• Title/Summary/Keyword: DSC(Differential scanning calorimetry)

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Physicochemical Characterization of Extrudate Solid Formulation of Angelica gigas Nakai Prepared by Hot Melt Extrusion Process

  • Azad, Md Obyedul Kalam;Cho, Hyun Jong;Koo, Ja Seong;Park, Cheol Ho;Kang, Wie Soo
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2018.04a
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    • pp.72-72
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    • 2018
  • The root of Angelica gigas Nakai (AGN) is used as a traditional herbal medicine in Korea for the treatment of many diseases. However, a major challenge associated with the usage of the active compounds from AGN is their poor water solubility. Therefore, this work aimed to enhance the solubility of active compounds by a chemical (viz. surfactant) and physical (hot melt extrusion) crosslinking method (CPC). Infrared Fourier transform spectroscopy (FT-IR) revealed multiple peaks in extrudate solids representing new functional groups including carboxylic acid, alkynes and benzene derivatives. Differential scanning calorimetry (DSC) analysis of the extrudate showed lower glass transition temperature (Tg) and lower enthalpy (${\Delta}H$) (Tg: $43^{\circ}C$; ${\Delta}H$: <6 (J/g)) compared to the non-extrudate (Tg $68.5^{\circ}C$; ${\Delta}H$: 123.2) formulations. X-ray powder diffraction (XRD) analysis revealed amorphization of crystal materials in extrudate solid. In addition, nanonization, enhanced solubility and higher extraction of phenolic compounds were achieved in the extrudate solid. Among the different extrudates, acetic acid- and Span 80-mediated formulations showed superior extractions. We conclude that the CPC method successfully enhanced the production of amorphous nano dispersions from extrudate solid formulations.

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The Effect of Dealumination on the Structure and Acidity of SAPO-11 Molecular Sieve (탈알루미늄화가 SAPO-11 분자체의 구조 및 산성도에 미치는 영향)

  • Park, Jong Yul;Lee, Chi Hun;Kim, Soo Kyung
    • Journal of the Korean Chemical Society
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    • v.40 no.3
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    • pp.202-208
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    • 1996
  • SAPO-11 was synthesized hydrothermally and dealuminated with $H_4$EDTA. The framework structure of SAPO-11 was maintained safely by 24 hours' dealumination, but further dealumination for 48 hours caused SAPO-11 collapsed and to be changed to variscite($AIPO_4{\cdot}2H_2O$) and tridymite($SiO_2$). Dealuminated SAPO-11 showed two structural hydroxyl bands at 3607 $cm^{-1}$ and 3453 $cm^{-1}$ respectively. The intensities of these two bands increased according to the extent of dealumination, and disappeared by the adsorption of methylamine. Dealuminated SAPO-11 showed higher desorption temperatures and greater activation energies in desorption of water and methylamine compared to non-dealuminated SAPO-11. All the phenomena may be due to the stronger interactions of Bronsted acid sites of structural hydroxyl groups generated by dealumination with adsorbed water and methylamine molecules respectively.

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Mechanical Properties of PVC Composite Containing Iron Dust (제철 분진을 함유한 PVC 복합체 수지의 기계적 성질)

  • Nah, Jae-Woon;Kim, Myung-Yul
    • Elastomers and Composites
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    • v.33 no.5
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    • pp.370-376
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    • 1998
  • Mechanical properties of PVC[poly(vinylchloride)] composites containing the dust from blast and converter (Kwangyang Iron Co.) were investigated as a function of dust content. Tensile strength is increased, when the blast dust is mixed with PVC to the extent of 8.83wt % and impact strength is not significantly changed. From these results, it is suggested that blast dust containing CaO, SiO, MgO, $A1_2O_3$ and metallugical particle is compatible with PVC. Thermogravimetric analysis(TGA) showed that residual weight(%) at temperature $600^{\circ}C$ increased with the amount of blast dust and differential scanning calorimetry(DCS) showed that the thermal stability of PVC composite was increased when the weight ratio of blast dust was 8.83wt % X-ray diffractometry measurement also showed their blends and structures.

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Lifetime Prediction and Aging Behaviors of Nitrile Butadiene Rubber under Operating Environment of Transformer

  • Qian, Yi-hua;Xiao, Hong-zhao;Nie, Ming-hao;Zhao, Yao-hong;Luo, Yun-bai;Gong, Shu-ling
    • Journal of Electrical Engineering and Technology
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    • v.13 no.2
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    • pp.918-927
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    • 2018
  • Based on the actual operating environment of transformer, the aging tests of nitrile butadiene rubber (NBR) were conducted systematically under four conditions: in air, in transform oil, under compression in air and under compression in transform oil to studythe effect of high temperature, transform oil and compression stress simultaneously on the thermal aging behaviors of nitrile butadiene rubber and predict the lifetime. The effects of liquid media and compression stress simultaneously on the thermal aging behaviors of nitrile butadiene rubber were studied by using characterization methods such as IR spectrosc-opy, thermogravimetric measurements, Differential Scanning Calorimetry (DSC) measurements and mechanical property measurements. The changes in physical properties during the aging process were analyzed and compared. Different aging conditions yielded materials with different properties. Aging at $70^{\circ}C$ under compression stress in oil, the change in elongation at break was lower than that aging in oil, but larger than that aging under compression in air. The compression set or elongation at break as evaluation indexes, 50% as critical value, the lifetime of NBR at $25^{\circ}C$ was predicted and compared. When aging under compression in oil, the prediction lifetime was lower than in air and under compression in air, and in oil. It was clear that when predicting the service lifetime of NBR in oil sealing application, compression and media liquid should be involved simultaneously. Under compression in oil, compression set as the evaluation index, the prediction lifetime of NBR was shorter than that of elongation at break as the evaluation index. For the life prediction of NBR, we should take into account of the performance trends of NBR under actual operating conditions to select the appropriate evaluation index.

Preparation and Characterization of Elastomeric Solid Electrolyte Based on $PEO-EDA-LiClO_4$ Blends ($PEO-EDA-LiClO_4$ 블렌드계 탄성체 전해질의 제조와 특성)

  • Chang, Young-Wook;Joo, Hyun-Seok
    • Elastomers and Composites
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    • v.39 no.1
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    • pp.36-41
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    • 2004
  • Solid polymer electrolytes were prepared by UV irradiation of the blends consisting of poly(ethylene oxide)(PEO), epoxy diacrylate(EDA) and LiClO_4$. Conductivities of the electrolyte films were measured as a function or blend composition, salt concentration and temperature. The electrolyte having the composition of poly(ethylene oxide) (70% by weight)/epoxy diacrylate (30% by weight) with mole ratio of 10 of ethylene $oxide/Li^+$ exhibited a high ionic conductivity of $1.2{\times}10^{-5} S/cm$ at $25^{\circ}C$. This blend is transparent and shows elastomeric properties. Morphological studies by means of differential scanning calorimetry, X-ray diffraction and polarized optical microscopy indicated that the cured epoxy chains in the blends inhibit the crystallization of poly (ethylene oxide) and thereby induce the blend systems to be completely amorphous in certain compositions.

Fabrication and Characterization of Modified Poly(2-hydroxyethyl methacrylate)(PHEMA) Hydrogels by Thermal/Photo Polymerization

  • Lee, Minsu;Lee, Junghyun;Jang, Jihye;Nah, Changwoon;Huh, Yang-il
    • Elastomers and Composites
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    • v.54 no.4
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    • pp.359-367
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    • 2019
  • Poly(2-hydroxyethyl methacrylate) (PHEMA) hydrogels modified with various co-monomers, such as N-vinyl pyrrolidone (NVP), glycidyl methacrylate (GMA), and glycerol monomethacrylate (GMMA), were prepared to investigate the effect of adding a co-monomer on the water contents, surface wettability, and tensile modulus. These polymers were synthesized by thermal- and photo-polymerization in the presence of azobisisobutyronitrile (AIBN) and diphenyl(2,4,6-trimethylbenzoyl)-phosphineoxide (TPO) as the initiators. The characteristics of the hydrogels were analyzed via FTIR and UV/Vis spectroscopies, contact angle measurements, and tensile modulus measurements with UTM. Regarding the properties of water in the hydrogels, the ratio between free to bound water was investigated using differential scanning calorimetry (DSC). The effects of adding the co-monomers on the water content, surface wettability, and tensile modulus for soft contact lenses were also investigated. In the case of p(HEMA-co-NVP) hydrogels, the increase in the equilibrium water content (EWC) was primarily due to the increase in the bound water content. For p(HEMA-co-GMMA) hydrogels, an increase in free water content was the main reason for the increased EWC. In contrast, in the case of p(HEMA-co-GMA) hydrogels, a decrease in bound water content was observed to be the main factor that reduced the EWC. Photo-polymerized PHEMA hydrogels showed enhanced surface wettability and tensile modulus as compared to those produced via thermal polymerization.

A Study on the molecular structure and molecular weight control of styrene films by plasma polymerization (플라즈마 중합법에 의한 스티렌 박막의 분자 구조 및 분자량 제어에 관한 연구)

  • 김종택;최충양;박종관;박응춘;이덕출
    • Journal of the Korean Vacuum Society
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    • v.6 no.3
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    • pp.213-219
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    • 1997
  • The plasma polymerized styrene films were prepared by using an inter-electrode capacitively coupled gas-flow-type reactor, and the effects of plasma polymerization condition on the molecular weight distribution were investigated by Fourier Transform Infrared (FT-IR), Pyrolysis Gas Chromatography(PyGC), Differential Scanning Calorimetry(DSC) and Gel Permeation Chromatography(GPC). From the above results, the very cross-linked films different from chemical characteristics of the starting monomer were taken out, and it is realized that the molecular structure, cross linking density, and molecular weight distribution could be controlled by changing the parameters such as deposition pressure, deposition power and gas flow rate. Accordingly, it is suggested that plasma polymerization method performed by inter-electrode capacitively coupled gas-flow-type reactor has good characteristics for manufacturing the functional organic thin films which can be applied in sensors, opto-electric device, photo-resist by changing the polymerization parameters.

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Specific Heat and Thermal Conductivity Measurement of XLPE Insulator and Semiconducting Materials (XLPE 절연층과 반도전층 재료의 비열 및 열전도 측정)

  • Lee Kyoung-Yong;Yang Jong-Seok;Choi Yong-Sung;Park Dae-Hee
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.55 no.1
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    • pp.6-10
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    • 2006
  • To improve mean-life and reliability of power cable, we have investigated specific heat (Cp) and thermal conductivity of XLPE insulator and semiconducting materials in 154(kV) underground power transmission cable. Specimens were respectively made of sheet form with EVA, EEA and EBA added $30[wt\%],$ carbon black, and the other was made of sheet form by cutting XLPE insulator in 154(kV) power cable. Specific heat (Cp) and thermal conductivity were measured by DSC (Differential Scanning Calorimetry) and Nano Flash Diffusivity. Specific-heat measurement temperature ranges of XLPE insulator were from $20[^{\circ}C]\;to\;90[^{\circ}C],$ and the heating rate was $1[^{\circ}C/mon].$ And the measurement temperatures of thermal conductivity were $25[^{\circ}C],\;55[^{\circ}C]\;and\;90[^{\circ}C].$ In case of semiconducting materials, the measurement temperature ranges of specific heat were from $20[^{\circ}C]\;to\;60[^{\circ}C],$ and the heating rate was $1[^{\circ}C/mon].$ And the measurement temperatures of thermal conductivity were $25[^{\circ}C],\;55[^{\circ}C].$ In addition we measured matrix of semiconducting materials to show formation and growth of carbon black in base resins through the SEM. From these experimental results, both specific heat and thermal conductivity were increased by heating rate because volume of materials was expanded according to rise in temperature.

Post space preparation timing of root canals sealed with AH Plus sealer

  • Kim, Hae-Ri;Kim, Young Kyung;Kwon, Tae-Yub
    • Restorative Dentistry and Endodontics
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    • v.42 no.1
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    • pp.27-33
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    • 2017
  • Objectives: To determine the optimal timing for post space preparation of root canals sealed with epoxy resin-based AH Plus sealer in terms of its polymerization and influence on apical leakage. Materials and Methods: The epoxy polymerization of AH Plus (Dentsply DeTrey) as a function of time after mixing (8, 24, and 72 hours, and 1 week) was evaluated using Fourier transform infrared (FTIR) spectroscopy and microhardness measurements. The change in the glass transition temperature ($T_g$) of the material with time was also investigated using differential scanning calorimetry (DSC). Fifty extracted human single-rooted premolars were filled with gutta-percha and AH Plus, and randomly separated into five groups (n = 10) based on post space preparation timing (immediately after root canal obturation and 8, 24, and 72 hours, and 1 week after root canal obturation). The extent of apical leakage (mm) of the five groups was compared using a dye leakage test. Each dataset was statistically analyzed by one-way analysis of variance and Tukey's post hoc test (${\alpha}=0.05$). Results: Continuous epoxy polymerization of the material with time was observed. Although the $T_g$ values of the material gradually increased with time, the specimens presented no clear $T_g$ value at 1 week after mixing. When the post space was prepared 1 week after root canal obturation, the leakage was significantly higher than in the other groups (p < 0.05), among which there was no significant difference in leakage. Conclusions: Poor apical seal was detected when post space preparation was delayed until 1 week after root canal obturation.

Thermal properties and mechanical properties of dielectric materials for thermal imprint lithography

  • Kwak, Jeon-Bok;Cho, Jae-Choon;Ra, Seung-Hyun
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2006.06a
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    • pp.242-242
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    • 2006
  • Increasingly complex tasks are performed by computers or cellular phone, requiring more and more memory capacity as well as faster and faster processing speeds. This leads to a constant need to develop more highly integrated circuit systems. Therefore, there have been numerous studies by many engineers investigating circuit patterning. In particular, PCB including module/package substrates such as FCB (Flip Chip Board) has been developed toward being low profile, low power and multi-functionalized due to the demands on miniaturization, increasing functional density of the boards and higher performances of the electric devices. Imprint lithography have received significant attention due to an alternative technology for photolithography on such devices. The imprint technique. is one of promising candidates, especially due to the fact that the expected resolution limits are far beyond the requirements of the PCB industry in the near future. For applying imprint lithography to FCB, it is very important to control thermal properties and mechanical properties of dielectric materials. These properties are very dependent on epoxy resin, curing agent, accelerator, filler and curing degree(%) of dielectric materials. In this work, the epoxy composites filled with silica fillers and cured with various accelerators having various curing degree(%) were prepared. The characterization of the thermal and mechanical properties wasperformed by thermal mechanical analysis (TMA), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), rheometer, an universal test machine (UTM).

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