Thermal Characteristics of SrO-2B(2)O(3) Glasses

Transparent SrO-2B(2)O(3) (SBO) glasses were fabricated via the conventional melt-quenching technique. X-ray diffraction (XRD) and differential thermal analysis (DTA) studies carried out on the as-quenched glasses confirmed their amorphous and glassy nature, respectively. The thermal parameters were evaluated for the as-quenched glass-plates using non-isothermal DTA experiments. The average values of the activation energies for the glass transition and crystallization of these glasses were 800 +/- 10 kJ/mol and 298 +/- 10 kJ/mol respectively. The values of the kinetic parameters that were obtained by different non-isothermal techniques were in close agreement.

Thermal ignition studies on metallized fuel-oxidizer systems

The thermal ignition behaviour of various mixtures of organic fuels, magnesium and ammonium nitrate (AN) has been examined by differential thermal analysis technique. It has been observed that the thermal decomposition/ignition of organic fuel-AN mixtures is modified significantly in the presence of magnesium metal. The decomposition characteristics of the binary mixtures of AN with various metals indicate the specific action of magnesium and zinc in lowering the decomposition temperature. A possible explanation for the low temperature decomposition is given in terms of the solid state reaction causing the fusion of AN which further reacts with the metal resulting in a highly exothermic reaction.

Thermal behaviours of sulphur-selenium mixtures

The thermal behaviours of sulphur, selenium and their mixtures have been studied over the range 40–450Dagger. It has been shown that the polymerization threshold temperature of sulphur,T Ø, decreases with increasing selenium content and follows the equilibrium copolymerization model proposed by Tobolsky and Owen. The formation of octa-atomic species Se8–xSx, where 8 >x > 4, takes place only after sulphur is in the liquid state. The rate of polymerization is enhanced by the addition of increasing amounts of selenium and this is reflected in the higher polymerization peak temperatures. The X-ray powder diffractograms show that all the sulphur-selenium melts belong to the same phase as that of SeS, though the constituent atoms are randomly distributed.

Thermal decomposition of zirconyl oxalates I. Barium zirconyl oxalate

Conditions for the preparation of stoichiometric barium zirconyl oxalate heptahydrate (BZO) have been standardized. The thermal decomposition of BZO has been investigated employing TG, DTG and DTA techniques and chemical and gas analysis. The decomposition proceeds through four steps and is not affected much by the surrounding gas atmosphere. Both dehydration and oxalate decomposition take place in two steps. The formation of a transient intermediate containing both oxalate and carbonate groups is inferred. The decomposition of oxalate groups results in a carbonate of composition Ba2Zr2OsCO3, which decomposes between 600 and 800 ~ and yields barium zirconate. Chemical analysis, IR spectra and X-ray powder diffraction data support the identity of the intermediate as a separate entity.

Thermal decomposition of zirconyl oxalates I. Barium zirconyl oxalate

Conditions for the preparation of stoichiometric barium zirconyl oxalate heptahydrate (BZO) have been standardized. The thermal decomposition of BZO has been investigated employing TG, DTG and DTA techniques and chemical and gas analysis. The decomposition proceeds through four steps and is not affected much by the surrounding gas atmosphere. Both dehydration and oxalate decomposition take place in two steps. The formation of a transient intermediate containing both oxalate and carbonate groups is inferred. The decomposition of oxalate groups results in a carbonate of composition Ba2Zr2O5CO3, which decomposes between 600 and 800° and yields barium zirconate. Chemical analysis, IR spectra and X-ray powder diffraction data support the identity of the intermediate as a separate entity.Die Bedingungen für die Herstellung von stöchiometrischem Barium-zirconyl-oxalat Heptahydrat (BZO) wurden standardisiert. Die thermische Zersetzung von BZO wurde unter Einsatz der TG-, DTG- und DTA, sowie der chemischen und Gasanalyse untersucht. Die Zersetzung verläuft über vier Stufen und wird von der umgebenden Gasathmosphäre nicht besonders beeinflusst. Sowohl die Dehydratisierung als auch die Oxalatzersetzung erfolgt in zwei Stufen. Die Bildung einer intermediären Übergangsverbindung mit sowohl Oxalat- als auch Carbonatgruppen wirken hierbei mit. Die Zersetzung der Oxalatgruppen ergibt ein Carbonat der Zusammensetzung Ba2Zr2O5CO3, das zwischen 600 und 800° zersetzt wird und Bariumzirconat ergibt. Die Angaben der chemischen Analyse, der IR-Spekren und der Röntgen-Pulver-Diffraktion unterstützen die Identität der Intermediärverbindung als eine separate Einheit.On a standardisé les conditions de préparation de l'oxalate heptahydraté de zirconyle et de baryum (BZO) stoechiométrique. On a étudié la décomposition thermique de BZO par TG, TGD et ATD ainsi que par analyses chimiques et analyses des gaz. La décomposition a lieu en quatre étapes et n'est pas trop influencée par l'atmosphère ambiante. La déshydratation et la décomposition de l'oxalate ont lieu en deux étapes. Il se forme un composé intermédiaire de transition contenant à la fois les groupes oxalate et carbonate. La décomposition des groupes oxalate fournit un carbonate de composition Ba2Zr2O5CO3 qui se décompose entre 600 et 800° pour fournir du zirconate de baryum. L'analyse chimique, les spectres IR et la diffraction des rayons X sur poudre, apportent les preuves de l'existence d'un composé intermédiaire comme entité séparée.

Thermal decomposition of ethylene diamine diperchlorate

Thermal decomposition of ethylene diamine diperchlorate (EDDP) has been studied by differential-thermal analysis (DTA), thermogravimetric analysis (TGA), isothermal weight-loss measurements and mass-spectrometric analysis of the decomposition products. It has been observed that EDDP decomposes in two temperature regions. The low-temperature decomposition stops at about 35 to 40 percent weight loss below 250°C. The reason for the low-temperature cessation may be the adsorption of excess ethylene diamine on the crystal surface of EDDP. An overall activation energy of 54 kcal per mole has been calculated for the thermal decomposition of EDDP. Mass-spectrometric analysis shows that the decomposition products are mainly CO2, H2O, HCl and N2. The following stoichiometry has been proposed for the thermal decomposition of EDDP: (−CH2NH3CIO4)2→2CO2O+2HCl+N2

Thermal properties of 3BaO–3TiO2–B2O3 glasses

Transparent glasses in the system 3BaO–3TiO2–B2O3 (BTBO) were fabricated via the conventional melt-quenching technique. The as-quenched samples were confirmed to be non-crystalline by differential thermal analysis (DTA). Thermal parameters were evaluated using non-isothermal DTA experiments. The Kauzmann temperature was found to be 759 K based on heating-rate-dependent glass transition and crystallization temperatures. A theoretical relation for the temperature-dependent viscosity is proposed for these glasses and glass-ceramics.

1-D Hydrogen bonded water in Cu(II)-picolinate coordination polymer: synthesis, crystal structure, and thermogravimetric analysis

A new Cu(II)-picolinate complex was synthesized and characterized by single crystal X-ray crystallography. The complex crystallizes in the centrosymmetric triclinic space group P (1) over bar (no. 2). Picolinate in the complex extends the neutral unit into a 1-D chain through mu(2)-bridging carboxylate. The complex has a hydrogen bonding acceptor in the second coordination sphere allowing lattice water to assemble neighboring chains. Water self-assembles to form a zig-zag 1-D chain. The adjacent chains are assembled by C-H center dot center dot center dot O interactions result in the formation 2-D hydrogen bonded network. The overall hydrogen bonding between water chain and Cu-picolinate network yields a 3-D hydrogen bonded coordination network. X-ray structural analysis, FTIR and thermal analysis have been used to characterize the reported compound in the solid state.

Thermal degradation kinetics of thermoresponsive poly(N-isopropylacrylamide-co-N,N-dimethylacrylamide) copolymers prepared via RAFT polymerization

Reversible addition-fragmentation chain transfer polymerization at 70 A degrees C in N,N-dimethylformamide was used to prepare poly(N-isopropylacrylamide-co-N,N-dimethylacrylamide) copolymers in various compositions to afford well-defined polymers with pre-determined molecular weight, narrow molecular weight distribution, and precise chain end structure. The copolymer compositions were determined by H-1 NMR spectroscopy. The reactivity ratios of N-isopropylacrylamide (NIPAM) and N,N-dimethylacrylamide (DMA) were calculated as r (NIPAM) = 0.838 and r (DMA) = 1.105, respectively, by the extended Kelen-Tudos method at high conversions. The lower critical solution temperature of PNIPAM can be altered by changing the DMA content in the copolymer chain. Differential scanning calorimetry and thermogravimetric analysis at different heating rates were carried out on these copolymers to understand the nature of thermal degradation and to determine its kinetics. Different kinetic models were applied to estimate various parameters like the activation energy, the order, and the frequency factor. These studies are important to understand the solid state polymer degradation of N-alkyl substituted polymers, which show great potential in the preparation of miscible polymer blends due to their ability to interact through hydrogen bonding.

A new 3D cadmium(II) coordination polymer having mu(4)-oxalato, mu-aquo and mu-chlorido bridges: crystal structure, solid state fluorescence and thermal behavior

A new 3D cadmium(II) coordination polymer, Cd(C2O4)(0.5)Cl(H2O)](n) (1) has been synthesized from a mixture of CdCl2. H2O and (NH4)(2)C2O4 in a slightly acidic pH. Its molecular structure was determined by single crystal X-ray diffraction which reveals that the new polymeric structure consists of simultaneous mu(4)-oxalato, mu-aquo, and mu-chlorido bridges between the metal centers, embedded in distorted pentagonal bipyramidal geometries. On thermal analysis compound exhibits high thermal stability up to 330 degrees C. Compound 1 also exhibits strong fluorescent emission. (c) 2013 Elsevier B.V. All rights reserved.

Structural, thermal and electrical properties of poly(methyl methacrylate)/CaCu3Ti4O12 composite sheets fabricated via melt mixing

Poly(methyl methacrylate) (PMMA) and CaCu3Ti4O12 (CCTO) composites were fabricated via melt mixing followed by hot pressing technique. These were characterized using X-ray diffraction, thermo gravimetric, thermo mechanical, differential scanning calorimetry, fourier transform infrared (FTIR) and Impedance analyser for their structural, thermal and dielectric properties. Composites were found to have better thermal stability than that of pure PMMA. However, there was no significant difference in the glass transition (T (g) ) temperature between the polymer and the composite. The appearance of additional vibrational frequencies in the range 400-600 cm(-1) in FTIR spectra indicated a possible interaction between PMMA and CCTO. The composite, with 38 vol% of CCTO (in PMMA), exhibited remarkably low dielectric loss at high frequencies and the low-frequency relaxation is attributed to the interfacial polarization/MWS effect. The origin of AC conductivity particularly in the high-frequency region was attributed to the electronic polarization.

Cross-linked Chitosan/Thermoplastic Starch Reinforced with Multiwalled Carbon Nanotubes Using Maleate Esters as Coupling Agent: Mechanical, Tribological and Thermal Characteristics

Bio-nanocomposites have been developed using cross-linked chitosan and cross-linked thermoplastic starch along with acid functionalized multiwalled carbon nanotubes (f-MWCNT). The nanocomposites developed were characterized for mechanical, wear, and thermal properties. The results revealed that the nanocomposites exhibited enhanced mechanical properties. The composites containing 3% f-MWCNT showed maximum compression strength. Tribological studies revealed that, with the addition of small amount of f-MWCNTs the slide wear loss reduced up to 25%. SEM analysis of the nanocomposites showed predominantly brittle fractured surface. Thermal analysis showed that the incorporation of f-MWCNTs has improved the thermal stability for the nanocomposites.

Mesostructured lamellar chromium oxide

Mesostructured lamellar chromium oxide with an interlayer separation of 29 Angstrom has been prepared by employing a cationic surfactant. The introduction of phosphate groups in the oxide increases the interlayer separation to 32 Angstrom.

Synthesis of nanoparticles of the giant dielectric material, CaCu3Ti4O12 from a precursor route

A complex oxalate precursor, CaCu3(TiO)(4)(C2O4)(8)center dot 9H(2)O, (CCT-OX), was synthesized and the precipitate that obtained was confirmed to be monophasic by the wet chemical analyses, X-ray diffraction, FTIR absorption and TG/DTA analyses. The thermal decomposition of this oxalate precursor led to the formation of phase-pure calcium copper titanate, CaCu3Ti4O12, (CCTO) at a parts per thousand yen680A degrees C. The bright-field TEM micrographs revealed that the size of the as synthesized crystallites to be in the 30-80 nm range. The powders so obtained had excellent sinterability resulting in high density ceramics which exhibited giant dielectric constants upto 40000 (1 kHz) at 25A degrees C, accompanied by low dielectric losses.