Lanthanide complexes with 3,4,5-triethoxybenzoic acid and 1,10-phenanthroline: synthesis, crystal structures, thermal decomposition mechanism and phase transformation kinetics

RSC Advances ◽  
2015 ◽  
Vol 5 (12) ◽  
pp. 9261-9271 ◽  
Author(s):  
Xiao-Xia Qi ◽  
Ning Ren ◽  
Su-Ling Xu ◽  
Jian-Jun Zhang ◽  
Guang-Cai Zong ◽  
...  

In the temperature range of 280 to 350 K, there is a solid-to-solid phase transition for each complex, which is further evidenced by four thermal circulating processes with the scanning rate of 10 K min−1.

2003 ◽  
Vol 39 (1-2) ◽  
pp. 353-368 ◽  
Author(s):  
N. Adhoum ◽  
J. Bouteillon ◽  
D. Dumas ◽  
J.C. Poignet

This paper deals with electrochemical insertion into a cathodic material. New results on modeling of the influence of a solid phase transformation on the shape of voltamograms are presented. The original experiments concern the insertion of sodium into carbon during the cathodic reduction of molten NaF at 1020 ?C, but in the present manuscript emphasis on the theoretical aspects of the work is put. Phase transformations during electrochemical insertion are taken into account, with various values for parameters such as the thermodynamic biphase equilibrium potential, the compared diffusion and phase transformation kinetics, and the electrode thickness. The voltamograms calculated present very specific features; some of them have already been observed experimentally in literature.


Author(s):  
Jako S. Eensalu ◽  
Kaia Tõnsuaadu ◽  
Jasper Adamson ◽  
Ilona Oja Acik ◽  
Malle Krunks

AbstractThermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III) (1), a precursor for Sb2S3 thin films synthesized from an acidified aqueous solution of SbCl3 and KS2COCH2CH3, was monitored by simultaneous thermogravimetry, differential thermal analysis and evolved gas analysis via mass spectroscopy (TG/DTA-EGA-MS) measurements in dynamic Ar, and synthetic air atmospheres. 1 was identified by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) measurements, and quantified by NMR and elemental analysis. Solid intermediates and final decomposition products of 1 prepared in both atmospheres were determined by X-ray diffraction (XRD), Raman spectroscopy, and FTIR. 1 is a complex compound, where Sb is coordinated by three ethyldithiocarbonate ligands via the S atoms. The thermal degradation of 1 in Ar consists of three mass loss steps, and four mass loss steps in synthetic air. The total mass losses are 100% at 800 °C in Ar, and 66.8% at 600 °C in synthetic air, where the final product is Sb2O4. 1 melts at 85 °C, and decomposes at 90–170 °C into mainly Sb2S3, as confirmed by Raman, and an impurity phase consisting mostly of CSO 2 2− ligands. The solid-phase mineralizes fully at ≈240 °C, which permits Sb2S3 to crystallize at around 250 °C in both atmospheres. The gaseous species evolved include CS2, C2H5OH, CO, CO2, COS, H2O, SO2, and minor quantities of C2H5SH, (C2H5)2S, (C2H5)2O, and (S2COCH2CH3)2. The thermal decomposition mechanism of 1 is described with chemical reactions based on EGA-MS and solid intermediate decomposition product analysis.


2010 ◽  
Vol 63 (4) ◽  
pp. 544 ◽  
Author(s):  
Anja-Verena Mudring

Ionic liquids (ILs) have become an important class of solvents and soft materials over the past decades. Despite being salts built by discrete cations and anions, many of them are liquid at room temperature and below. They have been used in a wide variety of applications such as electrochemistry, separation science, chemical synthesis and catalysis, for breaking azeotropes, as thermal fluids, lubricants and additives, for gas storage, for cellulose processing, and photovoltaics. It has been realized that the true advantage of ILs is their modular character. Each specific cation–anion combination is characterized by a unique, characteristic set of chemical and physical properties. Although ILs have been known for roughly a century, they are still a novel class of compounds to exploit due to the vast number of possible ion combinations and one fundamental question remains still inadequately answered: why do certain salts like ILs have such a low melting point and do not crystallize readily? This Review aims to give an insight into the liquid–solid phase transition of ILs from the viewpoint of a solid-state chemist and hopes to contribute to a better understanding of this intriguing class of compounds. It will introduce the fundamental theories of liquid–solid-phase transition and crystallization from melt and solution. Aside form the formation of ideal crystals the development of solid phases with disorder and of lower order like plastic crystals and liquid crystals by ionic liquid compounds are addressed. The formation of ionic liquid glasses is discussed and finally practical techniques, strategies and methods for crystallization of ionic liquids are given.


RSC Advances ◽  
2016 ◽  
Vol 6 (2) ◽  
pp. 859-865 ◽  
Author(s):  
Changping Guo ◽  
Dunju Wang ◽  
Bing Gao ◽  
Jun Wang ◽  
Bo Luo ◽  
...  

The comparison of solid–solid phase transition (ε → γ polymorph) of CL-20 and Cl-20/composites revealed by DSC curves.


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