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

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CHARACTERIZATION OF $YBa_2Cu_3O_{7-x}$ MADE BY A SOL-GEL PROCESS USING NITRATE SALTS AND SODIUM HYDROXIDE (질산염(窒酸鹽)과 수산화(水酸化)나트륨을 써서 졸-겔 법(法)으로 만든 $YBa_2Cu_3O_{7-x}$의 특성분석(特性分析))

  • Kim, Bong-Heup;Kang, Hyung-Boo;Kim, Hyun-Teak
    • Proceedings of the KIEE Conference
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    • 1990.11a
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    • pp.143-149
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    • 1990
  • A sol-gel processing of $YBa_2Cu_3O_{7-x}$ superconductor using metal nitrate salts and sodium hydroxide as the starting materials has been investigated because of the need to produce pure, hompgeneous superconducting materials. Since the precipitation of barium hydroxides can be obtained only at high basicities, the process has to be carried out Ca. pH 13 to get the simultaneous coprecipitation with the other metal hydroxides. The involved reaction mechanisms were investigated and intermediate and final products were characterized by means of thermogravimetric analysis(TGA), infra-red(IR) spectroscopy, X-ray diffraction(XRD) analysis, scanning electron microscopy(SEM), thermal mechanical analysis(TMA) and electrical measurement.

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Synthesis and Characterization of Fluorinated Polybenzimidazole Proton Exchange Membranes for Fuel Cell (연료전지용 불소화 폴리벤즈이미다졸 양성자 교환 멤브레인 합성 및 특성평가)

  • KIM, AE RHAN
    • Transactions of the Korean hydrogen and new energy society
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    • v.28 no.1
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    • pp.24-29
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    • 2017
  • A fluorinated polybenzimidazole (FPBI) was synthesized from 3,3-diaminobenzidine (DAB) of tetraamine, 2,2-bis(4-carboxyphenyl)hexafluoropropane of aromatic biscarboxylic acid, and 4,4-sulfonyldibenzoic acid of aromatic biscarboxylic acid in polyphosphoric acid (PPA). A FPBI was easily cast and made into clear films. The structure of condensation polymers and corresponding membranes were analyzed using GPC (gel permeation chromatography), $^1H$-NMR ($^1H$ nuclear magnetic resonance) and FT-IR (fourier transform infrared). TGA (thermogravimetric analysis) analysis showed that the prepared membranes were thermally stable, so that elevated temperature fuel cell operation would be possible. The proton conductivity of the FPBI membranes increased with increasing temperatures in the polymer. A FPBI membrane has a maximum ion conductivity of 45 mS/cm at $90^{\circ}C$ and 100% relative humidity.

Analysis on Activation Energy Measurement and Application of Nuclear Equipment Non-metallic Materials (원전기기 비금속재료의 활성화에너지 측정 및 적용성 분석)

  • Bhang, Keug-Jin;Hong, Jun-Hee
    • Journal of Power System Engineering
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    • v.20 no.4
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    • pp.38-43
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    • 2016
  • Safety-related equipments of Nuclear Power Plants(NPP) have to perform environmental qualification test in accordance with IEEE-323 standards. However, non-metallic materials replace new one regularly instead of the test because they are considered as consumable parts. In this study, the seven kinds of non-metallic materials are selected and their activation energy was experimentally evaluated with uncertainty analysis by using thermogravimetric analyzer(TGA). In order to obtain activation energy of non-metallic materials, mass difference, temperature raising rate and conversion rate on the specimen are analyzed. It is postulated that the three experiment conditions are important to get a reliable activation energy. This postulate was experimentally confirmed using Arrhenius equation and Flynn-Wall-Ozawa analysis.

Preparation of multi-component ceramic proton conductors for intermediate temperature fuel cell (중온형 연료전지를 위한 다성분계 세라믹 수소이온 전도체 제조)

  • Lim, Byeong-mu;Seo, Dong-ho;Park, Sang-sun;Lee, Hong-yeon;Shul, Yong-Gun
    • 한국신재생에너지학회:학술대회논문집
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    • 2009.06a
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    • pp.410-411
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    • 2009
  • The multi-component ceramic proton conductor, $BaZr(Y)O_3-SiO_2-TiO_2-ZrO_2$ (BZY-STZ) and $LaPO_4-SiO_2-TiO_2-ZrO_2$ (LP-STZ), were synthesized by micro-emersion and sol-gel technique. The characterization of proton conductors were carried out using X-ray diffraction(XRD), thermogravimetric analysis(TGA), differential thermal analysis(DTA), impedance analysis. The proton conductors indicate the possibility of application for the intermediate temperature up to $700^{\circ}C$.

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Thermal Analysis of Mica/Epoxy Composites used In Generator Stator Windings (발전기 고정자 권선에서 사용되는 마이카/에폭시의 열적 분석)

  • 김희동;김태완;김정훈
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1997.04a
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    • pp.330-333
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    • 1997
  • The thermal impact of mica/epoxy paper(130${\mu}{\textrm}{m}$) is investigated using XRD, DSC and TGL X-ray diffraction(XRD) analysis was performed to know the position and structure of mica crystal in insulation materials. A differential scanning calorimeter(DSC) was used to measure glass transition temperature and excess enthalphy of the composite materials that had been subjected to thermal aging. The glass transition temperature(T$_{g}$) measured by DSC is observed at 95.43$^{\circ}C$ and 113.43$^{\circ}C$, respectively. The T$_{g}$ also increases with increased aging time. Measurements performed by TGA(thermogravimetric analysis) have showed that weight loss profile of sound specimens are lower than those aged.ged.

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Phosgen-free Synthesis of Oligoureas Having Amino End-groups: Their Application to the Synthesis of Poly(urea-imide)

  • Chang, Ji-Young;Kim, Beom-Jin
    • Fibers and Polymers
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    • v.3 no.2
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    • pp.55-59
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    • 2002
  • The thermal reaction of acetoacetanilide in the presence of aniline or phenol yielded carbanilide in quantitative yields. This reaction was applied to the synthesis of polyurea. Bisacetoacetamides were prepared from diamines and diketene in DMF. They were thermally polymerized in the presence of phenol or a diamine (6FDA) to yield polyureas of low molecular weights. The polymers were soluble in DMSO and NMP. $^1{H-NMR}$ analysis showed that they had amino group terminated structures. Poly(urea-imide) was synthesized by the reaction of an oligourea diamine with pyromellitic dianhydride in NMP. The concentration of terminal amino groups was determined by an acid-base titration. The thermal property of poly(urea-imide) was evaluated by thermogravimetric analysis (TGA). Initial decompisition took place at 332-$350^{\circ}C$.

The Use of Pistachio Pollen for the Production of Nanostructured Porous Nickel Oxide

  • Atalay, F.E.;Yigit, E.;Biber, Z.S.;Kaya, H.
    • Nano
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    • v.13 no.12
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    • pp.1850143.1-1850143.9
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    • 2018
  • Natural biotemplates - such as bacteria, fungi and viruses - are used in nanostructured metal oxide production. The pollen can be found abundantly in nature, and their microcapsules can be easily isolated from the pollen by chemical treatments. To date, pollen microcapsules are mostly used as drug carriers and catalytic agent templates. In the present study, nanoporous-structured nickel oxide is produced using Pistachio pollen microcapsules. The raw pollen, chemically treated pollen and metal-coated pollen were characterized using scanning electron microscopy, Brunauer-Emmett-Teller (BET) surface area analysis, thermogravimetric analysis (TGA), differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. The natural Pistachio pollen which were procured from Gaziantep, Turkey, are spherical, with a diameter of approximately $23{\mu}m$. The maximum surface area obtained for nickel oxide-coated microcapsules is $228.82m^2/g$. This result shows that Pistachio pollen are an excellent candidate for the production of porous nanostructured materials for supercapacitor electrodes.

Thermal Characteristics of LaMnO3 Non-isothermal Synthesis Reaction (LaMnO3 비등온 합성반응의 열적특성)

  • Jeon, Jong Seol;Lee, Jung Hun;Yoon, Chang Hyeok;Yoo, Dong Jun;Lim, Dae Ho;Kang, Yong
    • Korean Chemical Engineering Research
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    • v.54 no.3
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    • pp.404-409
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    • 2016
  • Thermal Characteristics and kinetic parameters of $LaMnO_3$ synthesis reaction were investigated by means of TGA (Thermogravimetric analysis) at non-isothermal heating conditions (5.0, 10.0, 15.0 and 20.0 K/min). The reaction was occurred rapidly at 450~600K (X=0.4~0.7) depending on the heating rate. Activation energy for the synthesis of $LaMnO_3$ from the precursor, which was determined by different method such as Friedman, Ozawa-Flynn-Wall and Vyazovkin methods, was in the range of 23~243 kJ/g-mol depending on the fractional conversion level and estimation method. The reaction order decreased with increasing heating rate and fractional conversional level. The average reaction order was 4.50 in case of X=0.1~0.3, while it was 1.87 in case of X=0.7~0.9, respectively. The value of frequency factor of reaction rate increased with inceasing heating rate and fractional conversion level. The aveage value of frequency factor was 205.6 ($min^{-1}$) when X=0.1~0.3, while it was 475.2 ($min^{-1}$) when X=0.7~0.9, respectively.

Study on the Pyrolysis Kinetics of RDF(Refuse Derived Fuel) with Thermogravimetric Analysis (열중량 분석 기법을 통한 RDF의 열분해 특성 조사)

  • Kim, Dong-Won;Lee, Jong-Min;Kim, Jae-Sung
    • Korean Chemical Engineering Research
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    • v.47 no.6
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    • pp.676-682
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    • 2009
  • Devolatilization of the Refuse Derived Fuel(RDF) which is produced at WonJu in Korea was characterized in air atmosphere with variation of heating rate(10, 20 and $30^{\circ}C/min$) in TGA. The results of TG Analysis have shown that the pyrolysis and char combustion of the RDF occurred in the range of $350{\sim}700^{\circ}C$ depending on the heating rate. Activation energy of the RDF which was determined by using Friedman and Ozawa-Flynn-Wall method was in the range of 14.44~18.40 kcal/mol. Also, reaction order(n) and pre-exponential factors(A) were 1.219 and $3.02{\times}10^5$ by using Friedman method, respectively. In order to find out the devolatilization mechanism of the RDF, twelve solid-state mechanisms defined by Coats Redfern Method were tested. The results of the Coats Redfern Method have shown that chemical reaction is the effective mechanism by comparison with the value of the activation energy which was derived from the Friedman and Flynn-Wall-Ozawa method and correlation coefficient from twelve solid-state mechanisms of Coats Redfern Method. The solid state decomposition mechanism of the RDF was found to be a decelerated $F_1$ type, random nucleation with one nucleus on the individual particle.

Pyrolysis and Combustion Characteristics of an Oriental Oak Leaf (굴참나무 잎의 열분해 및 연소 특성 연구)

  • Seo, Young-Hoon;Park, Jin-Mo;Lee, Myung-Wook;Kim, Jin-Soo;Kim, Seung-Soo
    • Applied Chemistry for Engineering
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    • v.21 no.5
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    • pp.575-580
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    • 2010
  • Forest fires in Korea, having forest coverage of 70%, have kept increasing in number and scale since the middle of 1990's. Although deposited fallen leaves in forests such as herbaceous plants, conifers, and broadleaf trees are used as a medium for forest fires, the pyrolysis and combustion characteristics of the various species of trees are hardly studied. Oriental oak is the representative broadleaf tree in domestic forests, and pyrolysis and combustion of oriental oak leaf were carried out by thermogravimetic analysis (TGA). The leaf of oriental oak was ignited at $239^{\circ}C$ whereas pyrolysis started at $250^{\circ}C$. The corresponding kinetic parameters including activation energy and pre-exponential factor were determined by differential method over the degree of conversions. The values of activation energies for pyrolysis were increased as the conversion increases from 10% to 80%, whereas those of values were decreased during combustion.