• 제목/요약/키워드: Thermal Gravimetric Analysis

검색결과 154건 처리시간 0.032초

목질계 바이오매스로부터 가스화에 의한 합성가스 제조 연구 (Synthesis Gas Production from Gasification of Woody Biomass)

  • 조원준;모용기;송택용;백영순;김승수
    • 한국수소및신에너지학회논문집
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    • 제21권6호
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    • pp.587-594
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    • 2010
  • Hydrogen is an alternative fuel for the future energy which can reduce pollutants and greenhouse gases. Synthesis gas has played an important role of synthesizing the valuable chemical compounds, for example methanol, DME and GTL chemicals. Renewable biomass feedstocks can be potentially used for fuel and chemicals. Current thermal processing techniques such as fast pyrolysis, slow pyrolysis, and gasification tend to generate products with a large slate of compounds. Lignocellulose feedstocks such as forest residues are promising for the production of bio-oil and synthesis gas. Pyrolysis and gasification was investigated using thermogravimetric analyzer (TGA) and bubbling fluidized bed gasification reactor to utilize forest woody biomass. Most of the materials decomposed between $320^{\circ}C$ and $380^{\circ}C$ at heating rates of $5{\sim}20^{\circ}C$/min in thermogravimetric analysis. Bubbling fluidized bed reactor was used to study gasification characteristics, and the effects of reaction temperature, residence time and feedstocks on gas yields and selectivities were investigated. With increasing temperature from $750^{\circ}C$ to $850^{\circ}C$, the yield of char decreased, whereas the yield of gas increased. The gaseous products consisted of mostly CO, $CO_2$, $H_2$ and a small fraction of $C_1-C_4$ hydrocarbons.

Preparation of Anatase TiO2 Thin Films with (OiPr)2Ti(CH3COCHCONEt2)2 Precursor by MOCVD

  • Bae, Byoung-Jae;Lee, Kwang-Yeol;Seo, Won-Seok;Miah, Md. Arzu;Kim, Keun-Chong;Park, Joon T.
    • Bulletin of the Korean Chemical Society
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    • 제25권11호
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    • pp.1661-1666
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    • 2004
  • The reaction of titanium tetraisopropoxide with 2 equiv of N,N-diethyl acetoacetamide affords Ti($O^iPr)_2(CH_3COCHCONEt_2)_2$ (1) as colorless crystals in 80% yield. Compound 1 is characterized by spectroscopic (Mass and $^1H/^{13}C$ NMR) and microanalytical data. Molecular structure of 1 has been determined by a single crystal X-ray diffraction study, which reveals that it is a monomeric, cis-diisopropoxide and contains a six coordinate Ti(IV) atom with a cis($CONEt_2$), trans($COCH_3$) configuration (1a) in a distorted octahedral environment. Variable-temperature $^1H$ NMR spectra of 1 indicate that it exists as an equilibrium mixture of cis, trans (1a) and cis, cis (1b) isomers in a 0.57 : 0.43 ratio at -20$^{\circ}C$ in toluene-$d_8$ solution. Thermal properties of 1 as a MOCVD precursor for titanium dioxide films have been evaluated by thermal gravimetric analysis and vapor pressure measurement. Thin films of pure anatase titanium dioxide (after annealing above 500$^{\circ}C$ under oxygen) have been grown on Si(100) with precursor 1 in the substrate temperature range of 350- 500$^{\circ}$ using a bubbler-based MOCVD method.

Influence of fly ash and GGBFS on the pH value of cement mortar in different curing conditions

  • Shafigh, Payam;Yousuf, Sumra;Ibrahim, Zainah;Alsubari, Belal;Asadi, Iman
    • Advances in concrete construction
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    • 제11권5호
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    • pp.419-428
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    • 2021
  • The pH of cement-based materials (CBMs) is an important factor for their durability, sustainability, and long service life. Currently, the use of supplementary cementitious materials (SCMs) is becoming mandatory due to economic, environmental, and sustainable issues. There is a decreasing trend in pH of CBMs due to incorporation of SCMs. The determination of numerical values of pH is very important for various low and high volume SCMs blended cement mortars for the better understanding of different defects and durability issues during their service life. In addition, the effect of cement hydration and pozzolanic reaction of SCMs on the pH should be determined at initial and later ages. In this study, the effect of low and high-volume fly ash (FA) and ground granulated ballast furnace slag (GGBFS) cement mortars in different curing conditions on their pH values has been determined. Thermal gravimetric analysis (TGA) was carried out to support the findings from pH measurements. In addition, thermal conductivity (k-value) and strength activity indices of these cement mortars were discussed. The results showed that pH values of all blended cement mortars were less than ordinary Portland cement (OPC) mortar in all curing conditions used. There was a decreasing tendency in pH of all mortars with passage of time. In addition, the pH of cement mortars was not only dependent on the quantity of Ca(OH)2. The effect of adding SCMs on the pH value of cement mortar should be monitored and measured for both short and long terms.

산화조건에서 $PrCl_3$의 열적거동 (Thermal behavior of $PrCl_3$ in an oxidizing condition)

  • 은희철;양희철;조용준;이한수;김인태
    • 방사성폐기물학회지
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    • 제7권4호
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    • pp.207-212
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    • 2009
  • 본 연구에서는 산화조건하 LiCl-KCl 공융염내에서 란탄계 염화물의 하나인 $PrCl_3$의 열적거동을 살펴보았다. 먼저 산소를 주입하면서 $PrCl_3$의 열중량분석(TGA; thermogravimetric analysis)을 실시하였고, 이 때 얻어진 결과들을 바탕으로, 산소분산법을 이용하여 온도에 따른 LiCl-KCl 공융염내 $PrCl_3$의 산화실험을 수행하였다. $PrCl_3$의 열중량분석 결과에 따르면, 약 $380^{\circ}C$까지 $PrCl_3$에서 염소의 해 리가 급격하게 발생되었고 약 $600^{\circ}C$에서 $PrCl_3$가 PrOCl로 전환되는 반응이 종료되는 것으로 확인되었다. 산소분산법에 의한 LiCl-KCl 공융염내 $PrCl_3$의 열적거동은 산화조건에서 열중량분석시 나타난 $PrCl_3$의 열적거동과 유사하였고, 발생된 PrOCl은 공융염내에서 불용성 화합물로써 바닥으로 침전하였다. 산소분산법에 의한 공융염내 $PrCl_3$의 PrOCl로의 전환은 $650^{\circ}C$ 이상의 온도에서 활발하게 진행되었고, 이 때 발생되는 배기가스내 $Cl_2$의 농도분석을 통해 공융염내 $PrCl_3$의 전환상태를 예측할 수 있을 것으로 판단된다.

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NaCl/H3PO4 내염화 처리가 라이오셀 섬유의 열 안정 및 내산화 특성에 미치는 영향 (Effects of NaCl/H3PO4 Flame Retardant Treatment on Lyocell Fiber for Thermal Stability and Anti-oxidation Properties)

  • 김은애;배병철;이철위;전영표;이영석;인세진;임지선
    • 공업화학
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    • 제25권4호
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    • pp.418-424
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    • 2014
  • 본 연구에서는 NaCl/$H_3PO_4$ 혼합수용액을 사용하여 라이오셀 섬유의 내염화 처리를 수행하고 이에 따른 열 안정성과 내산화성의 향상 효과를 고찰하였다. 라이오셀 섬유를 다양한 공정조건으로 내염화 처리한 후 열 안정성과 내산화성을 측정 및 분석하고 그에 따른 메커니즘을 제시하였다. 실험결과, 내염화 처리된 라이오셀 섬유의 적분 열분해 온도(integral procedural decomposition temperature, IPDT)와 한계산소지수(limited oxygen index, LOI)는 약 23, 30% 증가하였으며, 활성화 에너지(activation energy, $E_a$) 값은 약 24% 향상된 것을 알 수 있었다. 이러한 결과는 $H_3PO_4$와 NaCl가 연소시 에스테르화 반응, 탈수소화 반응 및 C-C결합의 분해반응으로 char 형성을 촉진하고 섬유 표면에 형성된 탄소 층을 형성함으로써, 고분자 수지 내부로 산소와 열 공급을 물리적으로 차단하여 열 안정성과 내산화성이 향상된 것으로 판단된다. 이러한 결과를 바탕으로, NaCl/$H_3PO_4$ 혼합수용액을 이용한 내염화 처리 공정의 최적화된 인자 및 메커니즘을 제시하였고 열 안정성과 내산화성이 향상된 라이오셀을 성공적으로 제조하였다.

라이오셀의 열 안정 및 내산화 특성 향상을 위한 Na3PO4 내염화 처리 (Na3PO4 Flame Retardant Treatment on Lyocell Fiber for Thermal Stability and Anti-oxidation Properties)

  • 김형기;김은애;이영석;인세진
    • 한국화재소방학회논문지
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    • 제29권2호
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    • pp.25-32
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    • 2015
  • 라이오셀 섬유의 열 안정성과 내산화성을 향상시키기 위하여 $Na_3PO_4$ 수용액으로 내염화 처리를 실시하였다. 다양한 공정조건으로 라이오셀 섬유를 내염화 처리한 후 열 안정성과 내산화성을 측정 및 분석하고 그에 따른 메커니즘을 고찰하였다. 내염화 처리된 라이오셀 섬유의 적분 열분해 온도(integral procedural decomposition temperature, IPDT)와 활성화 에너지(activation energy, $E_a$)값은 각각 약 30, 160%로 향상된 것을 알 수 있었다. 이는 $Na_3PO_4$가 연소 시 에스테르화 반응, 탈수소화 반응 및 C-C 결합의 분해반응으로 char 형성을 촉진하여 섬유 표면에 보호층을 형성하여, 고분자 수지 내부로 산소와 열 공급을 물리적으로 차단하여 열 안정성과 내산화성이 향상된 것으로 판단된다. 이러한 결과를 바탕으로, $Na_3PO_4$ 수용액을 이용하여 열 안정성과 내산화성이 향상된 라이오셀을 제조하였고, 내염화 처리공정의 최적화된 인자 및 메커니즘을 고찰하였다.

나노 섬유를 혼합한 시멘트 페이스트의 미세구조와 강도에 대한 연구 (A Study about the Strength and Microstructure of Hardened Cement Pastes Including Nanofibers)

  • 응유옌 트리;김정중
    • 대한토목학회논문집
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    • 제40권2호
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    • pp.177-182
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    • 2020
  • 본 연구에서는 시멘트 페이스트에 혼합된 나노 섬유가 경화된 시멘트페이스트의 압축강도와 인장강도에 미치는 영향을 연구하였다. 2종류의 나노 섬유를 사용하였다. 나일론 66 나노 섬유와 카본 나노 튜브로 보강된 나일론 66 나노 섬유를 전기방사로 제작하여 시멘트 파우더에 각각 혼합하였다. 물-시멘트비 0.5의 시멘트 페이스트 시편을 제작하고 28일간 양생하였다. 실험 결과, 나노섬유의 혼합이 시멘트 페이스트 시편의 압축강도와 인장강도를 증가시킴을 확인하였다. 나노 섬유의 보강 매카니즘을 확인하기 위해 주사전자현미경(SEM) 분석, 전계방사 투과전자 현미경(FE-TEM) 분석 및 열 중량 분석(TGA)을 수행하여 나노섬유를 포함한 시멘트 페이스트의 미세 구조를 분석하였다.

A STUDY ON OXIDATION TREATMENT OF URANIUM METAL CHIP UNDER CONTROLLING ATMOSPHERE FOR SAFE STORAGE

  • Kim, Chang-Kyu;Ji, Chul-Goo;Bae, Sang-Oh;Woo, Yoon-Myeoung;Kim, Jong-Goo;Ha, Yeong-Keong
    • Nuclear Engineering and Technology
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    • 제43권4호
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    • pp.391-398
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    • 2011
  • The U metal chips generated in developing nuclear fuel and a gamma radioisotope shield have been stored under immersion of water in KAERI. When the water of the storing vessels vaporizes or drains due to unexpected leaking, the U metal chips are able to open to air. A new oxidation treatment process was raised for a long time safe storage with concepts of drying under vacuum, evaporating the containing water and organic material with elevating temperature, and oxidizing the uranium metal chips at an appropriate high temperature under conditions of controlling the feeding rate of oxygen gas. In order to optimize the oxidation process the uranium metal chips were completely dried at higher temperature than $300^{\circ}C$ and tested for oxidation at various temperatures, which are $300^{\circ}C$, $400^{\circ}C$, and $500^{\circ}C$. When the oxidation temperature was $400^{\circ}C$, the oxidized sample for 7 hours showed a temperature rise of $60^{\circ}C$ in the self-ignition test. But the oxidized sample for 14 hours revealed a slight temperature rise of $7^{\circ}C$ representing a stable behavior in the self-ignition test. When the temperature was $500^{\circ}C$, the shorter oxidation for 7 hours appeared to be enough because the self-ignition test represented no temperature rise. By using several chemical analyses such as carbon content determination, X-ray deflection (XRD), Infrared spectra (IR) and Thermal gravimetric analysis (TGA) on the oxidation treated samples, the results of self-ignition test of new oxidation treatment process for U metal chip were interpreted and supported.

Variation in optical, dielectric and sintering behavior of nanocrystalline NdBa2NbO6

  • Mathai, Kumpamthanath Chacko;Vidya, Sukumariamma;Solomon, Sam;Thomas, Jijimon Kumpukattu
    • Advances in materials Research
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    • 제2권2호
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    • pp.77-91
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    • 2013
  • High quality nanoparticles of neodymium barium niobium ($NdBa_2NbO_6$) perovskites have been synthesized using an auto ignition combustion technique for the first time. The nanoparticles thus obtained have been characterized by powder X-ray diffraction, thermo gravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy and transmission electron microscopy. UV-Visible absorption and photoluminescence spectra of the samples are also recorded. The structural analysis shows that the nano powder is phase pure with the average particle size of 35 nm. The band gap determined for $NdBa_2NbO_6$ is 3.9 eV which corresponds to UV-radiation for optical inter band transition with a wavelength of 370nm. The nanopowder could be sintered to 96% of the theoretical density at $1325^{\circ}C$ for 2h. The ultrafine cuboidal nature of nanopowders with fewer degree of agglomeration improved the sinterability for compactness at relatively lower temperature and time. During the sintering process the wide band gap semiconducting behavior diminishes and the material turns to a high permittivity dielectric. The microstructure of the sintered surface was examined using scanning electron microscopy. The striking value of dielectric constant ${\varepsilon}_r=43$, loss factor tan ${\delta}=1.97{\times}10^{-4}$ and the observed band gap value make it suitable for many dielectric devices.

Mass Balance Method for Purity Assessment of Organic Reference Materials: for Thermolabile Materials with LC-UV Method

  • Lee, Joonhee;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • 제35권11호
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    • pp.3275-3279
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    • 2014
  • A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.