• Title/Summary/Keyword: One-pot synthesis

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Synthesis of Ce-doped In2O3 nanoparticles via a microwave-assisted hydrothermal pathway and their application as an ultrafast breath acetone sensor

  • Byeong-Hun Yu;Sung Do Yun;Chan Woong Na;Ji-Wook Yoon
    • Journal of the Korean institute of surface engineering
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    • v.56 no.6
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    • pp.393-400
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    • 2023
  • Acetone, a metabolite detected from the exhaled breath of people doing a diet, can be used for non-invasive monitoring of diet efficiency. Thus, gas sensors with rapid response and recovery characteristics to acetone need to be developed. Herein, we report ultrafast acetone sensors using Ce-doped In2O3 nanoparticles prepared by the one-pot microwave-assisted hydrothermal method. The pure In2O3 sensor shows a high response and fast response time (τres = 6 s) upon exposure to 2 ppm acetone at 300 ℃, while exhibiting a relatively sluggish recovery speed (τrecov = 1129 s). When 20 wt% Ce is doped, the τrecov of the sensor significantly decreased to 45 s withholding the fast-responding characteristic (τres = 6 s). In addition, the acetone response (resistance ratio, S) of the sensor is as high as 5.8, sufficiently high to detect breath acetone. Moreover, the sensor shows similar acetone sensing characteristics even under a highly humid condition (relative humidity of 60%) in terms of τres (6 s), τrecov (47 s), and S (4.7), demonstrating its high potential in real applications. The excellent acetone sensing characteristics of Ce-doped In2O3 nanoparticles are discussed in terms of their size, composition, phase, and oxygen adsorption on the sensing surface.

Synthesis of Organized $TiO_2$ Electrodes Using Graft Copolymer and Their Applications to Dye-Sensitized Solar Cells (가지형 공중합체를 이용한 나노구조 $TiO_2$ 제조 및 염료감응 태양전지 응용)

  • Ahn, Sung Hoon;Koh, Joo Hwan;Park, Jung Tae;Kim, Jong Hak
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.64.1-64.1
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    • 2010
  • The morphology of mesoporous $TiO_2$ films plays an important role in the operation of a DSSC. For example, the energy conversion efficiency of DSSCs with well-organized mesoporous $TiO_2$ films is much higher than those with traditional films possessing a random morphology. In previous research, well-organized mesoporous $TiO_2$ films have mainly been synthesized using an amphiphilic block copolymer, e.g., a poly(ethylene oxide) (PEO)-based template. A graft copolymer is more attractive than a block copolymer due to its low cost and the ease with which it can be synthesized. In this work, we provide the first report on the successful synthesis of well-organized mesoporous $TiO_2$ films templated by an organized graft copolymer as a structure directing agent. Well-organized mesoporous $TiO_2$ films with excellent channel connectivities were developed via the sol gel processusing an organized PVC-g-POEM graft copolymer synthesized by one-pot ATRP. The careful adjustment of copolymer composition and solvent affinity using a THF/$H_2O$/HCl mixture was used to systematically vary the material structure. The influence of the material structure on solar cell performance was then investigated. A solid-state DSSC employing both the graft copolymer templated organized 700 nm-thick $TiO_2$ films and graft copolymer electrolytes exhibited a solar conversion efficiency of 2.2% at 100 $mW/cm^2$. This value was approximately two-fold higher than that attained from a DSSC employing a random mesoporous $TiO_2$ film. The solar cell performance was maximized at 4.6% when the film thickness was increased to $2.5{\mu}m$. We believe that this graft copolymer-directed approach introduces a new and simple route toward the synthesis of well-organized metal oxide films as an alternative to a conventional block copolymer-based template.

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Fabrication of various carbon nanostructures by using different catalysts (촉매에 따른 다양한 탄소나노구조체 합성)

  • Choi, Kang-Ho;Yoo, In-Joon;Lee, Hee-Soo;Lee, Kyu-Hwan;Lim, Dong-Chan
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.3
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    • pp.133-140
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    • 2010
  • Carbon fiber has many potential applications in a wide array of fields of solar cell, fuel cell, batteries, and polymer matrix composites due to an exceptional mechanical properties and chemical stability. In this study, the effects of catalysts on the property of carbon nanostructures grown on the carbon fiber were systematically investigated. The surface treatment of carbon fiber and catalysts synthesis for carbon nanostructures growth were carried out by one-pot ELP method and thermal CVD, respectively. The surface morphology and crystal structure of carbon nanostructures were examined using a field emission scanning electron microscope and transmission electron microscope. Depending on the type of catalysts and the molar ratio, various types of carbon nanostructures like carbon nanotube, carbon nanofilament, carbon nanospring and etc. were synthesized on the surface of carbon fibers surface.

Bimetallic Co/Zn-ZIF as an Efficient Photocatalyst for Degradation of Indigo Carmine

  • Nguyen, Thanh Nhan;Nguyen, Hoang Phuc;Kim, Tae-Ho;Lee, Soo Wohn
    • Korean Journal of Materials Research
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    • v.28 no.1
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    • pp.68-74
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    • 2018
  • Cobalt-incorporated zeolitic imidazolate framework ZIF-8 was synthesized by a simple one-pot synthesis method at room temperature. Powder X-ray diffraction patterns and energy dispersive X-ray spectrum confirmed the formation of the bimetallic Co/Zn-ZIF structure. UV-Vis diffuse reflectance spectra revealed that the bimetallic ZIF had a lower HOMO-LUMO gap compared with ZIF-8 due to the charge transfer process from organic ligands to cobalt centers. A hydrolytic stability test showed that Co/Zn-ZIF is very robust in aqueous solution - the most important criterion for any material to be applied in photodegradation. The photocatalytic efficiency of the synthesized samples was investigated over the Indigo Carmine (IC) dye degradation under solar simulated irradiation. Cobalt incorporated ZIF-8 exhibited high efficiency over a wide range of pH and initial concentration. The degradation followed through three distinct stages: a slow initial stage, followed by an accelerated stage and completed with a decelerated stage. Moreover, the photocatalytic performance of the synthesized samples was highly improved in alkaline environment rather than in acidic or neutral environments, which may have been because in high pH medium, the increased concentration of hydroxyl ion facilitated the formation of hydroxyl radicals, a reactive species responsible for the breaking of the Indigo Carmine structure. Thus, Co/Zn-ZIF is a promising and green material for solving the environmental pollution caused by textile industries.

Ultralow-n SiO2 Thin Films Synthesized Using Organic Nanoparticles Template

  • Dung, Mai Xuan;Lee, June-Key;Soun, Woo-Sik;Jeong, Hyun-Dam
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3593-3599
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    • 2010
  • In an original effort, this lab attempted to employ polystyrene nanoparticles as a template for the synthesis of ordered and highly porous macroporous $SiO_2$ thin films, utilizing their high combustion temperature and narrow size distribution. However, polystyrene nanoparticle thin films were not obtained due to the low interaction between individual particles and between the particle and silicon substrate. However, polystyrene-polyacrylic acid (PS-AA) colloidal particles of a core-shell structure were synthesized by a one-pot miniemulsion polymerization approach, with hydrophilic polyacrylic acid tails on the particle surface that improved interaction between individual particles and between the particle and silicon substrate. The PS-AA thin films were spin-coated in the thickness ranges from monolayer to approximately $1.0\;{\mu}m$. Using the PS-AA thin films as sacrificial templates, macroporous $SiO_2$ thin films were successfully synthesized by vapor deposition or conventional solution sol-gel infiltration methods. Inspection with field emission scanning electron microscopy (FE-SEM) showed that the macroporous $SiO_2$ thin films consist of interconnected air balls (~100 nm). Typical macroporous $SiO_2$ thin films showed ultralow refractive indices ranging from 1.098 to 1.138 at 633 nm, according to the infiltration conditions, which were confirmed by spectroscopy ellipsometry (SE) measurements. This research shows how the synthetic control of the macromolecule such as hydrophilic polystyrene nanopaticles and silicate sol precursors innovates the optical properties and processabilities for actual applications.

Carbonylation of Bromobenzyl Bromide Catalyzed by $Co_2(CO)_8(II)$. Selective Synthesis of Alkyl(alkoxymethyl)benzoate (코발트 카르보닐 촉매에 의한 브로모벤질 브로미드의 카르보닐화 (II). 알킬(알콕시메틸)벤조에이트의 선택성 합성)

  • Shim Sang Chul;Doh Chil Hoon;Youn Young Zoo;Cho Chan Sik;Woo Byung Won;Oh Dae Hee
    • Journal of the Korean Chemical Society
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    • v.35 no.1
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    • pp.90-95
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    • 1991
  • A method for the selective syntheses of alkyl (alkoxymethyl)benzoates from halobenzyl halides by two steps in one pot process is described. In the first step, benzyl halide moiety is etherified with alkoxide anion in alcohol by Williamson ether process. In the second step, aryl halide moiety is carbonylated to give alkyl (alkoxymethyl)benzoate with alcohol, Na$_2$CO$_3$, CH$_3$I, and carbon monoxide (1 atm) in the presence of a catalytic amount of Co$_2$(CO)$_8$ in excellent yield.

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One-pot synthesis of silica-gel-based adsorbent with Schiff base group for the recovery of palladium ions from simulated high-level liquid waste

  • Wu, Hao;Kim, Seong-Yun;Ito, Tatsuya;Miwa, Misako;Matsuyama, Shigeo
    • Nuclear Engineering and Technology
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    • v.54 no.10
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    • pp.3641-3649
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    • 2022
  • A simple solvothermal reaction was used to prepare a 3-aminopropyl-functionalized silica-gel-based adsorbent for adsorbing Pd(II) from the nitric acid solution. Scanning electron microscopy, fourier transform infrared spectroscopy, and thermogravimetry analysis were performed on the as-synthesized adsorbent to demonstrate the successful introduction of Schiff base groups. Batch experiments were used to investigate the effects of contact time, nitric acid concentration, solution temperature, and adsorption capacity. It is worth noting that the prepared adsorbent exhibited a higher affinity toward Pd(II) with the uptake approximately 100% even in a 2 M HNO3 solution. At an equilibrium time of 5 h, the maximum adsorption capacity of Pd(II) was estimated to be 0.452 mmol/g. The adsorbed Pd(II) could be completely eluted by dissolving 0.2 M thiourea solution in 0.1 M HNO3. Using a combination of particle-induced X-ray emission analysis and an X-ray photoelectron spectrometer, the adsorbed Pd was found to be uniformly distributed on the surface of the prepared adsorbent and the existing species were Pd(II) and zero-valent Pd(0). Due to the desirable performances, facile preparation method, and abundant raw material source, the prepared adsorbent demonstrated a high application potential in the recovery of Pd(II) from simulated high-level liquid waste treatment.

Compositions of fatty acids and structural identification in human breast milk (모유 중 지방산 조성 및 구조 분석)

  • Ji-Woo, Yoo;Young-Soo, Keum;Nam Mi, Kang
    • Analytical Science and Technology
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    • v.35 no.6
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    • pp.229-236
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    • 2022
  • Lipidomic analyses of transient breast milk are far more limited than those of other dairy products. As a preliminary analysis of breast milk lipidomes, analytical methods for polar and nonpolar lipids from transient breast milk were developed, and detailed fatty acid profiles were determined in this study. The newly developed methods include solvent fractionation of phospholipids and acyl glycerol, one-pot derivatization to FAMEs and pyridylcarbinol esters, and instrumental analysis, including GC-FID and GC-MS. The results indicate that breast milk contains 16 major common fatty acids with 8-22 carbons. Additionally, 29 minor fatty acids were identified, including odd-numbered fatty acids and branched analogues with 11-23 carbons. Their detailed concentrations in different fractions were measured using the internal standard method. In addition to ordinary fatty acids, breast milk contains several branched fatty acids, including iso/anteiso acids with 15-18 carbons. Structural studies have been performed on selected minor fatty acids via chemical synthesis.

Stereoselective Synthesis of Novel Bestatin Analogs (새로운 베스타틴 유사체의 입체선택적 합성)

  • Seo, Youngran;Lee, SooBeom;Kim, Young Gyu
    • Applied Chemistry for Engineering
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    • v.26 no.1
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    • pp.111-115
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    • 2015
  • Two new analogs of bestatin were prepared from $\small{D}$-leucine and $\small{D}$-valine in a stereoselective and efficient way. An aminopeptidase inhibitor bestatin shows significant biological effects on immunomodulation and is marketed for the treatment of acute myelocytic leukemia. The key intermediates, trans-oxazolidine methyl esters 2a and 2b, were obtained with more than 20 to 1 stereoselectivity in a one-pot procedure by the three cascade reactions between N-hydroxymethyl protected ${\alpha}$-amino aldehydes (4a and 4b) and phenylsulfonylnitromethane ($PhSO_2CH_2NO_2$) and the following in-situ ozonolysis. Basic hydrolysis of 2a and 2b, and then the peptide coupling with $\small{L}$-Leu-OMe produced the protected derivatives of two new bestatin analogs, 3a and 3b, respectively. The new isobutyl and isopropyl analogs of bestatin (1a and 1b) were produced in overall 51% and 38% yields, respectively, with high stereoselectivity from the corresponding protected ${\alpha}$-amino aldehydes 4 in a six-step process.

Separation of Aluminum and Iron from Platinum Mixture using Synthetic Extraction Resins (합성(合成) 추출(抽出) 수지(樹脂)를 이용(利用)한 백금용액(白金溶液)으로부터 알루미늄과 철(鐵)의 분리(分離))

  • Lim, Gwang-Il;Han, Dong-Hyuk;Hwang, In-Sung;Han, Choon;Lee, Jin-Young;Kim, Joon-Soo;Park, Hyung-Kyu
    • Resources Recycling
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    • v.20 no.3
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    • pp.68-76
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    • 2011
  • For the separation of aluminum and iron from platinum mixtures, extraction resins were synthesized and separation efficiencies were compared with those by commercial one, $P_{204}$. During synthesis, the suspension polymerization method was adopted with D2EHPA as an extractant. Also, benzoyl peroxide as a starter was divided into 3parts and injected for the uniform size and dispersion of resin particles. Comparison tests resulted in 100% separation of Fe and Pt for both synthetic and $P_{204}$ resins. In case of Al and Pt, synthetic and $P_{204}$ resin gave extraction efficiencies of 99.9% and 98.9%, respectively. Difference in extractant contents of synthetic resin(61.8%) and $P_{204}$(60%) was considered to give differences in separation efficiencies of aluminum and iron elements. For both resins, separation efficiencies of Al and Fe increased up to $55^{\circ}C$. According to FT-IR analyses of both resins, specific peaks of D2EHPA and crosslinked polystyrene were identified at the wavenumber of $1000cm^{-1}$ and $2900cm^{-1}$ respectively.