• Title/Summary/Keyword: In-situ XRD

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Effects of Vacuum Annealing on the Structural Properties of Sputtered Vanadium Oxide Thin Films (스퍼터된 바나듐 산화막의 구조적 특성에 미치는 진공 어닐링의 효과)

  • Whang, In-Soo;Choi, Bok-Gil;Choi, Chang-Kyu;Kwon, Kwang-Ho;Kim, Sung-Jin
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.05b
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    • pp.70-73
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    • 2002
  • Thin films of vanadium oxide($VO_{x}$) have been deposited by r.f. magnetron sputtering from $V_{2}O_{5}$ target in gas mixture of argon and oxygen. The oxygen/(oxygen+argon) partial pressure ratio of 0% and 8% is adopted. Crystal structure, chemical composition, molecular structure and optical properties of films sputter-deposited under different oxygen gas pressures and in-situ annealed in vacuum at $400^{\circ}C$ for 1h and 4h are characterized through XRD. RBS, FTlR and optical absorption measurements. The films as-deposited are amorphous and those annealed for time longer than 4h are polycrystalline. $V_{2}O_{5}$ and lower oxides co-exist in sputter-deposited films and as the oxygen partial pressure is increased the films become more stoichiometric $V_{2}O_{5}$. When annealed at $400^{\circ}C$, the as-deposited films are reduced to a lower oxide. It is observed that the oxygen atoms located on the V-O plane of $V_{2}O_{5}$ layer participate more readily in the oxidation and reduction process. The optical transmission of the films annealed in vacuum decreases considerably than the as-deposited films and the optical absorption of all the films increases rapidly between 400 and 550nm.

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Phase sequence in Codeposition and Solid State Reaction of Co-Si System and Low Temperature Epitaxial Growth of $CoSi_2$ Layer (Co-Si계의 동시증착과 고상반응시 상전이 및 $CoSi_2$ 층의 저온정합성장)

  • 박상욱;심재엽;지응준;최정동;곽준섭;백홍구
    • Journal of the Korean Vacuum Society
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    • v.2 no.4
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    • pp.439-454
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    • 1993
  • The phase sequence of codeposited Co-Si alloy and Co/si multilayer thin film was investigated by differential scanning calormetry(DSC) and X-ray diffraction (XRD) analysis, The phase sequence in codeposition and codeposited amorphous Co-Si alloy thin film were CoSilongrightarrow Co2Si and those in Co/Si multilayer thin film were CoSilongrightarrowCo2Silongrightarrow and CoSilongrightarrowCo2Si longrightarrowCoSilongrightarrowCoSi2 with the atomic concentration ration of Co to Si layer being 2:1 and 1:2 respectively. The observed phase sequence was analyzed by the effectvie heat of formatin . The phase determining factor (PDF) considering structural facotr in addition to the effectvie heat of formation was used to explain the difference in the first crystalline phase between codeposition, codeposited amorphous Co-Si alloy thin film and Co/Si multilayer thin film. The crystallinity of Co-silicide deposited by multitarget bias cosputter deposition (MBCD) wasinvestigated as a funcion of deposition temperature and substrate bias voltage by transmission electron microscopy (TEM) and epitaxial CoSi2 layer was grown at $200^{\circ}C$ . Parameters, Ear, $\alpha$(As), were calculate dto quantitatively explain the low temperature epitaxial grpwth of CoSi2 layer. The phase sequence and crystallinity had a stronger dependence on the substrate bias voltage than on the deposition temperature due to the collisional daxcade mixing, in-situ cleannin g, and increase in the number of nucleation sites by ion bombardment of growing surface.

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Stabilization of Heavy Metals-contaminated Soils Around the Abandoned Mine area Using Phosphate (인산염을 이용한 휴.폐광산 주변 중금속 오염토양의 안정화처리에 관한 연구)

  • Lee, Eun-Gi;Choi, Sang-Il
    • Journal of Soil and Groundwater Environment
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    • v.12 no.6
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    • pp.100-106
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    • 2007
  • The objective of this study was to evaluate the efficiency of $(NH_4)_2HPO_4$, $Na_2HPO_4{\cdot}12H_2O$, $CaHPO_4{\cdot}2H_2O$, $Ca(H_2PO_4)_2{\cdot}H_2O$ and $H_3PO_4$ for the stabilization of soils contaminated with multi-metals containing Pb, Cd and As. The application rate of stabilizers to soils was determined based on $PO_4/Pb_{total}$ molar ratio of 0.5, 1, 2, 4. The results of Korea Standard Test and TCLP (EPA Method 1311) showed the reduction of metal leachabilities below the regulatory limits for Pb and Cd when $H_3PO_4$ and $Ca(H_2PO_4)_2{\cdot}H_2O$ were applied. However, stabilization efficiency for Cd was low and in case of As leaching concentration increased rather. It is considered that $PO_4$ reacted effectively $Pb^{2+}$ due to leaching Pb under low pH condition created by adding $H_3PO_4$. Accordingly Pb was stabilized by dissolution and precipitation of hydroxypyromorphite. From the change of metals fraction using sequential extraction procedure when $H_3PO_4$ applied as a stabilizer, we confirmed that residual fraction increased more than 60% and this result was accorded with XRD analysis that detected only hydroxypyromorphite peak in $H_3PO_4$.

Development of Biomass-Derived Anode Material for Lithium-Ion Battery (리튬이온 전지용 바이오매스 기반 음극재 개발)

  • Jeong, Jae Yoon;Lee, Dong Jun;Heo, Jungwon;Lim, Du-Hyun;Seo, Yang-Gon;Ahn, Jou-Hyeon;Choi, Chang-Ho
    • Clean Technology
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    • v.26 no.2
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    • pp.131-136
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    • 2020
  • Biomass bamboo charcoal is utilized as anode for lithium-ion battery in an effort to find an alternative to conventional resources such as cokes and petroleum pitches. The amorphous phase of the bamboo charcoal is partially converted to graphite through a low temperature graphitization process with iron oxide nanoparticle catalyst impregnated into the bamboo charcoal. An optimum catalysis amount for the graphitization is determined based on the characterization results of TEM, Raman spectroscopy, and XRD. It is found that the graphitization occurs surrounding the surface of the catalysis, and large pores are formed after the removal of the catalysis. The formation of the large pores increases the pore volume and, as a result, reduces the surface area of the graphitized bamboo charcoal. The partial graphitization of the pristine bamboo charcoal improves the discharge capacity and coulombic efficiency compared to the pristine counterpart. However, the discharge capacity of the graphitized charcoal at elevated current density is decreased due to the reduced surface area. These results indicate that the size of the catalysis formed in in-situ graphitization is a critical parameter to determine the battery performance and thus should be tuned as small as one of the pristine charcoal to retain the surface area and eventually improve the discharge capacity at high current density.

Review and Strategy for Study on Korean Buffer Characteristics Under the Elevated Temperature Conditions: Mineral Transformation and Radionuclide Retardation Perspective

  • Park, Tae-Jin;Yoon, Seok;Lee, Changsoo;Cho, Dong Keun
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.19 no.4
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    • pp.459-467
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    • 2021
  • In the majority of countries, the upper limit of buffer temperature in a repository is set to below 100℃ due to the possible illitization. This smectite-to-illite transformation is expected to be detrimental to the swelling functions of the buffer. However, if the upper limit is increased while preventing illitization, the disposal density and cost-effectiveness for the repository will dramatically increase. Thus, understanding the characteristics and creating a database related to the buffer under the elevated temperature conditions is crucial. In this study, a strategy to investigate the bentonite found in Korea under the elevated temperatures from a mineral transformation and radionuclides retardation perspective was proposed. Certain long-term hydrothermal reactions generated the bentonite samples that were utilized for the investigation of their mineral transformation and radionuclide retardation characteristics. The bentonite samples are expected to be studied using in-situ synchrotron-based X-Ray Diffraction (XRD) technique to determine the smectite-to-illite transformation. Simultaneously, the 'high-temperature and high-pressure mineral alteration measurement system' based on the Diamond Anvil Cell (DAC) will control and provide the elevated temperature and pressure conditions during the measurements. The kinetic models, including the Huang and Cuadros model, are expected to predict the time and manner in which the illitization will become detrimental to the performance and safety of the repository. The sorption reactions planned for the bentonite samples to evaluate the effects on retardation will provide the information required to expand the current knowledge of repository optimization.

Direct Bonding of Cu/AlN using Cu-Cu2O Eutectic Liquid (Cu-Cu2O계 공융액상을 활용한 Cu/AlN 직접접합)

  • Hong, Junsung;Lee, Jung-Hoon;Oh, You-Na;Cho, Kwang-Jun;Riu, Doh-Hyung;Oh, Sung-Tag;Hyun, Chang-Yong
    • Journal of Powder Materials
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    • v.20 no.2
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    • pp.114-119
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    • 2013
  • In the DBC (direct bonding of copper) process the oxygen partial pressure surrounding the AlN/Cu bonding pairs has been controlled by Ar gas mixed with oxygen. However, the direct bonding of Cu with sound interface and good adhesion strength is complicated process due to the difficulty in the exact control of oxygen partial pressure by using Ar gas. In this study, we have utilized the in-situ equilibrium established during the reaction of $2CuO{\rightarrow}Cu_2O$ + 1/2 $O_2$ by placing powder bed of CuO or $Cu_2O$ around the Cu/AlN bonding pair at $1065{\sim}1085^{\circ}C$. The adhesion strength was relatively better in case of using CuO powder than when $Cu_2O$ powder was used. Microstructural analysis by optical microscopy and XRD revealed that the interface of bonding pair was composed of $Cu_2O$, Cu and small amount of CuO phase. Thus, it is explained that the good adhesion between Cu and AlN is attributed to the wetting of eutectic liquid formed by reaction of Cu and $Cu_2O$.

Preparation of Silver/Polystyrene Nanocomposites by Radical Polymerization Using Silver Carbamate Complex (은 카바메이트 복합체를 이용한 라디칼 중합에 의한 은/폴리스티렌 나노복합체의 제조)

  • Park, Heon-Su;Park, Hyung-Seok;Gong, Myoung-Seon
    • Polymer(Korea)
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    • v.34 no.2
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    • pp.144-149
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    • 2010
  • Ag/polystyrene(PS) nanocomposites were prepared by in situ reduction of silver 2-ethylhexylcarbamate (Ag-CB) complex and follwing radical polymerization only by heating at 110 $^{\circ}C$. In contrast to this conventional heating method, the microwave irradiation afforded well-dispersed silver nanoparticles(NPs) in styrene monomer without polymerization. The synthesis of Ag NPs proceeded uniformly throughout the reaction vessel only under microwave irradiation, completing the reaction simultaneously in the whole reaction solution. Successive polymerization of the monomer containing the resultant NPs has successfully produced a hybrid of the silver NPs dispersed in PS matrix. Ag/PS (0.1/100) nanocomposites were prepared successfully by melt-mixing process using Ag/PS(4.0/100) as a master-batch. UV-VIS spectroscopy, TEM, and X-ray diffraction techniques were used to investigate the process of formation of Ag/PS nanocomposites.

Structural Evolution of Layered $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ upon Electrochemical Cycling in a Li Rechargeable Battery

  • Hong, Ji-Hyeon;Seo, Dong-Hwa;Kim, Seong-Uk;Gwon, Hyeok-Jo;Park, Yeong-Uk;Gang, Gi-Seok
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2010.05a
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    • pp.37.2-37.2
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    • 2010
  • Recently $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ has been consistently examined and investigated by scientists because of its high lithium storage capacity, which exceeds beyond the conventional theoretical capacity based on conventional chemical concepts. Consequently, $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ is considered as one of the most promising cathode candidates for next generation in Li rechargeable batteries. Yet the mechanism and the origin of the overcapacity have not been clarified. Previously, many authors have demonstrated simultaneous oxygen evolution during the first delithiation. However, it may only explain the high capacity of the first charge process, and not of the subsequent cycles. In this work, we report a clarified interpretation of the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$, which is the key element in understanding its anomalously high capacity. We identify how the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ occurs upon the electrochemical cycling through careful study of electrochemical profiles, ex-situ X-ray diffraction (XRD), HR-TEM, Raman spectroscopy, and first principles calculation. Moreover, we successfully separated the structural change at subsequent cycles (mainly cation rearrangement) from the first charge process (mainly oxygen evolution with Li extraction) by intentionally synthesizing sample with large particle size. Consequently, the intermediate states of structural evolution could be well resolved. All observations made through various tools lead to the result that spinel-like cation arrangement and lithium environment are created and embedded in layered framework during repeated electrochemical cycling.

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One-step phyto-mediated fabrication of silver nanoparticles and its anti-microbial properties

  • Velmurugan Palanivel;Sung-Chul Hong;Veera Ravi Arumugam;Sivakumar Subpiramaniyam;Pyong-In Yi;Seong-Ho Jang;Jeong-Min Suh;Eun-Sang Jung;Je-Sung Park
    • Advances in nano research
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    • v.14 no.4
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    • pp.391-397
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    • 2023
  • This manuscript describes the one-step eco-friendly green fabrication of silver nanoparticles (AgNPs) through the in-situ bio-reduction of an aqueous solution of silver nitrate using Syzygium aromaticum leaf extract. UV-vis spectroscopy shows a characteristic SPR peak around 442 nm. FTIR spectroscopy showed that the AgNPs were capped with bioactive phyto-molecules. TEM images revealed oval and spherical particles with a mean diameter of ~12.6 nm. XRD analysis revealed crystalline and face-cantered cubic AgNPs. The phytosynthesized AgNPs showed broad-spectrum anti-microbial activity against two foodborne pathogenic bacteria, Listeria monocytogenes and Staphylococcus aureus. The AgNPs showed a prominent ability to inhibit biofilms formed by L. monocytogenes and S. aureus in laboratory conditions through a crystal violet assay. The results suggest that the AgNPs could be a novel nanotool to develop effective antimicrobial and anti-biofilm agents in food preservation.

Al2TiO5-machinable Ceramics Made by Reactive Sintering of Al2O3 and TiO2 (Al2O3와 TiO2의 반응소결로 제조한 Al2TiO5-기계가공성 세라믹스)

  • Park, Jae-Hyun;Lee, Won-Jae;Kim, Il-Soo
    • Journal of the Korean Ceramic Society
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    • v.47 no.6
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    • pp.498-502
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    • 2010
  • Aluminium titanate($Al_2TiO_5$) has extremely anisotropic thermal expansion properties in single crystals, and polycrystalline material spontaneously microcracks in the cooling step after sintering process. These fine intergranular cracks limit the strength of the material, but provide an effective mechanism for absorbing strain energy during thermal shock and preventing catastrophic crack propagation. Furthermore, since machinable BN-ceramics used as an insulating substrate in current micro-electronic industry are very expensive, the development of new low-cost machinable substrate ceramics are consistently required. Therefore, cheap $Al_2TiO_5$-machinable ceramics was studied for the replacement of BN ceramics. $Al_2O_3-Al_2TiO_5$ ceramic composite was fabricated via in-situ reaction sintering. $Al_2O_3$ and $TiO_2$ powders were mixed with various mol-ratio and sintered at 1400 to $1600^{\circ}C$ for 1 h. Density, hardness and strength of sintered ceramics were systematically measured. Phase analysis and microstructures were observed by XRD and SEM, respectively. Machinability of each specimens was tested by micro-hole machining. The results of research showed that the $Al_2TiO_5$-composites could be used for low-cost machinable ceramics.