• Title/Summary/Keyword: Calorimetry

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Residual Stress Behavior and Characterization of Polyimide Crosslinked Networks via Ring-opening Metathesis Polymerization (개환 복분해 중합을 통한 가교형 폴리이미드 박막의 잔류응력 거동 및 특성 분석)

  • Nam, Ki-Ho;Seo, Jongchul;Jang, Wonbong;Han, Haksoo
    • Polymer(Korea)
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    • v.38 no.6
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    • pp.752-759
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    • 2014
  • Crosslinked polyimides (PIs) were synthesized by reacting 4,4'-(hexafluoroisopropylidene)-diphthalic anhydride (6FDA) and 2,2'-bis(trifluoromethyl)benzidine (TFDB) with various ratios of the cross-linkable, end-capping agent cis-1,2,3,6-tetrahydrophthalic anhydride (CDBA) via ring-opening metathesis polymerization. Residual stress behaviors were investigated in-situ during thermal imidization of the crosslinked PI precursors using a thin film stress analyzer (TFSA) by wafer bending method. The thermal properties were investigated via differential scanning calorimetry (DSC), thermomechanical analysis (TMA), and thermogravimetric analysis (TGA). The optical properties were measured by ultraviolet-visible spectrophotometer (UV-vis) and spectrophotometry. All properties were interpreted with respect to their morphology of crosslinked networks. With increasing the amounts of the end-capping agent, the residual stress decreased from 27.9 to -1.3 MPa, exhibited ultra-low stress and high thermal properties. The minimized residual stress and enhanced thermal properties of the crosslinked PI makes them potential candidates for versatile high-density multi-layer structure applications.

Colorless Copolyimide Films: Thermo-mechanical Properties, Morphology, and Optical Transparency (무색 투명한 폴리이미드 공중합체 필름 : 열적-기계적 성질, 모폴로지, 및 광학 투명성)

  • Jin, Hyo-Seong;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.32 no.3
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    • pp.256-262
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    • 2008
  • Copolyimides containing pendant trifluoromethyl ($CF_3$) groups were synthesized from 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and bis[4-(3-aminophenoxy)phenyl]sulfone (BAPS) with various concentrations of 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane(BAPP) to poly(amic acid)(PAA), followed by thermal imidization. These copolyimides were readily soluble in N,N'-dimethylacetamide (DMAc) and could be solution-cast into a flexible and tough film. The thermomechanical properties, morphology and an optical transparency of the copolyimide films were determined using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), wide angle X-ray diffraction (XRD), scanning electron microscopy (SEM), universal tensile machine (UTM), and a UV-Vis spectrometer. The cast copolyimide films exhibited high optical transparency with a cut-off wavelength (${\lambda}_0$) of $275{\sim}319\;nm$ in UV-vis absorption and a low yellow index(YI) value of $3.65{\sim}10.37$. The thermo-mechanical properties of copolyimide films were enhanced linearly with increasing a BAPP content. In contrast, the optical transparency of the copolyimide films was found to get worse with increasing a BAPP content.

Curing Properties of UV-LED Curable Color Coating (UV-LED 경화형 칼라 코팅의 경화특성 연구)

  • Ho, Shin-Chan;Kim, Jong-Gu;Hong, Jin-Who;Ahn, Tae-Jung;Kim, Hyun-Kyoung
    • Journal of Adhesion and Interface
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    • v.13 no.1
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    • pp.31-37
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    • 2012
  • In this study, we investigated the curing properties of UV-LED curable color coating. Specially, the effects of UV-LED wavelength (365, 395, and 405 nm), inert gas, the concentration of photosensitizer, and dual curing on the curing behavior of UV-LED coating systems were studied. The photopolymerization behaviors and the unreacted acrylate groups at Film-air (FA) interface and Film-substrate (FS) interface were investigated by photo differential scanning calorimetry (Photo-DSC) and Fourier-transform infrared spectroscopy with attenuated total reflection (FT-IR/ATR), respectively. Photo-DSC results showed that the heat flow and the ultimate conversion for coating system cured by 405 nm UV-LED were higher than the corresponding values for coating systems cured by 395 and 365 nm UV-LED. FT-IR/ATR results showed that the UV-LED curing systems improved interior and through curing of the coating film, but significantly are affected by oxygen inhibition at FA-interface. The inert environment such as nitrogen purging and the dual curing improved the surface and interior curing of the coating films.

Effect of Sucrose and Gluten on Glass Transition, Gelatinization, and Retrogradation of Wheat Starch (밀전분의 유리전이와 호화 및 노화에 대한 sucrose와 글루텐의 영향)

  • Jang, Jae-Kweon;Pyun, Yu-Ryang
    • Korean Journal of Food Science and Technology
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    • v.36 no.2
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    • pp.288-293
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    • 2004
  • Differential scanning calorimetry (DSC) was used to study effects of sucrose and gluten on wheat starch glass transition, gelatinization, and retrogradation. Glass transition temperature ($T_{g}$) of wheat starch decreased as the ratio of sucrose or gluten to starch increased. Both peak temperature ($T_{G}$) and enthalpy values of gelatinization endotherm increased or decreased with increasing ratio of sucrose or gluten, respectively. Wheat starch gel with no sucrose and gluten recrystallized up to 4 weeks of storage at $4^{\circ}C$, whereas those with sucrose and gluten completed recrystallization within 1 week. Both wheat starch gels with no sucrose and gluten, and those with sucrose and gluten at storage temperature of $32^{\circ}C$ recrystallized up to 4 weeks, with wheat starch-sucrose-gluten (1 : 0.5 : 0.12) system, which had highest ratios of gluten and sucrose to starch, showing lowest recrystallization. Nucleation and propagation rates of starch gel recrystallization based on polymer crystallization principles can be converted into peak width (${\delta}T$) and peak temperature ($T_{R}$) of retrogradative endotherm by DSC, because higher nucleation rate at storage temperature of $4^{\circ}C$ close to $T_{g}$ showed higher ${\delta}T$, whereas higher propagation rate at $32^{\circ}C$ (close to $T_{G}$) had higher $T_{R}$.

Stabilization of Polyphenolic Antioxidants Using Inclusion Complexation with Cyclodextrin and Their Utilization as the Fresh-food Preservative (폴리페놀계 천연 항산화제의 cyclodextrin inclusion complexation을 통한 안정화와 식품 보존제로의 활용)

  • Kim, Tae-Kwon;Shin, Hyun-Dong;Lee, Yong-Hyun
    • Korean Journal of Food Science and Technology
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    • v.35 no.2
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    • pp.266-271
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    • 2003
  • Insoluble polyphenol antioxidants, quercetin and catechin, were stabilized through the complexation with cyclodextrin to increase heat and pH stabilities. Comparison of inclusion complex formabilities of quercetin and catechin with ${\alpha}-,\;{\beta}-$, and ${\gamma}-CDs$ revealed ${\beta}-CD$ to be the most suitable result. Optimal molar mixing ratio of ${\beta}-CD$ and quercetin or catechin for inclusion complex formation was found to be 1 : 1. Inclusion complexation was confirmed using differential scanning calorimetry. Solubility of ${\beta}-CD-antioxidant$ inclusion complexes increased compared with native antioxidants, Stability against temperature and pH of ${\beta}-CD-antioxidant$ inclusion complex analyzed revealed antioxidant activities of ${\beta}-CD-quercetin$ and catechin inclusion complexes have higher stabilization compare to raw quercetin and catechin. Peroxide value of linoleic acid dissolved in water decreased substantionally after using ${\beta}-CD-quercetin$ inclusion complex. ${\beta}-CD-antioxidant$ inclusion complex can be used effectively as a fresh-food preservative.

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.

An Experimental Study on Hydration and Strength Development of High Blain Cement at Low Temperature (저온환경에서 고분말도 시멘트의 수화반응 및 강도발현 특성에 관한 실험적 연구)

  • Mun, Young-Bum;Kim, Hyeong-Cheol;Choi, Hyun-Kuk;Kim, Jae-Young;Lee, Han-Seung;Kim, Mok-Kyu
    • Journal of the Korea Institute of Building Construction
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    • v.15 no.4
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    • pp.367-373
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    • 2015
  • In this study, fundamental properties of cement were reviewed to apply high fineness cement at low temperature environment. The classified high fineness cement has large proportion of particles below $10{\mu}m$ which affects early hydration: an overall reaction of cement hydration faster. As a result of using high fineness cement, setting time of concrete was reduced and compressive strength was higher than OPC at all ages. Especially, compressive strength was more than double its value compared with OPC after three days curing in low temperature. Faster reaction and higher heat of hydration was verified by calorimetry early and maximum heat of hydration was analyzed by adiabatic temperature raising test. The analysis of this study confirmed that high fineness cement can be suitable to be used in low temperature environment.

Effects of Various Additives on the Thermal Properties and Gel Structure of Mackerel Surimi Prepared by Alkaline Washing under Reduced Pressure (몇가지 첨가물이 감압 알칼리 수세한 고등어 Surimi의 열특성 및 Gel 조직에 미치는 영향)

  • Park, Hyung-Sun;Park, Sang-Woo;Yang, Seung-Taek
    • Korean Journal of Food Science and Technology
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    • v.30 no.6
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    • pp.1350-1356
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    • 1998
  • An attempt was made to investigate the effects of additives (3%) such as egg white, soybean protein, corn starch and Read Amity-N (green bean starch 85%+psyllium husk 10%) on the thermal properties and gel structures of mackerel surimi and to examine the quality of surimi by using differential scanning calorimetry (DSC), rheometry and scanning electron microscopy (SEM). The thermal transition temperatures of mackerel surimi protein were 40, 52, 67 and $79^{\circ}C$ after those temperatures were changed to 37, 46, 57 and $76^{\circ}C$ after adding salt (3% NaCl). Addition of Read Amity-N and corn starch to surimi showed new peak at the temperature of $90^{\circ}C\;and\;92^{\circ}C$, respectively. The enhancing effects of gel strengths of mackerel surimi cooked gels prepared from adding four kinds of additives, respectively, were egg white > soybean protein > Read Amity-N > corn starch in order. Scanning electron microscopy showed a difference in fine structures between the cooked gels which were prepared with and without additives. Dispersion profiles of protein were more thick in cooked gel prepared with additive than in cooked gel prepared without additive.

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Cyclic fatigue resistance, torsional resistance, and metallurgical characteristics of M3 Rotary and M3 Pro Gold NiTi files

  • Pedulla, Eugenio;Lo Savio, Fabio;La Rosa, Giusy Rita Maria;Miccoli, Gabriele;Bruno, Elena;Rapisarda, Silvia;Chang, Seok Woo;Rapisarda, Ernesto;La Rosa, Guido;Gambarini, Gianluca;Testarelli, Luca
    • Restorative Dentistry and Endodontics
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    • v.43 no.2
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    • pp.25.1-25.10
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    • 2018
  • Objectives: To evaluate the mechanical properties and metallurgical characteristics of the M3 Rotary and M3 Pro Gold files (United Dental). Materials and Methods: One hundred and sixty new M3 Rotary and M3 Pro Gold files (sizes 20/0.04 and 25/0.04) were used. Torque and angle of rotation at failure (n = 20) were measured according to ISO 3630-1. Cyclic fatigue resistance was tested by measuring the number of cycles to failure in an artificial stainless steel canal ($60^{\circ}$ angle of curvature and a 5-mm radius). The metallurgical characteristics were investigated by differential scanning calorimetry. Data were analyzed using analysis of variance and the Student-Newman-Keuls test. Results: Comparing the same size of the 2 different instruments, cyclic fatigue resistance was significantly higher in the M3 Pro Gold files than in the M3 Rotary files (p < 0.001). No significant difference was observed between the files in the maximum torque load, while a significantly higher angular rotation to fracture was observed for M3 Pro Gold (p < 0.05). In the DSC analysis, the M3 Pro Gold files showed one prominent peak on the heating curve and 2 prominent peaks on the cooling curve. In contrast, the M3 Rotary files showed 1 small peak on the heating curve and 1 small peak on the cooling curve. Conclusions: The M3 Pro Gold files showed greater flexibility and angular rotation than the M3 Rotary files, without decrement of their torque resistance. The superior flexibility of M3 Pro Gold files can be attributed to their martensite phase.

A Sustainable and Viable Method to Recycle Oyster Shell Waste as an Alternative of Limestone in Limestone Calcined Clay Cement (LC3) (석회석 소성 점토 시멘트(LC3) 내 석회석 대체재로서 굴 패각의 친환경적인 재활용 방안)

  • Her, Sung-Wun;Suh, Heong-Won;Park, Jae-Yeon;Im, Su-Min;Bae, Sung-Chul
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.8 no.2
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    • pp.219-226
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    • 2020
  • Over the last decades, great efforts have been devoted to reuse industrial wastes and by-products from various industries as supplementary cementitious materials in order to reduce carbon dioxide(CO2) emission by reducing the use of Portland cement in construction. Oyster shell waste, originating from the fishery industry, is available in huge quantities in certain areas, and is generally discarded or landfilled. In this study, we aimed to reuse oyster shell as an alternative to limestone in limestone calcined clay cement(LC3). The oyster shell calcined clay cement(OC3) paste were produced and were characterized via X-ray diffraction, isothermal calorimetry, compressive strength tests, and thermogravimetry. The results revealed that OC3 pastes exhibited similar strength development and reactivities by pozzolanic reaction with LC3, which implies that oyster shell could be used as a substitute for limestone in LC3.