Thermal decomposition of energetic materials. 16. Solid-phase structural analysis and the thermolysis of 1,4-dinitrofurazano[3,4-b]piperazine

1986 ◽  
Vol 90 (19) ◽  
pp. 4686-4690 ◽  
Author(s):  
Y. Oyumi ◽  
A. L. Rheingold ◽  
T. B. Brill
Keyword(s):  
Thermal Decomposition ◽  
Structural Analysis ◽  
Energetic Materials ◽  
Solid Phase

scholarly journals Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III)—a single-source precursor for antimony sulfide thin films

2021 ◽  
Author(s):  
Jako S. Eensalu ◽  
Kaia Tõnsuaadu ◽  
Jasper Adamson ◽  
Ilona Oja Acik ◽  
Malle Krunks
Keyword(s):  
Thin Films ◽  
Thermal Decomposition ◽  
Mass Loss ◽  
Solid Phase ◽  
Evolved Gas Analysis ◽  
Gas Analysis ◽  
Thermal Decomposition Mechanism ◽  
Product Analysis ◽  
Gaseous Species ◽  
Single Source Precursor

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.

scholarly journals Comparative thermal research on tetraazapentalene-derived heat-resistant energetic structures

2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Jing Zhou ◽  
Li Ding ◽  
Yong Zhu ◽  
Bozhou Wang ◽  
Xiangzhi Li ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Thermal Decomposition ◽  
Fourier Transform ◽  
Energetic Materials ◽  
Great Influence ◽  
Fourier Transform Infrared ◽  
Thermal Decomposition Mechanism ◽  
Scanning Calorimetry ◽  
In Situ Ftir Spectroscopy ◽  
Heat Resistant

AbstractOrganic inner salt structures are ideal backbones for heat-resistant energetic materials and systematic studies towards the thermal properties of energetic organic inner salt structures are crucial to their applications. Herein, we report a comparative thermal research of two energetic organic inner salts with different tetraazapentalene backbones. Detailed thermal decomposition behaviors and kinetics were investigated through differential scanning calorimetry and thermogravimetric analysis (DSC-TG) methods, showing that the thermal stability of the inner salts is higher than most of the traditional heat-resistant energetic materials. Further studies towards the thermal decomposition mechanism were carried out through condensed-phase thermolysis/Fourier-transform infrared (in-situ FTIR) spectroscopy and the combination of differential scanning calorimetry-thermogravimetry-mass spectrometry-Fourier-transform infrared spectroscopy (DSC-TG-MS-FTIR) techniques. The experiment and calculation results prove that the arrangement of the inner salt backbones has great influence on the thermal decompositions of the corresponding energetic materials. The weak N4-N5 bond in “y-” pattern tetraazapentalene backbone lead to early decomposition process and the “z-” pattern tetraazapentalene backbone exhibits more concentrated decomposition behaviors.

Thermal decomposition and isomerization ofcis-permethrin and β-cypermethrin in the solid phase

2001 ◽  
Vol 58 (2) ◽  
pp. 183-189 ◽  
Author(s):  
Paola González Audino ◽  
Susana A Licastro ◽  
Eduardo Zerba
Keyword(s):  
Thermal Decomposition ◽  
Solid Phase

Thermal decomposition of energetic materials

1991 ◽  
Vol 181 ◽  
pp. 71-77 ◽  
Author(s):  
J.K. Chen ◽  
T.B. Brill
Keyword(s):  
Thermal Decomposition ◽  
Energetic Materials

scholarly journals The influence of the nature and textural properties of different supports on the thermal behavior of Keggin type heteropolyacids

2006 ◽  
Vol 71 (3) ◽  
pp. 235-249 ◽  
Author(s):  
Alexandru Popa ◽  
Viorel Sasca ◽  
Mircea Stefanescu ◽  
Erne Kis ◽  
Radmila Marinkovic-Neducin
Keyword(s):  
Thermal Stability ◽  
Thermal Decomposition ◽  
Thermal Behavior ◽  
Solid Phase ◽  
Textural Properties ◽  
Nitrogen Adsorption ◽  
Active Phase ◽  
Support Surface ◽  
Sem Images ◽  
The Stability

In order to obtain highly dispersed heteropolyacids (HPAs) species, H3PMo12O40 and H4PVMo11O40 were supported on various supports: silica (Aerosil - Degussa and Romsil types) and TiO2. The structure and thermal decomposition of supported and unsupported HPAs were followed by different techniques (TGA-DTA, FTIR, XRD, low temperature nitrogen adsorption, scanning electron microscopy). All the supported HPAs were prepared by impregnation using the incipient wetness technique with a 1:1 mixture of water-ethanol. Samples were prepared with different concentrations to examine the effect of loading on the thermal behavior of the supported acid catalysts. The thermal stability was evaluated with reference to the bulk solid acids and mechanical mixtures. After deposition on silica types supports, an important decrease in thermal stability was observed on the Romsil types and a small decrease on the Aerosil type. The stability of the heteropolyacids supported on titania increased due to an anion-support interaction, as the thermal decomposition proceeded in two steps. The structure of the HPAs was not totally destroyed at 450 ?C as some IR bands were still preserved. A relatively uniform distribution of HPAs on the support surface was observed for all compositions of the active phase. No separate crystallites of solid phase HPAs were found in the SEM images.

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