• Title/Summary/Keyword: TEM-EDS

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One-Pot Synthesis of Alkyl-Terminated Silicon Nanoparticles by Solution Reduction (표면 알킬기를 갖는 실리콘 나노입자의 One-Pot 용액환원 합성)

  • Yoon, Taegyun;Cho, Mikyung;Sun, Yang-Kook;Lee, Jung Kyoo
    • Korean Chemical Engineering Research
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    • v.49 no.5
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    • pp.577-581
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    • 2011
  • Silicon nanoparticles have attracted a great deal of scientific interests due to its intense photoluminescence in the visible spectral region and its potential applications in biological fluorescence maker, RGB (red, green, blue) display, photonics and photovoltaics etc. Practical applications making use of optical and physicochemical properties of Si nanoparticles requires an efficient synthetic method which allows easy modulation of their size, size distribution as well as surface functionalities etc. In this study, a one-pot solution reduction scheme is attempted to prepare alkyl-terminated Si nanoparticles (<10 nm) with Si precursors, (Octyl)$SiCl_3$ or mixture of (Octyl)$SiCl_3$ and $SiCl_4$, containing alkyl-groups using Na(naphthalide) as reducing agent. The surface capping of Si nanoparticles with octyl-groups as well as Si nanoparticle formation was achieved in one-pot reaction. The hexane soluble Si nanoparticles with octyl-termination were in the range of 2-10 nm by TEM and some oxide groups (Si-O-Si) was present on the surface by EDS/FTIR analyses. The optical properties of Si nanoparticles measured by UV-vis and PL evidenced that photoluminescent Si nanoparticles with alkyl-termination was successfully synthesized by solution reduction of alkyl-containing Si precursors in one-pot reaction.

Microstructures and Electrochemical Properties of Si-M (M : Cr, Ni) as Alloy Anode for Li Secondary Batteries (리튬이차전지용 Si-M (M : Cr, Ni) 합금 음극의 미세구조와 전기화학적 특성)

  • Lee, Sung-Hyun;Sung, Jewook;Kim, Sung-Soo
    • Journal of the Korean Electrochemical Society
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    • v.18 no.2
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    • pp.68-74
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    • 2015
  • To compare the microstructure and electrochemical properties between two binary alloys (Cr-Si, Ni-Si), two composition of binary alloys with the same capacity were selected using phase-diagram and prepared by matrix-stabilization method to suppress the volume expansion of Si by inactive-matrix. Master alloys were made by Arc-melting followed by fine structured ribbon sample preparation by Rapid Solidification Process (RSP, Melt-spinning method) under the same conditions. Also powder samples were produced by wet grinding for X-Ray Diffraction (XRD) and electrochemical measurements. As predicted from the phase diagram, only active-Si and inactive-matrix ($CrSi_2$, $NiSi_2$) were detected. The results of Scanning Electron Microscope (SEM) and Transmission Electron Microscopy - Energy Dispersive X-ray Spectroscopy (TEM-EDS) show that Cr-Si alloy has finer microstructure than Ni-Si alloy, which was also predictable through phase diagram. The electrochemical properties related to microstructure were evaluated by coin type full- and half-cells. Separately, self-designed test-cells were used to measure the volume expansion of Si during reaction. Volume expansion of Cr-Si alloy electrode with finer microstructure was suppressed significantly and improved in cycle capability, in comparison Ni-Si alloy with coarse microstructure. From these, we could infer the correlation of microstructure, volume expansion and electrochemical degradation and these properties might be predicted by phase diagram.

Effect of Ni Catalyst Thickness on Carbon Nanotube Growth Synthesized by Hot-filament PECVD (Ni 촉매층의 두께가 탄소나노튜브의 성장 형태에 미치는 영향)

  • Kim, Jung-Tae;Park, Yong-Seob;Kim, Hyung-Jin;Choi, Eun-Chang;Hong, Byung-You
    • Journal of the Korean Vacuum Society
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    • v.16 no.2
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    • pp.128-133
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    • 2007
  • In this study, we observed the shapes of CNTs formed with the thinckness of catalyst. Catalyst layer was grown by magnetron sputtering method and the thickness of Ni catalyst is the range from 20 to 80 nm. Also, the synthesis of CNT with Ni catalyst thickness was grown by hot-filament PECVD method. And, we investigated the composition of CNTs by using EDS measurement, also observed the shapes of CNTs by using HRTEM and FESEM measurements. In the result, through the TEM analysis, we observed the empty inside of CNTs and the multiwall CNTs, also confirmed the tip of CNT containing Ni. The composition of CNTs are consisted of an element of C, Ti, and Ni. As you shown the growth shapes of CNTs, the pretreatment of the catalyst before te growth of CNTs changed the particle size of the catalysts and grown the CNTs of the different shapes. Consequently, the best vertically alined and well-arranged CNTs exhibited from the substrate deposited at the catalyst thickness of 40 nm.

Synthesis of Trimetallic (PtRu-Sn/VC, PtRu-Ni/VC) Catalysts by Radiation Induced Reduction for Direct Methanol Fuel Cell (DMFC) (방사선환원법을 이용한 직접메탄올연료전지용(DMFC) 삼성분계촉매(PtRu-Sn/VC, PtRu-Ni/VC)의 합성)

  • Kim, Sang Kyum;Park, Ji Yun;Hwang, Sun Choel;Lee, Do Kyun;Lee, Sang Heon;Rhee, Young Woo;Han, Moon Hee
    • Clean Technology
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    • v.19 no.3
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    • pp.320-326
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    • 2013
  • Nano-sized PtRu-Ni/VC and PtRu-Sn/VC electrocatalysts were synthesized by a one-step radiation-induced reduction (RIR) (30 kGy) process using distilled water as the solvent and Vulcan XC-72 as the supporting material. The obtained electrocatalysts were characterized by transmission electron microscopy (TEM), scanning electron microscope energy dispersive spectroscopic (SEM-EDS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), respectively. The catalytic efficiency of electrocatalysts was examined for oxygen reduction, MeOH oxidation and CO stripping decreased in the following order, Hydrogen stripping : PtRu-Sn/VC > PtRu-Ni/VC > PtRu/VC$^{(R)}$ (E-TEK). MeOH oxidation : PtRu-Sn/VC > PtRu-Ni/VC > PtRu/ VC$^{(R)}$ (E-TEK). Unit cell performance : PtRu-Sn/VC > PtRu-Ni/VC > PtRu/VC$^{(R)}$ (E-TEK) catalysts.

Synthesis of Pt-Sn/Carbon Electrodes by Reduction Method for Direct Methanol Fuel Cell (환원법에 의한 직접 메탄올 연료전지(DMFC)용 Pt-Sn/Carbon 전극제조)

  • Jung, So-Mi;Shin, Ju-Kyung;Kim, Kwan-Sung;Baeck, Sung-Hyeon;Tak, Yong-Sug
    • Applied Chemistry for Engineering
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    • v.21 no.5
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    • pp.537-541
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    • 2010
  • Pt-Sn with various ratios was supported on carbon black after pretreatment in an acidic solution by a reduction method. The Pt/Sn ratio was controlled by varying the concentration of each component in the solution, and the influence of the composition on the electrocatalytic activities was investigated. The crystallinity of the synthesized materials was investigated by XRD (X-ray Diffraction), and the oxidation states of both the platinum and tin were determined by XPS (X-ray Photoelectron Spectroscopy). SEM (Scanning Electron Microscopy)-EDS (Energy Dispersive Spectroscopy) was utilized to examine the morphology and composition of the synthesized electrode, and the particle size of the Pt-Sn was analyzed by TEM (Transmission Electron Microscopy). The electrocatalytic activity for oxygen reduction was evaluated in a 0.5 M $H_2SO_4$ solution using a rotating disk electrode system. The activity and stability were found to be strongly dependent on the electrode composition (Pt/Sn ratio). The catalytic activity and stability for methanol oxidation were also measured using cyclic voltammetry (CV) in a mixture of 0.5 M $H_2SO_4$ and 0.5 M $CH_3OH$ aqueous solution. The addition of proper amount of Sn was found to significantly improve both catalytic activity and stability for methanol oxidation.

Optical Properties and Phenol Destruction Performance of Pd-inserted TiO2 Photocatalysts (Pd이 삽입된 TiO2 광촉매의 광학 특성 및 페놀 분해 성능 평가)

  • Do, Jeong Yeon;Kim, Teho;Sim, Hwanseok;Jeong, Hamin;Choi, Jae Hoon;Kang, Misook
    • Applied Chemistry for Engineering
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    • v.28 no.5
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    • pp.547-553
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    • 2017
  • This study focused on the difference of photocatalytic performance by the incorporation of Pd into the $TiO_2$ framework and suggested five different catalysts composed of $TiO_2$ and x mol% $Pd-TiO_2$ (x = 0.25, 0.5, 0.75, and 1.0). A typical sol-gel method was used to synthesize catalysts, and the phenol photodegradation performance of each catalysts was evaluated. The physicochemical and optical properties of catalysts were confirmed by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy/energy dispersive spectrometer (SEM/EDS), ultraviolet/visible spectroscopy (UV/Vis), photoluminescence spectroscopy (PL), and photocurrent measurements. With the addition of Pd ions, the band gap of catalysts was shortened and the charge separation between photogenerated electrons and holes easily also occurred. As a result, the phenol photo-destruction performance over 0.75 mol% $Pd-TiO_2$ catalyst was 3 times higher than that of pure $TiO_2$. This is believed to be due to Pd ions acted as an electron capturing function during photocatalysis.

Synthesis of Mesoporous Pt-Au Alloy Electrode by Electrodeposition Method for Direct Methanol Fuel Cell (전기화학적 증착법에 의한 직접 메탄올 연료전지(DMFC)용 메조포러스 백금-금 합금전극제조)

  • Park, Eun-Kyung;Ahn, Jae-Hoon;Kim, Young-Soo;Kim, Kyung-Hwa;Baeck, Sung-Hyeon
    • Korean Chemical Engineering Research
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    • v.46 no.4
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    • pp.727-731
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    • 2008
  • Mesoporous Pt-Au alloy films were successfully fabricated on ITO-coated glass by electrodeposition method using tri-blockcopolymer (P123) as a templating agent. The electrolyte consisted of 10 mM hydrogen hexachloroplatinate ($H_2PtCl_6$), 10 mM hydrogen tetrachloroaurate ($HAuCl_4$), and proper amount of P123. For comparison, control samples were electrodeposited without $HAuCl_4$ and P123. Film composition was determined by EDS(Energy Dispersive X-ray Spectroscopy), and the mesoporous structure was confirmed by TEM(Transmission Electron Microscopy). SEM(Scanning Electron Microscopy) was utilized to examine surface morphology, and it was observed that the addition of P123 affected the particle growth, resulting in the significant change of surface morphology. Methanol oxidation and CO oxidation were carried out to investigate electrocatalytic activities of synthesized samples. It was observed that the catalytic activity was strongly dependent on the film compositions. Compared with nonporous electrode prepared without P123 templating, mesoporous films prepared with P123 templating showed much higher catalytic activities and stability for both methanol oxidation and CO oxidation. These enhanced electrocatalytic activities were due to the high surface area and facilitated charge transfer of mesoporous films.

Synthesis and Characterization of a Series of PtRu/C Catalysts for the Electrooxidation of CO (일산화탄소 산화를 위한 PtRu/C 시리즈 촉매의 합성 및 특성 연구)

  • Lee, Seonhwa;Choi, Sung Mook;Kim, Won Bae
    • Clean Technology
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    • v.18 no.4
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    • pp.432-439
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    • 2012
  • The electrocatalytic oxidation of CO was studied using carbon-supported 20 wt% PtRu (PtRu/C) catalysts, which were prepared with different Pt : Ru atomic ratios from 7 : 3 to 3 : 7 using a colloidal method combined with a freeze-drying procedure. The bimetallic PtRu/C catalysts were characterized by various physicochemical analyses, including X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). CO stripping voltammetry measurements indicated that the addition of Ru with a Pt catalyst significantly improved the electrocatalytic activity for CO electrooxidation. Among the tested catalysts, the $Pt_5Ru_5/C$ catalyst had the lowest onset potential (vs.Ag/AgCl) and the largest CO EAS. Structural modification via lattice parameter change and electronic modification in the unfilled d band states for Pt atoms may facilitate the electrooxidation of CO.

Synthesis of Multi-Terminalized Magnetic-Cored Dendrimer for Adsorption of Chromium and Enhancement of Magnetic Recovery (크롬 흡착 및 자성회수율 향상을 위한 멀티터미널 자성코어 덴드리머의 합성)

  • Yeo, In-Hwan;Jang, Jun-Won;Kim, Lyung-Joo;Park, Jae-Woo
    • Journal of Korean Society of Environmental Engineers
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    • v.34 no.9
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    • pp.613-622
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    • 2012
  • A chrome absorbent that is useful in rapid magnetic recovery and recycling was developed though a synthesis of Multi-Terminalized Magnetic-core Dendrimer (MTMD). Divergence through coprecipitation and rotation growth was used for synthesis. The dendrimer was multi-terminilized through methyl propionate and glutaric acid. The property analysis of the synthesized sample was performed through XRD, FT-IR, TEM, EDS, TGA and zeta potential analyzer. A magnetic-core of MTMD had a magnetite crystal and the size of 4th generation dendrimer was identified to be from 15 nm to 20 nm. Through the analysis of the TGA, the rate of the dendrimer branch for the first generation dendrimer was about 7% and 3% of diminished weight occurred as the generation grows. Also, the potential of the dendrimer when multi-terminalized, had variation from 25.26 mV to -6.53 mV. As a result of MTMD adsorption experiment, it absorbed more than 80% within 5 minutes and indicated absorptivity of 6.308 mg/g. When it was compared with COOH Dendrimer (COOH-D) after magnetic recovery, the recovery time was rapidly reduced by more than half and it could recover 100% within 30 minutes. In case of the regeneration experiment that used chrome, it was identified to maintain the same adsorptivity for four runs.

Selective Catalytic Reduction (SCR) of NOx with NH3 on Sb-promoted VWTi Catalysts (Sb 첨가에 따른 VWTi 촉매의 암모니아 선택적 촉매 환원(SCR)을 통한 질소산화물 저감)

  • Kim, Su Bin;Choi, Gyeong Ryun;Shin, Jung Hun;Hong, Sung Chang
    • Applied Chemistry for Engineering
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    • v.32 no.1
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    • pp.35-41
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    • 2021
  • VWTi, which is used as a commercial catalyst in NH3-SCR, exhibits excellent denitrification performance at 300 to 400 ℃, but there is a problem that efficiency decreases at low temperatures below 300 ℃. Research on catalysts containing promoter to increase low-temperature denitrification efficiency is steadily progressing. However, research on the cause of the improvement in low-temperature denitrification efficiency of the catalyst and the catalyst properties is insufficient. In this study, it was confirmed that by adding Sb to VWTi, denitrification performance was improved by more than 10% in NH3-SCR reaction below 300 ℃. At this time, the space velocity and the size of the catalyst particles were controlled to exclude the influence of external/internal diffusion. In addition, the catalytic properties according to the presence or absence of Sb were investigated by performing BET, TEM/EDS, O2-TPD, H2-TPR and DRIFTs analysis. It was judged that the addition of Sb increased the adsorbed oxygen species on the surface of the catalyst, thereby enhancing the redox properties of the catalyst at low temperature and exhibiting excellent denitrification performance.