• Title/Summary/Keyword: Kissinger method

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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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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.

Analyses of Nano Epoxy-Silica Degradation in LEO Space Environment (저궤도 우주환경에서 에폭시-실리카 나노 복합소재의 열화거동 분석)

  • Jang, Seo-Hyun;Han, Yusu;Hwang, Do Soon;Jung, Joo Won;Kim, Yeong Kook
    • Journal of the Korean Society for Aeronautical & Space Sciences
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    • v.48 no.12
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    • pp.945-952
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    • 2020
  • In this study, the effects of Low Earth Orbit(LEO) environments on the degradation behavior of epoxy nano silica composite materials were investigated. The nanocomposite materials containing silica particles in different weight ratios of 10% and 18% were prepared and degraded in a LEO simulator to compare with the neat epoxy cases. Thermogravimetric analysis (TGA) was performed on the degraded nanocomposites and the activation energies were calculated by Friedman method, Flynn-Wall-Ozawa (FWO) method, Kissinger method, and DAEM (Distributed Activation Energy Method) based on the iso-conversional method. As the results, for the neat epoxy sample cases, it was found that the average activation energy was increased as the degradation was progressed. When the nano particles were mixed, however, the energy increased to the 15 environmental test cycles, and decreased afterwards, meaning that the particle mixture contributed adversely to the thermal degradation. Discussions on the results of the different calculation methods were also given.

A Study on Effects of Vulcanization Systems on Cross-linking and Degradation Reactions of NR/CR Blends Using Dynamic DSC and TGA (Dynamic DSC와 TGA를 이용한 NR/CR 고무블렌드의 가황시스템이 가교 및 열화반응에 미치는 영향 연구)

  • Min, Byung-kwon;Park, DongRyul;Ahn, WonSool
    • Korean Chemical Engineering Research
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    • v.47 no.2
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    • pp.169-173
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    • 2009
  • Effects of variations sulfur/accelerator ratio on cross-linking and thermal degradation behavior of NR/CR rubber compounds were studied using both dynamic DSC and non-isothermal TGA. DSC thermograms of the given samples were obtained with several different heating rates, and after cross-liked in DSC, TGA thermograms with the same samples also obtained. Kissinger analysis was applied to assess the activation energies for the cross-linking and thermal decomposition processes. Results showed that the formation and thermal decomposition reaction of the samples occurred in the overall temperature range of $120{\sim}180^{\circ}C$ and $350{\sim}450^{\circ}C$, respectively, exhibiting that data could be well-fittable by Kissinger method. Furthermore, formation activation energy by DSC was estimated as $83.0{\pm}5.0kJ/mol$, which was much smaller than that of degradation by TGA, $147.0{\pm}2.0kJ/mol$. From these results, it was considered that, although variations of sulfur/accelerator ratio in the present experiments affected little on the formation mechanism and/or thermal degradation, they could play roles as the catalysts which lower the activation energy of formation. Because of stabilization after formation reaction, however, they have no more effects on the lowering the activation energy, showing higher values when decomposition, caused by main-chain scissions.

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.

Thermal Degradation Analyses of Epoxy-Silica Nano Composites (에폭시-실리카 나노 복합소재의 열화 특성 및 거동 분석)

  • Jang, Seo-Hyun;Han, Yusu;Hwang, Do Soon;Jung, Joo Won;Kim, Yeong K.
    • Composites Research
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    • v.33 no.5
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    • pp.268-274
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    • 2020
  • This paper analyzed the degradation behaviors of silica nano epoxy composite based on the isoconversional method. The size of the silica nano particle was about 12 nm and the particles were mixed by three different weight ratios to make the degradation test samples. The thermogravimetric analyses were performed under six different temperature increase rates to measure the weight changes. Four different methods, Friedman, Flynn-Wall-Ozawa, Kissinger and DAEM (Distributed Activation Energy Method), were employed to calculate the activation energies depending on the conversion ratios, and their calculation results were compared. The results represented that the activation energy was increased when the silica nano particles were mixed up to 10%, indicating the definite contribution of the particles to the degradation behavior enhancements. However, the enhancement was not proportional to the particle mixture ratio by demonstrating the similar activation energies between 10% and 18% samples. The calculation results by the different methods were also compared and discussed.

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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Cure Kinetics of DGEBA/MDA/SN/HQ Thermosetting Matrix (열경화성 DGEBA/MDA/SN/HQ 매트릭스의 경화반응 속도)

  • Lee, Jae-Yeong;Sim, Mi-Ja;Kim, Sang-Uk
    • Korean Journal of Materials Research
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    • v.5 no.6
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    • pp.667-672
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    • 1995
  • Cure kinetics of DGEBA(diglycidyl ether of bisphenol A)/MDA(4, 4'-methylene dianiline)/SN(succinonitrile) system and DGEBA/MDA/SN/HQ(hydroquinone) system was studied by Kissinger equation and Fractional life method through DSC in the temperature range of 85∼150$^{\circ}C$. As cure temperature was increased, reaction rate increased and reaction order was almost constant. The reaction rate of the system with HQ as a catalyst was more higher and activation energy of that was lower about 20% than those of the system without HQ. Starting temperature of cure reaction for DGEBA/MDA/SN/HQ system decreased about 30$^{\circ}C$ than that of DGEBA/MDA/SN system.

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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.

Study on Thermal Decomposition of Korean Diaspore (국내산 다이아스포아의 열분해에 관한 연구)

  • 이헌수;손명모;박희찬
    • Journal of the Korean Ceramic Society
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    • v.24 no.4
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    • pp.307-312
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    • 1987
  • The investigation has been performed to study thermal dehydration of Song-sug, Pyung-il-do and Chung-mu diapore in Korea. Thermal analysis of Korean diaspore showed two steps of dehydration by dispore and kaolinite. The activation energy of dehydration reation of each diaspore was calculated by kissinger's method, and the results obtained were 63.608, 37.867 and 54.885Kcal/mol, respectively.

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