• Title/Summary/Keyword: High-temperature XRD

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Preparation of Porous Glass-Ceramics by the Sintering (소결법에 의한 다공질 결정화유리의 제조)

  • 박용완;이준영
    • Journal of the Korean Ceramic Society
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    • v.31 no.10
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    • pp.1218-1230
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    • 1994
  • In manufacturing process of porous glass-ceramics by the filler method, the sintering behaviour of crystallizable glass powder mixed with various salts was studied and also the effects of precipitated crystal phases on the properties of porous glass-ceramics were investigated. Fine-grained crystallizable glass powder was homogeneously mixed with various slat having grain size 100~200 ${\mu}{\textrm}{m}$ and sintered for densification. After washing out the inorganic salt with distilled water, the porous sintered body was heat treated additionly for crystallization. The MgO-Al2O3-SiO2 base glass was used as crystallizable glass powder and the water soluble salts such as K2SO4 and MgSO4 were used as filler. When K2SO4 was used, leucite crystal phase was formed as a result of the ion exchange and porous glass-ceramics which exhibit high temperature resistance and high thermal expansion coefficient of 17$\times$10-6/$^{\circ}C$ could be obtained. On the contrary, when MgSO4 was used, only slight ion exchange is observed and $\mu$-cordierite and $\alpha$-cordierite crystal phases were formed and porous glass-ceramics which exhibit low thermal expansion coefficient schedule were determined with the results of DTA curves, thermal shrinkage curves and XRD patterns analysis. From DTA curves and thermal shrinkage curves, it was found that the sintering densification have been completed at the temperature range of exothermic peak for crystallization. The pore size distributions and pore diameters were measured by mercury porosimeter. The pore diameter of porous glass-ceramics was 10~15 ${\mu}{\textrm}{m}$ when 100~200${\mu}{\textrm}{m}$ grain size of K2SO4 was used and it was 25~30 ${\mu}{\textrm}{m}$ when the same grain size of MgSO4 was used. The porous glass-ceramics K2SO4 used shows bimodal pore size distribution and its porous skeleton structure was ascertained by SEM observation.

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Heteroepitaxial growth of 3C-SiC on 6H-SiC substrates by thermal chemi-cal vapor deposition (화학기상증착법에 의한 6H-SiC 기판상의 3C-SiC 이종박막 성장)

  • 장성주;박주훈
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.13 no.6
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    • pp.290-296
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    • 2003
  • The heteroepitaxial growth of crystalline 3C-SiC on 6H-SiC substrates using high purity silane ($SiH_4$) and prophane ($C_3H^8$) was carried out by thermal chemical vapor deposition, and growth characteristics were investigated in this study. In case that the flow ratio of C/Si and flow rate of $H_2$ were 4.0 and 5.0 slm, respectively, the growth rate of epilayers was about 1.8 $\mu$m/h at growth temperature of $1200^{\circ}C$. The Nomarski surface morphology, X-ray diffraction, Raman spectroscopy, and photoluninescence of grown epilayers were measured to investigate the crystallinity. In this study, the high quality of crystalline 3C-SiC heteropitaxial layers was observed at growth temperature of above $1150^{\circ}C$.

Fabrication of C2H2 Gas Sensors Based on Ag/ZnO-rGO Hybrid Nanostructures and Their Characteristics (Ag/ZnO-rGO 하이브리드 나노구조 기반 C2H2 가스센서의 제작과 그 특성)

  • Lee, Kwan-Woo;Chung, Gwiy-Sang
    • Journal of Sensor Science and Technology
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    • v.24 no.1
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    • pp.41-46
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    • 2015
  • In this work, pure hierarchical ZnO structure was prepared using a simple hydrothermal method, and Ag nanoparticles doped hierarchical ZnO structure was synthesized uniformly through photochemical route. The reduced graphene oxide (rGO) has been synthesized by typical Hummer's method and reduced by hydrazine. Prepared Ag/ZnO nanostructures are uniformly dispersed on the surface of rGO sheets using ultrasonication process. The synthesized samples were characterized by SEM, TEM, EDS, XRD and PL spectra. The average size of prepared ZnO microspheres was around $2{\sim}3{\mu}m$ and showed highly uniform. The average size of doped-Ag nanoparticles was 50 nm and decorated into ZnO/rGO network. The $C_2H_2$ gas sensing properties of as-prepared products were investigated using resistivity-type gas sensor. Ag/ZnO-rGO based sensors exhibited good performances for $C_2H_2$ gas in comparison with the Ag/ZnO. The $C_2H_2$ sensor based on Ag/ZnO-rGO had linear response property from 3~1000 ppm of $C_2H_2$ concentration at working temperature of $200^{\circ}C$. The response values with 100 ppm $C_2H_2$ at $200^{\circ}C$ were 22% and 78% for Ag/ZnO and Ag/ZnO-rGO, respectively. In additions, the sensor still shows high sensitivity and quick response/recovery to $C_2H_2$ under high relative humidity conditions. Moreover, the device shows excellent selectivity towards to $C_2H_2$ gas at optimal working temperature of $200^{\circ}C$.

LS-MOCVD OF BARIUM STRONTIUM TITANATE THIN FILMS USING NOVEL PRECURSORS

  • Kwon, Hyun-Goo;Oh, Young-Woo;Park, Jung-Woo;Lee, Young-Kuk;Kim, Chang-Gyoun;Kim, Do-Jin;Kim, Yunsoo
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.19-19
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    • 2002
  • Perovskite-type titanate dielectrics have attracted much attention in memory devices such as DRAMs or FeRAMs due to their high dielectric constants. However, low volatility of the Ba, Sr, Pb or Zr precursors with only thd ligands has limitations in obtaining high quality thin films by liquid source metal organic chemical vapor deposition (LS-MOCVD) processes. To improve the volatility of these precursors, many attempts have been made such as adding polyether ligands to satisfy the coordinative saturation. We report the synthesis of new precursors Ba(thd)₂(tmeea) and Sr(thd)₂(tmeea), where tmeea = tris[2-(2-methoxyethoxy)ethyl]amino, and LS-MOCVD of barium strontium titanate (BSTO) thin films using these precursors. Due to increased basicity of amines compared with ethers, it is expected that the nitrogen-donor ligand will make a strong bond to a metal than an analogous oxygen-donor ligand, consequently improving the volatility and thermal behavior of these precursors. Thin films of BSTO were grown on Pt(111)/SiO₂/Si(100) substrates by LS-MOCVD using a cocktail source consisting of the conventional Ti precursor Ti(thd)₂(O/sup i/Pr), and these new Ba and Sr precursors. As-grown films were characterized by XPS, SEM, XRD, XRF, and C-V and I-V measurements. BSTO films grown at 420℃ were stoichiometric barium strontium titanate with very smooth surface morphology and their dielectric constants were found to be as targe as 450. Dependence of the composition, microstructure and the electrical properties of the BSTO films on the growth temperature, annealing temperature, working pressure, and the composition of the cocktail source will be discussed.

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New Polytriazoleimides with High Thermal and Chemical Stabilities

  • E, Yanpeng;Wan, Liqiang;Li, Yujing;Huang, Farong;Du, Lei
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2193-2199
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    • 2012
  • A series of novel polytriazoleimides were prepared from various aromatic dianhydrides and a new kind of 1,2,3-triazole-containing aromatic diamine synthesized by the Cu (I)-catalyzed 1,3-dipolar cycloaddition reaction in DMAc, and characterized by FT-IR, $^1H$-NMR, XRD, DSC and TGA techniques. The results show the polytriazoleimides are soluble in most of strong polar solvents and have inherent viscosity values of 0.51-0.62 dL/g(DMAc). The polytriazoleimide films exhibit a tensile strength of 62.3-104.5 MPa and an elongation at breakage of 4.0-8.1%, a glass transition temperature ($T_g$) of $257-275^{\circ}C$, a decomposition temperature (at 5% weight loss) of $350-401^{\circ}C$ in $N_2$ atmosphere, and a dielectric constant of 2.47-3.01 at 10 MHz, which depend on the structure of the polymers. The polytriazoleimides perform good resistance to acid and alkali solution.

A Novel Acid-Base Catalyzed Sol-Gel Synthesis of Highly Active Mesoporous TiO2 Photocatalysts

  • Khan, Romana;Kim, Sun-Woo;Kim, Tae-Jeong;Lee, Hyo-Sun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.1951-1957
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    • 2007
  • A new synthetic strategy based on the acid-base catalyzed sol-gel method was developed for the preparation of a series of mesoporous TiO2 nanoparticles. A key feature of the method involves a gradual change in pH (0.8- 9) during the sol-gel transition, which guarantees easy introduction of mesoporosity without relying on the well-established sonochemical or template approach. In addition, this method leads to the exclusive formation of the anatase phase stable enough to the calcination temperature up to 600 oC. The physicochemical properties of the particles in the series were characterized by various spectroscopic and analytical techniques such as wide-angle XRD, SAXRD, BET surface area, FE-SEM, TEM, FT-IR, TGA, and XPS. The photocatalytic efficiency of these materials was investigated for the oxidation of toluene under UV-irradiation. All but T-ad in the series exhibited high photocatalytic activity pushing the reaction into completion within 3 h. The reaction followed the first order kinetics, and the rate reaches as high as 3.9 × 10?2/min which exceeds the one with the commercially available Degussa P-25 by a factor of 3.2. When comparison is made among the catalysts, the reactivity increases with increase in the calcination temperature which in turn increases the crystallinity of the anatase phase, thus revealing the following rate orders: T-3 < T-4 < T-5 < T-6.

The Properties of $Bi_2Mg_{2/3}Nb_{4/3}O_7$ Thin Films Deposited on Copper Clad Laminates For Embedded Capacitor (임베디드 커패시터의 응용을 위해 CCL 기판 위에 평가된 BMN 박막의 특성)

  • Kim, Hae-Won;Ahn, Jun-Ku;Ahn, Kyeong-Chan;Yoon, Soon-Gil
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.45-45
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    • 2007
  • Capacitors among the embedded passive components are most widely studied because they are the major components in terms of size and number and hard to embed compared with resistors and inductors due to the more complicated structure. To fabricate a capacitor-embedded PCB for in-line process, it is essential to adopt a low temperature process (<$200^{\circ}C$). However, high dielectric materials such as ferroelectrics show a low permittivity and a high dielectric loss when they are processed at low temperatures. To solve these contradicting problems, we studied BMN materials as a candidate for dielectric capacitors. processed at PCB-compatible temperatures. The morphologies of BMN thin films were investigated by AFM and SEM equipment. The electric properties (C-F, I-V) of Pt/BMN/Cu/polymer were evaluated using an impedance analysis (HP 4194A) and semiconductor parameter analyzer (HP4156A). $Bi_2Mg_{2/3}Nb_{4/3}O_7$(BMN) thin films deposited on copper clad laminate substrates by sputtering system as a function of Ar/$O_2$ flow rate at room temperature showed smooth surface morphologies having root mean square roughness of approximately 5.0 nm. 200-nm-thick films deposited at RT exhibit a dielectric constant of 40, a capacitance density of approximately $150\;nF/cm^2$, and breakdown voltage above 6 V. The crystallinity of the BMN thin films was studied by TEM and XRD. BMN thin film capacitors are expected to be promising candidates as embedded capacitors for printed circuit board (PCB).

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Mechanism of Tungsten Recovery from Spent Cemented Carbide by Molten Salt Electrodeposition

  • Hongxuan Xing;Zhen Li;Enrui Feng;Xiaomin Wang;Hongguang Kang;Yiyong Wang;Hui Jin;Jidong Li
    • Journal of Electrochemical Science and Technology
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    • v.14 no.1
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    • pp.75-84
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    • 2023
  • The accumulation of spent carbide (YG8), not only pollutes the environment but also causes waste of tungsten, cobalt and other rare metal resources. To better address this issue, we proposed a combined electrochemical separation process of low-temperature aqueous solution and high-temperature molten salt for tungsten and cobalt. H2WO4 was obtained from spent carbide in an aqueous solution, and we calcined it to obtain WO3, which was used as a raw material to obtain tungsten by using molten salt electrodeposition. The influence of the current efficiency and the electrochemical behavior of the discharge precipitation of W(VI) were also studied. The calcination results showed that the morphology of WO3 was regular and there were no other impurities. The maximum current efficiency of 82.91% was achieved in a series of electrodeposition experiments. According to XRD and SEM analysis, the recovered product was high purity tungsten, which belongs to the simple cubic crystal system. In the W(VI) reduction mechanism experiments, the electrochemical process of W(VI) in NaCl-Na2WO4-WO3 molten salt was investigated using linear scanning voltammetry (LSV) and chronoamperometry in a three-electrode system. The LSV showed that W(VI) was reduced at the cathode in two steps and the electrode reaction was controlled by diffusion. The fitting results of chronoamperometry showed that the nucleation mechanism of W(VI) was an instantaneous nucleation mode, and the diffusion coefficient was 7.379×10-10 cm2·s-1.

Preparation of nanoparticles CuInSe2 absorber layer by a non-vacuum process of low cost cryogenic milling (저가의 cryogenic milling 비진공법을 이용한 나노입자 CuInSe2 광흡수층 제조)

  • Kim, Ki-Hyun;Park, Byung-Ok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.2
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    • pp.108-113
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    • 2013
  • Chalcopyrite material $CuInSe_2$ (CIS) is known to be a very prominent absorber layer for high efficiency thin film solar cells. Current interest in the photovoltaic industry is to identify and develop more suitable materials and processes for the fabrication of efficient and cost-effective solar cells. Various processes have been being tried for making a low cost CIS absorber layer, this study obtained the CIS nanoparticles using commercial powder of 6 mm pieces for low cost CIS absorber layer by high frequency ball milling and cryogenic milling. And the CIS absorber layer was prepared by paste coating using milled-CIS nanoparticles in glove box under inert atmosphere. The chalcopyrite $CuInSe_2$ thin films were successfully made after selenization at the substrate temperature of $550^{\circ}C$ in 30 min, CIS solar cell of Al/ZnO/CdS/CIS/Mo structure prepared under various deposition process such as evaporation, sputtering and chemical vapor deposition respectively. Finally, we achieved CIS nanoparticles solar cell of electric efficient 1.74 % of Voc 29 mV, Jsc 35 $mA/cm^2$ FF 17.2 %. The CIS nanoparticles-based absorber layers were characterized by using EDS, XRD and HRSEM.

Characterization of various crystal planes of beta-phase gallium oxide single crystal grown by the EFG method using multi-slit structure (다중 슬릿 구조를 이용한 EFG 법으로 성장시킨 β-Ga2O3 단결정의 다양한 결정면에 따른 특성 분석)

  • Hui-Yeon Jang;Su-Min Choi;Mi-Seon Park;Gwang-Hee Jung;Jin-Ki Kang;Tae-Kyung Lee;Hyoung-Jae Kim;Won-Jae Lee
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.34 no.1
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    • pp.1-7
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    • 2024
  • β-Ga2O3 is a material with a wide band gap of ~4.8 eV and a high breakdown-voltage of 8 MV/cm, and is attracting much attention in the field of power device applications. In addition, compared to representative WBG semiconductor materials such as SiC, GaN and Diamond, it has the advantage of enabling single crystal growth with high growth rate and low manufacturing cost [1-4]. In this study, we succeeded in growing a 10 mm thick β-Ga2O3 single crystal doped with 0.3 mol% SnO2 through the EFG (Edge-defined Film-fed Growth) method using multi-slit structure. The growth direction and growth plane were set to [010]/(010), respectively, and the growth speed was about 12 mm/h. The grown β-Ga2O3 single crystal was cut into various crystal planes (010, 001, 100, ${\bar{2}}01$) and surface processed. The processed samples were compared for characteristics according to crystal plane through analysis such as XRD, UV/VIS/NIR/Spec., Mercury Probe, AFM and Etching. This research is expected to contribute to the development of power semiconductor technology in high-voltage and high-temperature applications, and selecting a substrate with better characteristics will play an important role in improving device performance and reliability.