Synthesis thermogravimetric analysis

The process known as transimidization has been employed to functionalize polyimide oligomers, which were subsequentiy used to produce polyimide—titania hybrids (59). This technique resulted in the successhil synthesis of transparent hybrids composed of 18, 37, and 54% titania. The effect of metal alkoxide quantity, as well as the oligomer molecular weight and cure temperature, were evaluated using differential scanning calorimetry (dsc), thermogravimetric analysis (tga) and saxs. 

In most of the studies discussed above, except for the meta-linked diamines, when the aromatic content (dianhydride and diamine chain extender), of the copolymers were increased above a certain level, the materials became insoluble and infusible 153, i79, lsi) solution to this problem with minimum sacrifice in the thermal properties of the products has been the synthesis of siloxane-amide-imides183). In this approach pyromellitic acid chloride has been utilized instead of PMDA or BTDA and the copolymers were synthesized in two steps. The first step, which involved the formation of (siloxane-amide-amic acid) intermediate was conducted at low temperatures (0-25 °C) in THF/DMAC solution. After purification of this intermediate thin films were cast on stainless steel or glass plates and imidization was obtained in high temperature ovens between 100 and 300 °C following a similar procedure that was discussed for siloxane-imide copolymers. Copolymers obtained showed good solubility in various polar solvents. DSC studies indicated the formation of two-phase morphologies. Thermogravimetric analysis showed that the thermal stability of these siloxane-amide-imide systems were comparable to those of siloxane-imide copolymers 183>. 

Ando and co-workers have reported the synthesis of a silyl-carborane hybrid diethynylbenzene-silylene polymer (108) (Fig. 66) possessing high thermal stability.136 The polymer contained Si and —C=C— group in the main chain and m-carborane and vinyl groups in the side chain. The 5% weight-loss temperature of the cured polymer in air was over 1000°C as determined by thermogravimetric analysis. 

The reaction product was isolated by distillation under reduced pressure as a white powder and employed immediately after the synthesis in the registration of the FT-IR spectrum and in the thermogravimetric analysis. 

A synthesis protocol of porous zirconia catalyst support, through a neutral Ci3(EO)6-Zr(OC3H7)4 assembly pathway has been developed. Our studies evidenced the role played by the surfactant. It has also been observed that the increase of hydrothermal treatment time and temperature have a benefical effect on tailoring the pore sizes. The synthesized materials will be used in preparation of Au / ZrOz, Au / VO / ZrOz catalysts, which will be tested in the benzene oxidation reaction. Thermogravimetric analysis shows that the recovered zirconia present a relatively low thermal stability. Then the structure collapses due to the crystallization to more stable tetragonal and monoclinic phase. 

In 1967, Lloyd et al. claimed the first synthesis of a bismuthonium ylide by heating triphenylbismuthine and diazotetraphenylcyclopentadiene at 140°C. However, experimental details confirming the product are not available [67CC1042, 88JCS(P2)1829], Thermogravimetric analysis of the reaction shows that the carbene, cyclopentadienylidene, is formed at the initial step [72CC912]. 

The YBa2Cu307 y series with 0starting material was prepared in the manner described in the synthesis section and its oxygen content was evaluated to be 6.96+0.1 by a thermogravimetric analysis method (TGA) described elsewhere (11). This value will be taken as 7.0 (i.e. y = 0) in the following. Different values of y were then obtained by a contolled heat treatment of rectangular bars of the compound in an argon ambient. 

Rao and co-workers [82] used an inverted emulsion process for the synthesis of the emeraldine salt of PAM using a novel oxidising agent, benzoyl peroxide. The polymerisation was carried out in a non-polar solvent in the presence of four different protonic acids as dopants and an emulsifier (sodium lauryl sulfate). The polymer salts were characterised spectroscopically by ultraviolet-visible, Fourier-transform infrared, Fourier-transform Raman and electron paramagnetic resonance spectroscopy. Thermogravimetric analysis, was used to determine the stability of the salts and the activation energy for the degradation. The conductivity of the salts was found to be in the order of 10 S/cm. 

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