• Title/Summary/Keyword: Hot stage microscopy

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Hot stage microscopy and its applications in pharmaceutical characterization

  • Arun Kumar;Pritam Singh;Arun Nanda
    • Applied Microscopy
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    • v.50
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    • pp.12.1-12.11
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    • 2020
  • Hot stage microscopy (HSM) is a thermal analysis technique that combines the best properties of thermal analysis and microscopy. HSM is rapidly gaining interest in pharmaceuticals as well as in other fields as a regular characterization technique. In pharmaceuticals HSM is used to support differential scanning calorimetry (DSC) and thermo-gravimetric analysis (TGA) observations and to detect small changes in the sample that may be missed by DSC and TGA during a thermal experiment. Study of various physical and chemical properties such sample morphology, crystalline nature, polymorphism, desolvation, miscibility, melting, solid state transitions and incompatibility between various pharmaceutical compounds can be carried out using HSM. HSM is also widely used to screen cocrystals, excipients and polymers for solid dispersions. With the advancements in research methodologies, it is now possible to use HSM in conjunction with other characterization techniques such as Fourier transform infrared spectroscopy (FTIR), DSC, Raman spectroscopy, scanning electron microscopy (SEM) which may have additional benefits over traditional characterization techniques for rapid and comprehensive solid state characterization.

Thermal Behaviors of Ag Conductive Thick Film with Firing Temperature for Plasma Display Panel (PDP용 Ag 전도성 후막의 열적거동)

  • Hwang, Seong-Jin;Lee, Sang-Wook;Kim, Hyung-Sun
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.278-278
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    • 2007
  • Ag conductive thick film has been used in bus and address electrodes of PDP (Plasma display panel). In PDP fabrication, the firing temperature of electrode is normally $550{\sim}580^{\circ}C$. For the application of PDP industry, we investigated an Ag conductive thick film with firing temperature. Low melting glass frit was used in the conductive thick film. The thermal properties of Ag and frit were determined by a hot stage microscopy. Based on the our results, we suggest that the Ag conductive thick film should be considered of the firing temperature which is correlated to the shrinkage, conductivity, and shape of thick film.

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Measurement of the interfacial tension value for the polymer blends by breaking thread method (섬유사 붕괴 법(breaking thread)에 의한 고분자 블렌드의 계면장력 측정)

  • Son, Young-Gon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.8 no.5
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    • pp.1211-1214
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    • 2007
  • In this paper, the experimental details of the interfacial tension measurement by breaking thread method, which measures the interfacial tension between different polymer pairs, are described. The apparatus needed are a hot state, which melts the polymers, and an optical microscopy. The measured interfacial tension values are in goog agreement with the literature's values.

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Syntheses of Thermotropic Liquid-Crystalline Copoly(ester amide)s Containing a Flexible Spacer in the Main Chain and Their Structure Interpretation (Thermotropic copoly(ester amide)의 합성과 구조해석)

  • ;;Tosiyuki Uryu
    • Textile Coloration and Finishing
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    • v.2 no.4
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    • pp.237-244
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    • 1990
  • Syntheses and liquid-Crystallinites of thermotropic copoly (ester amide)s were investigated. The three components melt polycondensation of 4,4'-dicarboxy-$\alpha$, $\omega$-diphenoxyalkane as an A component, 4-4'diacetoxybiphenyl as a B, and p-N-acetoxy-aminobenzoic acid as a C gave the thrmotropic copoly(ester amide)s containing a flexible splacer in the polymer backbone. Diacetylated hydroquinone, methyl hydroquinone, chlorohydroquinone, and phenyl hydroquinone were used as anther B components. A polymer(6BPAB) having 10 mol% of C component and hexamethylene space. showed a typical nematic texture between $245^{\circ}C(T_m)\; and\; more\; than\; 360^{\circ]C(T_i)$. The melting points of the members of this series of polymers increased with decreasing methylene spacer. The polymer structure and mesomorphic nature were examined by solid and solution ^{13}C-NMR4 spectroscopy, cross polarizing microscopy with a hot stage, and X-ray diffactometry.

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Synthesis of Thermotropic Liquid-Crystalline Polyamides and Copolyamides Containing a Different Spacer in the Main Chain and Their Structure Interpretation (Spacer 의 변화에 의한 Thermotropic Polyamide 및 Copolyamide 의 합성)

  • ;;Toshiyuki Uryu
    • Textile Coloration and Finishing
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    • v.5 no.2
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    • pp.109-116
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    • 1993
  • Synthesis and liquid-crystallinites of thermotropic polyamides and copolyamides were investigated. Thermotropic polyamides and copolyamides containing a flexible spacer in the backbone were obtained by the two or three components melt polycondensations of 4,4'-dicarboxy-${\alpha}$${\omega}$-diphenoxy alkane as an A components, 4,4'-diacetoamido-3,3' dimethoxybiphenyl as a B, 1,4-diacetoamido-benzene (diacetylated p-phenylenediamine) was used as another amide-group-forming minomer. The content of the amide groups in the thermotropic polyamide and Copolyamide widely varied depending on the structure of the amide-group forming diacetoamido monomers. A polymer (9CLDI) showed a typical nematic texture between 218$^{circle}C$ ($T_m$) and 345$^{circle}C$($T_i$) The melting points of the members of this series of polymers increased with decreasing methylene spacer. The polymer structure and mesmorphic nature were examined by solid and solution ${^13}C$-NMR spectroscopy, cross polarizing microscopy with a hot stage.

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Vapor Phase Deposition and Characterization of Diamond Thin Films on Refractory Metals (내열금속 기판위에 다이아몬드 박막의 증착과 특성분석)

  • 홍성현;형준호
    • Korean Journal of Crystallography
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    • v.5 no.1
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    • pp.39-50
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    • 1994
  • Diamond thin films were deposited on silicon, molybdebum, titanum and tugsten substrates, and were chlwntnizen using scanning electron microscopy, X-ray diffraction analysis and Raman spectroscopy. From the result of experiment in various deposition periods, it was found that found that were nucleated and grown on interlayed carbide layers, which were formed on refractory metal substrates at the initial stage of.

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Warpage of Co-fired High K/Low K LTCC Substrate (고유전율/저유전율 LTCC 동시소성 기판의 휨 현상)

  • Cho, Hyun-Min;Kim, Hyeong-Joon;Lee, Chung-Seok;Bang, Kyu-Seok;Kang, Nam-Kee
    • Journal of the Microelectronics and Packaging Society
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    • v.11 no.3 s.32
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    • pp.77-82
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    • 2004
  • In this paper, warpages of heterogeneous LTCC substrates comprised of high K/low K hi-layered structure were investigated. The effect of glass content in high K LTCC layer on the warpage of substrate during co-firing process was examined. Shrinkage and dielectric properties of high K and low K green sheets were measured. In-situ camber observation by hot stage microscopy showed different camber development of heterogeneous LTCC substrates according to glass content in high K green sheet. High K green sheet containing $50\%$ glass was matched to low K green sheet in the shrinkage. Therefore, LTCC substrate of Low K/High K+$50\%$ glass structure showed flat surface after sintering.

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Effect of B2O3 Addition on Thermal, Structure, and Sealing Properties V2O5-P2O5-ZnO Glass (B2O3첨가에 따른 V2O5-P2O5-ZnO계 유리의 물성 및 구조와 봉착특성)

  • Sung, Aram;Kim, Yurian;Kim, Hyungsun
    • Korean Journal of Materials Research
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    • v.26 no.10
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    • pp.549-555
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    • 2016
  • We have investigated a glass-forming region of $V_2O_5-P_2O_5-ZnO$ glass and the effects of the addition of modifier oxides ($B_2O_3$) to the glass systems as a sealing material to improve the adhesion between the glass frits and a soda lime substrate. Thermal properties and coefficient of thermal expansion were measured using a differential scanning calorimetry, a dilatometer and a hot stage microscopy. Structural changes and interfacial reactions between the glass substrate and the glass frit after sintering (at $400^{\circ}C$ for 1 h) were measured by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and scanning electron microscope. The results showed that the adhesion strength increases as the content of $B_2O_3$ at 5 mol% increases because of changes in the structural properties. It seems that the glass structures change with $B_2O_3$, and the $Si^{4+}$ ions from the substrate are diffused to the sealing glass. From these results, we could understand the mechanism of strengthening of the adhesion of soda lime silica substrate by ion-diffusion from the substrate to the glass.

Synthesis and Characterization of Wholly Aromatic Polyester Liquid Crystalline Thermosets (전방향족 폴리에스터 열경화성 액정의 합성과 특성)

  • Moon, Hyun-Gon;Jung, Myung-Sup;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.36 no.1
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    • pp.9-15
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    • 2012
  • We prepared a series of aromatic liquid crystals (LCs) based on wholly aromatic ester units with the reactive end group methyl maleimide by means of melt condensation method, and the resulting LCs were thermally crosslinked to produce liquid crystalline thermoset (LCT) films. The synthesized LCs and LCTs were characterized with Fourier transform infrared (FTIR) spectroscopy, wide angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), thermomechanical analysis (TMA), and polarizing optical microscopy (POM) with a hot stage. The glass transition temperature ($T_g$) and coefficient of thermal expansion are strongly affected by the mesogen units in their main chain structures. The $p$-substituted biphenyl LC was found to have the highest thermal property value.

Liquid Crystalline Thermoset Films Based on Wholly Aromatic Copolymers (전방향족 공중합체의 열경화성 액정필름)

  • Moon, Hyun-Gon;Ahn, Yong-Ho;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.34 no.4
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    • pp.369-375
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    • 2010
  • We used melt polymerization method to prepare a series of aromatic liquid crystals (LCs) based on aromatic ester and amide units with the reactive methyl-maleimide end group, and then the resulting thermally cross-linked LCs to produce LC thermoset films by means of solution casting and the followed heat treatment. The synthesized LCs and LCTs were characterized by Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), thermomechanical analysis (TMA), X-ray diffractometry (XRD), and polarizing optical microscopy (POM) with a hot stage. All of the LCs prepared by melt polymerization method formed smectic mesophases. The thermal properties of the LC and LCT films were strongly affected by the mesogen units in the main chain structures. The thermal expansion coefficients of samples were in the range of 27.72~50.95 ppm/$^{\circ}C$.