• 제목/요약/키워드: X-ray crystal diffraction

검색결과 1,556건 처리시간 0.034초

루비듐 증기와 반응한 제올라이트 4A에 대한 결정학적 연구 (Crystallographic Study on Zeolite 4A Reacted with Rubidium Vapor)

  • 송승환;김양;한영욱
    • 한국광물학회지
    • /
    • 제4권2호
    • /
    • pp.99-107
    • /
    • 1991
  • Three fully dehydrated fully Rb+-exchanged zeolite A single crystals have been prepared by the reduction of all Na+ ions in dehydrated Na12-A by rubidium vapor at various experimental conditions (220 $\leq$ T $\leq$ 33$0^{\circ}C$, 2 $\leq$ t $\leq$24 hours, and 0.1 $\leq$ PRb $\leq$ 1.1 Torr). Their structures were determined by single-crystal X-ray diffraction methods in the space group {{{{ RHO }}m3m (a=12.245(3) A) at 22(1)$^{\circ}C$. In these structures 12.6(2) to 13.5(2) Rb species are found per unit cell, more than the 12 Rb+ ions needed to balance the anionic charge of the zeolite framework, indication that the sorption of Rb0 has occurred. In each structure, three Rb+ ions per unit cell are located at the centers of 8-rings. Beyond that, the fractional occupancies observed are simply explained by two unit cell arrangments. In one, two Rb+ ions are in the sodalite unit near opposite 6-rings, six are in the large cavity near 6-ring, and one is in the large cavity near a 4-ring. In the other, three Rb species in the sodalite cavity (forming a triangle 3.7 A on an edge) each bond (3.4 A) through a 6-ring to an Rb species in the large cavity to give an (Rb6)4+ cluster of symmetry 3m (C3V). Five additional Rb+ ions fill the remaining large-cavity 6-ring sites.

  • PDF

활성화 이온빔 처리된 사파이어 기판상 MOCVD로 성장시킨 GaN의 열처리 효과 (Effects of Postannealing on GaN Grown by MOCVD on Reactive ion Beam Pretreated Sapphire Substrate)

  • 이상진;변동진;홍창희;김긍호
    • 한국재료학회지
    • /
    • 제11권3호
    • /
    • pp.191-196
    • /
    • 2001
  • 사파이어 (0001) 기판의 활성화 이온빔 (RIB) 처리 후 MOCVD에서 성장한 GaN박막의 열처리를 통한 구조 변화를 살펴보고, 전기적 성질의 변화를 관찰하기 위하여 전기로를 이용하여 열처리를 하였다. 시편의 분석을 위하여 DCXRD, Hall, TEM을 사용하였다. 100$0^{\circ}C$에서 시간을 변화시키면서 열처리한 시편에서 DCXRD의 FWHM는 약 50 arc-sec 정도 감소하였고, Hall 이동도는 약 80$\textrm{cm}^2$/V.sec 정도 향상되었다. 가장 좋은 Hall 이동도를 보인 처리된 시편과 처리 전 시편의 TEM 비교 관찰에서 전위 밀도는 56~69% 정도 감소하였고 격자의 변형도 줄어들었다. 이것은 결정의 질과 전기적 성질 사이의 상관관계를 암시하며, 기판의 RIB 처리와 성장 후 적절한 열처리의 조합이 MOCVD로 성장시킨 GaN 박막의 특성을 개선시키는 것을 명확하게 보여준다.

  • PDF

아연-공기전지용 페롭스카이트 산화물 촉매의 산소환원반응 특성 (Characterization of LaCoO3 Perovskite Catalyst for Oxygen Reduction Reaction in Zn-air Rechargeable Batteries)

  • 선호정;조명연;안정철;엄승욱;박경세;심중표
    • 한국수소및신에너지학회논문집
    • /
    • 제25권4호
    • /
    • pp.436-442
    • /
    • 2014
  • $LaCoO_3$ powders synthesized by Pechini process were pulverized by planetary ball-milling to decrease particle size and characterized as a catalyst in alkaline solution for oxygen reduction and evolution reaction (ORR & OER). The changes of physical properties, such as particle size distribution, surface area and electric conductivity, were analyzed as a function of ball-milling time. Also, the variations of the crystal structure and surface morphology of ball-milled powders were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The electrochemically catalytic activities of the intrinsic $LaCoO_3$ powders decreased with increasing ball-milling time, but their electrochemical performance as an electrode improved by the increase of the surface area of the powder.

Spectroscopic and Microstructural Analysis of Phase Transformation of Mg-PSZ/$Al_2O_3$ Fibers Prepared by Sol-Gel Method

  • Eun, Hee-Tai;Whang, Chin-Myung
    • The Korean Journal of Ceramics
    • /
    • 제2권2호
    • /
    • pp.102-110
    • /
    • 1996
  • The Mg-PSZ/$Al_2O_3$ fibers were fabricated by the sol-gel method. The added $Al_2O_3$ amounts were varied from 5 to 20 mol%. The phase transformation studies of a drawn Mg-PSZ/$Al_2O_3$ fibers were investigated by use of X-ray diffraction, IR and Raman spectroscopy. Microstructure and tensile strength of fibers were subjected to scanning electron microscopy and tensile strength tester. When $Al_2O_3$ was added to the Mg-PSZ fibers, it was found out from the analysis of XRD patterns and Raman spectra that a small amount of crystalline spinel($MgAl_2O_4$) started to form due to the reaction between $Al_2O_3$ and MgO, at $1000^{\circ}C$, and the phase transformation temperature of $ZrO_2$ crystal phase at different sintering temperatures increased. Also, the rapid grain growth with average size of 2.0 ${\mu}m$ shown in Mg-PSZ fiber at $1500^{\circ}C$ was considerably suppressed to 0.39 ${\mu}m$ by adding $Al_2O_3$ at the same temperature. When the Mg-PSZ/$Al_2O_3$ fibers containing 5 mol% $Al_2O_3$ were sintered $800^{\circ}C$ for 1 hr, average tensile strength of fibers was 0.9 GPs at diameters of 20 to 30 ${\mu}m$, but as the sintering temperatures was increased to $1000^{\circ}C$ for 1 hr, average tensile strength of fibers increased to 1.2 GPa in the same diameter range.

  • PDF

Effect of Reaction Conditions on the Particle Properties for Synthesis of Stabilized Zirconia by Modified Oxalate Method

  • Park, Hyun-wook;Lee, Young Jin;Kim, Jin-Ho;Jeon, Dae-Woo;Hwang, Hae Jin;Lee, Mi Jai
    • 한국세라믹학회지
    • /
    • 제53권5호
    • /
    • pp.529-534
    • /
    • 2016
  • Nanocrystalline powder of zirconia stabilized with 8 mol% yttria (YSZ) has been synthesized through oxalate process using $ZrOCl_2{\cdot}8H_2O$ and $Y(NO_3)_3{\cdot}6H_2O$ as starting materials. Understanding of the characteristic changes of YSZ powder as a function of processing conditions is crucial in developing dense and porous microstructures required for fuel cell applications. In this research, microstructure change, surface area, particle shape and particle size were measured as a function of different processing conditions such as calcination temperature, stirring speed and concentration of starting materials. The resultant crystallite sizes were calculated by XRD-LB (X-Ray Diffraction Line-Broadening) method, BET method, and morphology of the crystal was observed in TEM and FE-SEM. The TEM examination showed that the powder synthesized with 0.7 M of YSZ concentration had a spherical morphology with sizes ranging from 20 to 40 nm. However, the powder was gradually aggregated above 1.0 M of YSZ concentration with the aggregation being intensified as the YSZ concentration was increased.

Modified Oxalate Method로 의해 합성한 LSCF Cathode의 전기적 특성 (Electrical Properties of Synthesis LSCF Cathode by Modified Oxalate Method)

  • 이미재;김세기;지미정;박상선;최영현
    • 한국전기전자재료학회:학술대회논문집
    • /
    • 한국전기전자재료학회 2006년도 하계학술대회 논문집 Vol.7
    • /
    • pp.30-31
    • /
    • 2006
  • The LSCF cathode for Solid Oxide Fuel Cell was investigated to develop high performance unit cell at intermediate temperature by modified oxalate method with different electrolyte. The LSCF precursors using oxalic acid, ethanol and $NH_4OH$ solution were prepared at $80^{\circ}C$, and pH was controlled as 2, 6, 7, 8, 9 and 10. The synthesis precursor powders were calcined at $800^{\circ}C$, $1000^{\circ}C$ and $1200^{\circ}C$ for 4hrs. Unit cells were prepared with the calcined LSCF cathode, buffer layer between cathode and each electrolyte that is the LSGM, YSZ, ScSZ and CeSZ. The synthesis LSCF powders by modified oxalate method were measured by scanning electron microscope and X-ray diffraction. The interfacial polarization resistance of cell was characterized by Solatron 1260 analyzer. The crystal of LSCF powders show single phase at pH 2, 6, 7, 8 and 9, and the average particle size was about $3{\mu}m$. The electric conductivity of synthesis LSCF cathode which was calcined at $1200^{\circ}C$ shows the highest value at pH 7. The cell consist of GDC had the lowest interfacial resistance (about 950 S/cm@650) of the cathode electrode. The polarization resistance of synthesis LSCF cathode by modified oxalate method has the value from 4.02 to 7.46ohm at $650^{\circ}C$. GDC among the electrolytes, shows the lowest polarization resistance.

  • PDF

Selective Growth of Nanosphere Assisted Vertical Zinc Oxide Nanowires with Hydrothermal Method

  • Lee, Jin-Su;Nam, Sang-Hun;Yu, Jung-Hun;Yun, Sang-Ho;Boo, Jin-Hyo
    • 한국진공학회:학술대회논문집
    • /
    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
    • /
    • pp.252.2-252.2
    • /
    • 2013
  • ZnO nanostructures have a lot of interest for decades due to its varied applications such as light-emitting devices, power generators, solar cells, and sensing devices etc. To get the high performance of these devices, the factors of nanostructure geometry, spacing, and alignment are important. So, Patterning of vertically- aligned ZnO nanowires are currently attractive. However, many of ZnO nanowire or nanorod fabrication methods are needs high temperature, such vapor phase transport process, metal-organic chemical vapor deposition (MOCVD), metal-organic vapor phase epitaxy, thermal evaporation, pulse laser deposition and thermal chemical vapor deposition. While hydrothermal process has great advantages-low temperature (less than $100^{\circ}C$), simple steps, short time consuming, without catalyst, and relatively ease to control than as mentioned various methods. In this work, we investigate the dependence of ZnO nanowire alignment and morphology on si substrate using of nanosphere template with various precursor concentration and components via hydrothermal process. The brief experimental scheme is as follow. First synthesized ZnO seed solution was spun coated on to cleaned Si substrate, and then annealed $350^{\circ}C$ for 1h in the furnace. Second, 200nm sized close-packed nanospheres were formed on the seed layer-coated substrate by using of gas-liquid-solid interfacial self-assembly method and drying in vaccum desicator for about a day to enhance the adhesion between seed layer and nanospheres. After that, zinc oxide nanowires were synthesized using a low temperature hydrothermal method based on alkali solution. The specimens were immersed upside down in the autoclave bath to prevent some precipitates which formed and covered on the surface. The hydrothermal conditions such as growth temperature, growth time, solution concentration, and additives are variously performed to optimize the morphologies of nanowire. To characterize the crystal structure of seed layer and nanowires, morphology, and optical properties, X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, and photoluminescence (PL) studies were investigated.

  • PDF

높은 In 조성을 갖는 InGaN 구조의 열처리 변수에 따른 구조 및 광학적 특성

  • 이관재;조병구;이현중;김진수;이진홍;임재영
    • 한국진공학회:학술대회논문집
    • /
    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
    • /
    • pp.228.2-228.2
    • /
    • 2013
  • 본 논문은 InN와 GaN를 교대로 증착하는 교번성장법(Alternate Growth Method)을 이용해 형성한 높은 인듐(Indium) 조성을 갖는 InGaN (HI-InGaN) 구조의 열처리(Rapid Thermal Annealing, RTA) 온도 및 시간에 대한 구조와 광학적 특성을 Double Crystal X-ray Diffraction (DCXRD), Transmission Electron Microscopy와 Photoluminescence (PL) 장비를 사용하여 분석한 결과를 보고한다. DCXRD 스펙트럼에서 HI-InGaN 박막은 GaN(0002)로부터 $2.98^{\circ}$ 분리된 위치에서 회절 신호를 관찰 할 수 있다. 그리고 GaN와 HI-InGaN 신호 사이의 넓은 범위에서 미약하지만 신호가 관찰 되는데, 이는 InN와 GaN 계면에서 발생하는 상호확산 확률의 차이에 기인한 In 조성이 다른 InGaN 신호로 해석할 수 있다. 열처리 온도를 $775^{\circ}C$로 고정하고 시간을 10, 20, 30초로 각각 변화시켜 RTA를 진행한 DCXRD 스펙트럼에서 GaN(0002)로부터 $0.7{\sim}1.1^{\circ}$ 떨어진 위치에서 InGaN 피크를 확인 할 수 있다. RTA 시간이 증가 할수록 HI-InGaN 신호의 위치가 GaN 피크 방향으로 이동하며, 세기가 증가하는 것을 확인 할 수 있다. HI-InGaN의 PL 스펙트럼에서 상온 발광파장은 1369 nm 이며, 반치폭(Line-width)은 51.02 nm을 보였다. RTA 수행 후 발광파장에 따른 광세기가 각각 달라졌으며, 특히 900 nm 부근의 신호가 상대적으로 크게 증가하는 것을 확인할 수 있었다. RTA에 따른 HI-InGaN의 구조 및 광학적 특성 변화를 InN와 GaN 계면에서 In, Ga 원자의 상호확산 효과현상으로 논의할 예정이다.

  • PDF

Synthesis of CdS with Graphene by CBD(Chemical Bath Deposition) Method and Its Photocatalytic Activity

  • Pawar, R.C.;Lee, Jin-Yong;Kim, Eun-Jeong;Kim, Hyungsub;Lee, Caroline Sunyong
    • 한국재료학회지
    • /
    • 제22권10호
    • /
    • pp.504-507
    • /
    • 2012
  • Synthesis of RGO (reduced graphene oxide)-CdS composite material was performed through CBD (chemical bath deposition) method in which graphene oxide served as the support and Cadmium Sulfate Hydrate as the starting material. Graphene-based semiconductor photocatalysts have attracted extensive attention due to their usefulness for environmental and energy applications. The band gap (2.4 eV) of CdS corresponds well with the spectrum of sunlight because the crystalline phase, size, morphology, specic surface area and defects, etc., of CdS can affect its photocatalytic activity. The specific surface structure (morphology) of the photocatalyst can be effective for the suppression of recombination between photogenerated electrons and holes. Graphene (GN) has unique properties such as a high value of Young's modulus, large theoretical specific surface area, excellent thermal conductivity, high mobility of charge carriers, and good optical transmittance. These excellent properties make GN an ideal building block in nanocomposites. It can act as an excellent electron-acceptor/transport material. Therefore, the morphology, structural characterization and crystal structure were observed using various analytical tools, such as X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy. From this analysis, it is shown that CdS particles were well dispersed uniformly in the RGO sheet. Furthermore, the photocatalytic property of the resulting RGO-CdS composite is also discussed in relation to environmental applications such as the photocatalytic degradation of pollutants. It was found that the prepared RGO-CdS nanocomposites exhibited enhanced photocatalytic activity as compared with that of CdS nanoparticles. Therefore, better efficiency of photodegradation was found for water purification applications using RGO-CdS composite.

Characteristics of NbN Films Deposited on AISI 304 Using Inductively Coupled Plasma Assisted DC Magnetron Sputtering Method

  • Jun, Shinhee;Kim, Junho;Kim, Sunkwang;You, Yong Zoo;Cha, Byungchul
    • 한국표면공학회지
    • /
    • 제46권5호
    • /
    • pp.187-191
    • /
    • 2013
  • Niobium nitride (NbN) films were deposited on AISI 304 stainless steels by inductively coupled plasma (ICP) assisted dc magnetron sputtering method at different ICP powers, and the effects of ICP power on the phase formation, mechanical and chemical properties of the films were investigated. X-ray diffraction analysis (XRD) and field emission scanning electron microscopy (FESEM) were used to analyze the crystal structure and micro-knoop hardness was used to measure the hardness of the films. Also, 3-D mechanical profiler and a ball-on-disk wear tester were used to measure the thickness of the films and to estimate wear characteristics, respectively. The thickness of the films decreased but their hardness increased with increasing ICP power, and it was confirmed that only cubic ${\delta}$-NbN(200) remained at high ICP power. At lower ICP powers, a mixture of the hexagonal ${\delta}^{\prime}$-NbN and cubic ${\delta}$-NbN phases was obtained in the films and the hardness decreased. The corrosion potential value increased gradually with increasing ICP power, but the changes of ICP power did not significantly influence the overall corrosion resistance.