Fracture toughness, KIC, of the products increased from 3.1 to 5.9 MPa·m1/2 as the BN/Ti ratio increased from 0.11 to 0.20. However, products formed under nitrogen pressures higher than 6.0 MPa exhibited circumferential macrocracks due to thermal shock. [source] Grain-Boundary Viscosity of Preoxidized and Nitrogen-Annealed Silicon CarbidesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 10 2001Giuseppe Pezzotti Internal friction experiments were conducted on a model SiC polycrystal prepared from preoxidized (high-purity) SiC powder. This material contained high-purity SiO2 glass at grain boundaries in addition to a free-carbon phase, which was completely removed upon powder preoxidation. Comparative tests were conducted on a SiC polycrystal, obtained from the as-received SiC powder with the addition of 2.5 vol% of high-purity SiO2. This latter SiC material was also investigated after annealing at 1900°C for 3 h in a nitrogen atmosphere. Electron microscopy observations revealed a glass-wetted interface structure in SiC polycrystals prepared from both as-received and preoxidized powders. However, the former material also showed a large fraction of interfaces coated by turbostratic graphite. Upon high-temperature annealing in nitrogen, partial glass dewetting occurred, and voids were systematically observed at multigrain junctions. The actual presence of nitrogen could only be detected in a limited number of wetted interfaces. A common feature in the internal friction behavior of the preoxidized, SiO2 -added and nitrogen-annealed SiC was a relaxation peak that resulted from grain-boundary sliding. Frequency-shift analysis revealed markedly different characteristics for this peak: both the magnitude of the intergranular glass viscosity and the activation energy for grain-boundary viscous flow were much higher in the nitrogen-annealed material. Results of torsional creep tests were consistent with these findings, with nitrogen-annealed SiC being the most creep resistant among the tested materials. [source] Nanosized Barium Titanate Powder by Mechanical ActivationJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 1 2000Junmin Xue Mechanical activation, without any additional heat treatment, is used to trigger the formation of a perovskite BaTiO3 phase in an oxide matrix that consists of BaO and TiO2 in a nitrogen atmosphere. The resulting BaTiO3 powder exhibits a well-established nanocrystalline structure, as indicated by phase analysis using X-ray diffractometry. A crystallite size of ,14 nm is calculated, based on the half-width of the BaTiO3 (110) peak, using the Scherrer equation, and an average particle size of 20,30 nm is observed using transmission electron microscopy for the activation-derived BaTiO3 powder. [source] Tribological performances of heterocyclic-containing ether and/or thioether as additives in the synthetic diesterLUBRICATION SCIENCE, Issue 3 2009Peipei Liang Abstract The load-carrying capacity, wear and friction properties of 2-octoxyl methylthio-benzothiazole (DEOY) and 2-dodecylthio methylthio-benzothiazole (DEMB) added to a synthetic lubricant (diester) were evaluated using a four-ball test machine. The results indicate that the two compounds added to the diester possess good load-carrying capacities and excellent anti-wear and friction reduction properties. The thermal stability of the two compounds under nitrogen atmosphere was investigated by thermogravimetric analysis (TGA). It was found that the compounds DEOY and DEMB possess excellent thermal stability. The surface topography of the rubbed surface was investigated with scanning electron microscopy, the elemental chemical nature of the anti-wear films generated on steel counterface were investigated with X-ray photoelectron spectroscopy. Copyright © 2009 John Wiley & Sons, Ltd. [source] Synthesis and Characterization of Poly(N -vinylimidazole- co -acrylonitrile) and Determination of Monomer Reactivity RatiosMACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 8 2004Nursel Pekel Abstract Summary: Radical-initiated solution copolymerization of N -vinylimidazole (VIM) and acrylonitrile (AN) was carried out with 2,2, -azobisisobutyronitrile (AIBN) as an initiator in benzene at 70,°C in nitrogen atmosphere. The structure and composition of synthesized copolymers for a wide range of monomer feeds were determined by FTIR, 1H and 13C NMR spectroscopy with the aid of recorded analytical absorption bands for VIM (667 cm,1, CN of imidazole ring) and AN (2,242 cm,1, CN group), as well as by using the areas of proton and carbon atom signals from corresponding functional groups of monomer units. Monomer reactivity ratios for VIM (M1)-AN (M2) pair were determined by nonlinear regression (NLR), Kelen,Tüdös (KT) and Fineman,Ross (FR) methods. They were found to be r1,=,0.24 and r2,=,0.15 for the NLR method, r1,=,0.22 and r2,=,0.094 for the KT method, and r1,=,0.24 and r2,=,0.12 for the FR method, respectively. The relatively high activity observed of VIM growing macroradical and the results of FTIR and 1H NMR structural analysis of copolymers suggest the formation of complexed linkages between monomers and growing radicals in chain propagation reactions. Similar complexation between monomer,comonomer units in the structure of formed macromolecules showed an increase in isotactic triad fractions in the copolymer. Complex formation between the imidazole ring and nitrile group in both the monomer mixture and chain growing reactions. [source] 31P Solid state NMR study of structure and chemical stability of dichlorotriphenylphosphoraneMAGNETIC RESONANCE IN CHEMISTRY, Issue 6 2009Nina C. Gonnella Abstract Solid state 31P NMR spectroscopy was used to examine, monitor and quantify the compound integrity of the chemical reagent dichlorotriphenylphosphorane. Comparison was also made with solution 31P NMR spectra which showed that this highly reactive species could be observed in dry benzene prior to conversion to the hydrolyzed product. This is the first reported solid state NMR study of the stability and reactivity of dichlorotriphenylphosphorane and the first account of its observation and comparison in the solution state. In the solid state, the ionic and covalent forms for dichlorotriphenylphosphorane were observed along with hydrolyzed products, however, the degree of hydrolysis was dependent upon the rotor packing conditions. Calculation of the relative percent composition of dichlorotriphenylphosphorane with hydrolyzed product was made for samples prepared in air versus under nitrogen atmosphere. This information was critical in adjusting the amount of reagent used in chemical development syntheses and scale up laboratories. All hydrolyzed products were identified, based upon chemical comparisons with spectra of pure materials. Copyright © 2009 John Wiley & Sons, Ltd. [source] Combined STM/STS, TEM/EELS investigation of CNx -SWNTsPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 10 2008H. Lin Abstract Nitrogen doped single-walled carbon nanotubes (CNx -SWNTs) were successfully synthesized by vaporizing a C:Ni/Y target by a CO2 continuous laser under a nitrogen atmosphere. The as-grown nanotubes were investigated by combining TEM/EELS and STM/STS techniques. According to TEM observations, the tubes are mostly single-walled and few defects are found. Local chemical characterization was performed by EELS analysis, which proves the presence of nitrogen in both individual tubes and SWNTs bundles and indicates a nitrogen concentration around 1 at.%. STM observations of CNx -SWNTs have been then undertaken and atomic resolution images were obtained. First STM analyses of these nanotubes show some defects which have never been observed in pure carbon nanotubes before. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Growth peculiarities of silicon nanoparticles in an oxide matrix prepared by magnetron sputteringPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 8 2007L. Khomenkova Abstract The process of thermal decomposition of SiOx layers prepared by magnetron sputtering is studied by photoluminescence, AFM, Auger and SIMS methods. The dependence of the depth distribution of the chemical composition on excess silicon content is obtained. It is shown that as-sputtered SiOx layers are characterized by homogeneous enough chemical composition and do not exhibit photoluminescence. High-temperature annealing in nitrogen atmosphere stimulates not only Si nanoparticle formation but also the appearance of a Si depleted region near layer-substrate interface. This last process is found to be dependent on excess Si content. The decrease of silicon content in the depth of the annealed layers is accompanied by the decrease of Si particle sizes as proved by the blue shift of the photoluminescence maximum. The mechanisms of SiOx decomposition and possible reasons for the appearance of the Si depleted region are discussed. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Exceptional anoxia resistance in larval tiger beetle, Phaeoxantha klugii (Coleoptera: Cicindelidae)PHYSIOLOGICAL ENTOMOLOGY, Issue 2 2003Matthias Zerm Abstract. The tiger beetle Phaeoxantha klugii inhabits Central Amazonian floodplains, where it survives the annual inundation period in the third-instar larval stage submerged in the soil at approximately 29 °C for up to 3.5 months. Because flooded soils quickly become anoxic, these larvae should be highly resistant to anoxia. The survival of adult and larval P. klugii was therefore tested during exposure to a pure nitrogen atmosphere in the laboratory at 29 °C. Adult beetles were not resistant (< 6 h). Survival of larvae decreased over time, maximum survival was 15 days, whereas time to 50% mortality was 5.7 days (95% confidence interval 3.8,7.9). Anoxia resistance was additionally tested in third-instar larvae submerged within sediment for 40 days before anoxia exposure in the laboratory. Anoxia resistance was greatly enhanced in these larvae, showing a survival rate of 50% after 26 days of anoxia exposure. It appears that the gradual flooding process and/or the submersion phase induced a physiological alteration, most probably a strong depression in metabolic rate, which requires some days for induction. The degree of anoxia resistance in larval P. klugii is remarkable among terrestrial arthropods worldwide, even more so considering the high ambient temperatures. The species is well-suited to serve as a model organism for studying the physiological mechanisms of anoxia and submersion resistance in terrestrial arthropods inhabiting tropical floodplains. [source] Deposition of SiO, -Like Thin Films from a Mixture of HMDSO and Oxygen by Low Pressure and DBD Discharges to Improve the Corrosion Behaviour of SteelPLASMA PROCESSES AND POLYMERS, Issue S1 2007Camille Petit-Etienne Abstract Hexamethyldisiloxane was used to deposit silicon dioxide thin films using a low frequency plasma reactor at low pressure as well as a dielectric barrier discharge (DBD) at atmospheric pressure. FT-IR, XPS, EIS, SEM and ellipsometry were used to analyse the samples. The results show that, at low pressure, the deposited films which are smooth, continuous and dense present a polymer-like structure. By carrying out the film deposition after an oxygen plasma pretreatment step, a further improvement in the protective properties is achieved, which is observed in the case of SiO, coatings with 13.56 MHz RF generators.1 At atmospheric pressure, the deposited films present an inorganic character deposited in open air and a polymer-like one deposited under a controlled nitrogen atmosphere in our DBD reactor. The latter also allows continuous films which present the best anti-corrosive properties (which have been studied for the first time for anti-corrosive properties) when they contain some carbon incorporated. [source] | |||||||||||||||||||