• Title/Summary/Keyword: differential scanning calorimetry

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Synthesis, Morphology and Permeation Properties of poly(dimethyl siloxane)-poly(1-vinyl-2-pyrrolidinone) Comb Copolymer (폴리디메틸실록산-폴리비닐피롤리돈 빗살 공중합체 합성, 모폴로지 및 투과성질)

  • Patel, Rajkumar;Park, Jung Tae;Park, Min Su;Kim, Jong Hak
    • Membrane Journal
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    • v.27 no.6
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    • pp.499-505
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    • 2017
  • The increasing number of natural disasters resulting from anthropogenic greenhouse gas emissions has prompted the development of a gas separation membrane. Carbon dioxide ($CO_2$) is the main cause of global warming. Organic polymeric membranes with inherent flexibility are good candidates for use in gas separation membranes and poly(dimethyl siloxane)(PDMS) specifically is a promising material due to its inherently high $CO_2$ diffusivity. In addition, poly(vinyl pyrrolidine)(PVP) is a polymer with high $CO_2$ solubility that could be incorporated into a gas separation membrane. In this study, poly(dimethyl siloxane)-poly(vinyl pyrrolidine)(PDMS-PVP) comb copolymers with different compositions were synthesized under mild conditions via a simple one step free radical polymerization. The copolymerization of PDMS and PVP was characterized by FTIR. The morphology and thermal behavior of the produced polymers were characterized by transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). Composite membranes composed of PDMS-PVP on a microporous polysulfone substrate layer were prepared and their $CO_2$ separation properties were subsequently studied. The $CO_2$ permeance and $CO_2/N_2$ selectivity through the PDMS-PVP composite membrane reached 140.6 GPU and 12.0, respectively.

Enhanced Dissolution and Permeation of Biphenyl Dimethyl Dicarboxylate Using Solid Dispersions (고체분산체로부터 비페닐디메칠디카르복실레이트의 용출 및 투과 증전)

  • Moon, Jee-Hyun;Chun, In-Koo
    • Journal of Pharmaceutical Investigation
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    • v.29 no.3
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    • pp.227-234
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    • 1999
  • Solid dispersions were prepared to increase the dissolution rate of biphenyl dimethyl dicarboxylate (DDB) using water-soluble carriers such as povidone, copolyvidone, $2-hydroxypropyl-{\beta}-cyclodextrin (HPCD)$, sodium salicylate or sodium benzoate by solvent evaporation method. Solid dispersions were characterized by infrared spectrometry, differential scanning calorimetry (DSC) and powder X-ray diffractometry, dissolution and permeation studies. DDB tablets (7.5 mg) were prepared by compressing the powder mixtures composed of solid dispersions, lactose, com starch, crospovidone and magnesium stearate using a single-punch press. DDB capsules (7.5 mg) were also prepared by filling the mixtures in empty hard gelatin capsules (size No.1). From the DSC and powder x-ray diffractometric studies, it was found that DDB was amorphous in the HPCD or copolyvidone solid dispersions. Dissolution rates after 10 min of DDB alone and solid dispersions (1 : 10) in sodium benzoate, sodium salicylate and copolyvidone were 11.8, 23.5, 22.8 and 82.5%, respectively. Dissolution rates of DDB after 30 min from 1 : 10 and 1 : 20 copolyvidone solid dispersions were 80.5 and 95.0%, respectively. For the DDB tablets prepared using solid dispersions (1 : 20), the initial dissolution rate was dependent on carrier material, and was ranked in order, $Kollidon\;30\;{\ll}$ copolyvidone < HPCD. For the HPCD solid dispersion tablets, dissolution rate reached 97.4% after 15 min, but thereafter slowly decreased to 80.7% after 2 hr due to the precipitation of DDB. However, in the case of copolyvidone solid dispersion tablets, dissolution increased linearly and reached 93.4% after 2 hr. Reducing the volume of test medium from 900 to 300 ml markedly decreased the dissolution rate of the tablets containing 1 : 20 HPCD solid dispersions and 1 : 10 copolyvidone solid dispersion. For 1 : 20 copolyvidone solid dispersion tablets, there was no significant change in dissolution rate up to 1 hr with different volumes of test medium. Preparation of the copolyvidone solid dispersion (1 : 20) in capsules markedly delayed the dissolution (31.2 % after 2hr) due to the limited diffusion within capsules. The permeation rate $(13.4\;g/cm^2\;after\;8\;hr)$ of DDB through rabbit duodenal mucosa from copolyvidone solid dispersion (1 : 10) was markedly enhanced, when compared with drug alone or physical mixtures. From overall findings, DDB formulations containing copolyvidone solid dispersions (1 : 20) could be used to remarkably improve the dissolution rate in dosage form of powders and tablets.

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Study on the Texture and Staling of Breads with Addition of Various Hydrocolloids (Hydrocolloids를 첨가한 식빵의 텍스쳐와 노화에 관한 연구)

  • Lee, Seung Ju;Cho, Sook-Kyung;Lee, Seung-Joo
    • Korean journal of food and cookery science
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    • v.24 no.5
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    • pp.636-644
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    • 2008
  • The principal objective of this study was to assess the effects of hydrocolloids(xanthan gum, guar gum, sodium alginate, k-carrageenan, carboxy-methyl cellulose) on the suppression of retrogradation in the bread. The pasting properties of the doughs and the sensory properties were determined in the bread samples, to which xanthan gum, guar gum, sodium alginate, k-carrageenan, and CMC, were added at different ratios(0.2%, 0.6%, 1%). CMC and k-carrageenan with 0.6% level were selected for the further retrogradation studies. Changes in the firmness of the bread samples at room temperature for 15 days were assessed using a texture analyzer, and the type of retrogradation was calculated via the Avrami equation. The thermal properties of the samples were also determined via differential scanning calorimetry (DSC). The addition of hydrocolloids was shown to increase the viscosities of the doughs. Setback and breakdown viscosity were reduced significantly via the addition of CMC(0.6%, 1%), xanthan gum(1%), and k-carrageenan(1%). Sensory hardness was significantly increased when 1% hydrocolloids were added. Our textural analysis showed that the addition of CMC reduced the firmness of the bread, whereas k-carrageenan didn't. However, the retrogradation rate was reduced via the addition of k-carrageenan, as was also demonstrated in the results of our DSC analysis.

Comparison on Physicochemical Properties of Korean Kidney Bean Starch according to Varieties (품종에 따른 강낭콩 전분의 이화학적 성질비교)

  • Cho, Eun-Ja;Kim, Sung-Kon;Park, Sun-Hee
    • Korean Journal of Food Science and Technology
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    • v.30 no.4
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    • pp.787-793
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    • 1998
  • Physicochemical properties of starch of three cultivars of Korean kidney Bean Starches, Pink (PKB), Red (RKB) and White (WKB) were studied. Starch granule was oval/round and smooth in all samples. The amylograms showed a continuous increase of viscosity without peak during heating. The water-binding capacities of starches of PKB, RKB and WKB were 102.1%, 94.7% and 106.9%, respectively. The swelling powers were rapidly incresed in all samples. The amylose content, blue value and relative viscosity of kidney bean starches were $31.1{\sim}32.8%,{\;}0.64{\sim}0.66$ and $2.27{\sim}2.61{\;}mlg^{-1}$, respectively. The transmittance of starch suspension was linearly increased as the temperature raised from $65^{\circ}C{\;}to{\;}85^{\circ}C$. The gelatinization temperature ranges determined by differential scanning calorimetry (DSC) were $71.1{\sim}86.9^{\circ}C for PKB, $71.1{\sim}86.0^{\circ}C$ for RKB and $60.8{\sim}77.9^{\circ}C$ for WKB.

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Studies on the Thermal Stability and Color of Free Drip released from Pork Muscle with pH, Concentration of NaCl and Phosphate (pH, NaCl 및 phosphate 첨가에 따른 돈육 드립의 열안정성 및 색에 관한 연구)

  • Kim, Cheon-Jei;Lee, Chang-Hyun;Song, Min-Seok;Lee, Eui-Soo;Cho, Jin-Kook
    • Korean Journal of Food Science and Technology
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    • v.32 no.6
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    • pp.1285-1290
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    • 2000
  • The objective of this study was to evaluate the characteristics on the thermal denaturation of free drip released from pork loin during chilled storage using DSC (differential scanning calorimetry) with pH, concentration of NaCl and phosphate. The increasing of pH stabilized the heat resistance of the proteins in drip. A $T_1$ greatly increased of $T_{max}$ by $6.33^{\circ}C$ incline from pH 5.5 to 6.5. And increasing the concentration of NaCl destabilized the heat resistance of drip. $T_1$ showed the greatest reduction of $T_{max}\;(9.41^{\circ}C)$ in the presence of 5% NaCl. The presence of STPP (Sodium Tripolyphosphate) enchanced the thermal stability of pork drip by $5.84^{\circ}C$ in the presence of 0.5% STPP. As temperature increased from 40 to $100^{\circ}C$, lightness $(L^*)$ increased from 41.1 to 69.5, while redness $(a^*)$ decreased from 26.70 to 5.40. Particularly, both values of $L^*-$ and $a^*-$ greatly changed by 78% from 40 to $60^{\circ}C$.

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Preparation and characterization of high density polyethylene/silane treated pulverized-phenol resin composites (고밀도 폴리에틸렌과 실란 처리된 분쇄페놀수지 복합재의 제조 및 특성)

  • Park, Jun-Seo;Han, Chang-Gue;Nam, Byeong-Uk
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.17 no.9
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    • pp.27-33
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    • 2016
  • Phenolic resin has excellent heat resistance and good mechanical properties as a thermosetting resin. However, its thermosetting characteristics cause it to produce a non-recyclable waste in the form of sprue and runner which is discarded and represents up to 15~20% of the overall products. Forty thousand tons of phenolic resin sprue and runner are disposed of (annually). The (annual) cost of such domestic waste disposal is calculated to be 20 billion won. In this study, discarded phenol resin scraps were pulverized and treated by silanes to improve their interfacial adhesion with HDPE. The sizes of the pulverized pulverulent bodies and fine particles were (100um~1000um) and (1~100um), respectively. The pulverized phenol resin was treated with 3-(methacryloyloxy) propyltrimethoxysilane and vinyltrimethoxy silane and the changes in its characteristics were evaluated. The thermal properties were evaluated by DSC and HDT. The mechanical properties were assessed by a notched Izod impact strength tester. When the silane treated phenol resin was added, the heat distortion temperature of HDPE increased from $77^{\circ}C$ to $96^{\circ}C$ and its crystallinity and crystallization temperature also increased. Finally, its impact strength and tensile strength increased by 20% and 50%, respectively, in comparison with the non-treated phenol resin.

Polymerization Behavior of Self-healing Agents for Damage Repair in Composite Materials (복합재 손상보수용 자가치료제의 중합 거동)

  • Oh, Jinoh;Yoon, Sungho;Jang, Seyong
    • Journal of the Korean Society of Propulsion Engineers
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    • v.18 no.5
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    • pp.35-42
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    • 2014
  • Thermal analysis properties and adhesive properties of self-healing agents were evaluated through differential scanning calorimetry, reaction heat measurement, and adhesive shear test. D1E0, D3E1, D1E1, D1E3, and D0E1, depending on the mixing ratio of DCPD and ENB, were considered as self-healing agents. The amount of Grubbs' catalyst, depending on the type of self-healing agents, was varied from 0.1 wt% to 1.5 wt%. In the case of DCPD, the polymerization reaction occurred faster and the stabilized adhesive strength increased as the amount of catalyst increased; however, a large amount of catalyst was required. ENB had excellent reactivity with a small amount of the catalyst; however, high reaction heat was observed at the early stage of polymerization. Thermal analysis properties and adhesive properties of self-healing agents can be controlled by varying a mixing ratio of DCPD and ENB. Among the self-healing agents used for this study, the D3E1 would be one of the most preferable candidates with regard to maximum adhesive strength, reaching time to maximum adhesive strength, stabilized adhesive strength, and reaction heat.

Evaluation of Stamp Forming Process Parameters for CF/PEKK Thermoplastic Composite Using Finite Element Method (고속 열 성형 유한요소해석을 활용한 CF/PEKK 열가소성 복합재 구조물 제작 공정 예측 및 검증)

  • Lee, Keung-In;Choe, Hyeon-Seok;Kwak, June-Woo;Lee, Jun-Sung;Ju, Hyun-Woo;Kweon, Jin-Hwe;Nam, Young-Woo
    • Composites Research
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    • v.34 no.5
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    • pp.296-304
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    • 2021
  • This study presented the evaluation of the stamp forming process for L-shape CF/PEKK thermoplastic composite using the finite element model. The formability of three different trimming allowances has been examined for representative product geometry. The results showed that those manufactured by high trimming allowance showed more excellent formability in those areas. Moreover, the effects of the trimming allowances on the stress, thickness, wrinkle distributions of thermoplastic composites fabricated with the stamp forming process were evaluated. The comparison of the simulation and experimental results for the thickness and wrinkle distributions proved the accuracy of the stamp forming model. The crystallinity of the composite was performed by differential scanning calorimetry (DSC). The void content of the composite was evaluated by matrix digestion. Then, the fabricated structure was characterized and achieved high quality in crystallinity and void content. Consequently, the presented FEM modeling shows excellent potential for application in the aircraft product design process. This pragmatic approach could efficiently offer a valuable solution for the thermoplastic composite manufacturing field.

Synthesis and Characterization of Polymers with Azobenzene and Hexamethylene Groups in Main Chain (주사슬에 아조벤젠기와 헥사메틸렌기를 갖는 고분자의 합성 및 특성)

  • Gu, Su-Jin;Lee, Eung-Jae;Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.86-92
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    • 2019
  • Polymers with various compositions of azobenzene and hexamethylene groups in the main chain were synthesized by a Schotten-Baumann reaction and their properties were investigated. The chemical structures and physical properties of the synthesized polymers were investigated by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, thermogravimetric analysis, polarized optical microscopy, and x-ray diffraction. The polymers showed an inherent viscosity of 1.28-1.36 dl/g and were relatively insoluble in most organic solvents. The melt transition temperature increased rapidly with increasing number of azobenzene groups in the polymer. When the azobenzene monomer content was more than 50 mol%, no melting transition occurred below the decomposition temperature. Among the polymers with a melt transition temperature, the MP-A3C7 and MP-A5C5 polymers were liquid crystalline materials and exhibited a nematic phase with weak liquid crystallinity over a wide liquid crystal temperature range. This difference in the properties of the synthesized polymers is likely due to the changes in intermolecular forces resulting from the linearity and polarity of the trans-form of azobenzene.

Transient Liquid Phase Sinter Bonding with Tin-Nickel Micro-sized Powders for EV Power Module Applications (주석-니켈 마이크로 분말을 이용한 EV 전력모듈용 천이액상 소결 접합)

  • Yoon, Jeong-Won;Jeong, So-Eun
    • Journal of the Microelectronics and Packaging Society
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    • v.28 no.2
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    • pp.71-79
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    • 2021
  • In this study, we have successfully fabricated the Sn-Ni paste and evaluated the bonding properties for high-temperature endurable EV (Electric Vehicle) power module applications. From evaluating of the micro-structural changes in the TLPS (Transient Liquid Phase Sintering) joints with Sn and Ni contents in the Sn-Ni pastes, a lack of Ni powders and Ni particle agglomerations by Ni surplus were observed in the Sn-20Ni and Sn-50Ni joints (in wt.%), respectively. In contrast, relatively dense microstructures are observed in the Sn-30Ni and Sn-40Ni TLPS joints. From differential scanning calorimetry (DSC) thermal analysis results of the fabricated Sn-Ni paste and TLPS bonded joints, we confirmed that the complete reactions of Sn with Ni to form Ni-Sn intermetallic compounds (IMCs) at bonding temperatures occurred, and there is no remaining Sn in the joints after TLPS bonding. In addition, the interfacial reactions and IMC phase changes of the Sn-30Ni joints under various bonding temperatures were reported, and their mechanical shear strength were investigated. The TLPS bonded joints were mainly composed of residual Ni particles and Ni3Sn4 intermetallic phase. The average shear strength tended to increase with increasing bonding temperature. Our results indicated a high shear strength value of approximately 30 MPa at a bonding temperature of 270 ℃ and a bonding time of 30 min.