• Title/Summary/Keyword: XRD analysis

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Reaction Characterization of Y2Ba1CU1O5 Oxides by Solid State Reaction Method and Pyrophoric Synthesis Method (고상반응법과 발화합성법에 의한 Y2Ba1CU1O5 산화물의 반응특성)

  • Park, Jeong-Shik
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.772-777
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    • 1999
  • $Y_2Ba_1Cu_1O_5(Y211)$ powders were prepared by pyrophoric synthesis method and by solid state reaction method using $Y_2O_3(99.9%)$, $BaCO_3(99.9%)$, and CuO(99.9%) powders in both of these processes. The phase formation and reaction kinetics of $Y_2Ba_1Cu_1O_5$ powders have been studied using X-ray diffraction analysis(XRD) of samples at various heat treatment temperatures and reaction time. The reaction characterization suggested that the phase formation rate is mainly controlled by the particle size of Y211 powders. The activation energy(${\Delta}E_a$) of Y211 phase formation in this pyrophoric synthesis method was found to be 136.42 kJ/mol compared with 149.46 kJ/mol for that of solid state reaction method. These results data showed that the pyrophoric synthesis method is kineticaly more efficient than the solid state reaction method in this $Y_2Ba_1Cu_1O_5$ system.

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SURFACE CHARACTERISTICS AND BIOLOGICAL RESPONSES OF HYDROXYAPATITE COATING ON TITANIUM BY HYDROTHERMAL METHOD: AN IN VITRO STUDY

  • Kim, Dong-Seok;Kim, Chang-Whe;Jang, Kyung-Soo;Lim, Young-Jun
    • The Journal of Korean Academy of Prosthodontics
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    • v.43 no.3
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    • pp.363-378
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    • 2005
  • Statement of problem. Hydroxyapatite(HA) coated titanium surfaces have not yet showed the reliable osseointegration in various conditions. Purpose. This study was aimed to investigate microstructures, chemical composition, and surface roughness of the surface coated by the hydrothermal method and to evaluate the effect of hydrothermal coating on the cell attachment, as well as cell proliferation. Material and Methods. Commercially pure(c.p.) titanium discs were used as substrates. The HA coating on c.p. titanium discs by hydrothermal method was performed in 0.12M HCl solution mixed with HA(group I) and 0.1M NaOH solution mixed with HA(group II). GroupⅠ was heated at 180 $^{\circ}C$ for 24, 48, and 72 hours. GroupⅡ was heated at 180 $^{\circ}C$ for 12, 24, and 36 hours. And the treated surfaces were evaluated by Scanning electron microscopy(SEM), Energy dispersive X-ray spectroscopy(EDS), X-ray photoelectron spectroscopy(XPS), X-ray diffraction method(XRD), Confocal laser scanning microscopy(CLSM). And SEM of fibroblast and 3-(4,5- dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide(MTT) assay were used for cellular responses of the treated surfaces. Results. The color of surface changed in both groups after the hydrothermal process. SEM images showed that coating pattern was homogeneous in group II, while inhomogeneous in group I. H72 had rosette-like precipitates. The crystalline structure grew gradually in group II, according to extending treatment period. The long needle-like crystals were prominent in N36. Calcium(Ca) and phosphorus(P) were not detected in H24 and H48 in EDS. In all specimens of group II and H72, Ca was found. Ca and P were identified in all treated groups through the analysis of XPS, but they were amorphous. Surface roughness did not increase in both groups after hydrothermal treatment. The values of surface roughness were not significantly different between groups I and II. According to the SEM images of fibroblasts, cell attachments were oriented and spread well in both treated groups, while they were not in the control group. However, no substantial amount of difference was found between groups I and II. Conclusions. In this study during the hydrothermal process procedure, coating characteristics, including the HA precipitates, crystal growth, and crystalline phases, were more satisfactory in NaOH treated group than in HCl treated group. Still, the biological responses of the modified surface by this method were not fully understood for the two tested groups did not differ significantly. Therefore, more continuous research on the relationship between the surface features and cellular responses seems to be in need.

Effects of Boride on Microstructure and Properties of the Electroconductive Ceramic Composites of Liquid-Phase-Sintered Silicon Carbide System (액상소결(液狀燒結)한 SiC계(系)의 전도성(電導性) 복합체(複合體)의 미세구조(微細構造)와 특성(特性)에 미치는 Boride의 영향(影響))

  • Shin, Yong-Deok;Ju, Jin-Young;Ko, Tae-Hun
    • The Transactions of The Korean Institute of Electrical Engineers
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    • v.56 no.9
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    • pp.1602-1608
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    • 2007
  • The composites were fabricated, respectively, using 61[vol.%] SiC-39[vol.%] $TiB_2$ and using 61[vol.%] SiC-39[vol.%] $ZrB_2$ powders with the liquid forming additives of 12[wt%] $Al_2O_3+Y_2O_3$ by hot pressing annealing at $1650[^{\circ}C]$ for 4 hours. Reactions between SiC and transition metal $TiB_2$, $ZrB_2$ were not observed in this microstructure. The result of phase analysis of composites by XRD revealed SiC(6H, 3C), $TiB_2$, $ZrB_2$ and $YAG(Al_5Y_3O_{12})$ crystal phase on the Liquid-Phase-Sintered(LPS) $SiC-TiB_2$, and $SiC-ZrB_2$ composite. $\beta\rightarrow\alpha-SiC$ phase transformation was occurred on the $SiC-TiB_2$ and $SiC-ZrB_2$ composite. The relative density, the flexural strength and Young's modulus showed the highest value of 98.57[%], 249.42[MPa] and 91.64[GPa] in $SiC-ZrB_2$ composite at room temperature respectively. The electrical resistivity showed the lowest value of $7.96{\times}10^{-4}[\Omega{\cdot}cm]$ for $SiC-ZrB_2$ composite at $25[^{\circ}C]$. The electrical resistivity of the $SiC-TiB_2$ and $SiC-ZrB_2$ composite was all positive temperature coefficient resistance (PTCR) in the temperature ranges from $25[^{\circ}C]$ to $700[^{\circ}C]$. The resistance temperature coefficient of composite showed the lowest value of $1.319\times10^{-3}/[^{\circ}C]$ for $SiC-ZrB_2$ composite in the temperature ranges from $100[^{\circ}C]$ to $300[^{\circ}C]$ Compositional design and optimization of processing parameters are key factors for controlling and improving the properties of SiC-based electroconductive ceramic composites.

Solidification of Molten Salt Waste by Gel-Route Pre-treatment (겔화 전처리법을 이용한 폐용융염의 고형화)

  • Park Hwan Seo;Kim In Tae;Kim Hwan Young;Ryu Seung Kon;Kim Joon Hyung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.3 no.1
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    • pp.57-65
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    • 2005
  • This study suggested a new method for the solidification of molten salt waste generated from the electro-metallurgical process in the spent fuel treatment. Using binary material system, sodium silicate and phosphoric acid, metal chlorides were converted into metal phosphate in the micro-reaction module formed by SiO$_{2} particles. The volatile element in the reaction module would little vaporized below 1100$^{circ}$C After the gel product was mixed with borosilicate glass powder and thermally treated at 1000$^{circ}$C, li exists as Li$_{3}$PO$_4$ separated from glass phase and, Cs and Sr would be incorporated into an amorphous phase from XRD analysis. In case of the addition of ZrCl$_{4}$ to the binary system, the gel products were transformed into NZP structure considered as an prospective ceramic waste form after heat-treatment above 700 $^{circ}$C. From these results, the gel-route pretreatment can be considered as an effective approach to the solidincation of molten salt waste by the confirmed process or waste form and this also would be an alternative method on the ANL method using zeolites in USA by the confirmation of its chemical durability as an future work.

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Effects of Aging on Properties of MgO-Partially Stabilized Zirconia (마그네시아 부분안정화 지르코니아 소결체의 특성에 미치는 열처리 효과)

  • 정형진;오영제;이홍림
    • Journal of the Korean Ceramic Society
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    • v.24 no.3
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    • pp.243-250
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    • 1987
  • The effects aging on some properties and thermal-shock behavior of zirconia partially stabilized with 9 mol% MgO (9MZ) were studied. 9MZ specimens were aged over $1200^{\circ}$-$1400^{\circ}C$ for 12hours subsequently, after sintering at $1650^{\circ}C$ for 4 hours. Fracture strength(both before and after thermal-shock test), linear thermal expansion, monoclinic fraction and phase transition by XRD, density, galvanic potential and microstructure were measured. Quantitative chemical analysis around the grain-boundary of the specimen aged at $1350^{\circ}C$ was also conducted by EDX. The aging of 9MZ specimen causes a thermal decomposition of cubic-$ZrO^{2}$ into the formation metastable tetragonal-$ZrO^{2}$ and MgO. The former increases the residual strength after thermal-shock test and the latter improves the thermal-shock resistance due to thermal conduction through the continuous magnesia phase and the formation of monoclinic phase content in matrix were increased with decreasing the aging temperature from $1400^{\circ}C$ to $1200^{\circ}C$. Galvanic potential of the aged specimen exhibited a proper emf characteristic.

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Change of Electrochemical Characteristics Due to the Fe Doping in Lithium Manganese Oxide Electrode

  • Ju Jeh Beck;Kang Tae Young;Cho Sung Jin;Sohn Tae Won
    • Journal of the Korean Electrochemical Society
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    • v.7 no.3
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    • pp.131-137
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    • 2004
  • Sol-gel method which provides better electrochemical and physiochemical properties compared to the solid-state method was used to synthesize the material of $LiFe_yMn_{2-y}O_4$. Fe was substituted to increase the structural stability so that the effects of the substitution amount and sintering temperature were analyzed. XRD was used for the structural analysis of produced material, which in turn, showed the same cubic spinel structure as $LiMn_2O_4$ despite the substitution of $Fe^{3+}$. During the synthesis of $LiFe_yMn_{2-y}O_4$, as the sintering temperature and the doping amount of Fe(y=0.05, 0.1, 0.2)were increased, grain growth proceeded which in turn, showed a high crystalline and a large grain size, certain morphology with narrow specific surface area and large pore volume distribution was observed. In order to examine the ability for the practical use of the battery, charge-discharge tests were undertaken. When the substitution amount of $Fe^{3+}\;into\;LiMn_2O_4$ increased, the initial discharge capacity showed a tendency to decrease within the region of $3.0\~4.2V$ but when charge-discharge processes were repeated, other capacity maintenance properties turned out to be outstanding. In addition, when the sintering temperature was $800\~850^{\circ}C$, the initial capacity was small but showed very stable cycle performance. According to EVS(electrochemical voltage spectroscopy) test, $LiFe_yMn_{2-y}O_4(y=0,\;0.05,\;0.1,\;0.2)$ showed two plateau region and the typical peaks of manganese spinel structure when the substitution amount of $Fe^{3+}$ increased, the peak value at about 4.15V during the charge-discharge process showed a tendency to decrease. From the previous results, the local distortion due to the biphase within the region near 4.15V during the lithium extraction gave a phase transition to a more suitable single phase. When the transition was derived, the discharge capacity decreased. However the cycle performance showed an outstanding result.

Effect of Support Geometry on Catalytic Activity of Pt/CeO2 Nanorods in Water Gas Shift Reaction (Water Gas Shift 반응에서 Pt/CeO2 촉매의 지지체구조에 따른 촉매활성 연구)

  • Im, Hyo Been;Kwon, Soon Jin;Byun, Chang Ki;Ahn, Hee Sung;Koo, Kee Young;Yoon, Wang Lai;Yi, Kwang Bok
    • Transactions of the Korean hydrogen and new energy society
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    • v.25 no.6
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    • pp.577-585
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    • 2014
  • Nanorod and particle shape $CeO_2$ were synthesized via hydrothermal process and precipitation method, respectively, and used as supports of Pt catalyst for water gas shift (WGS) reaction. Three different durations (12, 48, and 96h) for hydrothermal process were applied for the preparation of nanorod type $CeO_2$. 1.0 wt% of Pt was loaded on the prepared supports with incipient wetness method prior to the catalytic activity tests that were carried out at a GHSV of $95,541h^{-1}$, and a temperature range of 200 to $360^{\circ}C$. Varying duration of hydrothermal process led to the difference in physical characteristics of $CeO_2$ nanorods, such as aspect ratio, BET surface area, pore diameter, and pore volume. Consequently, the catalytic activities of Pt/$CeO_2$ nanorods were affected by the physical characteristics of the supports and appeared to be in the order of Pt/$CeO_2$(12) > Pt/$CeO_2$(48) > Pt/$CeO_2$(96). The comparison of the catalytic activities and results of the analysis (XPS, XRD, SEM, BET and TPR) for the supports revealed that the activity of the catalysts depends on chemical states of the Pt and the support materials in the temperature range that is lower than $280^{\circ}C$. However, the activity is rather dependent on the physical characteristic of the supports because the increased gas velocity limits the mass transfer of reactants in micropores of the supports.

Growth of Li2B4O7 Single Crystal and Its Thermoluminescent Properties (Li2B4O7 단결정 성장과 열형광 특성)

  • Park, Kang-Soo;Ahn, Jung-Keun;Kim, Dong-Jin;Hwang, Yoon-Hwae;Kim, Hyung-Kook;Park, Myeong-Hwan;Kang, Hee-Dong;Kim, Do-Sung
    • Journal of Sensor Science and Technology
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    • v.12 no.1
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    • pp.16-23
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    • 2003
  • Thermoluminescent properties of $Li_2B_4O_7$ single crystal grown by Czochralski method have been investigated. The high quality $Li_2B_4O_7$ single crystal without core was obtained at rotation speed of 10 rpm for seed crystal and pulling speed below $0.18\;mm{\cdot}h^{-1}$. The structure of $Li_2B_4O_7$ single crystal was classified as tetragonal by XRD analysis. The TL glow curve was composed with three overlapped peaks which can be easily deconvoluted and the TL response of $Li_2B_4O_7$ single crystal TLD to X-ray radiation is linear within the range of $50\;mGy{\sim}1.5\;Gy$. Activation energies of three TL glow peaks analyzed by the various heating rates method and PL spectrum were 0.93, 1.78 and 2.25 eV, respectively.

A Study on the Low Temperature Epitaxial Growth of $CoSi_2$ Layer by Multitarget Bias cosputter Deposition and Phase Sequence (Multitarget Bias Cosputter증착에 의한 $CoSi_2$층의 저온정합성장 및 상전이에 관한 연구)

  • Park, Sang-Uk;Choe, Jeong-Dong;Gwak, Jun-Seop;Ji, Eung-Jun;Baek, Hong-Gu
    • Korean Journal of Materials Research
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    • v.4 no.1
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    • pp.9-23
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    • 1994
  • Epitaxial $CoSi_2$ layer has been grown on NaCl(100) substrate at low deposition temperature($200^{\circ}C$) by multitarget bias cosputter deposition(MBCD). The phase sequence and crystallinity of deposited silicide as a function of deposition temperature and substrate bias voltage were studied by X-ray diffraction(XRD) and transmission electron microscopy(TEM) analysis. Crystalline Si was grown at $200^{\circ}C$ by metal induced crystallization(M1C) and self bias effect. In addition to, the MIC was analyzed both theoretically and experimentally. The observed phase sequence was $Co_2Si \to CoSi \to Cosi_2$ and was in good agreement with that predicted by effective heat of formation rule. The phase sequence, the CoSi(l11) preferred orientation, and the crystallinity had stronger dependence on the substrate bias voltage than the deposition temperature due to the collisional cascade mixing, the in-situ cleaning, and the increase in the number of nucleation sites by ion bombardment of growing surface. Grain growth induced by ion bombardment was observed with increasing substrate bias voltage at $200^{\circ}C$ and was interpreted with ion bombardment dissociation model. The parameters of $E_{Ar}\;and \alpha(V_s)$ were chosen to properly quantify the ion bombardment effect on the variation in crystallinty at $200^{\circ}C$ with increasing substrate bias voltage using Langmuir probe.

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A Study on the Formation fo Epitaxial $CoSi_2$ Thin Film using Co/Ti Bilayer (Co/Ti이중박막을 이용한 $CoSi_2$에피박막형성에 관한 연구)

  • Kim, Jong-Ryeol;Bae, Gyu-Sik;Park, Yun-Baek;Jo, Yun-Seong
    • Korean Journal of Materials Research
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    • v.4 no.1
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    • pp.81-89
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    • 1994
  • Ti film of lOnm thickness and Co film of 18nm thickness were sequentially e-heam evaporated onto Si (100) substrates. Metal deposited samples were rapidly thermal-annt.aled(KTA) in thr N1 en vironment a t $900^{\circ}C$ for 20 sec. to induce the reversal of metal bilayer, so that $CoSi_{2}$ thin films could be formed. The sheet resistance measured by the 4-point probe was 3.9 $\Omega /\square$This valur was maintained with increase in annealing time upto 150 seconds, showing high thermal stab~lity. Thc XRII spectra idrn tified the silicide film formed on the Si substrate as a $CoSi_{2}$ epitaxial layer. The SKM microgr;iphs showed smooth surface, and the cross-sectional TKM pictures revealed that the layer formed on the Si substrate were composed of two Co-Ti-Si alloy layers and 70nm thick $CoSi_{2}$ epl-layer. The AES analysis indicated that the native oxide on Si subs~rate was removed by TI ar the beginning of the RTA, and Ihcn that Co diffused to clean surface of Si substrate so that epitaxial $CoSi_{2}$ film could bt, formed. In thc rasp of KTA at $700^{\circ}C$. 20sec. followed by $900^{\circ}C$, 20sec., the thin film showed lower sheet resistance, but rough surface and interface owing to $CoSi_{2}$ crystal growth. The application scheme of this $CoSi_{2}$ epilayer to VLSI devices and the thermodynarnic/kinetic mechan~sms of the $CoSi_{2}$ epi-layer formation through the reversal of Co/Ti bdayer were discussed.

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