• Title/Summary/Keyword: Isothermal TGA

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Kinetics of Thermal Degradation of Polypropylene/Nanoclay/Wood Flour Nanocomposites

  • Mohan, D. Jagan;Lee, Sun-Young;Kang, In-Aeh;Doh, Geum-Hyun;Park, Byung-Dae;Wu, Qinglin
    • Journal of the Korean Applied Science and Technology
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    • v.24 no.3
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    • pp.278-286
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    • 2007
  • As a part of enhancing the performance of wood-plastic composites (WPC), polypropylene (PP)/ nanoclay (NC)/ wood flour (WF) nanocomposites were prepared using melt blending and injection molding process to evaluate their thermal stability. Thermogravimetric analysis (TGA) was employed to investigate thermal degradation kinetics of the nanocomposites both dynamic and isothermal conditions. Dynamic scans of the TGA showed an increased thermal stability of the nanocomposites at moderate wood flour concentrations (up to 20 phr, percentage based on hundred percent resin) while it decreased with the addition of 30 phr wood flour. The activation energy $(E_a)$ of thermal degradation of nanocomposites increased when nanoclay was added and the concentration of wood flour increased. Different equations were used to evaluate isothermal degradation kinetics using the rate of thermal degradation of the composites, expressed as weight loss (%) from their isothermal TGA curves. Degradation occurred at faster rate in the initial stages of about 60 min., and then proceeded in a gradual manner. However, nanocomposites with wood flour of 30 phr heated at $300^{\circ}C$ showed a drastic difference in their degradation behavior, and reached almost a complete decomposition after 40 min. of the isothermal heating. The degree of decomposition was greater at higher temperatures, and the residual weight of isothermal degradation of nanocomposites greatly varied from about 10 to 90%, depending on isothermal temperatures. The isothermal degradation of nanocomposites also increased their thermal stability with the addition of 1 phr nanoclay and of wood flour up to 20 phr. But, the degradation of PP100/NC1/MAPP3/WF30 nanocomposites with 30 phr wood flour occurs at a faster rate compared to those of the others, indicating a decrease in their thermal stability.

Phase Transformation and Thermoelectric Properties of N-tyre β Processed by Mechanical Alloying (기계적 합금화로 제조한 N형 β의 상변화 및 열전 특성)

  • Eo, Sun-Cheol
    • Korean Journal of Materials Research
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    • v.12 no.5
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    • pp.375-381
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    • 2002
  • N-type ${\beta}-FeSi_2$ with a nominal composition of $Fe_{0.98}Co_{0.02}Si_2$ powders has been produced by mechanical alloying process and consolidated by vacuum hot pressing. As-milled powders were of metastable state and fully transformed to ${\beta}-FeSi_2$ phase by subsequent isothermal annealing. However, as-consolidated $Fe_{0.98}Co_{0.02}Si_2$ consisted of untransformed mixture of ${\alpha}-Fe_2Si_ 5$ and $\varepsilon$-FeSi phases. Isothermal annealing has been carried out to induce the transformation to a thermoelectric semiconducting ${\beta}-FeSi_2$ phase. The transformation behavior of ${\beta}-FeSi_2$ was investigated by utilizing DTA, a modified TGA under magnetic field, SEM, and XRD analyses. Isothermal annealing at $830^{\circ}C$ in vacuum led to the thermoelectric semiconducting ${\beta}-FeSi_2$ phase transformation, but some residual metallic $\alpha$ and $\varepsilon$ phases were unavoidable even after prolonged annealing. Thermoelectric properties were remarkably improved by isothermal annealing due to the transformation from metallic $\alpha$ and $\varepsilon$ phases to semiconducting phases.

Non-isothermal TGA Study on Thermal Degradation Kinetics of ACM Rubber Composites (비등온 TGA를 이용한 ACM 고무복합재료의 열분해 거동 연구)

  • Ahn, WonSool;Lee, Hyung Seok
    • Elastomers and Composites
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    • v.48 no.2
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    • pp.161-166
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    • 2013
  • Thermal degradation behavior of chlorine cure-site ACM and carboxylic cure-site ACM rubbers was studied by non-isothermal TGA thermal analysis. Carboxylic cure-site ACM rubber exhibited comparatively more thermally stable than chlorine cure-site ACM, showing higher peak temperature, at which maximum reaction rate occurred. Activation energies from Kissinger method were calculated as 118.6 kJ/mol for the chlorine cure-site ACM and 105.5 kJ/mol for the carboxylic cure-site ACM, showing similar values from Flynn-Wall-Ozawa analysis over the conversion range of 0.1~0.2. From the analysis of the reaction order change, both samples seemed thermally decomposed through the multiple reaction mechanism as is the common rubber materials.

A Study on the Thermal Life-Time Expectation of a NR Rubber Material using Isothermal TGA and TMA (등온 TGA 및 TMA를 이용한 NR고무소재의 내열수명 예측에 관한 연구)

  • Ahn, Won-Sool;Park, Ki-Ho
    • Elastomers and Composites
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    • v.44 no.3
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    • pp.269-273
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    • 2009
  • A study on the life-time expectation of a CR-modified NR rubber composite through the change of thermal degradation characteristics was performed using both isothermal thermogravimetric analysis (TGA) and thermomechanical analysis (TMA). Master curves at reference temperature of $90^{\circ}C$ could be obtained with shift factor $a_T$, which was determined empirically using Time-Temperature Superposition Principle (TTSP). Activation energies could be calculated from the slope of Arrhenius plot of shift factor and showed similar values of $E_{a,TGA}$= 41.2 and $E_{a,TMA}$= 54.5 kJ/mol, respectively. It was considered from the results that chemical degradation resulting weight loss of the sample might be closely related to a physical degradation such as the dimensional change of the sample.

Study on the Non-isothermal Crystallization Behavior of Polypropylene/Corn Starch-MB Blends (폴리프로필렌/옥수수전분 블렌드의 비등온결정화 거동 연구)

  • Kim, Youn-Cheol
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.9 no.5
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    • pp.1125-1129
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    • 2008
  • Polypropylene (PP)/corn starch master batch(starch-MB) blends with different PP compositions of 90, 80, 70, and 60 wt% were prepared by melt compounding at $200^{\circ}C$, using lab scale Brabender mixer. The chemical structures, thermal properties and non-isothermal crystallization behavior of the PP/starch-MB blends were investigated by FT-infrared spectrometry (FT-IR), differential scanning calorimetry (DSC), and thermogravimetric analyzer (TGA). The fabrication of the PP/starch-MB blend was confirmed by the existence of hydroxy group in FT-IR spectrum. There was no district change in melting temperature and melting enthalpy, and TGA curve indicates a decrease in degradation temperature with starch-MB content. The non-isothermal crystallization process was analyzed using by Avrami equation. The Avrami exponents were in the range of 2.71-3.97 for PP and 1.48-1.99 for PP/starch-MB blonds. The activation energies calculated by Kissinger method were 233 kJ/mol for PP, 484 kJ/mol for PP90, 541 kJ/mol for PP80, 553 kJ/mol for PP70, and 422 kJ/mol for PP60.

A Study on the Development of CVD Precursors VI-Thermal Properties of Co(III) β-Diketonates

  • Lee, Han-Bin;Lee, Choong-Hyuk;Oh, In-Sook;Lee, Ik-Mo
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.891-894
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    • 2010
  • Thermal properties of a series of Co $\beta$-diketonates have been systematically investigated and it is found that tris(3,5-heptanedionato) cobalt(III) ($Co(hd)_3$) with the lowest melting point among them can be a better precursor than tris(2,2,6,6-tetramethyl-3,5-heptanedionato cobalt(III) ($Co(tmhd)_3$), one of the most popular precursors to date, under suitable conditions. Isothermal TGA study shows that $Co(hd)_3$ would work better at higher temperature, while $Co(dmhd)_3$ would be a better precursor at lower temperature.

An Experimental Study on Measurement of the Reaction Order of a Liquid Fuel with Various Components (혼합 액체연료의 화학반응차수 계측에 관한 실험적 연구)

  • Choi, Hyo-Hyun;Lim, Jun-Seok;Kim, Chul-Jin;Sohn, Chae-Hoon
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2011.04a
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    • pp.421-424
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    • 2011
  • Thermal Analyses are conducted to measure various factors of a liquid fuel required for numerical analysis. Thermal Analyses are divided into two different methods of TGA (Thermo Gravimetric Analysis) and DSC (Differential Scanning Calorimetry). Non-isothermal experimental results are analyzed using by TGA. The results are filtered by a Freeman Carroll method. At the same time, chemical parameters of unknown liquid fuel, activation temperature and reaction order are measured to 6128.2 K and 1.4, respectively. Furthermore, the parameters can be obtained by various mathematical methods. It is found that tha parameters depend on the processing method.

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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.

Pyrolysis Properties of Lignins Extracted from Different Biorefinery Processes

  • Lee, Hyung Won;Jeong, Hanseob;Ju, Young-Min;Youe, Won-Jae;Lee, Jaejung;Lee, Soo Min
    • Journal of the Korean Wood Science and Technology
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    • v.47 no.4
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    • pp.486-497
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    • 2019
  • The non-isothermal and isothermal pyrolysis properties of H lignin and P lignin extracted from different biorefinery processes (such as supercritical water hydrolysis and fast pyrolysis) were studied using thermogravimetry analysis (TGA) and pyrolyzer-gas chromatography/mass spectrometry (Py-GC/MS). The lignins were characterized by ultimate/proximate analysis, FT-IR and GPC. Based on the thermogravimetry (TG) and derivative thermogravimetry (DTG) curves, the thermal decomposition stages were obtained and the pyrolysis products were analyzed at each thermal decomposition stage of non-isothermal pyrolysis. The isothermal pyrolysis of lignins was also carried out at 400, 500, and $600^{\circ}C$ to investigate the pyrolysis product distribution at each temperature. In non-isothermal pyrolysis, P lignin recovered from a fast pyrolysis process started to decompose and produced pyrolysis products at a lower temperature than H lignin recovered from a supercritical water hydrolysis process. In isothermal pyrolysis, guaiacyl and syringyl type were the major pyrolysis products at every temperature, while the amounts of p-hydroxyphenyl type and aromatic hydrocarbons increased with the pyrolysis temperature.

Non-isothermal pyrolysis of cashew shell cake-bituminous coal blends

  • Park, Yoon Hwa;Park, Ho Young;Kim, Hyun Hee;Park, Sang Bin
    • Environmental Engineering Research
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    • v.23 no.2
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    • pp.121-128
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    • 2018
  • This paper describes the non-isothermal pyrolysis of cashew shell cake (CSC) - bituminous coal blends. The blends exhibit two distinct stages in the thermogravimetric curves, which the first stage stems from CSC and the second one from the superposition of CSC and coal pyrolysis. The pyrolysis behavior of the blend was linearly proportional to the blending ratios. The overall behavior of the blends was evaluated in terms of the maximum rate of weight loss, characteristic temperatures, char yields, and the calculated and experimental thermogravimetric curves. The activation energies ranged up to 49 kJ/mol for the blends were obtained and used to evaluate the interaction in the blends. The present thermogravimetric study shows that there is no significant interaction between CSC and coal in the blends, and it was supported by the characteristic values which are linearly proportional to the weight percentages of cashew cake-shell in the blends. The no-interaction might be due to the fact that the main reaction zones are distinctively different for two constituents, so the additive rule is acceptable for describing pyrolysis behavior of the present blends.