• Title/Summary/Keyword: DSC curves

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A Study on Transformation of Dynamic DSC Results into Isothermal Data for the Formation Kinetics of a PU Elastomer

  • Ahn, WonSool
    • Elastomers and Composites
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    • v.53 no.2
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    • pp.52-56
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    • 2018
  • The present study examines the transformation of dynamic DSC data into the equivalent isothermal data for the formation kinetics of a polyurethane elastomer. The reaction of 2'-dichloro-4,4'-methylenedianiline (MOCA) with a PTMG/TDI-based isocyanate prepolymer was evaluated. DSC measurement was performed in the dynamic scanning mode with several different heating rates to obtain the reaction thermograms. Then, the data was transformed into the isothermal data through a procedure based on Ozawa analysis. The main feature of this procedure was the transformation of $({\alpha}-T)_{\beta}$ curves from dynamic DSC into $({\alpha}-t)_T$ curves using the isoconversional $(t-T)_{\alpha}$ diagram. Validity was discussed for the relationship between the dynamic DSC data and the transformed isothermal results.

A study of plastic plateau disappearance in stress-strain curve of annealed polypropylene films during stretching

  • Lei, Caihong;Wu, Shuqiu;Xu, Ruijie;Xu, Yunqi;Peng, Xinlong
    • Advances in materials Research
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    • v.2 no.2
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    • pp.111-118
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    • 2013
  • The changes of plastic plateau in the stress-strain curves of annealed polypropylene (PP) films during stretching under room temperature were followed and the corresponding melting properties and microstructure were characterized by differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). It was found that during stretching the plastic plateau disappeared progressively with the increase of drawing ratio. At the same time, the endotherm plateau in DSC curves also disappeared progressively. The presence of the plastic plateau was attributed to the stretching of unstable crystalline part which was formed by tie chains around initial row-nucleated lamellae structure during annealing. During stretching, the unstable part was stretched and converted to bridges connecting separated lamellae. There was direct relationship between the disappearance of plastic plateau and pore formation.

A Study on the Thermal Decomposition Characteristics of Nitrophenylhydrazine (니트로페닐하이드라진의 열분해 특성에 관한 연구)

  • 김관응;이근원
    • Journal of the Korean Society of Safety
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    • v.16 no.2
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    • pp.75-79
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    • 2001
  • For handling and storage of reactive chemicals, the hazard evaluations have been extremely important. In the chemical industry, the most concerns are focused on the thermal harzards such as runaway reactions and thermal decompositions, which are mostly governed by thermodynamics and reaction kinetics or these reactive chemical in the system. This study no investigated the thermal decomposition characteristics of nitrophenylhydrazine isomers by using differential scanning calorimeter(DSC) and accelerating rate calorimeter(ARC). Experimental results showed that exothermic onset-temperatures in nitrophenylhydrazine(NPH) isomers were about 160-$210^{\circ}C$ by DSC and 100-$150^{\circ}C$ by ARC. The decomposition temperature acquired by ARC was about 50-$60^{\circ}C$ lower than that by DSC. Reaction heats were about 40-100cal/g by DSC and 330-750ca1/g by ARC. While ortho isomer of NPH show two distinct exothermic peaks, para isomer shows a single peak in DSC curves. The first exothermic peak for 2-NPH is mainly due to intramolecular dehydration forming 1-hydroxybenzotriazole(HOBT) and the second exothermic peak is mainly due to the decomposition of HOBT formed in the first step of decomposition. The exothermin peak in the DSC curve for 4-NPH is mainly due to dissociation of hydrazino and nitro groups.

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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.

Comparison of transition temperature range and phase transformation behavior of nickel-titanium wires (니켈-타이타늄 호선의 상전이 온도 범위와 상전이 행동 비교)

  • Lee, Yu-Hyun;Lim, Bum-Soon;Lee, Yong-Keun;Kim, Cheol-We;Baek, Seung-Hak
    • The korean journal of orthodontics
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    • v.40 no.1
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    • pp.40-49
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    • 2010
  • Objective: The aim of this research was to evaluate the mechanical properties (MP) and degree of the phase transformation (PT) of martensitic (M-NiTi), austenitic (A-NiTi) and thermodynamic nickel-titanium wire (T-NiTi). Methods: The samples consisted of $0.016\;{\times}\;0.022$ inch M-NiTi (Nitinol Classic, NC), A-NiTi (Optimalloy, OPTI) and T-NiTi (Neo-Sentalloy, NEO). Differential scanning calorimetry (DSC), three-point bending test, X-ray diffraction (XRD), and microstructure examination were used. Statistical evaluation was undertaken using ANOVA test. Results: In DSC analysis, OPTI and NEO showed two peaks in the heating curves and one peak in the cooling curves. However, NC revealed one single broad and weak peak in the heating and cooling curves. Austenite finishing ($A_f$) temperatures were $19.7^{\circ}C$ for OPTI, $24.6^{\circ}C$ for NEO and $52.4^{\circ}C$ for NC. In the three-point bending test, residual deflection was observed for NC, OPTI and NEO. The load ranges of NC and OPTI were broader and higher than NEO. XRD and microstructure analyses showed that OPTI and NEO had a mixture of martensite and austenite at temperatures below Martensite finishing ($M_f$). NEO and OPTI showed improved MP and PT behavior than NC. Conclusions: The mechanical and thermal behaviors of NiTi wire cannot be completely explained by the expected degree of PT because of complicated martensite variants and independent PT induced by heat and stress.

An Investigation on the Crystal Growth Studies and Emission line shape in $Er^{3+}$-doped Sodium Tellurite Glasses

  • Joshi, Purushottam;Jha, Animesh
    • Ceramist
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    • v.10 no.3
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    • pp.67-74
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    • 2007
  • Crystallisation kinetics of the erbium doped soda-tellurite glasses were studied using the differential thermal analysis (DTA) and differential scanning calorimetery (DSC) techniques. The DTA curves in the temperature range of 350 K to 650 K were obtained from isochronal heating rates, chosen in the range of 2 to 20 K/min. DSC isothermal curves were used to calculate the fraction of crystals formed on reheating. The apparent activation energies for devitrification were derived by measuring the shifts in the values of $T_g$ and $T_x$ with heating rates, using the Kissinger method. The derived values of apparent activation energies for isochronal and isothermal methods varied in the range of $190-204\;{\pm}\;5\;kJ\;mol^{-1}$. The X-ray powder diffraction analysis of heat treated and transparent samples showed the presence of nano-scale size sodium-tellurite crystals. These crystallites were found to have a strong influence on the full width of half maxima of the transition in $Er^{3+}:\;^4I_{13/2}{\rightarrow}^4I_{15/2}$, which extended from 70 nm in the vitreous materials to 132 nm in glass-ceramic materials.

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Improvement of Solubility and Dissolution of Ketoconazole by Inclusion with Cyclodextrin (시클로덱스트린과의 포접에 의한 케토코나졸의 용해성 및 용출 증가)

  • Park, Gee-Bae;Ann, Hong-Jik;Chang, Young-Soo;Seo, Bo-Youn;Lee, Kwang-Pyo
    • Journal of Pharmaceutical Investigation
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    • v.24 no.2
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    • pp.85-94
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    • 1994
  • Inclusion complexes of ketoconazole (KT) with ${\alpha}-$, ${\beta}-cyclodextrin$ (CD) and dimethyl-${\beta}-cyclodextrin$ $(DM{\beta}CD)$ in a molar ratio of 1:2 were prepared by freeze-drying and solvent evaporation methods. The interactions of KT with ${\alpha}-CD$, ${\beta}-CD$ and $DM{\beta}CD$ in aqueous solution and in solid state were investigated by solubility study, infrared (lR) spectroscopy and differential scanning calorimetry (DSC). The stability constant of $KT-DM{\beta}CD$ inclusion complex (lC) was found to be the largest among three inclusion complexes. Clear differences in IR spectra and DSC curves were observed between inclusion complexes and physical mixtures (PM) of KT-CDs. It was also shown by IR spectra and DSC curves that solvent evaporation method might be. superior to the freeze-drying method in preparing the inclusion complexes of KT-CDs. The dissolution rate of KT was markedly increased by inclusion complex formation with CDs in the buffer solution at pH 4.0 and pH 6.8. The mean dissolution time (MDT,min), which represents the rapidity of dissolution, was in the order of $KT-DM{\beta}CD$ IC (3.20) < $KT-{\beta}-CD$ IC (4.36) < $KT-{\alpha}-CD$ IC (6.99) < $KT-{\alpha}-CD$ PM (17.46)< $KT-{\beta}-CD$ PM (19.36) < $KT-{\beta}-CD$ PM (28.53). The dissolution rates of KT-CD ICsprepared by solvent evaporation method were faster than those of KT-CD ICs prepared by freeze-drying method.

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The Precipitation Phenomena of Al-2.1Li-2.9Cu alloy by Differential Scanning Calorimetry(I) - Precipitation sequence - (열분석법에 의한 Al-2.1Li-2.9Cu합금의 석출현상(I) - 석출순서 -)

  • Park, Tae-Won
    • Journal of the Korean Society for Heat Treatment
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    • v.9 no.4
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    • pp.252-260
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    • 1996
  • A study was conducted to examine the precipitation phenomena of Al-2.1Li-2.9Cu alloy by differential scanning calorimetry and transmission electron microscopy. DSC curves were measured over the temperature range of $25{\sim}550^{\circ}C$ at a heating rate of $2{\sim}20^{\circ}C$/min.. Three heat evolution peaks and three heat absorption peaks were observed in the DSC curve for the as-quenched specimen. From DSC results and TEM analysis, it was proved that the precipitation sequence in the as-quenched specimen is supersaturated solid solution ${\rightarrow}$ GP zone ${\rightarrow}{\delta}^{\prime}{\rightarrow}T_1{\rightarrow}T_2$ and ${\theta}^{\prime}$ was detected in the peak aged specimen at $160^{\circ}C$. The major phase formed at peak hardeness in the aging at $160^{\circ}C$ was ${\delta}^{\prime}$ phase. The activation energies for the formation of ${\delta}^{\prime}$ and $T_1$ phases were 22.3kcal/mole and 24.3kcal/mole, respectively. These lower activation energies than those for diffusion of Cu and Li in Al are ascribed to the quenched-in excess vacancies.

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Effects of Emulsifier on the Thermal Behaviour in Palm Oil (유화제의 첨가가 팜유의 열 특성에 미치는 영향)

  • Chang, Young-Sang;Yi, Young-Soo;Kang, Woo-Suk;Shin, Zae-Ik
    • Korean Journal of Food Science and Technology
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    • v.21 no.6
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    • pp.857-862
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    • 1989
  • Palm oil was crystallized and melted in the differential scanning calorimeter (DSC) in the presence and the absence of sucrose fatty acid ester (SE) at the different scanning rate. In the presence of SE, the crystallization temperature of palm oil was lowered, because SE inhibited the formation of mother crystal at the initial cooling stage The melting curves of SE added palm oil changed irregularly in the ${\alpha}-form$ transition and fusion entropy. It was that the presence of SE affected the molecular diffusion in palm oil.

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Effects of Aluminum Nanoparticles on Thermal Decomposition of Ammonium Perchlorate

  • Zhu, Yan-Li;Huang, Hao;Ren, Hui;Jiao, Qing-Jie
    • Journal of the Korean Chemical Society
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    • v.57 no.1
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    • pp.109-114
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    • 2013
  • The effects of aluminum nanoparticles (AlNs) on the thermal decomposition of ammonia perchlorate (AP) were investigated by DSC, TG-DSC and DSC-TG-MS-FTIR. Addition of AlNs resulted in an increase in the temperature of the first exothermic peak of AP and a decrease in the second. The processing of non-isothermal data at various heating rates with and without AlNs was performed using Netzsch Thermokinetics. The dependence of the activation energy calculated by Friedman's isoconversional method on the conversion degree indicated the decomposition process can be divided into three steps. They were C1/D1/D1 for neat AP, determined by Multivariate Non-linear Regression, and changed to C1/D1/F2 after addition of AlNs into AP. The isothermal curves showed that the thermal stability of AP in the low temperature stage was improved in the presence of AlNs.