210 resultados para THERMAL CHARACTERIZATION


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This paper describes the chemical, thermal and thermomechanical characterization of curaua fiber. The research of the thermal and thermomechanical properties of natural fibers is of major interest, considering their increasing utilization in several applications, and the large temperature range to which the fibers are submitted.

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Pure BBN powders and with addition of 1 and 2 wt% in excess of bismuth were obtained by Pechini Method. The powders calcined at 300°C/4h were analyzed by TG/DTA to study the temperature of organic matter decomposition. A systematic study of calcination temperature and time to the formation of the BBN phase was performed and the phase formation was accompanied by XRD. The calcined powders at 800°C during 2h were analyzed by infrared spectroscopy and by BET. The powders were isostaticaly pressed and sintered at temperatures ranging from 900°C to 1000°C. The ceramics were characterized by XRD to control the crystalline phase and by SEM to analyze the microstructure.

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Synthesis, characterization, and biological activity of a new water-soluble Pd(II)-deoxyalliin (S-allyl-L-cysteine) complex are described in this article. Elemental and thermal analysis for the complex are consistent with the formula [Pd(C6H10NO2S)2]. 13C NMR, 1H NMR, and IR spectroscopy show coordination of the ligand to Pd(II) through S and N atoms in a square planar geometry. Final residue of the thermal treatment was identified as a mixture of PdO and metallic Pd. Antiproliferative assays using aqueous solutions of the complex against HeLa and TM5 tumor cells showed a pronounced activity of the complex even at low concentrations. After incubation for 24 h, the complex induced cytotoxic effect over HeLa cells when used at concentrations higher than 0.40 mmol/L. At lower concentrations, the complex was nontoxic, indicating its action is probably due to cell cycle arrest, rather than cell death. In agreement with these results, the flow cytometric analysis indicated that after incubation for 24 h at low concentrations of the complex cells are arrested in G0/G1. © 2005 NRC Canada.

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Two extracellular xylanases produced by the thermotolerant fungus Aspergillus caespitosus grown in sugar cane bagasse were purified and characterized. Estimated molecular masses were 26.3 and 27 kDa (xyl I); 7.7 and 17.7 kDa (xyl II) for gel filtration and SDS-PAGE, respectively. Optimal temperature for both xylanases was 50-55°C. Optimal pH was 6.5-7.0 for xyl I, and 5.5-6.5 for xyl II. The thermostability (T half) at 55°C was 27.3 min (xyl I) and >90 min (xyl II). Xylanase activity was inhibited by several ions. β-mercaptoethanol activated 59 and 102% xyl I and xyl II activities, respectively. These enzymes preferentially hydrolyzed birchwood xylan, and the K m and V max values were 2.5 mg/ml and 1679 U/mg protein (xyl I), and 3.9 mg/ml and 113 U/mg protein (xyl II). The action of both xylanases mainly that of xyl II, on kraft pulp reduced kappa number and increased pulp viscosity. © 2004 Elsevier Ltd. All rights reserved.

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Carbon/epoxy 8552 prepreg is a thermoplastic toughened high-performance epoxy being used in the manufacture of advanced army material. Understanding the cure behavior of a thermosetting system is essential in the development and optimization of composite fabrication processes. The cure kinetics and rheological behavior were evaluated using a differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA) and a rheometer. Values of the kinetic parameters were obtained from dynamic DSC scans using an nth order reaction model. Rheological measurements as a function of temperature and time were made for the prepreg system. The manufacturer's recommended cure cycle was evaluated and considered adequate to consolidated the studied system.

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The discovery of the spatial uniform coexistence of superconductivity and ferromagnetism in rutheno-cuprates, RuSr2GdCu2O8 (Ru-1212), has spurred an extraordinary development in the study of the competition between magnetism and superconductivity. However, several points of their preparation process and characterization that determine their superconductive behavior are still obscure. The improvement of sample preparation conditions involves some thermal treatments in inert atmosphere. The first treatment results in the immediate formation of Sr2GdRuO 6. Using the CuO composition as a precursor, we produced Ru-1212. To turn it metallic and superconductor, besides the previous treatment, a final sinterization is carried out in oxygen flow for several days. Three Ru-1212 samples were produced by varying the last sinterization time (two, four, and six days under oxygen flow). Through measurements of x-ray diffraction, scanning electron microscopy, differential thermal analysis, magnetic susceptibility and mechanical spectroscopy, it was studied the influence of the treatments under oxygen atmosphere on the structural and superconducting properties of the material.

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The extracellular tannase from Emericela nidulans was immobilized on different ionic and covalent supports. The derivatives obtained using DEAE-Sepharose and Q-Sepharose were thermally stable from 60 to 75 °C, with a half life (t50) >24 h at 80 °C at pH 5. 0. The glyoxyl-agarose and amino-glyoxyl derivatives showed a thermal stability which was lower than that observed for ionic supports. However, when the stability to pH was considered, the derivatives obtained from covalent supports were more stable than those obtained from ionic supports. DEAE-Sepharose and Q-Sepharose derivatives as well as the free enzyme were stable in 30 and 50 % (v/v) 1-propanol. The CNBr-agarose derivative catalyzed complete tannic acid hydrolysis, whereas the Q-Sepharose derivative catalyzed the transesterification reaction to produce propyl gallate (88 % recovery), which is an important antioxidant. © 2012 Springer Science+Business Media Dordrecht.

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New nanocomposites based on bacterial cellulose nanofibers (BCN) and polyurethane (PU) prepolymer were prepared and characterized by SEM, FT-IR, XRD, and TG/DTG analyses. An improvement of the interface reaction between the BCN and the PU prepolymer was obtained by a solvent exchange process. FT-IR results showed the main urethane band at 2,270 cm-1 to PU prepolymer; however, in nanocomposites new bands appear as disubstituted urea at 1,650 and 1,550 cm-1. In addition, the observed decrease in the intensity of the hydroxyl band (3,500 cm-1) suggests an interaction between BCN hydroxyls and NCO-free groups. The nanocomposites presented a non-crystalline character, significant thermal stability (up to 230 °C) and low water absorption when compared to pristine BCN. © 2013 Akadémiai Kiadó, Budapest, Hungary.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Synthesis, characterization and thermal decomposition of bivalent transition metal α-hydroxyisobutyrates, M(C4H7O 3)2·nH2O (M = Mn(II), Fe(II), Co(II), Ni(II), Cu(II), Zn(II)), as well as the thermal behaviour of α-hydroxyisobutyric acid and its sodium salt were investigated employing simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), infrared spectroscopy (FTIR), TG-DSC coupled to FTIR, elemental analysis and complexometry. All the compounds were obtained as dihydrated, except the copper one which was obtained in the anhydrous state. The thermal decomposition of the anhydrous compounds occurs in a single or two steps and the final residue up to 235 C (Mn), 300 C (Fe), 305 C (Co), 490 C (Ni), 260 C (Cu) and 430 C (Zn) is Mn2O3, Fe2O3, Co3O 4, NiO, CuO and ZnO, respectively. The results also provided information concerning the ligand's denticity and identification of the gaseous products evolved during the thermal decomposition of these compounds. Copyright © 2013 Published by Elsevier B.V. All rights reserved.

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Secondary phases such as Laves and carbides are formed during the final solidification stages of nickel based superalloy coatings deposited during the gas tungsten arc welding cold wire process. However, when aged at high temperatures, other phases can precipitate in the microstructure, like the γ″ and δ phases. This work presents a new application and evaluation of artificial intelligent techniques to classify (the background echo and backscattered) ultrasound signals in order to characterize the microstructure of a Ni-based alloy thermally aged at 650 and 950 °C for 10, 100 and 200 h. The background echo and backscattered ultrasound signals were acquired using transducers with frequencies of 4 and 5 MHz. Thus with the use of features extraction techniques, i.e.; detrended fluctuation analysis and the Hurst method, the accuracy and speed in the classification of the secondary phases from ultrasound signals could be studied. The classifiers under study were the recent optimum-path forest (OPF) and the more traditional support vector machines and Bayesian. The experimental results revealed that the OPF classifier was the fastest and most reliable. In addition, the OPF classifier revealed to be a valid and adequate tool for microstructure characterization through ultrasound signals classification due to its speed, sensitivity, accuracy and reliability. © 2013 Elsevier B.V. All rights reserved.

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Natural rubber/gold nanoparticles membranes (NR/Au) were studied by ultrasensitive detection and chemical analysis through surface-enhanced Raman scattering and surface-enhanced resonance Raman scattering in our previous work (Cabrera et al., J. Raman Spectrosc. 2012, 43, 474). This article describes the studies of thermal stability and mechanical properties of SERS-active substrate sensors. The composites were prepared using NR membranes obtained by casting the latex solution as an active support (reducing/establishing agents) for the incorporation of colloidal gold nanoparticles (AuNPs). The nanoparticles were synthesized by in situ reduction at different times. The characterization of these sensors was carried out by thermogravimetry, differential scanning calorimetry, scanning electron microscopy (SEM) microscopy, and tensile tests. It is suggested an influence of nanoparticles reduction time on the thermal degradation of NR. There is an increase in thermal stability without changing the chemical properties of the polymer. For the mechanical properties, the tensile rupture was enhanced with the increase in the amount of nanoparticles incorporated in the material. © 2013 Wiley Periodicals, Inc.

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Synthesis, structural and spectroscopic characterizations, molecular modeling and antimycobacterial assays of new silver(I) complexes with two Schiff bases - MBDA and MBDB - are reported. The complexes [Ag(MBDA) 2]NO3, or AgMBDA, and [Ag(MBDB)NO3] or AgMBDB, were obtained by the reaction of the respective ligands with silver(I) nitrate in methanol. The Schiff bases were previously obtained by mixing ethylenediamine or 1,3-diaminopropane with p-anisaldehyde. The characterizations of the complexes were based on elemental (C, H and N) and thermal (TG-DTA) analyses and 13C and 1H NMR and FT-IR spectroscopic measurements, as well as X-ray structure determination for AgMBDA. Spectroscopic data predicted by DFT calculations are in agreement with the experimental data for the AgMBDA complex. The AgMBDA complex has a monomeric structure with a molar proportion 1:2 Ag/ligand, while AgMBDB presents a 1:1 proportion. The complexes AgMBDA and AgMBDB showed to be more effective against Mycobacterium tuberculosis than antibacterial agent silver sulfadiazine - SSD. © 2013 Elsevier Ltd. All rights reserved.

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The novel coordination polymer with the formula {[Nd2(2,5-tdc)3(dmf)2(H2O)2].dmf.H2O}n (2,5-tdc2-=2,5-thiophedicarboxylate anion and dmf=dimethylformamide) has been synthesized and characterized by thermal analysis (TG/DTA), vibrational spectroscopy (FTIR) and single crystal X-ray diffraction analysis (XRD). Structure analysis reveals that Nd(III) ions show dicapped trigonal prism coordination geometry. The 2,5-tdc2- ligands connect four Nd(III) centers, adopting (κ1 - κ1) - (κ1 - κ1) - μ4 coordination mode, generating an interesting 6-connected uninodal 3D network. Photophysical properties were studied using diffuse reflectance spectroscopy (DR) and excitation/emission spectra. The photoluminescence data show the near infrared emission (NIR) with the characteristic 4F3/2→4IJ (J=9/2, 11/2 and 13/2) transitions of Nd(III) ion, indicating that 2,5-tdc2- is able to act as a sensitizer for emission in NIR region. © 2013 Elsevier B.V.

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A polymeric complex [Eu(α-tpc)3(α-Htpc) 2]n and its characterization by single crystal X-ray and thermal analysis, infrared and photoluminescence spectroscopies are described. The compound crystallizes in the monoclinic Cc space group. The asymmetric unit is formed from a europium ion bonded to one carboxyl oxygen of five different thiophene carboxylic moieties. Three of these moieties are deprotonated and bridge between neighboring europium ions giving rise to an infinite polymer along the c axis. Besides the europium characteristic emission lines, the emission spectra show unambiguously the crystal size effect on the 5D0 → 7F0 transition. The complex thermal decomposition at 220 C leads to a stable luminescent complex in which the 5D0 → 7F4 transition reveals a monomeric characteristic. The Judd-Ofelt intensity parameters to the polymeric and the monomeric compound with the same ligand and coordination number were compared. © 2013 Published by Elsevier Ltd.