• Title/Summary/Keyword: Thermogravimetric analysis (TGA)

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Thermal Behavior of LixCoO2 Cathode and Disruption of Solid Electrolyte Interphase Film

  • Doh, Chil-Hoon;Kim, Dong-Hun;Lee, Jung-Hun;Lee, Duck-Jun;Jin, Bong-Soo;Kim, Hyun-Soo;Moon, Seong-In;Hwang, Young-Gi;Veluchamy, Angathevar
    • Bulletin of the Korean Chemical Society
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    • v.30 no.4
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    • pp.783-786
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    • 2009
  • Thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and ion chromatography(IC) were employed to analyze the thermal behavior of $Li_xCoO_2$ cathode material of lithium ion battery. The mass loss peaks appearing between 60 and 125 ${^{\circ}C}$ in TGA and the exothermic peaks with 4.9 and 7.0 J/g in DSC around 75 and 85 ${^{\circ}C}$ for the $Li_xCoO_2$ cathodes of 4.20 and 4.35 V cells are explained based on disruption of solid electrolyte interphase (SEI) film. Low temperature induced HF formation through weak interaction between organic electrolyte and LiF is supposed to cause carbonate film disruption reaction, $Li_2CO_3\;+\;2HF{\rightarrow}\;2LiF\;+\;CO_2\;+\;H_2O$. The different spectral DSC/TGA pattern for the cathode of 4.5 V cell has also been explained. Presence of ionic carbonate in the cathode has been identified by ion chromatography and LiF reported by early researchers has been used for explaining the film SEI disruption process. The absence of mass loss peak for the cathode washed with dimethyl carbonate (DMC) implies ionic nature of the film. The thermal behavior above 150 ${^{\circ}C}$ has also been analyzed and presented.

Combustion Characteristics of High Moisture Indonesia Coal as a Pulverized Fuel at Thermal Power Plant (미분탄 화력발전소 연료로서 고수분 인도네시아탄의 연소특성)

  • Kim, Jae-Kwan;Lee, Hyun-Dong
    • Journal of the Korean Society of Combustion
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    • v.14 no.3
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    • pp.16-23
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    • 2009
  • It is strongly desired for coal-fired power plants to utilize not only low-rank coals with high moisture contents, but also lowering cost with diversifying fuel sources. In this study, combustion characteristics of low rank coal with high moisture, and standard pulverized coals are experimentally investigated using TGA (Thermogravimetric Analysis) and DTF (drop tube furnace). The coals tested are three kinds of coal with moisture content ranging from 8.32 to 26.82%. The results show that under the air combustion condition, the burn-out time at TGA rises as moisture content increases, and standard pulverized coal with 8.32% moisture content showed the lowest activation energy of 55.73 kJ/mol. In case of the high amount of moisture, the combustion efficiency decreases due to evaporation heat loss, and unburned carbon in ash produced at combustion process in DTF increased. Aslo, initial deformation temperature of slag attached in alumina tube of DTF decreased with lowering the crytallinity of anorthite and augite. To improve the combustion reactivity and efficiency, it is effective to upgrade through drying the high moisture coal to moisture level (less than 10%) of standard pulverized coal.

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A Kinetic Studies of Pyrolysis and Combustion of Sewage Sludge (하수 슬러지의 열분해 및 연소 Kinetics 연구)

  • Roh, Seon Ah
    • Resources Recycling
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    • v.23 no.6
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    • pp.47-53
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    • 2014
  • Effective treatment and energy conversion technologies are necessary due to the ban of the dumping of organic waste including the sewage sludge. In this study, the kinetics of pyrolysis and combustion were derived in a TGA and thermobalance reactor, which is essential for thermal conversion of sewage sludge to energy. Three steps are shown for the pyrolysis in TGA and the different pre-exponential factors and activation energies are derived depending on the temperature range. Three models of gassolid reaction were applied to the reaction kinetics analysis for the combustion of sewage sludge char and shrinking core model was an appropriated model. Apparent activation energy and pre-exponential factor were evaluated and the effect of oxygen partial pressure was examined.

Study on Flame Retardancy and Thermal Resistance Properties of Phenolic Foam and Polyurethane Foam (페놀 폼과 폴리우레탄 폼의 난연 및 내열성 연구)

  • Lee, Ju-Chan;Seo, Jung-Seok;Kim, Sang Bum
    • Journal of the Korean Institute of Gas
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    • v.17 no.1
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    • pp.35-41
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    • 2013
  • In this study, flame retardancy of polyurethane foam and phenolic foam were investigated by addition of phosphorous flame retardants. The thermal degradation behavior of polyurethane foam and phenolic foam in the presence of flame retardants has been studied by thermogravimetric analysis(TGA). Heat release rate(HRR), mean HRR, mass loss rate(MLR), total smoke released(TSR) and limited oxygen index(LOI) were tested by cone calorimeter. From the test results, Phenolic foam showed low HRR, MLR and TSR than polyurethane foam.

Effect of Crystal Form on Dissolution of Prednisolone (프레드니솔론의 용출에 미치는 결정형의 영향)

  • Sohn, Young-Taek;Do, Eui-Sun
    • Journal of Pharmaceutical Investigation
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    • v.33 no.2
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    • pp.99-103
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    • 2003
  • Four different crystal forms of prednisolone, two polymorphic forms and two pseudopolymorphic forms, were obtained by the recrystallization from different organic solvents under varying conditions. The isolated crystal forms were characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and X-ray powder diffraction (XRD). Form 1 was the most stable form that had the highest melting point and melt at $250.1^{\circ}C$. Form 2 was a monohydrate and Form 3 was a methanol solvate. The endothermic peak of Form 4 was shown at $230.2^{\circ}C$. When stored at different relative humidity over the period of 3 months, all of the modifications did not undergo transformation. The dissolution patterns of these four modifications were also checked in distilled water at $37{\pm}0.5^{\circ}C$, for 120 minutes. The dissolution rate of Form 4 was highest and those of Form 3, Form 2, Form 1 followed. Form 2, Form 3 and Form 4 had higher dissolution rate than Form 1.

Intercalation of Polycarbonate/Montmorillonite Nanocomposites (폴리카보네이트와 몬모릴로나이트 나노복합체의 층간삽입)

  • 이양훈;홍성권;윤광수;최일석;이성구
    • Polymer(Korea)
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    • v.25 no.6
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    • pp.818-825
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    • 2001
  • Polycarbonate(PC)/montmorillonite (MMT) nanocomposites were prepared by solution and melt mixing methods. A d-spacing of the nanocomposites was measured by an X-ray diffractometer. Neat montmorillonite (MMT-Na) and MMTs modified by dodecyl ammonium (MMT-DA) or dimethyl hydrogenated tallow 2-ethylhexyl ammonium (MMT-25A) were used. The d-spacing value of PC/MMT-25A and PC/MMT-DA was higher than that of PC/MMT-Na. The d-spacing increased from around 12 to $37AA$ depending on the mixing method. PC was more readily introduced to the gallery of MMT as the molecular weight of PC reduced and the mixing time increased. PC/MMT-25A showed higher thermal stability by thermogravimetric analysis (TGA) than PC/MMT-DA and PC/MMT-Na.

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Synthesis and Application of Oligo(3-Methylthiothiophene) Using Palladium Catalyst (Palladium 촉매를 이용한 Oligo(3-methylthiothiophene)의 합성과 응용)

  • Park, Sang-Ho;Jung, Moon-Young;Bae, Jin-Young
    • Polymer(Korea)
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    • v.31 no.6
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    • pp.469-473
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    • 2007
  • In this study, oligo(3-methylthiothiophene) was synthesized from thiophene derivative according to the method of reductive coupling using palladium catalyst. For the preparation of monomer, 3-methylthiothiophene was first synthesized through the metal-halogen exchange reaction of 3-bromothiophene with n-butyllithiuim, and the corresponding 2,5-dibromo-3-methylthiothiophene was formed by bromination. Their synthesis and characterization were determined by $^1H-NMR$ and ATR analyses. Thermal stability of the oligothiophene was monitored by thermogravimetric analysis (TGA). Thermal evaporation of the oligo(3-methylthiothiophene) on the substrate was attempted for OTFT applications.

Poly(lactic acid)/Wood Flour/Montmorillonite Nanocomposites (II) : Thermal properties

  • Kim, Jin-Sung;Lee, Sun-Young;Doh, Geum-Hyun;Kang, In-Aeh;Yoon, Ho-Gyu
    • Journal of the Korean Wood Science and Technology
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    • v.37 no.5
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    • pp.434-439
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    • 2009
  • This study investigates the thermal properties of nanocomposites prepared from poly(lactic acid) (PLA), wood flour (WF) and montmorillonite (MMT) by melt compounding with a twin screw extruder. In order to enhance the mechanical properties of PLA/WF composites, maleic anhydride grafted PLA (MAPLA) is synthesized as a compatibilizer. MAPLA prepared in the laboratory is characterized using FR-IR. From SEM microphotographs, the presence of MAPLA has a positive effect on the mechanical properties of WF-reinforced PLA composites. The addition of WF/MAPLA into neat PLA increased the glass transition temperature ($T_g$). The addition of 1 to 5 wt% MMT into PLA/WF/MAPLA composite decreases the $T_g$. The cold crystallization temperature ($T_{cc}$) was decreased by the addition of MMT. The MMT could act as effective nucleating sites of PLA crystallization. The thermal stability evaluated by thermogravimetric analysis (TGA) is improved with the contents of MMT up to 3 wt%.

A Comparative Study on Electron-Beam and Thermal Curing Properties of Epoxy Resins (에폭시 수지의 전자선 및 열경화 특성에 관한 연구)

  • 이재락;허건영;박수진
    • Polymer(Korea)
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    • v.26 no.1
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    • pp.80-87
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    • 2002
  • A comparative study using electron-beam(EB) and thermal curing techniques was carried out to determine the effect of cure behavior and thermal stability of epoxy resins. In this work, benzylquinoxalinium hexafluoroantimonate(BQH) was used as a latent cationic catalyst for an epoxy resin. According to the thermogravimetric analysis(TGA), the decomposed activation energy based on Coats-Redfern method was higher in the case of thermal curing technique. This could be interpreted in terms of slow thermal diffusion rate resulted from high crosslink density of the thermally cured epoxy resin. However, the increase of hydroxyl group in the epoxy resin cured by EB technique was observed in near-infrared spectroscopy(NIRS) measurements, resulting in improving the stable short aromatic chain structure, integral procedural decomposition temperature, and finally ductile properties for high impact strengths.

Synthesis and Characterization of Nickel(II) Tetraaza Macrocyclic Complex with 1,1-Cyclohexanediacetate Ligand

  • Lim, In-Taek;Kim, Chong-Hyeak;Choi, Ki-Young
    • Journal of the Korean Chemical Society
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    • v.62 no.6
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    • pp.427-432
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    • 2018
  • The reaction of [$[Ni(L)]Cl_2{\cdot}2H_2O$ (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[$14,4,0^{1.18},0^{7.12}$]docosane) with 1,1-cyclohexanediacetic acid ($H_2cda$) yields mononuclear nickel(II) complex, [$Ni(L)(Hcda^-)_2$] (1). This complex has been characterized by X-ray crystallography, electronic absorption, cyclic voltammetry and thermogravimetric analyzer. The crystal structure of 1 exhibits a distorted octahedral geometry with four nitrogen atoms of the macrocycle and two 1,1-cyclohexanediacetate ligands. It crystallizes in the triclinic system P-1 with a = 11.3918(7), b = 12.6196(8), $c=12.8700(8){\AA}$, $V=1579.9(2){\AA}^3$, Z = 2. Electronic spectrum of 1 also reveals a high-spin octahedral environment. Cyclic voltammetry of 1 undergoes one wave of a one-electron transfer corresponding to $Ni^{II}/Ni^{III}$ process. TGA curve for 1 shows three-step weight loss. The electronic spectra, electrochemical and TGA behavior of the complex are significantly affected by the nature of the axial $Hcda^-$ ligand.