• Title/Summary/Keyword: X-Ray diffraction measurement

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The Effect of polyethlenglycol on Electrocrystallization of zine Coat (아연전기도금의 존착성에 미치는 폴리에탈렌글리콜의 영향)

  • 김현태;정원섭;조남웅
    • Journal of the Korean institute of surface engineering
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    • v.30 no.2
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    • pp.128-135
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    • 1997
  • The effect of the polyethyledglycol(PEG) on the surface morphology and crystal orientation of electrodeposited zinc from a chloride (1.5M Zinc+7.0M chloriode) have been studied by means of electrochemical methodes, scanning electron microscopy, surface appearance measurement and X-ray diffraction patterns. The resistance of electrodeposit increased, whereas the evolution of hydrogen decreased with incrasing of molecular weight of the PEG. Large grains of electrodeposit were obtained from bath in the absence of organid additive. When the PEG was added, fine grained crystals were observed and the surface roughness was relatively small, but surface appearance deteriorated. The preferred orientation with a(101) plane parallel to the surface was obtained from the PEG addited bath.

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Morphological Control of Periodic Mesoporous Organosilica with Agitation

  • Park, Seong Su;Lee, Chi Heon;Jeon, Jong Hyeon;Jo, Sang Jun;Park, Dong Ho
    • Bulletin of the Korean Chemical Society
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    • v.22 no.9
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    • pp.948-952
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    • 2001
  • Periodic mesoporous organosilicas with rope-based morphology from a reaction gel composition of 1 BTME : 0.57 ODTMABr : 2.36 NaOH : 353 H2O were synthesized. While long rope-shaped product dominated in case of static synthesis condition , gyroid type products instead of rope shaped product appeared and rope shaped product disappeared with agitation. PMO with such a long rope shaped morphology is firstly reported. Additionally, various rope-based morphologies depending on the degree of bending, twisting, folding and winding of rope such as spirals, discoids, toroids, and worm-like aggregates were observed. White powdered products were characterized by X-ray diffraction, N2 sorption measurement, SEM and TEM. From XRD pattern and TEM image, ODTMA-PMO with hexagonal symmetry was identified. The pore diameter and BET surface area of ODTMA-PMO are $32.9{\AA}$ and 799 m2g-1 , respectively. Hexagonally arrayed channels run with long axis of rope and rope-based shapes with various degree of curvature, which was elucidated by using TEM images.

Characterization of Zirconium Sulfate Supported on Zirconia and Activity for Acid Catalysis

  • Son, Jong Rak;Gwon, Tae Dong;Kim, Sang Bok
    • Bulletin of the Korean Chemical Society
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    • v.22 no.12
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    • pp.1309-1315
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    • 2001
  • Zirconium sulfate supported on zirconia catalysts were prepared by impregnation of powdered $Zr(OH)_4$ with zirconium sulfate aqueous solution followed by calcining in air at high temperature. The characterization of prepared catalysts was performed using Fourier transform infrared (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and by the measurement of surface area. The addition of zirconium sulfate to zirconia increased the phase transition temperature of $ZrO_2$ from amorphous to tetragonal due to the interaction between zirconium sulfate and zirconia, and the specific surface area and acidity of catalysts increased in proportion to the zirconium sulfate content up to 10 wt% of $Zr(SO_4)_2$. Infrared spectra of ammonia adsorbed on $Zr(SO_4)2}ZrO_2$ showed the presence of Bronsted and Lewis acid sites on the surface. $10-Zr(SO_4)_2}ZrO_2$ calcined at $600^{\circ}C$ exhibited maximum catalytic activities for 2-propanol dehydration and cumene dealkylation. The catalytic activities for both reactions were correlated with the acidity of catalysts measured by ammonia chemisorption method.

Synthesis of LiFePO4 nano-fibers for cathode materials by electrospinning process

  • Kang, Chung-Soo;Kim, Cheong;Son, Jong-Tae
    • Journal of Ceramic Processing Research
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    • v.13 no.spc2
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    • pp.304-307
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    • 2012
  • Nano-fibers of LiFePO4 were synthesized from a metal oxide precursor by adopting electrospinning method. After calcination of the above precursor nano-fibers at 800 ℃, LiFePO4 nano-fibers with a diameter of 300 ~ 800 nm, were successfully obtained. Measurement were performed using X-ray diffraction (XRD), fourier transform infrared spectrometer (FT-IR), videoscope, scanning electron microscope (SEM) and atomic force microscope (AFM), respectively, were performed to characterize the properties of the as-prepared materials. The results showed that the crystalline phase and morphology of the fibers were largely influenced the starting materials and electrospinning conditions.

ELECTROCHEMICAL STUDY ON THE CORROSION BEHAVIOUR OF DENTAL AMALGAM IN ARTIFICIAL SALIVA (인공타액에서 아말감의 부식거동에 관한 전기화학적 연구)

  • Kim, Yeoung-Nam;Um, Chung-Moon
    • Restorative Dentistry and Endodontics
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    • v.13 no.2
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    • pp.221-235
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    • 1988
  • The purpose of this study was to observe characteristic properties through the polarization curves and EMPA images from 4 different types of amalgam obtained by using the potentiostats (EG & G PARC) & EPMA (Jeol JSM-35), to investigate the degree of corrosion of each phase of amalgam on the oxidation peak, and to identify corrosion products from the corroded amalgam by use of X-ray diffractometer(Rigaku). After each amlgam alloy and Hg were triturated as the direction of the manufacturer by means of the mechanical amalgamator(Shofu), the triturated mass was inserted into the cylindrical metal mold which was 12mm in diameter and 10mm in height and was condensed by means of routine manner. The specimen was removed from the mold and stored at room temperature for about 7 days. The standard surface preparation was routinely carried out. Anodic polarization measurement was employed to compare the corrosion behaviours of the amalgams in 0.9% saline solution(pH6.8~7.0) and artificial saliva (pH6.8~7.0) at $37^{\circ}C$. The open circuit potential was determined after 30 minutes' immersion of specimen in electrolyte and the potential scan was begun at the potential of 100mV cathodic from the corrosion potential. The scan rate was 1mV/sec and the surface area of amalgam exposed to the solution was 0.64$cm^2$ for each specimen. All the potentials reported are with respect to a saturated calomel electrode (SCE). EPMA images on the determined oxidation peaks of each amalgam in artificial saliva were observed. X-ray diffraction patterns of each sample were recorded before and after polarization in artificial saliva (Aristaloy, Caulk Spherical, Dispersalloy and Tytin: at +770mV, +585mV, +8.10m V and +680m V respectively) by use of a recording diffractometer. Nickel filtered Cu $K_{{\alpha}_1}$ radiation was used and sample was scanned at $4^{\circ}(2{\theta})/min.$ from $25^{\circ}$ to $80^{\circ}$. The following results were obtained. 1. Oxidation peak potential in artificial saliva shifted to more anodic direction than that in saline solution. 2. The corrosion potential of high copper amalgam was more anodic than the potential of low copper amalgam. 3. The current density was lower in artificial saliva than in saline solution. 4. One of the corrosion products, AgCl was identified by X-ray diffraction analysis. 5. ${\gamma}_2$ phase was the most susceptible to corrosion and e phase was stable in low copper amalgam and ${\eta}$' phase and Ag-Cu eutectic were susceptible to corrosion in high copper amalgam.

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Synthesis and Characterizations of Mn1+XCo2-XO4 Solid Solution Catalysts for Highly Efficient Li/Air Secondary Battery (고효율의 리튬/공기 이차전지 공기전극용 Mn1+XCo2-XO4 고용체 촉매 합성 및 분석)

  • Park, Inyeong;Jang, Jaeyong;Lim, Dongwook;Kim, Taewoo;Shim, Sang Eun;Park, Seok Hoon;Baeck, Sung-Hyeon
    • Journal of the Korean Electrochemical Society
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    • v.18 no.4
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    • pp.137-142
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    • 2015
  • $Mn_{1+X}Co_{2-X}O_4$ solid solutions with various Mn/Co ratios were synthesized by a combustion method, and used as cathode catalysts for lithium/air secondary battery. Their electrochemical and physicochemical properties were investigated. The morphology was examined by transmission electron microscopy (TEM), and the crystallinity was confirmed by X-ray diffraction (XRD) analyses. For the measurement of electrochemical properties, charge and discharge measurements were carried out at a constant current density of $0.2mA/cm^2$, monitoring the voltage change. Electrochemical impedance spectroscopy (EIS) analyses were also employed to examine the change in charge transfer resistance during charge-discharge process. $Mn_{1+X}Co_{2-X}O_4$ solid solutions showed enhanced cycleability as a cathode of Li/air secondary battery, and the performance was found to be strongly dependent on Mn/Co ratio. Among synthesized catalysts, $Mn_{1.5}Co_{1.5}O_4$ exhibited the best performance and cycleability, due to high charge transfer rate.

Morphological Structural and Electrical Properties of DC Magnetron Sputtered Mo Thin Films for Solar Cell Application

  • Fan, Rong;Jung, Sung-Hee;Chung, Chee-Won
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.389-389
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    • 2012
  • Molybdenum is one of the most important materials used as a back ohmic contact for $Cu(In,Ga)(Se,S)_2$ (CIGS) solar cells because it has good electrical properties as an inert and mechanically durable substrate during the absorber film growth. Sputter deposition is the common deposition process for Mo thin films. Molybdenum thin films were deposited on soda lime glass (SLG) substrates using direct-current planar magnetron sputtering technique. The outdiffusion of Na from the SLG through the Mo film to the CIGS based solar cell, also plays an important role in enhancing the device electrical properties and its performance. The structure, surface morphology and electrical characteristics of Mo thin films are generally dependent on deposition parameters such as DC power, pressure, distance between target and substrate, and deposition temperature. The aim of the present study is to show the resistivity of Mo layers, their crystallinity and morphologies, which are influenced by the substrate temperature. The thickness of Mo films is measured by Tencor-P1 profiler. The crystal structures are analyzed using X-ray diffraction (XRD: X'Pert MPD PRO / Philips). The resistivity of Mo thin films was measured by Hall effect measurement system (HMS-3000/0.55T). The surface morphology and grain shape of the films were examined by field emission scanning electron microscopy (FESEM: Hitachi S-4300). The chemical composition of the films was obtained by the energy dispersive X-ray spectroscopy (EDX). Finally the optimum substrate temperature as well as deposition conditions for Mo thin films will be developed.

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Preparation of Bismuth Thin Films by RF Magnetron Sputtering and Study on Their Electrical Transport Properties (RF 마그네트론 스퍼터링을 이용한 Bismuth 박막의 제조와 그 전기적 특성 연구)

  • Kim Dong-Ho;Lee Gun-Hwan
    • Journal of the Korean institute of surface engineering
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    • v.38 no.1
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    • pp.7-13
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    • 2005
  • Bismuth thin films were prepared on glass substrate with RF magnetron sputtering and effects of substrate temperature on surface morphology and their electrical transport properties were investigated. Grain growth of bismuth after nucleation and the onset of coalescense of grains at 393 K were observed with field emission secondary electron microscopy. Continuous thin films could not be obtained above 473 K because of grain segregation and island formation. Hall effect measurements showed that substrate heating yields the decrease of carrier density and the increase of mobility. Resistivity of bismuth film has its minimum (about 0.7 x 10/sup -3/ Ωcm) in range of 403~433 K. Annealing of bismuth films deposited at room temperature was carried out in a radiation furnace with flowing hydrogen gas. The change of resistivity was not significant due to cancellation of the decrease of carrier density and the increase of mobility. The abrupt change of electrical properties of film annealed above 523 K was found to be caused by partial oxidation of bismuth layer in x-ray diffraction analysis.

The Study of Growth and Characterization of CuGaSe$_2$ Sing1e Crystal Thin Films for solar cell by Hot Wall Epitaxy (HWE(Hot Wall Epitaxy)에 의한 태양 전지용 박막성장과 특성에 관한 연구)

  • 홍광준
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.07a
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    • pp.237-242
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    • 2001
  • The stochiometric mix of evaporating materials for the CuGaSe$_2$ single crystal thin films was prepared from horizontal furnace. To obtain the single crystal thin films, CuGaSe$_2$ mixed crystal was deposited on thoroughly etched semi-insulating GaAs(100) substrate by the Hot Wall Epitaxy (HWE) system. The source and substrate temperature were 610$^{\circ}C$ and 450$^{\circ}C$, respectively The crystalline structure of single crystal thin films was investigated by the photoluminescence and double crystal X-ray diffraction (DCXD). From the photocurrent spectrum by illumination of perpendicular light on the c-axis of the CuGaSe$_2$ single crystal thin film, we have found that the values of spin orbit splitting Δ So and the crystal field splitting ΔCr were 91 meV and 249.8 meV at 20 K, respectively. From the Photoluminescence measurement on CuGaSe$_2$ single crystal thin film, we observed free excition (Ex) existing only high quality crystal and neutral bound exiciton (D$^{\circ}$,X) having very strong peak intensity. Then, the full-width-at-half-maximum(FWHM) and binding energy 7f neutral acceptor bound excision were 8 meV and 35.2 meV, respectivity. By Haynes rule, an activation energy of impurity was 355.2 meV

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Effect of Geometrical shape and Cold work on Deformation and Hydrogen absorption behaivor in Palladium (팔라듐에서의 변형 및 수소흡수거동에 미치는 형상 및 가공의 영향)

  • Jung, Y.G.;Kim, K.H.;Kim, S.W.
    • Transactions of the Korean hydrogen and new energy society
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    • v.12 no.4
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    • pp.247-255
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    • 2001
  • The relation between the deformation and the geometrical shape, and the effect of cold work on the hydrogen absorption behavior in palladium were investigated. The Pd specimens used were plates and wires as cold worked and annealed states. The palladium plates and wires were loaded with hydrogen by electrochemical method. Experimental analyses were carried out through X -ray diffraction, micrometer measurement and decimal balance measurement. As the results, it is found that the effect of cold work on hydrogen absorption capacity was relatively small. The deformation of the palladium plates in thickness direction is larger than in other lateral directions whereas the palladium wires showed the same deformation ratio in all radius directions because of the circular distribution of coexisting $\alpha$ and $\beta$ phases. The products of plastic deformation such as slip lines and voids etc. were observed abundantly in all specimens although the specimens had undergone only once of a hydrogen absorption and desorption.

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