• Title/Summary/Keyword: Thermo-optical 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.

Analysis of Thermo-Acoustic Emission from Damage in Composite Laminates under Thermal Cyclic Loading (열하중을 받는 복합재료 적층판의 손상에 대한 열-음향방출해석)

  • Kim, Young-Bok;Min, Dae-Hong;Lee, Deok-Bo;Choi, Nak-Sam
    • Journal of the Korean Society for Nondestructive Testing
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    • v.21 no.3
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    • pp.261-268
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    • 2001
  • An investigation on nondestructive evaluation of thermal stress-nduced damage in the composite laminates (3mm in thickness and $[+45_6/-45_6]_s$ lay-up angles) has been performed using the thermo-acoustic emission technique. Reduction of thermo-AE events due to repetitive thermal load cycles showed a Kaiser effect. An analysis of the thermo-AE behavior determined the stress free temperature of composite laminates. Fiber fracture and matrix cracks were observed using the optical microscopy, scanning electron microscopy and ultrasonic C-sean. Short-Time Fourier Transform of thermo-AE signals offered the time-frequency characteristics which might classily the thermo-AE as three different types to estimate the damage processes of the composites.

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Design of Dynamically Focus-switchable Fresnel Zone Plates Based on Plasmonic Phase-change VO2 Metafilm Absorbers

  • Kyuho Kim;Changhyun Kim;Sun-Je Kim;Byoungho Lee
    • Current Optics and Photonics
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    • v.7 no.3
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    • pp.254-262
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    • 2023
  • Novel thermo-optically focus-switchable Fresnel zone plates based on phase-change metafilms are designed and analyzed at a visible wavelength (660 nm). By virtue of the large thermo-optic response of vanadium dioxide (VO2) thin film, a phase-change material, four different plasmonic phase-change absorbers are numerically designed as actively tunable Gires-Tournois Al-VO2 metafilms in two and three dimensions. The designed phase-change metafilm unit cells are used as the building blocks of actively focus-switchable Fresnel zone plates with strong focus switching contrast (40%, 83%) and high numerical apertures (1.52, 1.70). The Fresnel zone plates designed in two and three dimensions work as cylindrical and spherical lenses in reflection type, respectively. The coupling between the thermo-optic effect of VO2 and localized plasmonic resonances in the Al nanostructures offer a large degree of freedom in design and high-contrast focus-switching performance based on largely tunable absorption resonances. The proposed method may have great potential in photothermal and electrothermal active optical devices for nonlinear optics, microscopy, 3D scanning, optical trapping, and holographic displays over a wide spectral range including the visible and infrared regimes.

The Characteristics of Bonding for Thermo-plastic using Solar Energy (태양에너지를 이용한 열경화성 플라스틱 접합특성)

  • Kim, Ok-Sam;Kim, Il-Soo;Son, Joon-Sik;Seo, Joo-Hwan;Moon, Chae-Joo
    • Transactions of the Korean Society of Machine Tool Engineers
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    • v.16 no.2
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    • pp.106-111
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    • 2007
  • In this research work attempts were made to study the bonding of thermo-plastics with adhesives using solar radiation. In order to study the curing behaviour necessary experiments were conducted under varying conditions of temperature, exposure time and power of solar energy. The cured samples were then studied under the optical microscope before subjecting to tensile testing in order to study their mechanical properties of thermo-plastics. The fracture surfaces were further studied under the Scanning Electron Microscopy(SEM) in order to research the microstructural changes that are taken place during curing. In order to measure the performance of solar energy cured joints the parameters such as; bond strength, surface morphology, the microstructual changes, variation in properties of adhesives bonded joints are compared to that of specimen cured at ambient conditions and specimen cured using microwave techniques.

A study on Adhesion and Wear Resistance of Vanadium Carbide Coating on Die Steels by Immersing in Molten Borax Bath (용융 붕사욕 침지법에 의해 금형용 강에 형성된 VC coating층의 밀착성과 내마모성에 관한 연구)

  • Lee, B.K.;Nam, T.W.
    • Journal of the Korean Society for Heat Treatment
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    • v.13 no.2
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    • pp.71-84
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    • 2000
  • A study on adhesion and wear resistance of VC(vanadium carbide) coating on die steels, STD11 and STD61, has been carried out. The VC coating on the die steels was made by immersing them in molten borax bath, a kind of TRD(thermo-reactive deposition and diffusion). Adhesion strength and wear resistance were investigated using scratch test, indentation test and plate-disc test(Ogoshi type) respectively. The influence of sliding distance on the amount of wear has been determined and dominant wear mechanisms has been characterized using optical microscopy, scanning electron microscopy and EDS spectroscopy. The critical adhesion strength($L_c$) between VC coating layer and substrate(STD11) was increased to 60N($L_c$) in the scratch test. In the case of STD61, the strength increased to 24N. The wear resistance of VC coated die steels was excellent because the diffusion layer formed just below the coating layer. The dominant wear mechanism was identified as adhesive wear for VC coating die steels which were worn by combination of cracking and plucking of VC fragments and disc.

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Detection and Evaluation of Microdamages in Composite Materials Using a Thermo-Acoustic Emission Technique (열-음향방출기법을 이용한 복합재료의 미세손상 검출 및 평가)

  • 최낙삼;김영복;이덕보
    • Composites Research
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    • v.16 no.1
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    • pp.26-33
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    • 2003
  • Utilizing a thermo-acoustic emission (AE) technique, a study on detection and evaluation of microfractures in cross-ply laminate composites was performed. Fiber breakages and matrix fractures formed by a cryogenic cooling at $-191^{\circ}C$ were observed with ultrasonic C-scan, optical and scanning electron microscopy. Those microfractures were monitored in a non-destructive in-situ state as three different types of thermo-AE signals classified on the basis of Fast-Fourier Transform and Short-Time Fourier Transform. Thus, it was concluded that real-time estimation of microfracture processes being formed during cryogenic cooling could be accomplished by monitoring such different types of thermo-AEs in each time-stage and then by analyzing thermo-AE behaviors for the respective AE types on the basis of the AE signal analysis results obtained during thermal heating and cooling load cycles.

Synthesis and Characterization of CuInS2 Semiconductor Nanoparticles and Evolution of Optical Properties via Surface Modification (CuInS2 나노 반도체 합성 및 표면 개질을 통한 광학적 효율 분석 연구)

  • Yang, Hee-Seung;Kim, Yoo-Jin
    • Journal of Powder Materials
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    • v.19 no.3
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    • pp.177-181
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    • 2012
  • Copper composite materials have attracted wide attention for energy applications. Especially $CuInS_2$ has a desirable direct band gap of 1.5 eV, which is well matched with the solar spectrum. $CuInS_2$ nanoparticles could make it possible to develop color-tunable $CuInS_2$ nanoparticle emitter in the near-infrared region (NIR) for energy application and bio imaging sensors. In this paper, $CuInS_2$ nanoparticles were successfully synthesized by thermo-decomposition methods. Surface modification of $CuInS_2$ nanoparticles were carried out with various semiconductor materials (CdS, ZnS) for enhanced optical properties. Surface modification and silica coating of hydrophobic nanoparticles could be dispersed in polar solvent for potential applications. Their optical properties were characterized by UV-vis spectroscopy and photoluminescence spectroscopy (PL). The structures of silica coated $CuInS_2$ were observed by transmission electron microscopy (TEM).

Prediction of Solidification Path in Al-Si-Fe Ternary System and Experimental Verification (Al-Si-Fe 3원계 조성의 응고경로 예측 및 실험적 검증)

  • Lee, Sang-Hwan;Lee, Sang-Mok
    • Journal of Korea Foundry Society
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    • v.30 no.1
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    • pp.34-45
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    • 2010
  • The effects of alloy elements and cooling rate on the solidification path and the formation behavior of $\beta$ phase in Fe-containing Al-Si alloys were studied based on the thermodynamic analysis and the pertinent experiments. The thermodynamic calculation was systematically performed by using Thermo-Calc program. For the thermodynamic analysis in high alloy region of Al-Si-Fe ternary system, a thermodynamic database for Thermo-Calc was correctly updated and revised by the collected up-to-date references. For the thermodynamic-based prediction of various solidification paths in Fe-containing Al-Si system, liquidus projection of Al-Si-Fe ternary system, including isotherms, invariant, monovariant, bivariant reactions and equilibrium temperatures, was calculated and analyzed as functions of composition and temperature. The calculated results were compared to the experimental results using various casting specimens. In order to analyze various solidification sequences as functions of Si and Fe content, 4 representative alloy compositions, low Fe content in both low and high Si contents and high Fe content again in both low and high Si contents, were designed in this study. For better understanding of the influence of cooling rate on the formation behavior of $\beta$ phase, 4 alloys were solidified under furnace and rapidly cooled conditions. Cooling curves of solidified alloys were recorded by thermal analysis. Various important solidification events were evaluated using the first derivative-cooling curves. Microstructures of the casting samples were studied by the combined analysis of optical microscopy (OM) and scanning electron microscopy (SEM).

Characterizations of Flexible Clay-PVA Hybrid Films: Thermo-optical Properties, Morphology, and Gas Permeability (유연한 점토-폴리(비닐 알코올) 하이브리드 필름의 특성 연구: 열적.광학적 성질, 모폴로지, 및 가스 투과성)

  • Shin, Ji-Eun;Ham, Mi-Ran;Kim, Jeong-Cheol;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.35 no.5
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    • pp.402-408
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    • 2011
  • To improve $Na^+$-saponite(SPT) film flexibility, we prepared SPT hybrid clay films with various poly(vinyl alcohol) (PVA) concentrations(0~10 wt%) using the solution intercalation method. In this study, we investigated the thermo-optical properties, morphology, and gas permeability of the SPT hybrid films. We also examined the relationship between the film properties and PVA content using wide angle X-ray diffraction measurements(XRD), field emission scanning electron microscopy(FESEM), differential scanning calorimetry(DSC), thermogravimetric analysis(TGA), thermomechanical analysis(TMA), ultraviolet-visible(UV-vis) spectroscopy, and oxygen transmission rate($O_2$TR) testing. The properties of the clay hybrid films were strongly affected by PVA filler content. The presence of a small amount of PVA was sufficient to improve the flexibility of SPT hybrid films.

SBA-15 Supported Fe, Ni, Fe-Ni Bimetallic Catalysts for Wet Oxidation of Bisphenol-A

  • Mayani, Suranjana V.;Mayani, Vishal J.;Kim, Sang Wook
    • Bulletin of the Korean Chemical Society
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    • v.35 no.12
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    • pp.3535-3541
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    • 2014
  • Bisphenol A is considered as pollutant, because it is toxic and hazardous to living organisms even at very low concentrations. Biological oxidation used for removing this organic from waste water is not suitable and consequently application of catalytic wet oxidation has been considered as one of the best options for treating bisphenol A. We have developed Fe/SBA-15, Ni/SBA-15 and Fe-Ni/SBA-15 as heterogeneous catalysts using the advanced impregnation method for oxidation of bisphenol A in water. The catalysts were characterized with physico-chemical characterization methods such as, powder X-ray diffraction (PXRD), FT-IR measurements, N2 adsorption-desorption isotherm, thermo-gravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis. This work illustrates activity of the catalysts for heterogeneous catalytic degradation reaction revealed with excellent conversion and recyclability. The degradation products identified were not persistent pollutants. GC-MS analysis identified the products: 2,4-hexadienedioic acid, 2,4-pentadienic acid and isopropanol or acetic acid. The leachability study indicated that the catalysts release very little metals to water. Therefore, the possibility of water contamination through metal leaching was almost negligible.