• Title/Summary/Keyword: Kissinger's method

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A Study on Thermal Decomposition of RDX According to the Size using TGA (TGA를 이용한 RDX의 입자 크기에 따른 열적 분해 특성 연구)

  • Bum, Kil-Ho;Kim, Seung-Hee;Kim, Jin-Seuk
    • Journal of the Korea Institute of Military Science and Technology
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    • v.15 no.1
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    • pp.81-85
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    • 2012
  • This work is related to study the thermal decomposition of 1,3,5-trinitro-1,3,5-triazacylohexane(RDX) by differential scanning calorimeter and thermo-gravimetry with Kissinger's & Iso-conversional method under nonisothermal conditions, with heating rate from 2 to $8^{\circ}C$/min or given heating rate. We calculated and compared activation energy with these two methods. Iso-conversional method is better than Kissinger's method to study decomposition mechanism. We also investigated activation energy and frequency factor by Kissinger's & Iso-conversional method with the influence of particle size. In case of single crystal, Cl-3(large crystal) has better thermal stability than Cl-5(small crystal). The activation energy increased according to the size of the particle size.

Effect of Particle Size on Thermal Property of RDX and HMX (HMX와 RDX의 열적 특성에 미치는 입자 크기의 영향)

  • Kim, Seung Hee
    • Applied Chemistry for Engineering
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    • v.23 no.3
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    • pp.352-357
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    • 2012
  • Techniques of thermal analyses such as DSC and TGA have been used in the study of activation energy (Ea) and frequency factor (A) depending on the particle size of RDX and HMX. Activation energy and frequency factor were calculated by Kissinger's method and Vyazovkin's method. As the particle size of RDX increased, TGA showed activation energy increased, but DSC didn't show. However, In case of HMX, as the particle size increased, both of DSC and TGA showed increase in activation energy. Moreover, Vyazovkin's method can obtain activation energy and mechanism according to decomposition of RDX and HMX.

Non-isothermal TGA Analysis on Thermal Degradation Kinetics of Modified-NR Rubber Composites (비등온 TGA에 의한 개질NR고무복합재료지 열분해 Kinetics에 관한 해석)

  • Oh, Jeong-Seok;Lee, Joon-Mann;Ahn, Won-Sool
    • Polymer(Korea)
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    • v.33 no.5
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    • pp.435-440
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    • 2009
  • Thermal degradation behavior of CR (chloroprene) -modified NR (natural rubber) compounds, having different sulfur/accelerator compositions, was studied by non-isothermal TGA method. Data were analyzed using both Kissinger and Flynn-Wall-Ozawa analysis to assess the activation energies. Activation energy obtained from Kissinger analysis was $147.0{\pm}2.0$ kJ/mol for all samples, showing little effect of sulfur/accelerator composition changes in the samples. On the other hand, activation energy from Flynn-Wall-Ozawa analysis exhibited much variations with conversion, showing average value of $211.6{\pm}19.0$ kJ/mol. From the results, it was considered that whole thermal degradation processes of the samples were composed of complex multiple step processes, of which reaction mechanisms were different from each other.

Cure Kinetcs of DGEBA/MDA/GN/HQ System by DSC Analysis (DSC 분석에 의한 DGEBA/MDA/GN/HQ계의 경화반응 속도론)

  • Lee, J.Y.;Shim, M.J.;Kim, S.W.
    • Applied Chemistry for Engineering
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    • v.5 no.5
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    • pp.904-909
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    • 1994
  • Cure kinetics of DGEBA(diglycidyl ether of bisphenol A)/MDA(4,4'-methylene dianiline)/GN(glutaronitrile) system with and without HQ(hydroquinone) as a catalyst was studied by Kissinger equation and Fractional life method. The activation energy of the system with HQ was somewhat lower and the pre-exponential factor of that was higher by about 30% than those of the system without HQ. As 1.25phr of HQ was added, reaction rates increased about 1.8 times.

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A Study of Thermal Decomposition Characteristics and Toxicity of Product on PS/SAN/ABS (PS/SAN/ABS의 열분해특성과 생성물의 독성에 관한 연구)

  • Kang Yun Jin;Lee Nae Woo;Seul Soo Duk
    • Journal of the Korean Institute of Gas
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    • v.4 no.1 s.9
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    • pp.16-25
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    • 2000
  • To estimate the thermal characteristics and toxic parameters on styrene copolymers, We have investigated the activation energy, physical features and generation possibility of toxic material like narcotic gases. The activation energy was 25${\~}$50 Kcal/mol by the Kissinger's and DSC method at high temperature decomposition. It will be good information to estimate the possibility of fire occurrence. From calculations of FED, the values of $LC_{50}$ for PS, SAN and ABS were checked as 8,580, 265 and 308 $mg/m^3$ The mechanisms of thermal decomposition were mainly estimated by main chain scission, not by side group on FT-IR analysis.

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A Study of Crystallization and Fracture Toughness of Glass Ceramics in the $ZrO_2.SiO_2$ Systems Prepared by the Sol-Gel Method (졸-겔법으로 제조한 $ZrO_2.SiO_2$계 결정화유리의 결정화 및 파괴인성에 관한 연구)

  • 신대용;한상목;강위수
    • Journal of the Korean Ceramic Society
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    • v.37 no.1
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    • pp.50-56
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    • 2000
  • Precursor gels with the composition of xZrO2·(100-x)SiO2 systems (x=10, 20 and 30 mol%) were prepared by the sol-gel method. Kinetic parameters, such as activation energy, Avrami's exponent, n, and dimensionality crystal growth value, m, have been simultaneously calculated from the DTA data using Kissinger and Matusita equations. The crystallite size dependence of tetragonal to monoclinic transformation of ZrO2 was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal ZrO2 occurred through 3-dimensional diffusiion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about 310∼325±10kJ/mol. The growth of t-ZrO2, in proportion to the cube of radius, increased with increasing heating temperature and hteat-treatment time. It was suggested that the diffusion of Zr4+ ions by Ostwald ripening was rate-limiting process for thegrowth of t-ZrO2 crystallite size. The fracture toughness of xZrO2·(100-x)SiO2 systems glass ceramics increased with increasing crystallite size of t-ZrO2. The fracture toughness of 30ZrO2·70SiO2 system glass ceramics heated at 1,100℃ for 5h was 4.84 MPam1/2 at a critical crystaliite size of 40 nm.

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A Study on Formation and Thermal Decomposition Kinetics of PU Elastomers by Dynamic DSC and TGA Analysis (Dynamic DSC 및 TGA 열분석을 이용한 PU Elastomer의 중합반응 및 열분해 반응 Kinetics에 관한 연구)

  • Yoon, Soo-Koong;Ahn, Won-Sool
    • Elastomers and Composites
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    • v.42 no.1
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    • pp.47-54
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    • 2007
  • Reaction kinetics of polyurethane elastomers (PU) were studied using dynamic DSC and TGA for three PU samples of general purpose (Sample A), high temperature cross-likable CASE purpose with MOCA (Sample B), and RT cross-likable CASE purpose grade (Sample C). From DSC results, sample with MOCA(Sample B) showed lower shift of peak temperature, while showing broader thermograms than those of general purpose grade (Sample A). On the other hand, RT cross-linkable PU grade (Sample C) showed an interesting double mode reaction patterns, i.e., a lower temperature reaction at about $70\;^{\circ}C$, and a higher temperature reaction in the range of $140{\sim}170\;^{\circ}C$, indicating that it requires 2-step reaction process in order to complete the reaction. Once the cross-linking reaction completed, however, TGA results showed that all the samples would be considered to have similar chemical structures, showing similar decomposition processes. Sample C, especially, had showed decomposition properties of both Sample A and Sample B. Formation activation energies calculated from Kissinger method showed 10.39, 65.85, 36.52(Low $T_p$) and 18.21(High $T_p$) kcal/mol, while decomposition activation energies were 31.94, 30.84, 24.16 kcal/mol, respectively.

Kinetic Studies of the Catalytic Low Rank Coal Gasification under CO2 Atmosphere (CO2분위기하에서 저급석탄 촉매가스화 반응 특성 연구)

  • Park, Chan Young;Park, Ji Yun;Lee, Si Hoon;Rhu, Ji Ho;Han, Moon Hee;Rhee, Young Woo
    • Korean Chemical Engineering Research
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    • v.50 no.6
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    • pp.1086-1092
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    • 2012
  • In this study, kinetic studies and analysis of the produced syngas were conducted for low rank coal gasification under $CO_2$ atmosphere. 6 coals were analyzed to measure amount of sulfur and ash by proximate and ultimate analyses. And then they were analyzed to select suitable sample by using Thermogravimetric analyzer (TGA). Selected coal sample Samhwa was mixed with catalysts. Mixed samples with catalysts were used to get activation energy under $CO_2$ atmosphere by using Kissinger's method and shrinking core model (SCM). Also, analysis of produced syngas was performed by Gas Chromatography (GC). In this experiment, activation of the $K_2CO_3$ was the best performance, and result of the analysis of the syngas showed similar trend with result of the activation energy.

The crystallization behavior of glass made from coal bottom ash (석탄 바닥재로 제조된 유리의 결정화 거동 분석)

  • Jang, Seok-Joo;Kang, Seung-Gu
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.1
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    • pp.58-63
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    • 2010
  • The glass-ceramics made from the mixture of coal bottom ash, produced from a thermal power plant mixed with $Na_2O$ and $Li_2O$ was fabricated and their crystallization behavior was studied using a non-isothermal analyzing method. The temperature for 50% crystallization was higher than the exothermic peak temperature $T_p$ at DTA curve and the quickest crystallization temperature was much the same as $T_p$ as identified from the relationships of crystallized fraction and crystallization rate with temperature. By using Kissinger equation describing a crystallization behavior, the activation energy (262 kJ/mol), the Avrami constant (1.7) and the frequency ($5.7{\times}10^{16}/s$) for crystallization were calculated from which the nepheline crystal could be expected as showing an 1~2-dimensional surface crystallization behavior mainly with some bulk crystallization tendency at the same time. The actual observation of microstructure using SEM showed the considerable amount of surface crystals of dendrite and the bulk crystals with low fraction, so the prediction by the Kissinger equation was in accord with the crystallization behavior of glass-ceramics fabricated in this study.

The Study on Thermal Analysis and Thermodynamic Characteristics of Spinel Compounds(ZnCo2O4, NiCo2O4) (스피넬 구조를 가지는 전이금속화합물(ZnCo2O4, NiCo2O4)의 열적 분석 및 열역학적 특성 연구)

  • Kim, Jae-Uk;Ji, Myoung-Jin;Cha, Byung-Kwan;Kim, Chul-Hyun;Jang, Won-Cheoul;Kim, Jong-Gyu
    • Journal of the Korean Chemical Society
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    • v.54 no.2
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    • pp.192-197
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    • 2010
  • The spinel compound was obtained by the thermal decomposition of Zn-Co and Zn-Ni gel prepared by sol-gel method using oxalic acid as a chelating agent. The formation of spinel compound has been comfirmed by thermogravimetric analysis (TGA), x-ray powder diffraction (XRD) and infrared spectroscopy (IR). The particle size of 13 nm~16 nm was calculated by Scherrer's equation. The sol-gel method provides a practicable and effective route for the synthesis of the spinel compound at low temperature ($350^{\circ}C$). The kinetic parameters such as activation energy (Ea) and pre-exponential factor (A) for each compound were found by means of the Kissinger method and Arrhenius equation. The decomposition of spinel compound has an activation energy about 155 kJ/mol. Finally, the thermodynamic parameters (${\Delta}G^{\varphi}$, ${\Delta}H^{\varphi}$, ${\Delta}S^{\varphi}$) for decomposition of spinel compound was determined.