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Formation and Structure of $CaO-P_2O_5-SiO_2$ Glasses ($CaO-P_2O_5-SiO_2$계 유리의 형성 및 구조)

  • 조정식;김철영
    • Journal of the Korean Ceramic Society
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    • v.29 no.9
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    • pp.729-738
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    • 1992
  • The glass formation and structural change with the glass compositions were investigated in the CaO-P2O5-SiO2 system with less than 40 wt% of P2O5. The glass formation range was determined by XRD, SEM and EDS techniques for water quenched specimens. The structural analyses were made for binary CaO-SiO2 glasses and ternary CaO-P2O5-SiO2 glasses by using FT-IR and Raman spectroscopy. The glass formation was affected by CaO/SiO2 mole ratio, P2O5 content and primary crystalline phase. The stable glass formation range was found when the transformed CaO/SiO2 mole ratio (new factor derived from structural changes) was in the range of 0.72~1.15 with less than 10 mol% of P2O5. The structural analyses of CaO-SiO2 glasses indicated that as the CaO/SiO2 ratio was increased, the nonbridging oxygens in the structural unit of the glasses were increased. With addition of P2O5 to CaO-SiO2 glasses, the P2O5 enhanced the polymerization of [SiO4] tetrahedra unit in CaO-SiO2 glasses, which contained a large portion of nonbridging oxygen. The phosphate eliminated nonbridging oxygens from silicate species, forcing polymerization of silicate structures and produced in [PO4] monomer in glasses. When added P2O5 was kept constant, the structural change with various CaO/SiO2 ratio was very similar to that of CaO-SiO2 glasses.

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Preparation of $MgO-ZrO_2$ Fibers by Sol-Gel Method and Their Characterization (졸-겔법에 의한 $MgO-ZrO_2$ 섬유의 제조와 특성)

  • 황진명;은희태
    • Journal of the Korean Ceramic Society
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    • v.31 no.10
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    • pp.1147-1158
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    • 1994
  • From Zr(O-nC3H7)4-H2O-C2H5OH-HNO3 starting solutions, MgO-doped stabilized zirconia fibers with varying content of MgO (10~18 mol%) from different MgO sources were fabricated by sol-gel method. The MgO sources used are magnesium nitrate hexahydrate, magnesium acetate tetrahydrate, and magnesium ethylate. The phase transformation studies of a drawn MgO-ZrO2 fiber were carried out using X-ray diffraction, IR spectroscopy, and Raman spectroscopy. The microstructure, tensile strength, and microporosity of fibers were investigated using SEM, tensile strength test, and microporosimeter. Although various MgO sources such as magnesium nitrate, acetate, and ethylate were used, the crystallization behavior of MgO-ZrO2 fibers at different temperatures could be summarized as follows: CubiclongrightarrowMetastable TetragonallongrightarrowMonocliniclongrightarrowCoexistence of Monoclinic and CubiclongrightarrowCubic(trace of monoclinic). At 150$0^{\circ}C$, the phase transformation of MgO-ZrO2 fibers shows the following change depending on the amount of MgO[Mg(NO3)2.6H2O]: At 10 mol%, both monoclinic and cubic phase coexist, at 12 mol%, monoclinic phase decreases rapidly, and then at 14 mol%, only cubic phase remains. When the MgO-ZrO2 fibers containing 12 mol% magnesium nitrate were heated at 80$0^{\circ}C$ for 1hr, average tensile strength of fibers is 4.0 GPa at diameters of 20 to 30 ${\mu}{\textrm}{m}$. As the heat-treatment temperatures increase to 100$0^{\circ}C$ for 1 hr, tensile strength of MgO-ZrO2 fibers decreases rapidly to 0.7 GPa.

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Pyrolysis kinetics and microstructure of thermal conversion products on toluene soluble component from two kinds of modified pitch

  • Zhu, Yaming;Zhao, Xuefei;Gao, Lijuan;Cheng, Junxia
    • Carbon letters
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    • v.28
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    • pp.38-46
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    • 2018
  • Modified pitch A (MPA) and modified pitch B (MPB) were prepared by oxidative polymerization and thermal polycondensation reaction with refined pitch as the raw material, respectively. The toluene soluble components (TS-1 and TS-2) were obtained by solvent extraction from MPA and MPB, separately. The Flynn-Wall-Ozawa method and Kissinger-Akahira-Sunose method were used to calculate the pyrolysis activation energy of TS. The Satava-Sestak method was used to investigate the pyrolysis kinetic parameters of TS. Moreover, the optical microstructure of the thermal conversion products (TS-1-P and TS-2-P) by calcination shows that TS-1-P has more contents of mosaic structure and lower contents of fine fiber structure than TS-2-P. The research result obtained by a combination of X-ray diffraction and the curve-fitting method revealed that the ratios of ordered carbon crystallite (Ig) in TS-1-P and TS-2-P were 0.3793 and 0.4417, respectively. The distributions of carbon crystallite on TS-1-P and TS-2-P were calculated by Raman spectrum and curve-fitting analysis. They show that the thermal conversion product of TS-2 has a better graphite crystallite structure than TS-1.

Structure and Thermal Properties of SnO2-(1-x)P2O5-xB2O3 Glasses (SnO2-(1-x)P2O5-xB2O3 유리의 열적, 구조적 특성)

  • An, Yong-Tae;Choi, Byung-Hyun;Ji, Mi-Jung;Chang, Woo-Suk;Bae, Hyun;Hwang, Hae-Jin
    • Journal of the Korean Ceramic Society
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    • v.47 no.2
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    • pp.117-121
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    • 2010
  • $SnO_2-(1-x)P_2O_5-xB_2O_3$ glass system were prepared by melt-quenching technique in the compositional series containing 50, 55 and 60 mol% of $SnO_2$. Local structure of the glasses was investigated by Raman and FT-IR measurements. A large glass-forming region was found at the phosphate side of the ternary system with homogeneous glasses containing up to 5~25 mol% of $B_2O_3$. According as content of $B_2O_3$ increases, theraml expansion coefficient of glass decreased but transition temperature and softening temperature increased. Because these phenomenon changed local structure of glass. According as content of $B_2O_3$ increases, quantity of bridging oxygen increased. Also, according as content of $SnO_2$ increases, confirmed that quantity of non-bridging oxygen increases.

A Study on the Comparison between an Optical Fiber and a Thermal Sensor Cable for Temperature Monitoring (온도 모니터링을 위한 광섬유 센서와 온도센서 배열 케이블의 비교 연구)

  • Kim, Jung-Yul;Kim, Yoo-Sung;Song, Yoon-Ho
    • Proceedings of the Korean Geotechical Society Conference
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    • 2006.03a
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    • pp.1100-1109
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    • 2006
  • In this study, two different technologies which can measure temperature simultaneously at many points are introduced. One is to use a thermal sensor cable that is comprised of addressable thermal sensors connected in parallel within a single cable. The other is to use an optic fiber with Distributed Temperature Sensing (DTS) system. The difference between two technologies can be summarized as follows. A thermal sensor cable has a concept of 'point sensing' that can measure temperature at accurate position of a thermal sensor. So the accuracy and resolution of temperature measurement are up to the ability of the thermal sensor. Whereas optic fiber sensor has a concept of 'distributed sensing' because temperature is measured by ratio of Stokes and anti-Stokes component intensities of Raman backscatter that is generated when laser pulse travels along an optic fiber. It's resolution is determined by measuring distance, measuring time and spatial resolution. The purpose of this study is that application targets of two temperature measurement techniques are checked in technical and economical phases by examining the strength and weakness of them. Considering the functions and characteristics of two techniques, the thermal sensor cable will be suitable to apply to the assessment of groundwater flow, geothermal distribution and grouting efficiency within 300m distance. It is expected that the optic fiber sensor can be widely utilized at various fields (for example: pipe line inspection, tunnel fire detection, power line monitoring etc.) which need an information of temperature distribution over relatively long distance.

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Direct Methanation of Syngas over Activated Charcoal Supported Molybdenum Catalyst (활성탄 담지 몰리브덴 촉매를 이용한 합성가스 직접 메탄화 반응)

  • KIM, SEONG-SOO;LEE, SEUNG-JAE;PARK, SUNG-YOUL;KIM, JIN-GUL
    • Transactions of the Korean hydrogen and new energy society
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    • v.31 no.5
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    • pp.419-428
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    • 2020
  • The kinetics of direct methanation over activated charcoal-supported molybdenum catalyst at 30 bar was studied in a cylindrical fixed-bed reactor. When the temperature was not higher than 400℃, the CO conversion increased with increasing temperature according to the Arrhenius law of reaction kinetics. While XRD and Raman analysis showed that Mo was present as Mo oxides after reduction or methanation, TEM and XPS analysis showed that Mo2C was formed after methanation depending on the loading of Mo precursor. When the temperature was as high as 500℃, the CO conversion was dependent not only on the Arrhenius law but also on the catalyzed reaction by nanoparticles, which came off from the reactor and thermocouple by metal dusting. These nanoparticles were made of Ni, Fe, Cr and alloy, and attributed to the formation of carbon deposit on the wall of the reactor and on the surface of the thermocouple. The carbon deposit consisted of amorphous and disordered carbon filaments.

Synthesis and Formation Mechanism of Cobalt Doped Willemite Blue Pigments (Co-Doped Willemite 파란색 안료의 합성과 생성기구)

  • Hwang, Dong-Ha;Han, Kyong-Sop;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.47 no.6
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    • pp.603-607
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    • 2010
  • Turquoise blue pigment of Vanadium-zircon blue (DCMA number 14-42-2), which was already commercialized, was stable to be reproduced but insufficient to give strong blue. However, it possible to obtain more intense blue by partially substituting cobalt ions into the willemite($Zn_2SiO_4$) lattice classified into DCMA number 7-10-2 for blue ceramic pigment. By the composition of willemite $Co_xZn_{2-x}SiO_4$(X=0.01, 0.03, 0.05, 0.07, 0.09 mole), this study used reagent grade zinc oxide, cobalt oxide and silicon dioxide as starting materials, carrying out the synthesis with solid reaction method by adding $H_3BO_3$ as a mineralizer. The firing temperature was between $1200^{\circ}C$ and $1400^{\circ}C$. The characteristics of synthesized pigment were analyzed by X-ray diffraction, Raman spectroscopy and SEM and the characteristics of color tones were analyzed by UV-Vis spectroscopy and CIE-$L^*a^*b^*$ measurement. As a result, the optimal composition was $Zn_{1.95}Co_{0.05}$ with 1wt% of $H_3BO_3$ as a mineralizer and firing condition was $1350^{\circ}C$/3 h. $L^*a^*b^*$ value was 29.25, 41.03, -59.93 for on glaze pigment and 37.03, 36.41, -60.03 for under glaze pigment.

Effect of Color Development of Willemite Crystalline Glaze by Adding NiO (Willemite 결정유에 NiO 첨가가 발색에 미치는 영향)

  • Lee, Chi-Youn;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.47 no.6
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    • pp.598-602
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    • 2010
  • When metal oxides are added into crystalline glaze, colors of glaze and crystals are similar as colorants generally. But the case of NiO in zinc crystalline glaze is different from general color development. When NiO is added to zinc crystalline glaze it can develop two or three colors. The active use of color development mechanism by adding NiO to the zinc crystalline glaze to control color of the base glaze and crystal with stability is investigated. This report is expected to contribute to the ceramic industry in improving application of zinc crystalline glaze. For the experiment of NiO, the quantity of NiO additives is changed to the base glaze for the most adequate formation of willemite crystal from previous research and firing condition: temperature increasing speed $5^{\circ}C/min$, holding 1 h at $1270^{\circ}C$, annealing speed $3^{\circ}C/min$ till $1170^{\circ}C$, holding 2 h at $1170^{\circ}C$ then naturally annealed. The samples are characterized by X-ray diffraction (XRD), UV-vis, and Micro-Raman. The result of the procedure as follows; Ni substitutes for Zn ion then glaze develops blue willemite crystals, as if cobalt is used, on brown glaze base. When NiO quantity is increased to over 5 wt%, willemite size is decreased, and the density of the crystal is increased, at the same time $Ni_2SiO_4$ (olivine) phase, the second phase, has been developed. The excessive NiO is reacted with silicate in the glass then developed green $Ni_2SiO_4$ (olivine), and quantity of $Ni_2SiO_4$ (olivine) is increased as quantity of willemite is decreased. It is proved to create three colors, blue, brown and green by controlling the quantity of NiO to the zinc crystalline glaze and it will improve the multiple use of colors to the ceramic design.

Water-Assisted Synthesis of Carbon Nanotubes at Low Temperature and Low Pressure (물을 첨가한 탄소나노튜브의 저온 저압 합성)

  • Kim, Young-Rae;Jeon, Hong-Jun;Lee, Nae-Sung
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.395-395
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    • 2008
  • Water-assisted synthesis of carbon nanotubes (CNTs) has been intensively studied in recent years, reporting that water vapor enhances the activity and lifetime of metal catalyst for the CNT growth. While most of these studies has been focused on the supergrowth of CNTs at high temperature, rarely has the similar approach been made for the CNT synthesis at low temperature. Since the metal catalyst are much less active at lower temperature, we expect that the addition of water vapor may increase the activity of catalyst more largely at lower temperature. We synthesized multi-walled CNTs at temperature as low as $360^{\circ}C$ by introducing water vapor during growth. The water addition caused CNTs to grow ~3 times faster. Moreover, the water-assisted growth prolonged the termination of CNT growth, implying the enhancement of catalyst lifetime. In general, a thinner catalyst layer is likely to produce smaller-diameter, longer CNTs. In a similar manner, the water vapor had a greater effect on the growth of CNTs for a smaller thickness of catalyst in this study. To figure out the role of process gases, CNTs were grown in the first stage and then exposed to each of process gases in the second stage. It was shown that water vapor and hydrogen did not etch CNTs while acetylene led to the additional growth of CNTs even faster in the second stage. As-grown CNTs were characterized by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM), and Raman spectroscopy.

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Effect of Acid Treatment on Transparent Conductive Films of Single-Walled Carbon Nanotubes Prepared Using Various Surfactants in Aqueous Solutions (계면 활성제로 분산한 SWCNT 투명 전도성 필름의 산 처리 효과)

  • Kim, Myoung-Su;Goak, Jeung-Choon;Han, Jong-Hun;Lee, Nae-Sung
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.396-396
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    • 2008
  • 투명 전도성 탄소나노튜브(carbon nanotube, CNT) 필름을 터치스크린이나 디스플레이 소자 등의 전극에 응용할 목적으로, CNT 필름의 전기저항 및 광 투과도를 향상시키기 위한 연구가 활발히 진행되고 있다. 본 연구에서는 단일벽 CNT (single-walled CNT)를 여러 가지 계면활성제로 분산시킨 수용액으로부터 제조한 CNT 필름을 산 처리하여 저항 및 투과도의 변화를 관찰하였다. 우선 계면활성제로 분산시킨 CNT 수용액을 알루미나 재질의 필터에서 정량적으로 진공 필터링하여 CNT 필름을 제조하였다. 알루미나 필터를 sodium hydroxide (NaOH) 수용액으로 용해시켜 제거함으로써 얻은 CNT 필름을 유리기판 위에 부착시킨 후 광 투과도와 먼 저항 (sheet resistance)을 측정하였다. CNT 필름을 질산 ($HNO_3$) 용액에 처리하였을 때 투과도는 1~5 % 향상되었으며, 면 저항은 계면활성제로 분산시킨 CNT 필름 대부분에서 감소하였다. 이는 CNT 표면에 코팅되어 있던 계면활성제들이 산에 의해 제거되었기 때문일 것으로 추측된다. 특히 sodium dodecylbenzene sulfonate (NaDDBS)로 제조한 CNT 필름의 경우, 질산을 처리 전에는 투과도 83%, 면 저항 450 $\Omega$/sq.의 특성을 보였으나, 처리 후에는 각각 86 %, 350 $\Omega$/sq.로 향상되었다. Polyvinyl pyrrolidone (PVP)과 cetyltrimethylammonium bromide (CTAB)를 사용하여 제조한 CNT 필름의 면 저항이 가장 뚜렷한 감소를 보였다. 제조된 필름과 삼 처리된 필름 특성을 Raman spectroscopy, scanning electron microscopy, UV-Vis spectroscopy 등을 이용하여 분석하였고, 4-point probe로 면 저항을 측정하였다.

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