• Title/Summary/Keyword: 시차 주사 열분석

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Formation of Mesoporous Membrane by Reverse Thermally induced Phase Separation (RTIPS) Process Using Flash Freezing (Mesoporous 막 제조를 위한 급냉법에 의한 역 열유도상전이공정)

  • Yeom, Choongkyun;Kim, Jiwon;Park, Heeyoung;Park, Seong Eun;Lee, Kee Yoon;Lee, Kew-Ho
    • Membrane Journal
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    • v.31 no.1
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    • pp.67-79
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    • 2021
  • Mesoporous polystyrene (PS) and polyethersulfone (PES) membranes have been fabricated by reverse-thermally induced phase separation (RTIPS) process, using flash freezing. The mesoporous pores can be created by the nano-scaled phase separation induced by the formation and growth of solvent crystals in the dope solution in RTIPS process. RTIPS process has been characterized through analysis on the enthalpy change in the solvent of the dope solution, the morphology of the membrane fabricated with different polymer content, and the pore size distribution and its standard deviation of pore size of the membrane with polymer content via DSC, SEM, and BET, respectively. It is found that the kinetic aspect of the dope solution, i.e., the crystallization of solvent is a crucial factor to determine the structure of membrane fabricated in RTIPS rather than the thermodynamic aspect of the dope solution.

The Properties Analysis of 600V Grade Polyvinyl Chloride Insulated Wire with Variation of Thermal Stress (열적 스트레스 변화에 따른 600V 비닐절연전선의 특성 분석)

  • 최충석
    • Fire Science and Engineering
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    • v.15 no.1
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    • pp.108-115
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    • 2001
  • In this paper, we analyzed the properties change of electric wire when the thermal stress was applied to 600V grade polyvinyl chloride insulated wire (IV). In the structure analysis, normal wire has the properties of direction on the surface, but in case of deteriorated wire at above $400^{\circ}c$, it formed the carbide, the crack and the crystal. The surface composition rate of normal wire was Cu : 100%, but the section composition of the deteriorated wire at $800^{\circ}c$ showed Cu : 78.89%, O : 21.11%. In result of analyzing the differential scanning calory of copper wire, the new reaction peak was observed on the deteriorated wire at above $700^{\circ}c$. In case of the deteriorated wire as $150^{\circ}c$ at the differential thermal analysis, an endothermic reaction appeared at $264^{\circ}c$ lower than the reactive point of normal wire. The occupation rate of oxygen according to the deterioration of copper wire is about 20% at $500^{\circ}c$.

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Characterization of energetic meterials using thermal calorimetry (등전환 방법을 이용한 고에너지 물질의 노화 효과 예측)

  • Kim, Yoocheon;Oh, Juyoung;Ambekar, Aniruda;Yoh, Jai-ick
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2017.05a
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    • pp.547-553
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    • 2017
  • Thermal analysis of three energetic materials used in pyroelectric device was performed using Differential Scanning Calorimetry (DSC). The theoretical method for extracting the reaction rate equation of energetic materials using DSC experimental data is proposed and the reaction rate extraction is performed. The results of the DSC were analyzed by the conversion method such as Friedman. Activation energy and frequency factor according to mass fraction were extracted to complete the reaction rate equation. The extracted reaction rate equation has a form that represents the entire chemical reaction process, not the assumption that the chemical reaction process of the high energy material is a main step in several stages. It has considerable advantages in terms of theoretical and accuracy as compared with the chemical reaction rate form extracted through conventional thermal analysis experiments. Using the derived reaction rate equation, we predicted the performance change of three energetic materials operating on actual storage condition over 20 years.

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Thermal Analysis of Nickel-Base Superalloys by Differential Scanning Calorimetry (시차주사열량측정법에 의한 니켈기 초내열 합금의 열분석)

  • Yun, Jihyeon;Oh, Junhyeob;Kim, Hongkyu;Yun, Jondo
    • Korean Journal of Materials Research
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    • v.26 no.5
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    • pp.235-240
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    • 2016
  • Appropriate thermo-mechanical properties of nickel-based superalloys are achieved by heat treatment, which induces precipitation and solid solution hardening; thus, information on the temperature ranges of precipitation and dissolution of the precipitates is essential for the determination of the heat treatment condition. In this study, thermal analyses of nickel-based superalloys were performed by differential scanning calorimetry method under conditions of various heating rates of 5, 10, 20, or 40K/min in a temperature range of 298~1573K. Precipitation and dissolution temperatures were determined by measuring peak temperatures, constructing trend lines, and extrapolating those lines to the zero heating rate to find the exact temperature under isothermal condition. Determined temperatures for the precipitation reactions were 813, 952, and 1062K. Determined onset, peak, and offset temperatures of the first dissolution reaction were 1302, 1388, and 1406K, respectively, and those values of the second dissolution reaction were 1405, 1414, and 1462K. Determined solvus temperature was 1462K. The study showed that it was possible to use a simple method to obtain accurate phase transition temperatures under isothermal condition.

Preparation of Quaternary Energetic Composites by Crystallization and Their Thermal Decomposition Characteristics (결정화에 의한 4성분계 에너지 복합체 제조 및 열분해 특성)

  • Kim, Byoung-Soo;Kim, Jae-Kyeong;Ahn, Ik-Sung;Kim, Hyoun-Soo;Koo, Kee-Kahb
    • Applied Chemistry for Engineering
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    • v.30 no.2
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    • pp.178-185
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    • 2019
  • Three spherical quaternary composites composed of metal/metal oxide/high explosive/oxidizer were prepared by a crystallization/agglomeration process. From the characteristics of composites by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), the shortening of the decomposition zone of high explosives in the quaternary composite was observed, which may be attributed to the autocatalytic reaction caused by $ClO_2$ or HCl which are ammonium perchlorate (AP) degradation products. The activation energy analysis showed that the activation energy abruptly decreases at the end of the decomposition zone of high explosives, and it was considered to be caused by $HNO_2$ which is common in decomposition products of high explosives. The activation energy predicted from complex pyrolysis results by the distributed activation energy model (DAEM) showed much better in accuracy than those by model-fitting methods such as Kissinger-Akahira-Sunose and Flynn-Wall-Ozawa models.

Characteristic of Underfill with Various Epoxy Resin (에폭시 수지에 따른 언더필의 특성에 관한 연구)

  • Noh, Bo-In;Lee, Jong-Bum;Jung, Seung-Boo
    • Journal of the Microelectronics and Packaging Society
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    • v.13 no.3 s.40
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    • pp.39-45
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    • 2006
  • This study was investigated the thermal properties of underfill with various epoxy resins using thermal analysis methods such as differential scanning calorimetry (DSC), thermo gravimetry analysis (TGA), dynamic mechanical analysis (DMA) and thermo-mechanical analysis (TMA). And, the adhesion strength of the underfills/FR-4 substrate was evaluated. The glass transition temperature (Tg) of underfill which was composed the cycolaliphatic epoxy resin was lower than that of underfill which was not composed the cycolaliphatic epoxy resin. The thermal degradation of underfill was composed of two processes, which involved chemical reactions between the degrading polymer and oxygen from the air atmosphere. The coefficient of thermal expansion (CTE) of underfill which was composed the cycolaliphatic epoxy resin was higher than that of underfill which was not composed the cycolaliphatic epoxy resin. The excessive curing temperatures caused a weak boundary layer of epoxy resin, which resulted in a deterioration of mechanical properties in the epoxy resin and thus led to poor adhesion property between the underfill/FR-4 substrate.

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Miscibility and Transesterification Reaction of blends of Polyarylate and Thermotropic Liquid Crystalline Polymer (Polyarylate와 열방성 액정고분자 블렌드의 상용성 및 에스터 교환반응에 대한연구)

  • 진선우
    • The Korean Journal of Rheology
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    • v.10 no.1
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    • pp.50-56
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    • 1998
  • 폴리아릴레이트(PAr)와 열방성 액정고분자(LCP)블렌드의 상용성과 두 고분자 사이 의 에스터 교환반응을 시차 주사 열분석기 (DSC)와 Fourier transform 적외선 분광분석기 (FT-IR spectroscopy)로 연구하였다. DSC를 이용하여 PAr-LCP 블렌드의 유리전이온도 (Tg)를 관찰한 결과, 두 개의 Tg가 관찰되었다. 측정된 Tg 결과로부터 블렌드 각 상에 녹아 있는 두성분의 상거동을 조사했으며 그결과 LCP가 PAR-rich 상에 녹아 들어간 양이 PAr 이 LCP-rich 상에 녹아 들어간 양보다 더 많음을 알수 있었다. 이러한 결과는 두 고분자 사 이에 부분적으로 상용성이 있음을 의미한다. 액정고분자의 이방성을 고려하여 PAr-LCP 블 렌드의 고분자-고분자 상호작용계수($\chi$12)는 0.069~0.076의 값으로 계산되었다. 두 고분자사 이의 에스터 교환반응를 조사하기 위하여 DSC내에서 열처리한 결과, 열처리 후에 PAr과 LCp의 Tg는 열처리하기 전에 비해 더 큰폭으로 두 Tg의중간값으로 이동하였다. 열처리한 PAr-LCP 블렌드를 FT-IR spectroscopy로 분석한 결과, 순수한 PAr과 LCP에 없는 새로운 에스터기의 특성피이크가 발견되었다. 이와 같은 열분석과 FT-IR spectroscopy 연구 결과 로부터 주어진 열처리 조건에서 PAr과 LCP 사이에 에스터 교환반응이 일어났음을 확인할 수 있었다.

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Polypropylene-Natural Fiber Composites: Rheological Properties during Mixing and Thermal Properties (폴리프로필렌-천연섬유 복합재료의 혼합시 유변학적 물성 및 열적 특성)

  • Kim, Sam-Jung;Yoo, Chong Sun;Kim, Gue-Hyun;Ha, Chang-Sik
    • Journal of Adhesion and Interface
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    • v.9 no.4
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    • pp.24-29
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    • 2008
  • Polypropylene-natural fiber composites have been prepared and their rheological properties during mixing and thermal properties were investigated. Two types of natural fibers (cotton fiber and wood fiber) were compared. On increasing fiber contents, the torque values of composites were increased, where the cotton fiber exhibited higher increase in torques. The torque values of composites were higher as the MI of PP decreased. X-ray diffraction and differential scanning calorimetry results showed an increase in the crystallization temperature but a decrease of crystallinity of the PP/natural fiber composites on increasing fiber contents.

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Poly(4-vinylpyridine)/Vinyl Acetate-Vinyl Alcohol Copolymer Blends : 9. Phase. Behavior (폴리(4-비닐피리딘)/비닐아세테이트-비닐알코올 공중합체 블렌드 :2. 상 거동)

  • Lee, Joon-Youl;Choi, Dong-Hoon;Lee, Hyeok
    • Polymer(Korea)
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    • v.25 no.5
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    • pp.649-656
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    • 2001
  • Miscibility of poly(4-vinylpyridine) (P4VP) blends with poly(vinyl acetate-co-vinyl alcohol) (VAc-VAL copolymers) was investigated as a function of comonomer composition of VAc-VAL copolymers. Differential scanning calorimetry (DSC) and thermo-optical microscopic (TOM) analysis confirmed that P4VP is miscible with VAc-VAL copolymers containing more than 30 mole% VAL. Fourier transform inflated (FT-IR) spectroscopic analysis revealed that the strong intermolecular hydrongen bonding interaction between the vinylpyridine and VAL hydroxyl group was formed. Theoretical phase diagram was constructed by the calculation using the Association model, a thermodynamic model for hydrogen-bonded polymer blend systems developed by Coleman et al. The calculated theoretical binodal phase diagrams were in good agreement with the experimentally determined cloud point curves.

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The Effects of Silica-Alumina Type Inorganic Compounds on the Pyrolysis Reaction of EVA to Produce Fuel-Oil (EVA 수지 이용 연료유 생성을 위한 열분해 반응에서 실리카-알루미나 계열 무기물의 영향)

  • Bak, Young-Cheol;Choi, Joo-Hong;Oh, Se-Hui
    • Transactions of the Korean hydrogen and new energy society
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    • v.22 no.5
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    • pp.706-713
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    • 2011
  • The effects of silica-alumina type catalysts addition on the thermal decomposition of ethylene vinyl acetate (EVA) resin have been studied in a thermal analyzer (TGA, DSC) and a small batch reactor. The silica-alumina type compounds tested were kaolinite, bentonite, perlite, activated clay and clay. As the results of TGA experiments, pyrolysis starting temperature for EVA resin had the 1st pyrolysis temperature range of 300~$400^{\circ}C$ and the 2nd pyrolysis temperature range of 425~$525^{\circ}C$. The silica-alumina type catalysts did not affect the pyrolysis rate in EVA pyrolysis reaction. In the DSC experiments, addition of kaolinite and bentonite catalysts reduced the heat of fusion and heat of 2nd pyrolysis reaction. In the batch system experiments, the mixing of silica-alumina type catalysts enhanced the yield of fuel oil, and affected to the distribution of carbon numbers. In the silica-alumina type inorganic material used in this experiments, bentonite was the most effective from the pyrolysis heat, yields, and the characteristics of fuel oil.