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

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Microstructures and Thermal Properties of Polycaprolactone/Epoxy Resin/SiO2 Hybrids

  • He, Lihua;Liu, Pinggui;Ding, Heyan
    • Journal of Adhesion and Interface
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    • v.7 no.4
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    • pp.32-38
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    • 2006
  • A series of organic-inorganic hybrids, PCL/EP/$SiO_2$, involving epoxy resin and triethoxysilane-terminated polycaprolactone elastomer (PCL-TESi) were prepared via polymerization of diglycidyl ether of bisphenol A (DGEBA) with amine curing agent KB-2 and sol-gel process of PCL-TESi. The curing reactions were started from the initially homogeneous mixture of DGEBA, KB-2 and the PCL-TESi. The organicinorganic hybrids containing up to 4.95% (wt) of $SiO_2$ were obtained and characterized by FT-IR, transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and thermogravimetry analysis (TGA). It was experimentally shown that the swelling property in toluene, morphologies and thermal properties of the resulting hybrids were quite dependent on the contents of $SiO_2$. The crosslink network density decreases with increasing of the PCL-TESi. And in TEM, the phase separated morphology of these hybrids was found, which resulted from the coagulation of Si-O-Si networks resulting from $-Si(OC_2H_5)_3$ of PCL-TESi self-curing by hydrolytic silanol condensation, with the advancement of the curing reaction in the modified epoxy resin systems. Meanwhile, the change of the $SiO_2$ content made the morphologies changed from aggregated particles of Si-O-Si in the hybrid to nanocluster of interconnected Si-O-Si particles, then to aggregated Si-O-Si dispersing in the continuous cured epoxy phase again, and last to co-continuous interpenetrating network. The glass transition behavior of the hybrid material was cooperative motion of large chain segments, which were hindered by the inorganic Si-O-Si network. And in TG analysis, the characteristic temperature at 5% of weight loss was evidently increased from $120.5^{\circ}C$ of pure cured epoxy to $277.6^{\circ}C$ of 3.84% (wt) of $SiO_2$ modified epoxy due to the existence of Si-O-Si when PCL-TESi was added in the hybrid.

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Aging Effect of Poly(vinyl alcohol) Membranes Crosslinked with Poly(acrylic acid-co-maleic acid)

  • Rhim Ji Won;Hwang Ho Sang;Kim Dae Sik;Park Ho Bum;Lee Chang Hyun;Lee Young Moo;Moon Go Young;Nam Sang Yong
    • Macromolecular Research
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    • v.13 no.2
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    • pp.135-140
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    • 2005
  • Poly(vinyl alcohol) (PVA) membranes crosslinked with poly(acrylic acid-co-maleic acid) (PAM) were prepared to investigate the effect of aging on their morphology by swelling them for up to 7 days. PAM was used both as a crosslinking agent and as a donor of the hydrophilic-COOH group. A $30 wt\%$ weight loss of the dry membrane was observed in the swelling test after 6 days. The surface of the membrane was dramatically changed after the swelling test. The surface roughness of the PVA/PAM membrane was increased, as determined by atomic force microscopy (AFM). The swelling loosened the polymer structure, due to the release of the unreacted polymer and the decomposition of the ester bond, thereby resulting in an increase in the free volume capable of containing water molecules. The water molecules present in the form of free water were determined by differential scanning calorimetry (DSC). The fraction of free water increased with increasing swelling time. The swelling of the membrane may provide space for the transport of protons and increase the mobility of the protonic charge carriers. The proton conductivity of the membranes measured at T= 30 and $50^{\circ}C$ was in the range of $10^{-3} to 10^{-2} S/cm$, and slightly increased with increasing swelling time and temperature.

Chemoenzymatic Synthesis of H-shaped Amphiphilic Pentablock Copolymer and Its Self-assembly Behavior (H-형태 양친매성 펜타블록 공중합체의 화학효소적 합성과 자기회합거동 평가)

  • Chen, Peng;Li, Ya-Peng;Li, Cai-Jin;Meng, Xin-Lei;Zhang, Bao;Zhu, Ming;Liu, Yan-Jing;Wang, Jing-Yuan
    • Polymer(Korea)
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    • v.37 no.3
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    • pp.332-341
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    • 2013
  • H-shaped amphiphilic pentablock copolymers $(PSt)_2-b-PCL-b-PEO-b-PCL-b-(PSt)_2$ was synthesized via chemoenzymatic method by combining enzyme-catalyzed ring-opening polymerization (eROP) of ${\varepsilon}$-caprolactone (${\varepsilon}$-CL) and atom transfer radical polymerization (ATRP) of styrene. By this process, we obtained copolymers with controlled molecular weight and low polydispersity. The structure and composition of the obtained copolymers were characterized by nuclear magnetic resonance (NMR), gel permeation chromatography (GPC) and infrared spectroscopy analysis (IR). The crystallization behavior of the copolymers was analyzed by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The crystallization behavior of the H-shaped block copolymers demonstrated a PCL dominate crystallization. The self-assembly behavior of the copolymers was investigated in aqueous media. The hydrodynamic diameters of the copolymer micelles in aqueous solution were measured by dynamic light scattering (DLS). The morphology of the copolymer micelles was observed by atomic force microscopy (AFM) and transmission electron microscopy (TEM). The hydrodynamic diameters of spherical micelles declined gradually with the increase of the hydrophobic chain lengths of the copolymers. The critical micelle concentration (CMC) values were determined from fluorescence emission, and it was found that the CMCs decreased with an increase of PSt hydrophobic block lengths.

Thermal Properties of Al-Ni-Y Alloy Amorphous Ribbons and High Temperature Deformation Behavior of Al-Ni-Y Alloy Extrudates Fabricated with Amorphous Ribbons (Al-Ni-Y 합금 비정질 리본의 열적 특성 및 리본 압출재의 고온변형 특성)

  • Ko, Byung-Chul;Yoo, Yeon-Chul
    • Transactions of Materials Processing
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    • v.7 no.4
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    • pp.333-339
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    • 1998
  • Hot torsion tests were conducted to investigate the high temperature deformation behavior of $Al_{85}Ni_{10}Y_5$ alloy extrudates fabricated with amorphous ribbons. The powder metallurgy routes, hot pressing and hot extrusion were used to fabricate the extrudates. Thermal properties of amorphous ribbons with different thickness as a function of aging temperature were studied by thin film x-ray dif-fraction (XRD) and differential scanning calorimetry(DSC). The Al phase crystallite firstly formed in the amorphous ribbons and its crystallization temperature($T_x$)Was ~210${\circ}C$ During the processings of consolidation and extrusion, nano-grained structure(~100 nm) was formed in the Al85Ni10Y5 alloy extrudates. The as-extrudated Al85Ni10Y5 alloy and the $Al_{85}Ni_{10}Y_5$ alloy annealed at 250${\circ}C$ for 1 hour showed a flow curve of DRV(dynamic recovery) during hot deformation at 400-550${\circ}C$. On the other hand, the $Al_{85}Ni_{10}Y_5$ alloy annealed at 400${\circ}C$ for 1 hour showed a flow curve of DRX(dynamic recrys-tallization) during hot deformation at 450-500${\circ}C$. Also the flow stress and flow strain of the $Al_{85}Ni_{10}Y_5$ alloy extrudate annealed at 400${\circ}C$ were higher than those at 250${\circ}C$.

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Study on Characteristics of Sn-0.7wt%Cu-Xwt%Re Solder (Sn-0.7wt%Cu-Xwt%Re 솔더의 특성에 관한 연구)

  • Noh, Bo-In;Won, Sung-Ho;Jung, Seung-Boo
    • Journal of the Microelectronics and Packaging Society
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    • v.14 no.4
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    • pp.21-25
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    • 2007
  • In this study, the properties of Sn-0.7wt%Cu-Xwt%Re(X=$0.01{\sim}1.0$) older were investigated by using DSC(differential scanning calorimetry), wetting balance, victors hardness and tensile testers. The melting temperature of solder was increased with increasing the contents of rare earth element, and the melting temperature range of Sn-0.7Cu-($0.01{\sim}1.0$)Re solder was $233.9{\sim}234.7^{\circ}C$. The wettability with Sn-0.7Cu-0.1Re solder was higher than that of Sn-0.7Cu-0.01Re and Sn-0.7Cu-1.0Re solders, and the wettability of Sn-0.7Cu-0.1Re solder was higher than that of Sn-0.7wt%Cu-0.01w%P solder. Also, the hardness and tensile strength of solder were increased with increasing the contents of rare earth element.

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Comparison of Inclusion Complex Formation Capacity of Cyclodextrins with Various Molecules and Characterization of Cyclodextrin-fatty Acid Complex (Cyclodextrin의 Inclusion Complex 형성능과 Fatty Acid와의 Complex 형성조건과 특성)

  • 이용현;정승환박동찬
    • KSBB Journal
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    • v.10 no.2
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    • pp.149-158
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    • 1995
  • The capacity of inclusion complex formation between ${\alpha}$-, ${\beta}$-, ${\gamma}$-cyclodextrins(CDs) and various compounds, such as pH indicators, biloslalns, glycoside, amino acid, and fatty acids, was compared. Fatty acid was identified as the most suitable ligand for fractionation of CDs in terms of capacity and selectivity. The effects of complex formation conditions, such as, mixing ratio of CD and fatty acid, pH, ionic strength, and temperature, on the capacity of fatty acrid-CD complex was also investigated. The carbon number of fatty acids was identified as the most significant factor determining the capacity and selectivity of inclusion complex formation of CDs. Capric acid(C10) and palmitic acid(C16) showed high specificity for ${\alpha}$- and ${\beta}$-CDs, respectively. Under the optimal conditions, the molar ratio of complex formed was found to be 1.0:2.6 for ${\alpha}$-CD/capric acid and 1.0:1.9 for ${\beta}$-CD/palmitic acid. X-ray diffraction and infrared spectrum of the formed inclusion complex were analyzed. The changes of enthalpy($\Delta$H) of the inclusion complex formation reaction was evaluated by differential scanning calorimetry, showed that the reaction was endothermic.

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Electrical conduction phenomena of $C_{22}$--quinolium(TCNQ) langmuir-blodgett films under the high-electric field ($C_{22}$-quinolium(TCNQ) LB막의 고전게 전기전도 현상)

  • 신동명;김태완;홍언식;송일식;유덕선;강도열
    • Electrical & Electronic Materials
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    • v.7 no.2
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    • pp.138-144
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    • 1994
  • Electrical conduction phenomena of $C_{22}$-quinolium(TCNQ) Langmuir- Blodgett(LB) films are reported through a study of current-voltage(I-V) characteristics along a perpendicular direction. The I-V characteristics were investigated by applying a step or a pulse voltage to the specimen as well as changing temperatures in the range of 20-250[.deg. C] It show an ohmic behavior in low-electric field, and a nonohmic behavior in high-electric field. This nonohmic behavior has been interpreted in terms of a conduction mechanism of space-charge limited current and Schottky effect. When the electric field is near the strength of 10$_{6}$ V/cm, there occur anomalous phenomena similar to breakdown. When step or pulse voltage is applied, the breakdown voltage shifts to the higher one as the step or pulse time width becomes shorter. To see the influence of temperature, current was measured as a function of temperature under the several bias voltages, which are lower than that of breakdown. It shows that the current increases to about 103 times near 60-70[.deg. C], and remains constant for a while up to around 150[.deg. C] and then suddenly drops. We have also performed a DSC(differential scanning calorimetry) measurement with $C_{22}$-quinolium(TCNQ) powder in the range of 30-300[.deg. C]. These results imply that the anomalous phenomena occuring in the high electric field are caused by the electrical and internal thermal effect such as a joule heating.ating.

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Comparison of Physicochemical Properties of Several Korean Potato Starches - Physicochemical Properties of Defatted potato starch - (품종별 한국산 감자의 전분 특성 비교(II) -탈지한 감자전분의 이화학적 특성 -)

  • 김경애;김선민
    • Korean journal of food and cookery science
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    • v.5 no.2
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    • pp.43-50
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    • 1989
  • Physicochemical properties on defatted potato starches, Irish Cobbler and Dejima, were investigated. The average diameter of the Irish Cobbler and Dejima starch were $22.5-29.8\mu\textrm{m}$, and both the starches had birefringence. Irish Cobbler starch was lower than that of Dejima starch in water binding capacity, swelling power and solubility. Relative crystallinity of both the starches was decreased after defatted. The blue value of Irich Cobbvler and Dejima starch was measured 0.37 and 0.35 respectively Transmittnace of 0.1% starch suspensions was higher on defatted starch than on untreated starch. Differential Scanning Calorimetry of untreated potato starch showeed higher gelatinization temperature in Irish Cobbler starch than in Dejiam starch. The gelatinization enthalpy of untreated starch was higher in Irisch Cobbler starch than in Dejima starch, but, after defatted, it was decreased.

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Effect of Cowpea Precipitate Flour Protein on Characteristics of Gel (동부앙금의 단백질 함량이 Gel화 특성에 미치는 영향)

  • 김경애;이선영;정난희;전은례
    • Korean journal of food and cookery science
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    • v.13 no.5
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    • pp.627-634
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    • 1997
  • The purpose of this study is to examine the effect of protein content on the physicochemical properties, gelatinized characteristics and textural properties of cowpea precipitate gels stored for 24 hrs and 48 hrs at room temperature. The contents of protein, total fat, and ash ranged from 0.35%∼1.38%, 0.54%∼0.64%, and 0.21%∼0.25%, respectively. The X-ray diffraction patterns were all Ca-type, showing no difference according to the protein content. Protein content did not make any difference in the blue values of cowpea precipitate. The blue value of cowpea precipitate powder as protein content was decreased. The water-binding capacity of cowpea precipitate powder increased as the protein content increased. Swelling power and solubility of cowpea precipitate powder increased as protein content decreased. The transmittance of cowpea precipitate powder was not different according to the protein content. The initial pasting temperature of cowpea precipitate powder by differential scanning calorimetry (DSC) and rapid visco analyser (RVA) showed no differences according to the protein content. In sensory evaluation, the color and clarity of cowpea precipitate gels stored for 24 hrs and 48 hrs at room temperature as the protein content increased, and the hardness, cohesiveness, springiness, acceptability were greater when the gels were stored for 48 hrs. Instrumental analyses using a rheometer showed that the hardness, gumminess, and chewiness of cowpea precipitate gels stored for 24 hrs, which was increased as the high protein content increased. For the gels stored for 48 hrs, all other factors are significantly different except cohesiveness as the protein content increased.

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Effects of the Type and Percentage of a Lipid on the Quality Characteristics of Rice Bread Depending on the Use of Wet and Dry Rice Flour (습식 및 건식 쌀가루의 유지 종류 및 첨가 비율에 따른 쌀빵 품질 특성)

  • Kim, Sang Sook;Chung, Hae Young
    • The Korean Journal of Food And Nutrition
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    • v.31 no.4
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    • pp.511-519
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    • 2018
  • The baking properties of rice bread with different percentages of butter and oil in wet and dry rice flour were investigated. The moisture, damaged starch, mean diameter, pasting properties by amylogram and RVA (Rapid Visco Analyzer), as well as thermal properties by DSC (Differential Scanning Calorimetry) of wet and dry rice flour were analyzed. The specific gravity and color (L, a, b) of the dough, as well as the appearance, color (L, a, b) and texture of the rice bread with different percentages of butter and oil in wet and dry rice flour were also analyzed. As a result, the wet rice flour were composed of a noted higher content in moisture, compared to the dry rice flour (p<0.001). The wet rice flour had lower values of damaged starch, higher values of mean diameter and a higher peak viscosity than was noted in the dry rice flour (p<0.001). The wet rice flour showed a higher degree of hydration and gelatinization than was seen in the dry rice flour (p<0.001). The prevailing principle to utilize the replacement of wet rice flour with oil had a significant effect on the volume, specific volume and hardness of the rice bread (p<0.001). The hardness of the rice bread also showed a decreasing trend as the amount of the added oil was increased into the mixture. These results suggest that the replacement of wet rice flour with 5.8% oil is effective for the production of rice bread.