• Title/Summary/Keyword: secondary crystallization.

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Preparation and Characteristics of $Y_2O_3-CeO_2-ZrO_2$Structural Ceramics ; I. Synthesis and Sinterability of Powder ($Y_2O_3-CeO_2-ZrO_2$ 구조세라믹스의 제조 및 특성 : I 분말의 합성 및 소결성)

  • 오혁상;이윤복;김영우;오기동;박흥채
    • Journal of the Korean Ceramic Society
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    • v.33 no.9
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    • pp.1057-1063
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    • 1996
  • Y2O3-CeO2-ZrO2 powders were prepared from water-soluble salts using a coprecipitation method. The forming process of oxide and the characteristics of the calcined powders treated in different drying conditions were investigated. The oxidation was occurred at the temperature of around 40$0^{\circ}C$ and the main crystallization of ZrO2 around $600^{\circ}C$. On calcination at $600^{\circ}C$ heating lamp-dried powders consisted of agglomerates of globular morphology with average agglomerate size of 2.27${\mu}{\textrm}{m}$ and specific surface area of 68.3m2/g and spray dried powders contained dense spheric particles with average agglomerate size of 1.35${\mu}{\textrm}{m}$ and specific surface area of 11.0m2/g which exhibited low agglomeration tendency. Removal of the water by a freeze-drying technique produced calcined powders containing flake-like secondary particle structures with wide agglomerate size distri-bution of 0.1-60${\mu}{\textrm}{m}$ and specific surface area of 24.5${\mu}{\textrm}{m}$. The 20 MPa-pressed density (36.8-41.4% T,D) of calcined powders did not nealy depend on drying methods whilst compaction ratio of calcined powders derived from freeze-drying was the highest ( 6.24) among three drying methods. On continuous heating up to 150$0^{\circ}C$ the sinterability of calcined powders derived from heating lamp-drying was superior to those derived from spray-and freeze-drying. The final sintered density of calcined powders was the highest (96% T,D at 150$0^{\circ}C$) in case of heating lamp-drying.

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Structural and Electrochemical Properties of Spin Coated LiCoO2 Cathode Thin Film in Lithium Secondary Batteries (스핀코팅법에 의한 리튬 2차전지용 산화물 양전극 LiCoO2 박막의 구조 및 전기화학적 특성에 대한 연구)

  • Gang, Seong-Gu;Yu, Gi-Cheon
    • Journal of the Korean Chemical Society
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    • v.50 no.3
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    • pp.243-246
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    • 2006
  • The LiCoO2 thin films were prepared on the Pt/Ti/SiO2/Si substrate by spin coating using citrate sol. The citrate sol was spin-coated on substrate and dried at 380oC for 15 min. to evaporate the solvents and remove the organic materials. The as-deposited films were annealed at 750oC for 10 min. in air for crystallization. The X-ray diffraction patterns for the film have been indexed hexagonal system with space group R3m. The active area of LiCoO2 films for electrochemical test was about 11cm2. A Li foil and 1M LiClO4 in propylene carbonate(PC) and ethylene carbonate(EC) (1:1)were used as an anode and an electrolyte, respectively. The galvanostatic charge-discharge test was carried out at constant current density ranging from 5 A/cm2 in the voltage window between 4.2 and 3.0 V. The first discharge capacity of the film is 0.35Ah/cm2-m. The cycling behavior of the LiCoO2 film is also reported.

Heavy Metal Retention by Secondary Minerals in Mine Waste Rocks at the Abandoned Seobo Mine (서보광산 폐광석 내 2차 광물에 의한 중금속 고정화)

  • 이평구;강민주;최상훈;신성천
    • Economic and Environmental Geology
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    • v.36 no.3
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    • pp.177-189
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    • 2003
  • The main purposes of this study are to utilize mineralogical studies such as optical microscope, XRD and SEM/EDS analyses to characterize the oxidation of sulfide minerals and the mechanisms controlling the movement of dissolved metals from waste rocks at the abandoned Seobo mine. Mineralogical research of the waste rocks confirms the presence of anglesite, covellite, goethite, native sulfur and nsutite as secondary minerals, suggesting that these phases control the dissolved concentrations of As, Cu, Fe, Mn, Pb and Zn. The dissolved metals are precipitated, adsorbed and/or coprecipitated with(or within) Fe(Mn)-hydroxides and Mn(Fe)-hydroxides. The main phases of secondary mineral, Fe-hydroxide, can be classified as amorphous or poorly crystalline and more crystallized phases(e.g. goethite) by crystallinity. Amorphous or poorly crystalline Fe-hydroxide has relatively high As contents(9-24 wt.%). This poorly crystalline Fe-hydroxide changes toward more crystallized phase(e.g. goethite) which contains relatively low As(0.6-7.7 wt.%). These results are mainly due to the progressive release of As with the crystallization evolution of the As-trapping poorly crystalline Fe-hydroxides. It is also attributed to the differences of specific surface areas between the poorly crystalline Fe-hydroxides and well crystallized phases. The dissolved metals from waste rocks at Seobo mine area are naturally attenuated by a series of precipitation(as Fe, Mn, Cu, Pb), coprecipitation(Fe, Mn) and adsorption(As, Cu, Pb, An) reactions. The results of mineralogical researches permit to assess the environmental impacts of mine waste rocks in the areas, and can be used as a useful data to lay available mine restoration plan.

Preparation of Al@Fe2O3 Core-Shell Composites Using Amphiphilic Graft Copolymer Template

  • Patel, Rajkumar;Kim, Sang Jin;Kim, Jin Kyu;Park, Jung Su;Kim, Jong Hak
    • Korean Chemical Engineering Research
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    • v.52 no.2
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    • pp.209-213
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    • 2014
  • A graft copolymer of poly(vinyl chloride)-g-poly(oxyethylene methacrylate) (PVC-g-POEM) was synthesized via atom transfer radical polymerization (ATRP) and used as a structure-directing agent to prepare $Al@Fe_2O_3$ core-shell nanocomposites through a sol-gel process. The amphiphilic property of PVC-g-POEM allows for good dispersion of Al particles and leads to specific interaction with iron ethoxide, a precursor of $Fe_2O_3$. Secondary bonding interaction in the sol-gel composites was characterized by Fourier transform-infrared (FT-IR) spectroscopy. The well-organized morphology of $Al@Fe_2O_3$ core-shell nanocomposites was observed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) were used to analyze the elemental composition and crystallization structure of the composites.

Properties of CulnSe$_{2}$ thin films selenizing indium/copper layers prepared by D.C. magnetron sputtering (D.C. magnetron sputtering에 의해 indium/copper 층이 selenizing된 $CuInSe_2$막의 특성)

  • Han, Sang-Kyu;Kim, Sun-Jae;Lee, Hyung-Bock;Lee, Byung-Ha;Park, Sung
    • Electrical & Electronic Materials
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    • v.8 no.3
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    • pp.298-305
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    • 1995
  • Copper-indium diselenide, $CuInSe_2$, thin films have been fabricated by selenizing Cu/In stacked layers with different sputtered Cu/(Cu+ln) mole ratios at 450.deg. C for 1hr on alumina substrates. The selenium source was selenium vapor. Microstructure, crystallization, and composition of the selenized $CuInSe_2$ films were examined by using scanning electron microscope, X-ray diffraction, Auger electron spectroscopy, and secondary ion mass spectrometry. Electrical resistivity and hall effects were also measured to investigate the electrical properties. As the sputtered Cu/(Cu+In) mole ratio of In/Cu layer increased, the amounts of void and CuSe phase in the selenized films increased but the composition of $CuInSe_2$ phase was the same regardless of the sputtered mole ratio. Comparing the electrical properties of $CuInSe_2$ thin film before and after the chemical etching, it was seen that the electrical resistivity, carrier concentration, and carrier mobility of the selenized films were affected by the amount of CuSe phase which seemed to increase primarily the hole concentration of the selenized films.

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Effects of annealing under oxygen atmosphere of PZT thin films on LTCC substrates (LTCC 기판위에 성장시킨 PZT 박막의 열처리시 $O_2$가 미치는 영향)

  • Lee, Kyung-Chun;Hur, Won-Young;Hwang, Hyun-Suk;Lee, Tae-Yong;Lee, Jong-Duk;Song, Joon-Tae
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.205-205
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    • 2010
  • Recently, low temperature co-fired ceramic (LTCC) technology is widely used in sensors, actuators and microsystem fields because of its very good electrical and mechanical properties, high stability as well as possibility of making 3D micro structures. In this study, we investigated the effects of on $O_2$ annealing treatment on the electrical properties of Pb(ZrTi)$O_3$ (PZT) thin films deposited on LTCC substrate. The LTCC substrates with thickness of $400\;{\mu}m$ were fabricated by laminating 4 green tapes which consist of alumina and glass particle in an organic binder. The PZT thin films were deposited on Au / LTCC substrates by RF magnetron sputtering method. The change of the crystallization of the films were investigated under various atmosphere. The structural variation of the films were analyzed by using X-Ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) and secondary ion mass spectrometry (SIMS).

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A study on the relationship of various characterizations for undoped ZnO thin films (Undoped ZnO 박막의 다양한 특성의 상관관계에 대한 연구)

  • Baek, Kyung-Hyun;Park, Hyeong-Sik;Jang, Kyung-Soo;Jung, Sung-Wook;Ryu, Kyung-Yul;Yun, Eui-Jung;Yi, J.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.147-147
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    • 2010
  • PTC Thermistors specimens were fabricated by added $MnO_2$ as donors, and $Nb_2O_5$ as acceptors and sintered $1250^{\circ}C$/2hrs. Average grain size decreased with increased in added $MnO_2$, and increased with added in $Nb_2O_5$. But, appeared liquid phase as $Bi_2O_3$ and $TiO_2$, affect to grain growth. XRD result, peak strength waslowed then crystallization not well, but, secondary phase were not showed all specimens. All specimens resistance were so high, about $40M{\Omega}$ over, couldn't measured to those resistance and doesn't appear PTCR effect.

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Efficiency Characteristics of Cu(In,Ga)Se2 Photovoltaic Thin Films According to the Mo:Na Thickness (Mo:Na두께에 따른 Cu(In,Ga)Se2 태양전지 박막의 효율 특성)

  • Shin, Younhak;Kim, Myunghan
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.26 no.9
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    • pp.701-706
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    • 2013
  • We have focused on the conversion efficiency of CIGS thin film solar cell prepared by co-evaporation method as well as the optimization of process condition. The total thickness of back electrode was fixed at 1 ${\mu}m$ and the structural, electric and optical properties of CIGS thin film were investigated by varying the thickness of Mo:Na bottom layer from 0 to 500 nm. From the experimental results, the content of Na was appeared as 0.28 atomic percent when the thickness of Mo:Na layer was 300 nm with compactly densified plate-shape surface morphology. From the XRD measurements, (112) plane was the strongest preferential orientation together with secondary (220) and (204) planes affecting to the crystallization. The lowest roughness and resistivity were 2.67 nm and 3.9 ${\Omega}{\cdot}cm$, respectively. In addition, very high carrier density and hole mobility were recorded. From the optimization of Mo:Na layer, we have achieved the conversion efficiency of 9.59 percent.

Structure and Magnetic Properties of a Fe73.5Si13.5B9Nb3Cu1 Alloy Nanopowder Fabricated by a Chemical Etching Method and Milling Procedure

  • Hong, Seong-Min;Kim, Jeong-Gon;Kim, Cheol-Gi
    • Journal of Magnetics
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    • v.14 no.2
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    • pp.71-74
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    • 2009
  • The magnetic and structural properties of FINEMET (the Hitachi product name of the Fe-Si-B-Nb-Cu alloy) nanopowder with a composition of $Fe_{73.5}Si_{13.5}B_9Nb_3Cu_1$ atomic percent were investigated after annealing, chemical etching, and mechanical milling. The primary and secondary crystallization temperatures were 523 and $550^{\circ}C$, respectively. The grain size of the particles was adjusted by annealing time. Optimally annealed particles exhibited a homogenous microstructure composed of nanometer-sized crystalline grains. The grain boundary of the annealed particles was etched preferentially by chemical etching. Chemically etched particles were broken at the grain boundary by high-energy ball milling. As a result, a nanometer-sized FINEMET powder with a uniform size of crystalline grains was fabricated.

Studied on the Crystallization of $Li_2O-Al_2O_3-SiO_2$ Glass by Adding $TiO_2$ and $ZrO_2$ ($TiO_2$$ZrO_2$의 첨가에 따르는 $Li_2O-Al_2O_3-SiO_2$ 계 유리의 결정화에 관한 연구)

  • 박용완;전문덕
    • Journal of the Korean Ceramic Society
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    • v.18 no.3
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    • pp.187-191
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    • 1981
  • The effect of additions, $TiO_2$ and $ZrO_2$ as nucleant on the base glass which composition was determined to 0.97 $Li_2O-Al_2O_3-SiO_2$ has been investigated by means of D.T.A., X-ray diffraction and dilatation. $TiO_2$ and $ZrO_2$ as nucleant were added 0.06mole, in which ratios of $TiO_2$/$ZrO_2$ were varied 1/0, 2/1, 1/1, 1/2 and 0/1. The crystalline phases were appeared to $\beta$-spodumene as principal, $\beta$-eucryptite and $ZrO_2$ as secondary, regardless of nucleant variations. The crystallinity of the crystallized glass added $TiO_2$, $ZrO_2$ mixture as nucleant was higher than that of the glass added $TiO_2$ or $ZrO_2$ only. The crystallinity of the glass added $TiO_2$/$ZrO_2$ =1/1 was highest. Increasing the addition of $ZrO_2$, it has been observed that the crystal growing temperature became higher.

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