Synthesis, characterization and thermal studies on solid compounds of 2-chlorobenzylidenepyruvate of heavier trivalent lanthanides and yttrium(III)

Solid-state compounds of general formula LnL(3)center dot nH(2)O, where Ln represents heavier lanthanides and yttrium and L is 2-chlorobenzylidenepyruvate, have been synthesized. Chemical analysis, simultaneous thermogravimetry-differential analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, elemental analysis and infrared spectroscopy have been employed to characterize and to study the thermal behaviour of these compounds in dynamic air atmosphere.On heating these compounds decompose in four (Gd, Tb, Ho to Lu, Y) or five (Eu, Dy) steps. They lose the hydration water in the first step and the thermal decomposition of the anhydrous compounds up to 1200 degrees C occurs with the formation of the respective oxide, Tb4O7 and Ln(2)O(3) (Ln=Eu, Gd, Dy to Lu and Y) as final residue. The dehydration enthalpies found for these compounds (Eu, to Lu and Y) were: 65.77, 55.63, 86.89, 121.65, 99.80, 109.59, 131.02, 119.78, 205.46 and 83.11 kJ mol(-1), respectively.

Synthesis, characterization and thermal behaviour of solid 4-methoxybenzoates of heavier trivalent lanthanides

Solid-state Ln-4-MeO-Bz compounds, where Ln stands for trivalent Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Y and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, phase transition, coordination mode, structure, thermal behaviour and thermal decomposition of the isolated compounds. The phase transition observed in the some compounds has been reported for the first time. (C) 2006 Elsevier B.V. All rights reserved.

Influence of processing conditions on the thermal decomposition of SrTiO3 precursors

The present work investigates the influence of milling and calcination atmosphere on the thermal decomposition of SrTiO3 powder precursors. Both pure and neodymium-modified SrTiO3 samples were studied. Milling did not significantly influence numerical mass loss value, but reduced the number of decomposition steps, modifying the profiles of the TG and DTA curves. on the other hand, milling increases the amount of energy liberated by the system upon combustion of organic matter. It was also observed that the milling process, associated to the calcination in an oxygen atmosphere, considerably decreases the amount of organic matter and increases the final mass loss temperature.

Preparation and thermal behavior of mixture of basic carbonate and 4-dimethylaminocinnamylidenepyruvate with lanthanides (III) and yttrium (III) in the solid state

Solid Ln-OKCO3-DMCP compounds, where Ln represents lanthanides (III) and yttrium (III) ions and DMCP is the anion 4-dimethyiaminocinnamylidenepyruvate, have been prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and elemental analysis have been used to characterize the compounds. The thermal stability as well as the thermal decomposition of these compounds were studied using an alumina crucible in an air atmosphere.

SiO2-PbF2-CdF2 glasses and glass ceramics

Lead-Cadmium fluorosilicate stable glasses were prepared and the vitreous domain region determined in the composition diagram. Characteristic temperatures were obtained from thermal analysis and the structural studies performed illustrate clearly the role played by lead atoms in the glasses crystallization behavior and the glass-forming ability of cadmium atoms. The occurrence of either a cubic lead fluoride or a lead-cadmium fluoride solid solution in crystallizing samples was found to be dependent on Er3+ doping. The optically active ions were found to concentrate in the crystalline phase and in fact play the role of nucleating agent as suggested from X-ray diffraction and EXAFS measurements. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Synthesis, characterisation and thermal behaviour of solid state compounds of 4-methylbenzylidenepyruvate with some bivalent metal ions

Solid state M-4-Me-BP compounds, where M stands for bivalent Mn, Fe, Co, Ni, Cu, Zn, Pb and 4-Me-BP is 4-methylbenzylidenepyruvate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis, and complexometry were used to characterise and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated complexes. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Development of alpha-SiAlON-SiC ceramic composites by liquid phase sintering

In this work, in situ alpha-SiAlON-SiC ceramic composites were obtained,by, liquid phase sintering, using SiC as reinforcement. Different beta-SiC powder contents (0-20 wt.%), were added to Si3N4-AlN-RE2O3. powder mixtures, and compacted by cold isostatic pressing. The samples were sintered at 1950 degrees C for 1 h, in N-2 atmosphere. Sintered: samples were characterized by relative density, weight loss, X-ray diffraction and scanning electron microscopy. Furthermore, mechanical properties such as hardness and fracture toughness were determined by Vickers indentation method. Lattice parameters of the alpha' phase did not considerably change with increase of SiC content. However, morphology, average grain size and aspect ratio of the alpha' phase were considerably changed with increase of the SiC content. These behavior influences significantly the mechanical properties of this hard ceramic composite. (C) 2006 Elsevier Ltd. All rights reserved.

Thermal studies on nickel(II) 4-iodopyrazole complexes

This work describes the synthesis, IR and UV-Vis spectroscopic characterization as well the thermal behavior of the [NiCl2(HIPz)(4)]center dot C3H6O (1), [Ni(H2O)(2)(HIPz)(4)](NO3)(2) (2), [Ni(NCS)(2)(HIPz)(4)] (3) and [Ni(N-3)(2)(HIPz)(4)] (4) (HIPz = 4-iodopyrazole) pyrazolyl complexes. TG experiments reveal that the compounds 1-4 undergo thermal decomposition in three or four mass loss steps yielding NiO as final residue, which was identified by X-ray powder diffraction.

Sol-gel Eu3+/Tm3+ doped transparent glass-ceramic waveguides

Eu3+ and Tm3+ doped lanthanum fluoride and lanthanum oxyfluoride are obtained from Eu3+, Tm3+ containing lanthanum fluoracetate solutions. The nature of the crystal phase obtained could be controlled by the temperature of heat treatment. Spectral characteristics of Eu3+ doped crystal phases were sufficiently different to allow utilization of Eu3+ as structural probes. Tm3+ emission at the technologically important spectral region of 1450nm could be observed for the fluoride and oxyfluoride crystal phases. The large bandwidth obtained (around 120nm) suggests potential applications in optical amplification. SiO2-LaF3-LaOF composite materials were also prepared. It is observed that for heat treatments above 800degreesC, fluorine loss, probably in the form of SiF4 hinder the observation of Tm3+ emission. Eu3+ spectroscopic characteristics clearly show the evolution of a fluoride like environment to an amorphous oxide one as the temperature of heat treatment increased. Thin films obtained by dip-coating on V-SiO2 substrates and treated at 300degreesC, 500degreesC and 800degreesC display guided modes in the visible and infrared regions. Optical characteristics (refractive index and films thickness) were obtained at 543.5, 632.8 and 1550nm. Attenuation as low as 1.8dB/cm was measured at 632.8nm. (C) 2004 Published by Elsevier B.V.

Thermoregulatory responses of Alpine goats during thermal stress

Eight non-lactating Alpine goats, averaging 57kg, were paired according to weight and assigned randomly to 2 groups of 4 animals, control (CG) and treatment (TG) with feed and water ad libitum. An adjustment period of 7 days with all animals at thermoneutral conditions was followed by a 28-day period when TG was exposed to air temperatures averaging 35.0 degrees C, from 0800 to 1700h, including simulated solar radiation, and thermoneutral conditions from 2700 to 0800h. CG remained under thermoneutral conditions. Respiratory frequency was greater, tidal volume lower, and respiratory minute volume greater for TG than CG (176 vs 30 breaths/min, P<.001, 105 vs 293ml, P<.01; 18.4 vs 9.21, P<.05). Respiratory evaporation and sweating rate as well as rectal and skin temperatures were greater for TG than CG (14.59 vs 6.32 kcal h(-1), P<.01; 43.97 vs.00 g m(-2) h(-1), P<.001; 40.0 vs 38.9 degrees C, P<.001; 39.3 vs 35.8 degrees C, P<.01). There was no difference between groups for hematocrit and feed intake, but water consumption was greater for stressed goats than control ones (28.3 vs 29.7%; 1.44 vs 1.49 kg/day; 3.07 vs 1.26 I/day, P<.05), Final body weights of both groups were similar to initial ones. It was concluded that non-lactating goats tolerated well a 35 degrees C day temperature which is 5 degrees C above the upper critical temperature, with a black-globe temperature of 39.1 degrees C and a Botsball temperature of 28.3 degrees C, though a certain degree of hyperthermia may occur, as long as thermoneutral conditions have prevailed during the night.

Thermal behaviour of polymetallic metal carbonyls with Fe-Fe, Fe-Hg and Hg-Hg bonds containing Lewis bases.

The thermal behaviour of polymetallic metal carbonyls containing Fe-Fe, Fe-Hg and Hg-Hg bonds and Lewis bases, such as [Fe-3(CO)(8)(L)(2)] (L = 1,10-phenantroline,2,2'-bipyridine), [Fe(CO)(4)(HgCl)(2)] and [Fe(CO)(4)(HgCl)(2)(L)(2)] (L = 1,10-phenantroline,2-quinolinethiol), have been investigated by thermal analysis (TG), Thermal studies give evidence that the thermal decomposition mechanisms and starting temperatures are strongly influenced by the Lewis bases. The thermal decompositions under synthetic air yielded, in all cases, the final solid product Fe2O3 which presence was confirmed by X-ray powder diffraction technique.

Preparation of SrBi2Ta2O9 ferroelectric thick films by electrophoretic deposition using aqueous suspensions

SrBi2Ta2O9 ferroelectric thick films were prepared by electrophoretic deposition (EPD). For that, ceramic powders were prepared by chemical method in order to obtain compounds with chemical homogeneity. The polymeric precursor method was used for the synthesis of the SrBi2Ta2O9 powder. The crystallographic structure of the powder was examined by X-ray diffraction, and the surface area was determined by single point BET adsorption. The 0.03 vol% suspension was formed by dispersing the powder in water using two different polymers as dispersants: an ester polyphosphate (C213) and an ammonium polyacrilate (Darvan 821-A). The influence of the different dispersants on the powder surface properties were investigated by zeta potential measurements. The films were deposited on platinum-coated alumina and Pt/Ti/SiO2/Si substrates by electrophoretic deposition using a 4 mA constant current, for 10 min, with two parallel electrodes placed at a separation distance of 3 min in the suspension. Several cycles of deposition-drying of the deposit was carried out until the desired thickness was obtained. After thermal treatment at temperatures ranging from 700 to 1000degreesC, the films were characterized by X-ray diffraction and scanning electron microscopy.

Study on the thermal behavior of the complexes of the type [PdX2(tdmPz)] (X = Cl-, Br-, I-, SCN-)

Four new mononuclear Pd(II) complexes of the type [PdX2(tdmPz)] {X = Cl- (1); Br- (2); I- (3); SCN- (4); tdmPz = 1-thiocarbamoyl-3,5-dimethylpyrazole} have been synthesized and characterized by elemental analysis, IR spectroscopy, H-1 and C-13{H-1}-NMR experiments. The thermal behavior of the complexes 1-4 has been investigated by means of thermogravimetry (TG) and differential thermal analysis (DTA). From the initial decomposition temperatures, the thermal stability of the complexes can be ordered in the sequence: 3 < 4 a parts per thousand 2 < 1. The final products of the thermal decompositions were characterized as metallic palladium by X-ray powder diffraction.

Oxygen plasma treatment of sisal fibers and polypropylene: Effects on mechanical properties of composites

Polypropylene powder and sisal fibers were oxygen plasma treated, and the mechanical properties of their composites were tested. Two main effects were investigated: the incorporation of oxygen polar groups in the polypropylene surface and the surface degradation and chain scission of both polypropylene and sisal fibers. Prior to these treatments, three reactor configurations were tested to investigate the best condition for both effects to occur in PP film. Results showed that polypropylene-cellulose adhesion forces are about an order of magnitude higher for PP film treatments at 13.56 MHz than at 40 kHz owing to much higher chain scission at lower frequencies, although it probably also occurs at high frequency and high power. Polypropylene powder treated with oxygen plasma in optimum conditions for polar group incorporation did not result in improvement in any composite mechanical property, probably owing to the polymer melting. Sisal fibers and PP powder treated In conditions of surface degradation did not improve flexural or tensile properties but resulted in higher impact resistance, comparable to the improvement obtained with the addition of compatibilizer.

Influence of the thermal treatment in the crystallization of NiWO4 and ZnWO4

NiWO4 and ZnWO4 were synthesized by the polymeric precursor method at low temperatures with zinc or nickel carbonate as secondary phase. The materials were characterized by thermal analysis (TG/DTA), infrared spectroscopy, UV-Vis spectroscopy and X-ray diffraction. NiWO4 was crystalline after calcination at 350 A degrees C/12 h while ZnWO4 only crystallized after calcination at 400 A degrees C for 2 h. Thermal decomposition of the powder precursor of NiWO4 heat treated for 12 h had one exothermic transition, while the precursor heat treated for 24 h had one more step between 600 and 800 A degrees C with a small mass gain. Powder precursor of ZnWO4 presented three exothermic transitions, with peak temperatures and mass losses higher than NiWO4 has indicating that nickel made carbon elimination easier.