scholarly journals Study on Thermal Decomposition Behavior, Gaseous Products, and Kinetic Analysis of Bis-(Dimethylglyoximato) Nickel(II) Complex Using TG-DSC-FTIR-MS Technique

Catalysts ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 331
Author(s):  
Ergang Yao ◽  
Siyu Xu ◽  
Fengqi Zhao ◽  
Taizhong Huang ◽  
Haijian Li ◽  
...  

The fiber-like bis-(dimethylglyoximato) nickel(II) complex, Ni(DMG)2 was successfully synthesized. The obtained samples were characterized by SEM-EDS, FT-IR, XRD, and XPS. The TG-DSC-FTIR-MS coupling technique was used to characterize the thermal decomposition behavior and evolved gas analysis of Ni(DMG)2. The non-isothermal decomposition reaction kinetic parameters were obtained by both combined kinetic analysis and isoconversional Vyazovkin methods. It was found that Ni(DMG)2 begins to decompose at around 280 °C, and a sharp exothermic peak is observed in the DSC curve at about 308.2 °C at a heating rate of 10 °C·min−1. The main gaseous products are H2O, NH3, N2O, CO, and HCN, and the content of H2O is significantly higher than that of the others. The activation energy obtained by the combined kinetic analysis method is 170.61 ± 0.65 kJ·mol−1. The decomposition process can be described by the random nucleation and growth of the nuclei model. However, it was challenging to attempt to evaluate the reaction mechanism precisely by one ideal kinetic model.

2015 ◽  
Vol 71 ◽  
pp. 112-122 ◽  
Author(s):  
Yoshihiko Sato ◽  
Takehiro Matsunaga ◽  
Shin-ichi Koyama ◽  
Tatsuya Suzuki ◽  
Masaki Ozawa

Materials ◽  
2018 ◽  
Vol 11 (11) ◽  
pp. 2082
Author(s):  
Shih-Yung Huang ◽  
Jian-Cheng Lin ◽  
Sin-Liang Ou

This study investigates the thermal decomposition behavior of GaN-based epilayers on patterned sapphire substrates (GaN-epi/PSSs) in a quartz furnace tube under a hydrogen atmosphere. The GaN-epi/PSS was decomposed under different hydrogen flow rates at 1200 °C, confirming that the hydrogen flow rate influences the decomposition reaction of the GaN-based epilayer. The GaN was completely removed and the thermal decomposition process yielded gallium oxyhydroxide (GaO2H) nanostructures. When observed by transmission electron microscopy (TEM), the GaO2H nanostructures appeared as aggregates of many nanograins sized 2–5 nm. The orientation relationship, microstructure, and formation mechanism of the GaO2H nanostructures were also investigated.


2008 ◽  
Vol 110 (5) ◽  
pp. 2924-2931 ◽  
Author(s):  
M. Farmahini-Farahani ◽  
S. H. Jafari ◽  
H. A. Khonakdar ◽  
F. Böhme ◽  
A. Yavari ◽  
...  

2001 ◽  
Vol 11 (PR3) ◽  
pp. Pr3-675-Pr3-682 ◽  
Author(s):  
Y. S. Min ◽  
Y. J. Cho ◽  
D. Kim ◽  
J. H. Lee ◽  
B. M. Kim ◽  
...  

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.


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