• Title/Summary/Keyword: Differential Scanning Thermal Analysis

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Study on the Thermal Property and Aging Prediction for Pressable Plastic Bonded Explosives through ARC(Heat-wait-search method) & Isothermal Conditions (ARC(Heat-wait-search method)와 Isothermal 조건을 이용한 압축형 복합화약의 열적 특성 및 노화 예측 연구)

  • Lee, Sojung;Kim, Seunghee;Kwon, Kuktae;Jeon, Yeongjin
    • Journal of the Korean Society of Propulsion Engineers
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    • v.22 no.4
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    • pp.55-60
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    • 2018
  • The thermal property is one of the most important characteristics in the field of energetic materials. Because energy materials release decomposition heat, differential scanning calorimetry (DSC) is frequently used for thermal analysis. However, thermodynamic events, such as melting can interfere with DSC kinetic analysis. In this study, we use isothermal mode for DSC measurement to avoid thermodynamic issues. We also merge accelerating rate calorimetry(ARC) data with DSC data to obtain a robust prediction results for small scale samples and for large scale samples as well. For the thermal property prediction, advanced kinetics and technology solutions(AKTS) programs are used.

Epoxidized Polybutadiene as a Thermal Stabilizer for Poly(3-hydroxybutyrate). II. Thermal Stabilization of Poly(3-hydroxybutyrate) by Epoxidized Polybutadiene

  • Choi, Ju-Yol;Lee, Jong-Keun;You, Young;Park, Won-Ho
    • Fibers and Polymers
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    • v.4 no.4
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    • pp.195-198
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    • 2003
  • Epoxidized polybutadiene (EPB) was prepared by polybutadiene (PB) with m-chloroperbenzoic acid (MCPBA) in homogeneous solution. EPB was blended with poly(3-hydroxybutyrate) (PHB) up to 30 wt% by solution-precipitation procedure. The thermal decomposition of PHB/EPB blends was studied by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and differential thermal analysis (DTA). The thermograms of PHB/EPB blends contained a two-step degradation process, while that of pure PHB sample exhibited only one-step degradation process. This degradation behavior of PHB/EPB blends, which have a higher thermal stability as measured by maximum decomposition temperature and residual weight, is probably due to crosslinking reactions of the epoxide groups in the EPB component with the carboxyl chain ends of PHB fragments during the degradation process, and the occurrence of such reactions can be assigned to the exothermic peaks in their DTA thermograms.

Hot stage microscopy and its applications in pharmaceutical characterization

  • Arun Kumar;Pritam Singh;Arun Nanda
    • Applied Microscopy
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    • v.50
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    • pp.12.1-12.11
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    • 2020
  • Hot stage microscopy (HSM) is a thermal analysis technique that combines the best properties of thermal analysis and microscopy. HSM is rapidly gaining interest in pharmaceuticals as well as in other fields as a regular characterization technique. In pharmaceuticals HSM is used to support differential scanning calorimetry (DSC) and thermo-gravimetric analysis (TGA) observations and to detect small changes in the sample that may be missed by DSC and TGA during a thermal experiment. Study of various physical and chemical properties such sample morphology, crystalline nature, polymorphism, desolvation, miscibility, melting, solid state transitions and incompatibility between various pharmaceutical compounds can be carried out using HSM. HSM is also widely used to screen cocrystals, excipients and polymers for solid dispersions. With the advancements in research methodologies, it is now possible to use HSM in conjunction with other characterization techniques such as Fourier transform infrared spectroscopy (FTIR), DSC, Raman spectroscopy, scanning electron microscopy (SEM) which may have additional benefits over traditional characterization techniques for rapid and comprehensive solid state characterization.

Differential Scanning Calorimetric and Thermogravimetric Analysis of Silk Fibroin / poly (Vinyl pyrrolidone) (견단백질 / Poly (Vinyl pyrrolidone)의 열특성)

  • Kweon, Hae-Yong;Lee, Kwang-Gill;Yeo, Joo-Hong;Woo, Soon-Ok;Han, Sang-Mi
    • Journal of Sericultural and Entomological Science
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    • v.49 no.2
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    • pp.77-80
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    • 2007
  • Silk fibroin/poly (vinyl pyrrolidone) conjugates were prepared and characterized through differential thermal calorimeter and thermogravimetry. The glass transition temperature (Tg) of poly (vinyl pyrrolidone) was not changed by reaction with silk fibroin. However, abnormal exothermic peak was observed at the silk fibroin/poly (vinyl pyrrolidone) conjugates. Thermogravimetric analysis showed that thermal stability of silk fibroin was relatively increased by reaction with PVP.

Thermal Decomposition Kinetics of ZPP as a Primary Charge of Initiators (착화기용 ZPP의 열분해 특성)

  • Kim, Junhyung;Seo, Taeseok;Ko, Seungwon;Ryu, Byungtae
    • Journal of the Korean Society of Propulsion Engineers
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    • v.19 no.5
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    • pp.15-21
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    • 2015
  • The thermal decomposition characteristics of the ZPP(Zirconium/Potassium perchlorate), widely used as a primary charge of initiators, were investigated by differential scanning calorimetry(DSC). The DSC results with different heating rates were elaborated with AKTS-Thermokinetics software for the determination of the kinetic parameters of the thermal decomposition of ZPP. There was good agreement between the experimental and the simulation curves, based on the determined kinetic parameters, which indicates the validity of the kinetic description of the thermal decomposition process of ZPP.

Kinetics on the Thermal Decomposition of Cellulose (셀룰로오스의 열분해 반응속도론)

  • 최승찬;박영수
    • Journal of the Korean Society of Tobacco Science
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    • v.5 no.2
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    • pp.55-62
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    • 1983
  • Four of non- isothermal methods evaluating kinetics have been studied by using differential scanning calorimetry (DSC) and thermogravimetry (TG) and applied for kinetics of the thermal decomposition of cellulose. It is concluded that the heating evolution methods with DSC and approximative methods with TC can lead to satisfactory kinetic analysis. Results calculating the reacting order and the activation energy of cellulose decomposition were 1/2 order and 42kcaB/mol, respectively.

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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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Influence of Dilauroyl Peroxide on Mechanical and Thermal Properties of Different Polypropylene Matrices (Dilauroyl Peroxide의 PP에 대한 기계적, 열적 성질 변화)

  • Sirin, Kamil;Yavuz, Mesut;Canli, Murat
    • Polymer(Korea)
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    • v.39 no.2
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    • pp.200-209
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    • 2015
  • In this study, the influence of dilauroyl peroxide on mechanical and thermal properties of different polypropylene (PP) matrices was investigated. Polypropylene matrices, different molecular weight isotactic PP containing 0.01, 0.02, 0.04, 0.06, 0.08, and 0.1 wt% of dilauroyl peroxide (DLP) were prepared by using a single-screw extruder. The effect of the visbreaking agent (DLP) on mechanical, physical, thermal and morphological properties of different molecular weight PP had been studied. Mechanical properties (tensile strength at break point, at yield and elongation at break point), melt flow index (MFI), scanning electron microscope (SEM) and differential scanning calorimetric (DSC) analyses of these matrices were examined. Melting ($T_m$) and crystallization ($T_c$) temperatures, crystallinity ratio (%) and enthalpies were determined. The microstructure of isotactic polypropylene matrix was investigated by scanning electron microscopy (SEM). From SEM analysis, it was observed that the surface disorder increased by the increasing amount of DLP. As a result of DSC analyses, the crystallinity ratio of the PP matrices has varied between 1.64-7.27%. Mechanical properties of the matrices have been improved. Particularly, the mechanical tests of PP have given interesting results when compounded with 0.06-0.08 wt% dilauroyl peroxide (DLP). Mechanical properties and thermal decomposition processes were all changed by increasing the amount of DLP in the matrix structure.

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.

Estimation of fire-temperature through instrumental analysis of Fire- Damaged Concrete (화재 입은 콘크리트의 기기분석을 통한 화재온도 추정)

  • Kim, Seong-Su;Park, Kwang-Pil;Nam, Ba-Reum;Yoo, Ju-Hwan
    • Proceedings of the Korea Concrete Institute Conference
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    • 2006.11a
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    • pp.913-916
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    • 2006
  • In this study, we conducted machinery analysis, such as differential thermal analysis, X-ray diffraction analysis and scanning electron microscope analysis, in order to predict fire temperature and to analyze fire damage in the case of fire on concrete structure. according to the machinery analysis and differential thermal analysis, concrete bought big creak over $300^{\circ}C$. these result can be utilized as good data in design for repair and reinforcement through rationally evaluating fire damage on concrete structure exposed to high heat or fire in the future.

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