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Abstract  

This paper examines the polymerization of acrylonitrile to poly(acrylonitrile)(PAN), and its cyclization, in bulk form and using N,N-dimethylformamide (DMF) as solvent in which both monomer and polymer are soluble. Thermal analysis of the resultant products after polymerization has been performed by DSC and pyrolysis gas chromatography/mass spectrometry (Py-GC/MS). Scanning electron microscopy has been used to study the morphology of the resultant products and after thermal treatments. The DSC thermal curve of PAN-DMF sample is quite different from the PAN bulk sample, showing a single sharp exothermic peak associated with nitrile group polymerization (cyclization) of PAN at lower temperature (240°C) than that of bulk PAN sample (314°C). Cyclization of PAN was confirmed by IR spectroscopy. It was found that the amide molecules are difficult to eliminate completely in the product obtained after the polymerization reaction, even after prolonged heating at 110°C, and remain occluded. The formation of a complex by dipolar bonding is also possible and it is discussed. It is concluded that the amount of heat evolved as well as the temperature interval over which it is released are influenced by the chemical processing of PAN when using DMF as solvent of both monomer and polymer. Pyrolysis of these PAN samples revealed the release of occluded molecules of DMF, and several compounds containing nitrogen produced from the thermal degradation processes. All these results are interesting to know the chemical processing of carbon fibres and activated carbon fibres from PAN modified precursors.

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Journal of Thermal Analysis and Calorimetry
Authors:
J. Pascual
,
F. Corpas
,
J. López-Beceiro
,
M. Benítez-Guerrero
, and
R. Artiaga

Abstract  

A Spanish red mud was thermally characterized. Chemical and mineralogical composition were determined by XRF and XRD.The thermal events observed in the range from room temperature to 1300°C were related to the sample composition. The first mass loss step was related to free water content, while many of the other processes were related to dehydration processes. It was found that most of the decomposition reactions of hydrohematite, ferrihydrite, aluminogoethite, boehmite, silicates and carbonates were strongly overlapping. It was also explained the formation of silicates and calcium titanate, which presence was confirmed at 1000°C by XRD.

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Abstract  

Chromium doped spinels LiCrYMn2−YO4 (0.2≤Y≤0.8) has been synthesized by the sucrose-aided combustion procedure. The thermal behaviour, phase homogeneity and structural characteristics of the samples were studied by thermal analysis, coupled mass spectrometry, and room-and high-temperature X-ray diffraction methods. It was found that the ‘as prepared’ samples contained residual organic impurities undetectable for X-ray diffraction, that burn out completely at 400°C. Samples treated between 400 and 750°C are single phase spinels, whose crystallites size increase from 10 to 50 nm on increasing the temperature. Cr-doping enhances the thermal stability of the spinels, which augments on increasing the Cr content Y. The enhanced thermal stability of the spinels has been accounted for based on the high excess stabilization energy of Cr3+ in octahedral ligand field.

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Journal of Thermal Analysis and Calorimetry
Authors:
V. Balek
,
M. Beneŝ
,
J. Ŝubrt
,
J. Pérez-Rodriguez
,
P. Sánchez-Jiménez
,
L. Pérez-Maqueda
, and
J. Pascual-Cosp

Abstract  

Emanation thermal analysis (ETA), thermogravimetry and high temperature XRD were used to characterize the thermal behavior during dehydration of natural Na montmorillonite (Upton Wyoming, USA) and homoionic montmorillonite (MMT) samples saturated with different cations, i.e. Li+, Cs+, NH4 +, Mg2+ and Al3+. ETA results characterized radon mobility and microstructure changes that accompanied the mass loss of the samples due to dehydration on heating in air. A collapse of interlayer space between the silicate sheets after water release from the MMT samples was characterized by a decrease of the radon release rate, ΔE. Decreases in c-axis basal spacing (d 001) values determined from XRD patterns for the different montmorillonite samples follow the sequence:

\documentclass{aastex} \usepackage{amsbsy} \usepackage{amsfonts} \usepackage{amssymb} \usepackage{bm} \usepackage{mathrsfs} \usepackage{pifont} \usepackage{stmaryrd} \usepackage{textcomp} \usepackage{upgreek} \usepackage{portland,xspace} \usepackage{amsmath,amsxtra} \pagestyle{empty} \DeclareMathSizes{10}{9}{7}{6} \begin{document} $$Mg - MMT > Al - MMT > Li - MMT > Na - MMT > NH_4 - MMT > Cs - MMT$$ \end{document}
The decrease of the radon release rate (ΔE) determined by ETA that characterized microstructure changes due to collapse of interlayer space corresponded well to differences in the c-axis basal spacing (Δd 001) values determined from the XRD patterns before and after samples dehydration.

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Journal of Thermal Analysis and Calorimetry
Authors:
V. Ramírez-Valle
,
M. Jiménez de Haro
,
M. Avilés
,
L. Pérez-Maqueda
,
A. Durán
,
J. Pascual
, and
J. Pérez-Rodríguez

Abstract  

Static and dynamic heating of vermiculite samples from Santa Olalla, Huelva, Spain, saturated with different cations, i.e. Na+, Cs+, NH4 +, Mg2+, Ca2+, Ba2+ and Al3+, have been studied. The characterization of the phases formed during heating has been carried out by X-ray diffraction. The phases formed depend on the cation present in the interlamellar position and the heating process. The phases identified in the vermiculite samples saturated with different cations and heated at different temperatures are the following: enstatite, forsterite, spinel, cordierite, anorthite, pollucite, nepheline, coesite, celsian and others various mixed silicates; also some dehydrated and amorphous phases have been observed. On static heating, at the maximum temperature reached in this work, the phases formed appear mixed with a glassy phase.

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