• Title/Summary/Keyword: ATR-FTIR spectroscopy

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Solid-phase Synthesis of 7-Aryl-benzo[b][1,4]oxazin-3(4H)-one Derivatives on a BOMBA Resin Utilizing the Smiles Rearrangement

  • Lee, Ji-Min;Yu, Eun-Ae;Park, Joo-Yeon;Ryu, In-Ae;Shin, Dong-Soo;Gong, Young-Dae
    • Bulletin of the Korean Chemical Society
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    • v.30 no.6
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    • pp.1325-1330
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    • 2009
  • A general method has been developed for the solid phase synthesis of drug-like 7-aryl-benzo[b][1,4]oxazin-3(4H)- one derivatives 6. The method relies on a novel, microwave irradiation promoted cyclization reaction of the BOMBA resin bound, N-substituted-$\alpha$-(2-chloro-4-bromophenoxy)acetamide 3 that takes place via a Smiles rearrangement. The 7-bromobenzo[1,4]oxazine 4, produced in this process is converted to 7-aryloxazin analogs 5 by utilizing Suzuki coupling with various substituted arylboronic acids. Finally, the target 7-aryl-benzo[b][1,4]oxazin-3(4H)-ones 6 are liberated from the resin by treatment with 5% TFA. The progress of the reactions involved in this preparative route can be monitored by using ATR-FTIR spectroscopy on a single bead. The target compounds, obtained by using this five-step sequence, are produced in high yields and purities.

Direct Bonding Characteristics of 2" 3C-SiC Wafers for Harsh Environment MEMS Applications (극한 환경 MEMS용 2" 3C-SiC기판의 직접접합 특성)

  • 정귀상
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.16 no.8
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    • pp.700-704
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    • 2003
  • This paper describes on characteristics of 2" 3C-SiC wafer bonding using PECVD (plasma enhanced chemical vapor deposition) oxide and HF (hydrofluoride acid) for SiCOI (SiC-on-Insulator) structures and MEMS (micro-electro-mechanical system) applications. In this work, insulator layers were formed on a heteroepitaxial 3C-SiC film grown on a Si (001) wafer by thermal wet oxidation and PECVD process, successively. The pre-bonding of two polished PECVD oxide layers made the surface activation in HF and bonded under applied pressure. The bonding characteristics were evaluated by the effect of HF concentration used in the surface treatment on the roughness of the oxide and pre-bonding strength. Hydrophilic character of the oxidized 3C-SiC film surface was investigated by ATR-FTIR (attenuated total reflection Fourier transformed infrared spectroscopy). The root-mean-square suface roughness of the oxidized SiC layers was measured by AFM (atomic force microscope). The strength of the bond was measured by tensile strength meter. The bonded interface was also analyzed by IR camera and SEM (scanning electron microscope), and there are no bubbles or cavities in the bonding interface. The bonding strength initially increases with increasing HF concentration and reaches the maximum value at 2.0 % and then decreases. These results indicate that the 3C-SiC wafer direct bonding technique will offers significant advantages in the harsh MEMS applications.ions.

UV-curing Behaviors and Mechanical Properties of UV-cured Polylactic Acid (PLA)

  • Lee, Seung-Woo;Park, Ji-Won;Park, Cho-Hee;Kim, Hyun-Joong;Eom, Young-Geun
    • Journal of the Korean Wood Science and Technology
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    • v.41 no.2
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    • pp.134-140
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    • 2013
  • UV curing was introduced via a chemical treatment by adding small amounts of a hexafunctional acrylic monomer and a photoinitiator to improve the mechanical properties of PLA. This study also employed a semi-interpenetrated structured polymer network through the process of UV-curing. The UV curing behaviors were investigated using FTIR-ATR spectroscopy and gel fraction determination. Also, the tensile strength was investigated with different hexafunctional acrylic monomer contents and UV doses. The results showed that the crosslinking of UV-induced chemically treated PLA started at a low content of hexafunctional acrylic monomer, resulting in a significant improvement of the mechanical properties compared to those of neat PLA due to crosslinking.

Improved performance of polyamide nanofiltration membranes by incorporating reduced glutathione during interfacial polymerization

  • Jiao, Zhiwei;Zhou, Linjie;Wu, Mengyuan;Gao, Kang;Su, Yanlei;Jiang, Zhongyi
    • Korean Journal of Chemical Engineering
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    • v.35 no.12
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    • pp.2487-2495
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    • 2018
  • Inspired by the specific amino acid sequence Asn-Pro-Ala (NPA) of water channel aquaporins (AQPs), we fabricated polyamide (PA) nanofiltration (NF) membranes by introducing reduced glutathione (GSH) in interfacial polymerization (IP) method. Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectrometry (XPS), scanning electron microscope (SEM), atomic force microscopy (AFM), zeta potential and static water contact angle measurement were employed to characterize the chemical composition, morphology, electronegativity and hydrophilicity of the NF membranes. The water flux of GSH/PIP-TMC NF membrane reached $32.00L\;m^{-2}h^{-1}$ at 0.2 MPa, which was approximately twice than that of pristine PIP-TMC NF membrane when the ratio of GHS to piperazidine (PIP) was 40% during IP process. More water channels were built as GSH was embedded into PA layer. The fabricated NF membranes also took on potent rejection for dyes and $Na_2SO_4$. This study presents a simple and facile method to simulate water channels-based biological materials which may find potential application in water treatment.

Crystallinity change of silkworm variety cocoons by heat treatment

  • Bae, Yu Jeong;Noh, Si Kab;Um, In Chul
    • International Journal of Industrial Entomology and Biomaterials
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    • v.42 no.1
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    • pp.7-13
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    • 2021
  • In the present study, the effect of heat treatment on the crystallinity of the outside of silkworm cocoon in nine different silkworm varieties was studied using ATR-FTIR spectroscopy. Additionally, the morphological structure and moisture regain of the cocoon were examined. The silkworm cocoon showed different colors and external features depending on the silkworm variety. Moreover, the thickness of the filament (15.3-27.6 ㎛) and moisture regain of the cocoon (9.0%-11.0%) were quite different depending on the silkworm variety. The crystallinity index of the cocoon outside varied from 52.1% to 56.1%, depending on the silkworm variety. J300 and MO42 showed the highest (56.1%) and the lowest (52.1%) crystallinity index, respectively, indicating that the microstructure of sericin of the outside of the cocoon was affected by the silkworm variety. Regardless of silkworm variety, their crystallinity indexes decreased from 52.1%-56.1% to 49.9%-43.6% depending on the silkworm variety by the heat treatment at 250 ℃. Interestingly, the crystallinity degree decrease was somewhat different depending on the silkworm variety, implying that the cocoon sericin microstructure is strongly influenced by the silkworm variety.

Characterization and experimental investigation for gamma-ray shielding competence of basalt-doped polyethylene nanocomposites

  • I.A. El-Mesady;F.I. El-Agawany;H. El-Samman;Y.S. Rammah;A. Hussein;R.A. Elsad
    • Nuclear Engineering and Technology
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    • v.56 no.2
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    • pp.477-484
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    • 2024
  • Experimental investigations on gamma - rays attenuation parameters and dielectric spectroscopic properties were done on a polymeric mixture with chemical composition (100-x) polyethylene + x basalt, where x = 0, 1, 3, 5, 10, and 20 wt%. Using the melting blending technique,six nanocomposite polymeric samples were prepared. The linear attenuation coefficient µ of each prepared set of samples was measured using a gamma-ray spectrometer including High Purity Germanium detector (HPGe) at energies 662.5, 1173.24, and 1332.51 keV. Based on the measured values of (µ) and sample density, the other effective shielding parameters were calculated. The values of µ showed an increase with increasing the dopant ratios from 0.0 up to 20.0 wt%. In addition, the µ values decreased with the photon's energy. The µ values were found 0.0847 up to 0.1175 cm-1, 0.0571 up to 0.0855 cm-1, and 0.0543 up to 0.075 cm-1 at 662.5, 1173.24, and 1332.51 keV. for B0 up to B20, respectively. The ATR spectroscopy was done on the prepared samples, and a good evidence of adding the filler to the pure polyethylene (HDPE) was obtained. Besides, an enhancement in dielectric constant by insertion of basalt NPs also recorded and can be attributed to the large dielectric constant of basalt compared to pure HDPE.

Study on the Copper-Arsenic Green Pigments used on Shamanic Paintings in the 19~20th century (19~20세기 무신도 등에 사용된 구리-비소 녹색 안료에 대한 연구)

  • Oh, Joon Suk;Choi, Jung Eun;Choi, Yoon Hee
    • Journal of Conservation Science
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    • v.31 no.3
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    • pp.193-214
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    • 2015
  • The green pigments of shamanic paintings (83 items) in the 19~20th century were analyzed with X-ray fluorescent spectrometer(XRF), scanning electron microscopy (SEM) and fourier transform infrared spectroscopy (ATR-FTIR). In 60 items, copper and arsenic were detected in green pigments of the paintings by XRF spectra. Cu $K{\alpha}$/As $K{\beta}$ (peak intensity ratio of copper and arsenic) of shamanic paintings of Bokgaedang (shrine), solemn paintings (romance of three kingdoms) of Donggwanwangmyo and unknown enshrined place were 5.93~12.04 and higher compared to 5.67-6.26 of standard emerald greens and 4.01~7.89 of remaining shamanic paintings. The SEM images of crystal forms of copper-arsenic green pigments were various. Crystal forms were divided into oval and round spherulite with intersecting plate crystals and spherulite with agglomerate plate crystals. The crystals of the latter were found in shamanic paintings of Bokgaedang (shrine), solemn paintings (romance of three kingdoms) of Donggwanwangmyo and unknown enshrined place and the former were found in the rest of shamanic paintings. Copper-arsenic green pigments of shamanic paintings were identified as Scheele's green from shamanic paintings of Bokgaedang (shrine) and romance of three kingdoms. Emerald green from the rest of shamanic paintings by ATR-FTIR. From analytical results, it is confirmed that Scheele's green of shamanic paintings of Bokgaedang and romance of three kingdoms was used in the 1850s~1870s and emerald green had been widely used from late 19th century to 1970 in the rest of shamanic paintings.

Characterization of Crosslinks of Maleic Anhydride-Grafted EPDM/Zinc Oxide Composite Using Dichloroacetic Acid/Toluene Cosolvent and Extraction Temperature (디클로로아세트산/톨루엔 공용매와 추출 온도를 이용한 무수말레산-그래프트 EPDM/산화 아연 복합체의 가교 특성 분석)

  • Kwon, Hyuk-Min;Choi, Sung-Seen
    • Elastomers and Composites
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    • v.48 no.4
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    • pp.288-293
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    • 2013
  • Crosslink characteristics of maleic anhydride-grafted EPDM (MAH-g-EPDM)/zinc oxide composite were investigated by weight losses after dichloroacetic acid (DCA)/toluene cosolvent extraction at different temperatures and by measurement of crosslink densities. The chemical changes were analyzed using attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). The weight losses by extraction at high temperature ($90^{\circ}C$) were remarkably greater than those at room temperature and those by DCA/toluene cosolvent extraction were greater than those by toluene one by more than 5 times. The crosslink densities were measured after the solvent extraction, and the second crosslink densities were higher than the first ones. The first crosslink density was lower when the extraction temperature was high, and it was much lower for the toluene extraction than for the DCA/toluene cosolvent extraction. The second crosslink density of the sample extracted with DCA/toluene cosolvent was greater than that extracted with toluene. The extracted components were depending on the extraction solvents and temperatures, for example; only strong crosslinked networks were remained when extracting with DCA/toluene cosolvent at high temperature, while only uncrosslinked polymer chains were extracted when extracting with toluene at room temperature. Therefore, crosslink characteristics of the MAH-g-EPDM/zinc oxide composite can be analyzed by comparison of the extracted components according to the extraction solvents and temperatures and by measurement of successive crosslink densities.

Mechanical Characteristics of CF Laminated Prepreg with UV-thermal Dual Curable Epoxy Resin (광·열경화형 수지를 이용한 탄소섬유 프리프레그의 물리적 특성)

  • Sim, Ji-hyun;Kim, Ji-hye;Park, Sung-min;Koo, Kwang-hoe;Jang, Key-wook;Bae, Jin-seok
    • Textile Coloration and Finishing
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    • v.29 no.1
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    • pp.37-44
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    • 2017
  • An issue of major concern in the utilization of laminated composites based epoxy resin is associated with the occurrence of delaminations or interlaminar cracks, which may be related to manufacturing defects or are induced in service by low-velocity impacts. A strong interfacial filament/brittle epoxy resin bonding can, however, be combined with the high fracture toughness of weak interfacial bonding, when the filaments are arranged to have alternate sections of shear stress. To improve this drawback of the epoxy resin, UV-thermal dual curable resin were developed. This paper presents UV-thermal dual curable resin which were prepared using epoxy acrylate oligomer, photoinitiators, a thermal-curing agent and thermoset epoxy resin. The UV curing behaviors and characteristics of UV-thermal dual curable epoxy resin were investigated using Photo-DSC, DMA and FTIR-ATR spectroscopy. The mechanical properties of UV-thermal dual curable epoxy resin impregnated CF prepreg by UV curable resin content were measured with Tensile, Flextural, ILSS and Sharpy impact test. The obtained results showed that UV curable resin content improves the epoxy toughness.

Synthesis and Comparison of EB- and UV-curable Monomers for Anti-fogging Coatings (전자선 및 자외선 경화형 방무코팅용 모노머의 합성 및 물성비교)

  • Cho, Jung-Dae;Lee, Jae-Sung;Kim, Yang-Bae;Hong, Jin-who
    • Applied Chemistry for Engineering
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    • v.16 no.3
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    • pp.449-455
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    • 2005
  • Electron beam (EB) and ultraviolet (UV) curable monomers (AF-1 with mono functionality and AF-2 with tetra functionality) containing hydroxy and acrylate group for anti-fogging coating were synthesized and applied to EB and UV-curable coating systems. The synthesized reactive AF-1 and AF-2 monomers were first formulated into UV-curable system and the optimization of film properties for anti-fogging coating was investigated. The 5:17.5 ratio for AF-1 and AF-2 was found to be the best optimized formulation for anti-fogging coating without destroying the other essential properties such as hardness, solvent resistance, and adhesion. The optimized formulation was applied to the EB-curable system, and EB and UV-curable systems were compared. The results demonstrated that both EB and UV-cured films coated on PC sheet showed excellent anti-fogging properties; however, the EB-cured film exhibited better hardness, adhesion, and water repellent properties than the UV-cured film.