• Title/Summary/Keyword: In-situ XRD

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Study on the Composition and Crystallization of TiNi Thin Films Fabricated by Pulsed Laser Deposition in Ambient Ar Gas (Ar가스 분위기에서 PLD방법으로 제작된 TiNi박막의 조성 및 결정성에 관한 연구)

  • Cha, J.O.;Shin, C.H.;Yeo, S.J.;Ahn, J.S.;Nam, T.H.
    • Journal of the Korean Vacuum Society
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    • v.16 no.2
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    • pp.116-121
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    • 2007
  • TiNi shape memory alloy(SMA) was fabricated by PLD(plused laser deposition) using equiatomic TiNi target. Composition and crystallization of TiNi thin films which were fabricated in ambient Ar gas(200m Torr)and vacuum($5{\times}10^{-6}\;Torr$) were investigated. Composition of TiNi thin films was characterized by energy-dispersive X-ray spectrometry (EDXS) and crystallization was confirmed by X-ray diffraction (XRD). The composition of films depends on the distance between target and substrate but does not sensitively depend on the substrate temperature. It is found that the composition of films can be easily controlled when substrate is placed inside plume in ambient Ar gas. It is also found that the in situ crystallization temperature ($ca.\;400^{\circ}C$) in ambient Ar gas is lowered in comparison with that of TiNi film prepared under vacuum. The low crystallization temperature in ambient Ar gas makes it possible to prepare the crystalline TiNi thin film without contamination.

Effect of Milling Medium Materials on Mechanical Alloying of Mo-65.8at%Si Powder Mixture (Mo-65.8at%Si 혼합분말의 기계적 합금화에 미치는 밀링매체 재료의 영향)

  • 박상보
    • Journal of Powder Materials
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    • v.4 no.3
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    • pp.179-187
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    • 1997
  • Milling media of steel and zirconia were used to produce $MoSi_2$ by mechanical alloying (MA) of Mo and Si powders. The effect of milling media on MA of Mo-65.8at%Si powder mixture has been investigated by SEM, XRD, DTh and in-situ thermal analysis. The powders mechanically alloyed by milling medium of steel for 8 hours showed the structure of fine mixture of Mo and Si, and those mechanically alloyed by milling medium of zirconia for longer milling time showed the structure of fine mixture of Mo and Si. The tetragonal $\alpha$-$MoSi_2$ Phase and the tetragonal $Mo_5Si_3$ phase appeared with small Mo peaks in the powders milled by milling medium of steel for 4 and 8 hours. The $\alpha$-$MoSi_2$ phase and the hexagonal $\beta$-$MoSi_2$ phase were formed after longer milling time. The $\alpha$-$MoSi_2$ phase appeared with large Mo peaks in the powders milled by milling medium of zirconia for 4 hours. The phases, $\alpha$-$MoSi_2$ and $\beta$-$MoSi_2$. were formed in the powders milled for longer milling time. DTA and annealing results showed that Mo and Si were transformed into $\alpha$-$MoSi_2$ and $Mo_5Si_3$, while $\beta$-$MoSi_2$ into $\alpha$-$MoSi_2$. In-situ thermal analysis results demonstrated that there were a sudden temperature rise at 212 min and a gradual increase in temperature in case of milling media of steel and zirconia, respectively. The results indicate that MA can be influenced by materials of milling medium which can give either impact energy on powders or thermal energy accumulated in vial.

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Preparation and Electrochemical Properties of PANI/TiO2 Composites for Supercapacitor Electrodes (수퍼커패시터 전극을 위한 폴리아닐린/TiO2 복합체의 제조 및 전기화학적 성질)

  • Park, Sukeun;Kim, Kwang Man;Lee, Young-Gi;Jung, Yongju;Kim, Seok
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.50-54
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    • 2012
  • In this study, PANI and PANI/$TiO_2$ composites were prepared as electrode materials for a supercapacitor application. Cyclic voltammetry (CV) was performed to investigate the supercapacity properties of these electrodes in an electrolyte solution of 6 M KOH. The PANI/$TiO_2$ composites were polymerized by amount of various ratios through a simple in-situ method. The morphological properties of composites were analyzed by SEM and TEM method. The crystallinity of the composite and $TiO_2$ particle size were identified using X-ray diffraction (XRD). In the electrochemical test, The electrode containing 10 wt% $TiO_2$ content against aniline units showed the highest specific capacitance (626 $Fg^{-1}$) and delivered a capacitance of 286 $Fg^{-1}$ reversibly at a 100 $mVs^{-1}$ rate. According to the surface morphology, the increased capacitance was related to the fact that nano-sized $TiO_2$ particles (~6.5 nm) were uniformly connected for easy charge transfer and an enhanced surface area for capacitance reaction of $TiO_2$ itself.

X-ray Scattering Study of Reactive Sputtered Ta-N/Ta/Si(001)Film as a Barrier Metal for Cu Interconnection (구리배선용 베리어메탈로 쓰이는 Ta-N/Ta/Si(001)박막에 관한 X-선 산란연구)

  • Kim, Sang-Soo;Kang, Hyon-Chol;Noh, Do-Young
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.05b
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    • pp.79-83
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    • 2001
  • In order to compare the barrier properties of Ta-N/Si(001) with those of Ta-N/Ta/Si(001), we studied structural properties of films grown by RF magnetron sputtering with various $Ar/N_2$ ratios. To evaluate the barrier properties, the samples were annealed in a vacuum chamber. Ex-situ x-ray scattering measurements were done using an in-house x-ray system. With increasing nitrogen ratio in Ta-N/Si(001), the barrier property of Ta-N/Si(001) was enhanced, finally failed at $750^{\circ}C$ due to the crystallization and silicide formation. Compared with Ta-N/Si(001), Ta-N/Ta/Si(001) forms silicides at $650^{\circ}C$. However it does not crystallize even at $750^{\circ}C$. With increasing nitrogen composition in Ta-N/Ta/Si(001), the formation of tantalum silicide was reduced and the surface roughness was improved. To observe the surface morphology of Ta-N/Ta/Si(001) during annealing, we performed an in-situ x-ray scattering experiment using synchrotron radiation of the 5C2 at Pohang Light Source(PLS). Addition of Ta layer between Ta-N and Si(001) improved the surface morphology and reduced the surface degradation at high temperatures. In addition, increasing $N_2/Ar$ flow ratio reduced the formation of tantalum silicide and enhanced the barrier properties.

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A Study on the Characteristics of a Pt/TiO2 Catalyst Prepared by Liquid-Phase Ruduction for Formaldehyde Oxidation at Room Temperature (액상환원 기반 Pt/TiO2 촉매 제조를 이용한 포름알데히드 상온 산화 반응 특성 연구)

  • Jae Heon Kim;Younghee Jang;Geo Jong Kim;Sung Chul Kim;Sung Su Kim
    • Applied Chemistry for Engineering
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    • v.34 no.6
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    • pp.612-618
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    • 2023
  • Modern society spends more than 80% of its daily life indoors, emphasizing the need for attention to indoor air pollution due to the improvement in living standards. In this study, the performance and reaction characteristics of the Pt/TiO2 catalysts prepared by liquid-phase reduction for the removal of formaldehyde (HCHO), one of the indoor air pollutants, at room temperature without the need for additional light or heat were investigated. As a result, it showed that catalysts prepared by the same method showed approximately 40~80% various activities depending on the type of TiO2. XRD, BET, and XPS analyses were performed to investigate the particle size, crystal structure, specific surface area, and O/Ti molar ratio of the support material, and it revealed that the correlation between the properties and performance was insignificant. To explore the oxidation reaction pathway of formaldehyde (HCHO), in situ DRIFT analysis using carbon monoxide and H2-TPR was perfomed. The results revealed that the performance was demonstrated by the oxidation state of the active metal and the adsorption-desorption characteristics of the adsorbate species.

Correlation between terahertz characteristics and defect states in LTG-InGaAs

  • Park, Dong-U;Kim, Jun-O;Lee, Sang-Jun;Kim, Chang-Su;Lee, Dae-Su;No, Sam-Gyu;Gang, Cheol;Gi, Cheol-Sik;Kim, Jin-Su
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.08a
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    • pp.243-243
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    • 2010
  • Low-temperature grown (LTG) InGaAs epilayers were grown by MBE technique for studying a correlation between terahertz (THz) emission and the intrinsic defects. The 1.2-um-thick Be-compensated LTG-InGaAs epilayers were prepared on SI-InP:Fe substrate at $200-250^{\circ}C$, and subsequently in-situ annealed under As environment at $550^{\circ}C$ for 5-30 minutes. The carrier concentration/mobility and the crystalline structure were analyzed by the Hall effect and the x-ray diffraction (XRD), respectively, and the carrier lifetime were determined by the fs time-resolved pump-probe spectroscopy. THz generation from LTG-InGaAs was carried out by a Ti-sapphire laser (800 nm) of a pulse width of 190 fs at a repetition of 76 MHz. Figure shows the spectral amplitude of generated waves in the THz region. As the growth temperature of epilayer increases, the amplitude is enhanced. However, two samples grown at $200^{\circ}C$, as-grown and annealed, show almost no difference in the spectral amplitude. This suggests that the growth temperature is critical in the formation of defect states involved in THz emission. We are now investigating the correlations between the XRD band attributed to defects, the Hall parameter, and the spectral amplitude of generated THz wave.

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Fabrication of Fe-TiC Composite Powder by High-Energy Milling and Subsequent Reaction Synthesis (고에너지 밀링 및 합성반응에 의한 Fe-TiC 복합분말 제조)

  • Ahn, Ki-Bong;Lee, Byung-Hun;Lee, Young-Hee;Khoa, Hyunh Xuan;Kim, Ji-Soon
    • Journal of Powder Materials
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    • v.20 no.1
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    • pp.53-59
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    • 2013
  • Fe-TiC composite powder was fabricated via two steps. The first step was a high-energy milling of FeO and carbon powders followed by heat treatment for reduction to obtain a (Fe+C) powder mixture. The optimal condition for high-energy milling was 500 rpm for 1h, which had been determined by a series of preliminary experiment. Reduction heat-treatment was carried out at $900^{\circ}C$ for 1h in flowing argon gas atmosphere. Reduced powder mixture was investigated by X-ray Diffraction (XRD), Field Emission-Scanning Electron Microscopy (FE-SEM) and Laser Particle Size Analyser (LPSA). The second step was a high-energy milling of (Fe+C) powder mixture and additional $TiH_2$ powder, and subsequent in-situ synthesis of TiC particulate in Fe matrix through a reaction of carbon and Ti. High-energy milling was carried out at 500 rpm for 1 h. Heat treatment for reaction synthesis was carried out at $1000{\sim}1200^{\circ}C$ for 1 h in flowing argon gas atmosphere. X-ray diffraction (XRD) results of the fabricated Fe-TiC composite powder showed that only TiC and Fe phases exist. Results from FE-SEM observation and Energy-Dispersive X-ray Spectros-copy (EDS) revealed that TiC phase exists uniformly dispersed in the Fe matrix in a form of particulate with a size of submicron.

Se-coated Cu-Ga-In 금속전구체 셀렌화 반응메카니즘 연구

  • Kim, U-Gyeong;Gu, Ja-Seok;Park, Hyeon-Uk
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.47.2-47.2
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    • 2011
  • 광전환 효율 20% (AM1.5G) 이상의 고효율 화합물 박막태양전지의 광흡수층으로 많은 관심을 받고 있는 $Cu(In,Ga)Se_2$ (CIGS) 태양전지의 광흡수층은 다양한 공정에 의해 제조가 가능하다. 현재 고효율 CIGS 셀 생성을 위해 널리 사용되고 있는 CIGS 흡수층 성장공정은 "co-evaporation (동시증발법)"과 2-step 공정이라 불리는 "precursorselenization(전구체-셀렌화)" 방법이다. 동시증발법은 개별원소 Cu, In, Ga, Se들을 고진공 분위기에서 고온(550~600$^{\circ}C$) 기판위에 증착하는 방법으로 소면적에서 가장 좋은 효율(~20%)을 보이는 공정이다. 하지만, 고온, 고진공 공정조건과 대면적 증착시 온도 및 조성 불균일 등의 문제점 등으로 상용화에 어려움이 있다. 전구체-셀렌화 공정은 1단계에서 다양한 방식(예: 스퍼터링, 전기도금, 프린팅 등) 방식으로 CuGaIn 전구체를 증착하고, 2단계에서 고온(550~600$^{\circ}C$)하에 H2Se gas 혹은 Se vapor와 반응시켜 CIGS를 생성한다. 일본의 Showa Shell와 Honda Soltec 등에 의해 이미 상업화 되었듯이, 저비용 대면적으로 상업화 가능성이 높은 공정으로 평가되고 있다. 하지만, 2단계에서 사용되는 H2Se 및 Se vapor의 유독성, 기상 Se과 금속전구체 간의 느린 셀렌화 반응속도, 셀렌화반응 후 생성된 CIGS 박막 두께방향으로의 Ga 불균일 분포, 생성된 CIGS/Mo 계면 접착력 저하 등의 문제점들이 개선, 해결되어야만 상업화에 성공할 수 있을 것이다. 본 연구에서는 Se layer가 코팅된 금속전구체의 셀렌화 반응메카니즘을 in-situ high-temperature XRD를 이용하여 연구하였다. 금속전구체는 스퍼터링, 스프레이 등 다양한 방법으로 제조되었고, 반응메카니즘 연구결과를 바탕으로 Se 코팅된 금속전구체를 이용한 급속열처리 공정의 최적화를 시도하였다.

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Influence of Reactivity of Reinforcing Nanoparticles with Aqueous Solution on Electroplating Copper Films (강화상 나노입자의 용액 반응성이 구리 도금 박막에 미치는 영향)

  • Park, Jieun;Oh, Minju;Kim, Yiseul;Lee, Dongyun
    • Korean Journal of Materials Research
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    • v.23 no.12
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    • pp.695-701
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    • 2013
  • To understand how reactivity between reinforcing nanoparticles and aqueous solution affects electrodeposited Cu thin films, two types of commercialized cerium oxide (ceria, $CeO_2$) nanoparticles were used with copper sulfate electrolyte to form in-situ nanocomposite films. During this process, we observed variation in colors and pH of the electrolyte depending on the manufacturer. Ceria aqueous solution and nickel sulfate ($NiSO_4$) aqueous solutions were also used for comparison. We checked several parameters which could be key factors contributing to the changes, such as the oxidation number of Cu, chemical impurities of ceria nanoparticles, and so on. Oxidation number was checked by salt formation by chemical reaction between $CuSO_4$ solution and sodium hydroxide (NaOH) solution. We observed that the color changed when $H_2SO_4$ was added to the $CuSO_4$ solution. The same effect was obtained when $H_2SO_4$ was mixed with ceria solution; the color of ceria solution changed from white to yellow. However, the color of $NiSO_4$ solution did not show any significant changes. We did observe slight changes in the pH of the solutions in this study. We did not obtain firm evidence to explain the changes observed in this study, but changes in the color of the electrolyte might be caused by interaction of Cu ion and the by-product of ceria. The mechanical properties of the films were examined by nanoindentation, and reaction between ceria and electrolyte presumably affect the mechanical properties of electrodeposited copper films. We also examined their crystal structures and optical properties by X-ray diffraction (XRD) and UV-Vis spectroscopy.

Microstructural ananalysis of AlN thin films on Si substrate grown by plasma assisted molecular beam epitaxy (RAMBE를 사용하여 Si 기판 위에 성장된 AIN 박막의 결정성 분석)

  • 홍성의;한기평;백문철;조경익;윤순길
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.22-26
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    • 2001
  • Microstructures of AlN thin films on Si substrates grown by plasma assisted molecular beam epitaxy were analyzed with various growth temperatures and substrate orientations. Reflection high energy electron diffraction (RHEED) patterns were checked for the in-situ monitoring of the growth condition. X-ray diffraction(XRD), double crystal X-ray diffraction (DCXD), and transmission electron microscopy/diffraction (TEM/TED) techniques were employed to characterize the microstructure of the films after growth. On Si(100) sub-strates, AlN thin films were grown mostly along the hexagonal c-axis orientation at temperature higher than $850^{\circ}C$. On the other hand the AlN films on Si(111) were epitaxially grown with directional coherencies in AlN(0001)/Si(111), AlN(1100)/Si(110), and AlN(1120)/Si(112). The microstructure of AlN thin films on Si(111) substrates, with a full width at half maximum of almost 3000 arcsec at 2$\theta$=$36.2^{\circ}$, showed that the single crystal films were grown, even if they includ a lot of crystal defects such as dislocations and stacking faults.

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