• 제목/요약/키워드: energy dispersive X-ray spectroscopy

검색결과 639건 처리시간 0.026초

K-Birnessite를 이용한 Li-Mn Spinel 나노입자 합성 및 전기화학적 특성 평가 (Hydrothermal Synthesis of Li-Mn Spinel Nanoparticle from K-Birnessite and Its Electrochemical Characteristics)

  • 김준일;이재원;박선민;노광철;선양국
    • 공업화학
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    • 제21권5호
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    • pp.590-592
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    • 2010
  • 본 연구에서는 리튬 2차 전지의 양극물질 중 하나인 Li-Mn spinel ($LiMn_2O_4$)을 합성하기 위해 전구체로 K-Birnessite ($K_xMnO_2{\cdot}{yH_2O}$)를 이용하였다. K-Birnessite는 과망간산칼륨[$KMnO_4$]과 우레아[$CO(NH_2)_2$]를 사용하여 수열합성법으로 합성하였고, K-Birnessite와 LiOH를 수열 반응시켜 Li-Mn spinel 나노입자를 제조하였다. 리튬함량에 따른 Li-Mn spinel 의 구조 및 형상 변화와 전기화학적 특성에 대한 경향성을 알아보기 위해 LiOH와 K-Birnessite의 몰 비를 조절하여 Li-Mn spinel를 합성하였다. 합성된 분말은 X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), thermogravimetry (TG)를 이용하여 물질의 구조 및 형상을 분석하였고, 정전류법으로 양극재의 용량과 율 특성을 비교 분석하였다. 그 결과 LiOH/K-Birnessite의 몰 비가 0.8일 때 가장 큰 용량($117\;mAhg^{-1}$)을 나타냈고, 몰 비가 증가할수록 Li-Mn spinel 중 리튬함량이 증가하여 용량은 감소하였으나, 입자크기는 작아져서 율 특성은 점점 향상되는 경향을 보였다.

Facile and Room Temperature Preparation and Characterization of PbS Nanoparticles in Aqueous [EMIM][EtSO4] Ionic Liquid Using Ultrasonic Irradiation

  • Behboudnia, M.;Habibi-Yangjeh, A.;Jafari-Tarzanag, Y.;Khodayari, A.
    • Bulletin of the Korean Chemical Society
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    • 제30권1호
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    • pp.53-56
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    • 2009
  • At room-temperature, a facile, seedless, and environmentally benign green route for the synthesis of star like PbS nanoclusters at 7 min in aqueous solution of 1-ethyl-3-methylimidazolium ethyl sulfate, [EMIM] [$EtSO_{4}$], room-temperature ionic liquid (RTIL), via ultrasonic irradiation is proposed. The X-ray diffraction studies display that the products are excellently crystallized in the form of cubic structure. An energy dispersive X-ray spectroscopy (EDX) investigation reveals the products are extremely pure. The absorption spectra of the product exhibit band gap energy of about 4.27 eV which shows an enormous blue shift of 3.86 eV that can be attributed to very small size of PbS nanoparticles produced and quantum confinement effect. A possible formation mechanism of the PbS nanoparticles using ultrasonic irradiation in aqueous solution of the RTIL is presented.

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

  • 정소미;신주경;김관성;백성현;탁용석
    • 공업화학
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    • 제21권5호
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    • pp.537-541
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    • 2010
  • 금속물질의 분산도를 높여주기 위해 열처리와 산처리를 수행한 carbon black에 다양한 비율의 Pt와 Sn을 담지 시킨 촉매를 환원법을 이용하여 합성하였다. Pt/Sn의 비율은 전구체 용액 내에서 상대적인 농도를 변화시켜 조절하였으며, Pt/Sn 비율에 따른 반응 특성을 조사하였다. XRD (X-ray Diffraction) 분석을 통해 합성된 촉매의 결정도를 확인하였고, XPS (X-ray Photoelectron Spectroscopy) 분석으로 Pt와 Sn의 산화가를 확인하였다. 합성된 촉매의 조성과 구조를 분석하기 위해 SEM (Scanning Electron Microscopy)-EDS (Energy Dispersive Spectroscopy) 분석과 TEM (Transmission Electron Microscopy) 분석을 수행하였다. 산소 환원 반응 특성은 0.5 M $H_2SO_4$ 수용액에서 RDE (Rotating Disk Electrode)를 이용하여 조사하였으며, 산소환원 촉매활성은 Pt/Sn의 비율에 크게 의존함을 확인하였다. 합성한 전극의 메탄올 산화반응은 전기화학분석장치(Potentiostat ; Princeton applied research, VSP)를 이용하여 0.5 M $CH_3OH$와 0.5 M $H_2SO_4$의 혼합수 용액에서 수행하였다. 메탄올 산화에 대한 전기화학적 촉매활성과 안정성을 평가한 결과 적절한 양의 Sn을 첨가한 촉매가 높은 촉매활성과 안정성을 나타냄을 확인하였다.

비 독성 셀레늄 팰릿을 이용하여 급속 열처리한 CIGS 흡수층 형성 (Fabrication of Cu(Inx,Ga1-x)Se2 absorber layers using non-toxic rapid thermal selenziation)

  • 천성현;권용현;조형균
    • 한국표면공학회:학술대회논문집
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    • 한국표면공학회 2013년도 춘계학술대회 논문집
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    • pp.160-160
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    • 2013
  • 본 실험에서는 CIGS 흡수층을 스퍼터링 방식과 급속열처리 장비를 이용한 2-step 방식을 이용하여 형성시켰다. 전구체는 DC 스퍼터링 방법으로 $Cu_{0.75}Ga_{0.25}/In$의 다층 전구체를 구성 후, 독성이 없는 셀레늄 팰릿을 graphite 상자에 넣어 급속열처리 장비로 온도를 $475{\sim}680^{\circ}C$로 온도를 조절하면서 셀렌화 하였다. 이렇게 구성된 CIGS 흡수층의 특성을 scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray differection (XRD)를 통해서 측정을 하였다.

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Zn/HA Coating on the Ti-xNb Alloys after Nanotube Formation for Dental Implant

  • Byeon, In-Seop;Choe, Han-Cheol
    • 한국표면공학회:학술대회논문집
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    • 한국표면공학회 2015년도 추계학술대회 논문집
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    • pp.139-140
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    • 2015
  • Zn/HA coating on the Ti-xNb alloys after nanotube formation for dental lmplant was researched using various experimental methods. Due to g ood biocompatibility and osteoconductivity, hydroxyapatite (HA) coating s on metallic biomedical implants were widely employed in orthopedic and dental applications. To improve biocompatibilities, Zinc (Zn) plays very important roles in the bone formation and immune reg ulations. The nanotube formed Zn-HA films were characterized with X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS).

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Surface Analysis of Copper-Tin Thin Films Synthesized by rf Magnetron Co-sputtering

  • 강유진;박주연;강용철
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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    • pp.272.2-272.2
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    • 2016
  • Copper-Tin (CuSn) thin films were synthsized by rf magnetron co-sputtering method with pure Cu and Sn metal targets with various rf powers and sputtering times. The obtained CuSn thin films were characterized by a surface profiler (alpha step), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), X-ray induced Auger electron spectroscopy (XAES), and contact angle measurement. The deposition rates were calculated by the thickness of CuSn thin films and sputtering times. We observed hexagonal Cu20Sn6 and cubic Cu39Sn11 phases from the films by XRD measurement. From the survey XPS spectra, the Cu and Sn main peaks were observed. Therefore, we could conclude CuSn thin films were successfully fabricated on the substrate in this study. The changes of oxidation states and chemical environment of the films were investigated with high resolution XPS spectra in the regions of Cu 2p, Cu LMM, and Sn 3d. Surface free energy (SFE) and wettability of the CuSn thin films were studied with distilled water (DW) and ethylene glycol (EG) using the contact angle measurement. The total SFE of CuSn thin films decreased as rf power on Cu target increased. The contribution to the total SFE of dispersive SFE was relatively superior to polar SFE.

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CORROSION BEHAVIOR OF AUSTENITIC AND FERRITIC STEELS IN SUPERCRITICAL WATER

  • Luo, Xin;Tang, Rui;Long, Chongsheng;Miao, Zhi;Peng, Qian;Li, Cong
    • Nuclear Engineering and Technology
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    • 제40권2호
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    • pp.147-154
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    • 2008
  • The general corrosion behavior of austenitic and ferritic steels(316L, 304, N controlled 304L, and 410) in supercritical water is investigated in this paper. After exposure to deaerated supercritical water at $480^{\circ}C$/25 MPa for up to 500 h, the four steels studied were characterized using gravimetry, scanning electron microscopy/energy dispersive X-ray spectroscopy(SEM/EDS), X-ray photoelectron spectroscopy(XPS), and X-ray diffraction(XRD). The results show that the 316L steel with a higher Cr and Ni content has the best corrosion-resistance performance among the steels tested. In addition to the oxide layer mixed with $Fe_{3}O_{4}$ and $(Fe,Cr)_{3}O_{4}$ that formed on all the samples, a $Fe_{3}O_{4}$ loose outer layer was observed on the 410 steel. The corrosion mechanism of stainless steels in supercritical water is discussed based on the above results.

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

  • 이성현;성재욱;김성수
    • 전기화학회지
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    • 제18권2호
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    • pp.68-74
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    • 2015
  • 본 실험에서는 리튬이차전지의 고용량 음극활물질로 주목받는 Si 합금의 부피팽창을 억제하기 위한 방법의 하나인 비활성-matrix상을 이용하고, 상태도를 이용하여 동일한 용량을 발현하는 Si계 이원계 합금 (Cr-Si, Ni-Si) 조성에서의 미세구조 및 전기화학적 특성을 비교/분석하였다. 급속응고공정(Rapid Solidification Process, Melt-spinning법)를 이용하여 동일조건하에서 리본 모양의 합금을 제작하였고, 제작된 리본합금은 동일조건에서 분쇄하여 X-선회절 (X-Ray Diffraction) 분석을 실시하였다. XRD 분석 결과, 상태도에서 예측된 것과 같이, 두 합금 모두 Si 상 및 비활성-matrix상($CrSi_2$$NiSi_2$)이 관찰되었으며, 이외의 제3의 상은 관찰되지 않았다. 또한, 주사전자현미경(SEM, Scanning Electron Microscope) 및 투과전자현미경-에너지분산분광법(TEM-EDS, Transmission Electron Microscopy - Energy Dispersive X-ray Spectroscopy)으로 미세구조를 살펴본 결과 Cr-Si 합금의 미세구조가 Ni-Si 합금보다 fine한 것을 알 수 있었고 이것은 상태도로부터 예측 가능하였다. 두 합금 조성에서 미세구조에 따른 전기화학적 특성을 비교 평가하기 위해 코인형 하프셀과 풀셀로 충방전 실험을 진행하였고 이와 별도로, 전극의 두께변화 측정이 가능하게 설계된 시험셀을 이용하여 반응 중 Si의 수축팽창을 측정하였다. coarse한 미세구조를 가진 Ni-Si 합금보다 fine한 미세구조를 갖는 Cr-Si 합금의 전극팽창이 비교적 잘 억제됨을 확인하였고, 충방전에 따른 수명 내구성도 우수함을 확인하였다. 이런 결과들로부터 합금의 조성에 따른 미세구조, 체적변화 및 전기화학적 열화와의 연관성을 유추할 수 있었다.

Enhanced Electrochemical Properties of Surface Modified LiMn2O4 by Li-Fe Composites for Rechargeable Lithium Ion Batteries

  • Shi, Jin-Yi;Yi, Cheol-Woo;Liang, Lianhua;Kim, Keon
    • Bulletin of the Korean Chemical Society
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    • 제31권2호
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    • pp.309-314
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    • 2010
  • The surface modified $LiMn_2O_4$ materials with Li-Fe composites were prepared by a sol-gel method to improve the electrochemical performance of $LiMn_2O_4$ and were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), and transmission electron microscopy (TEM)-EDS. XRD results indicate that all the samples (modified and pristine samples) have cubic spinel structures, and XRD, XPS, and TEM-EDS data reveal the formation of $Li(Li_xFe_xMn_{2-2x})O_4$ solid solution on the surface of particles. For the electrochemical properties, the modified material demonstrated dramatically enhanced reversibility and stability even at elevated temperature. These improvements are attributed to the formation of the solid solution, and thus-formed solid solution phase on the surface of $LiMn_2O_4$ particle reduces the dissolution of Mn ion and suppresses the Jahn-Teller effect.

Syntheses of Cu-In-Ga-Se/S nano particles and inks for solar cell applications

  • Jung, Duk-Young
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2010년도 제39회 하계학술대회 초록집
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    • pp.295-295
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    • 2010
  • Nanoparticles of the compound semiconductor, Cu(In, Ga)Se2 (CIGS), were synthesized in solution under ambient pressure below $100^{\circ}C$ and characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), optical absorption spectroscopy and energy-dispersive X-ray (EDX) analyses. These materials have chalcopyrite crystal structures and the particle sizes less than 100 nm. Synthetic conditions were studied for the crystallized CIGS nanoparticles formation to prevent from side products of Cu2Se, Cu2-xSe, and CuSe etc. The single phase CIGS nanoparticles were applied to coating of thin films photovoltaic cells. The electro deposition of CIGS thin films is also a good non-vacuum technology and under investigation. In aqueous solutions, the different chemical compositions of CIGS thin films were obtained, depending on pH, concentration of starting materials and deposition potentials. The surface morphology of the prepared CIGS thin films depends on the complexing ligands to the solutions during the electrochemical deposition.

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