• Title/Summary/Keyword: X-선 분말회절

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Synthesis and Characterization of Aluminosilicate Prepared Using Structure Directing Agent Containing Piperidine Moiety (피페리딘형 구조유도분자를 이용한 알루미노실리케이트 제올라이트의 합성 및 특성 연구)

  • Kim, Su Hyun;Park, Sung Jun;Shin, Na Ra;Cho, Sung June
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.203-207
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    • 2013
  • Zeolites with different structures were synthesized from the hydrothermal synthesis condition employing simple structure directing agent (SDA) containing piperidine moiety. The gel containing $1.0SiO_2$:0.9SDA:$0.062NaAlO_2$:0.217NaOH:$20H_2O$ was subject to hydrothermal synthesis at 413~453 K for 7 days. FER type zeolite was obtained at 433 K when piperidine was employed as SDA, whereas TON and MFI type zeolites were also obtained at 433 K when 2,6-dimethylpiperidine and 2,2,6,6-tetramethylpiperidine were used, respectively. Further increase of hydrothermal synthesis temperature to 453 K resulted in the formation of TON type zeolite when 2-mtheylpiperidine was used. The structural analysis of powder X ray diffraction pattern over FER type zeolite suggested that the SDA, piperidine interacted intimately with the zeolite where it located close to the framework.

Synthesis of Borosilicate Zeotypes by Steam-assisted Conversion Method (수증기 쪼임법에 의한 제올라이트형 보로실리케이트 제조방법)

  • Mansour, R.;Lafjah, M.;Djafri, F.;Bengueddach, A.
    • Journal of the Korean Chemical Society
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    • v.51 no.2
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    • pp.178-185
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    • 2007
  • Intermediate pentasil borosilicate zeolite-like materials have been crystallized by a novel method named steam-assisted conversion, which involves vapor-phase transport of water. Indeed, amorphous powders obtained by drying Na2O.SiO2.B2O3.TBA2O gels of various compositions using different boron sources are transformed into crystalline borosilicate zeolite belonging to pentasil family structure by contact with vapors of water under hydrothermal conditions. Using a variant of this method, a new material which has an intermediate structure of MFI/MEL in the ratio 90:10 was crystallized. The results show that steam and sufficiently high pH in the reacting hydrous solid are necessary for the crystallization to proceed. Characterization of the products shows some specific structural aspects which may have its unique catalytic properties. X-ray diffraction patterns of these microporous crystalline borosilicates are subjected to investigation, then, it is shown that the product structure has good crystallinity and is interpreted in terms of regular stacking of pentasil layers correlated by inversion centers (MFI structure) but interrupted by faults consisting of mirror-related layers (MEL structure). The products are also characterized by nitrogen adsorption at 77 K that shows higher microporous volume (0.160 cc/g) than that of pure MFI phase (0.119 cc/g). The obtained materials revealed high surface area (~600 m2/g). The infrared spectrum reveals the presence of an absorption band at 900.75 cm-1 indicating the incorporation of boron in tetrahedral sites in the silicate matrix of the crystalline phase.

Characteristics of $TiH_2$ under High Pressure (고압하에서 $TiH_2$의 특성화 연구)

  • Kim, Young-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.5 no.2
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    • pp.72-78
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    • 1992
  • The Earth outer core accomodates moderately considerable amount of lighter elements than pure iron itself. Hydrogen is one of the possible candidates of minor constituents in the outer core. It would be worth while to extend for the pressure effect on the solubility of hydrogen in the metal-hydrides including iron hydride. In view of hydrogen being one of the potential substitutes for petroleum, searching a more efficient way for storing hydrogen in the form of hydrides is of considerable value. For two purposes, $TiH_2$was selected among lot of hydrides for its characteristics under pressure and temperature. There have been two kinds of experiment carried out on $TiH_2$ under different experimental conditions. As one of these attempts, polycrystalline $TiH_2$ was loaded up to 15 GPa stepwise at the constant temperature 500${\circ}$ using a piston-cylinder diamond anvil cell equipped with a miniature furnace of an electric power supply. The X-ra diffraction technique was employed on the quenched samples after the simultaneous high pressure and temperature treatments. During these high pressure-temperature runs, and irreversible phase of $TiH_2$ has been observed at the pressures higher than 11.3 GPa, which would be assigned to the orthorhombic crystal system as one of the new phase(s) of $TiH_2$. Molar volume change on this phase transition is ∼10%.

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Solid-state reaction kinetics for the formation of aluminium titanate ($AL_2TiO_5$) from amorphous $TiO_2$ and $\alpha-AL_2O_3$ (비정질 $TiO_2$$\alpha-AL_2O_3$부터 $AL_2TiO_5$를 합성하기 위한 고체상태 반응속도)

  • Ik Jin Kim;Oh Seong Kweon;Young Shin Ko;Constantin Zografou
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.2
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    • pp.259-270
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    • 1997
  • Reaction kinetics for the solid-state reaction of $\alpha-Al_2O_3$ with amorphous $TiO_2$ to produce $Al_2TiO_5$ (Tialite) was studied in the temperature range of $1200~1300^{\circ}C$. Rate of kinetic reaction were determined by using $TiO_2$-coated $Al_2O_3$ compact containing 50 mol% $TiO_2$ and heating the reactant mixtures in MgO at definite temperature for various times. Amount of products and unreacted reactants were determined by X-ray diffractometry. Data from the volume fraction and ratio of peak intensities of $\beta-Al_2TiO_5$ indicated that the reaction of $\alpha-Al_2O_3$ with $TiO_2$ to form pseudobrookite starts between 1280 and $1300^{\circ}C$. The activation energy for solid-state reaction was determined by using the Arrhenius equation ; The activation energy was 622.4 kJ/mol.

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유리화 비정형 탄소(vitreous carbon)를 이용하여 제작한 전계방출 소자의 균일성 증진방법

  • 안상혁;이광렬
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.53-53
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    • 1999
  • 전계방출을 이용한 평판 표시장치는 CRT가 가진 장점을 모두 갖는 동시에 얇고 가벼우며 낮은 전력소모로 완벽한 색을 구현할 수 있는 차세대 표시장치로서 이에 대한 여국가 활발히 이루어지고 있다. 여기에 사용되는 음극물질로서 실리콘이나 몰리 등을 팁모양으로 제작하여 사용해 왔다. 하지만 잔류가스에 의한 역스퍼터링이나 화학적 반응에 의해서 전계방출 성능이 점차 저하되는 등의 해결해야할 많은 문제가 있다. 이러한 문제들을 해결하기 위하여 탄소계 재료로서 다이아몬드, 다이아몬드상 카본 등을 이용하려는 노력이 진행되어 왔다. 이중 유리화 비정형 탄소는 다량의 결함을 가지고 있는 유리질의 고상 탄소 재로로서, 전기전도도가 우수하면서 outgassing이 적고 기계적 강도가 뛰어나며 고온에서도 화학적으로 안정하여 전계방출 소자의 음극재료로서 알맞은 것으로 생각된다. 유리화 비정형 탄소가루를 전기영동법으로 기판에 코팅하여 전계방출 소자를 제작하였다. 전기영동 용액으로 이소프로필알코올에 질산마그네슘과 소량의 증류수, 유리화 비정형 탄소분말을 섞어주었고 기판으로는 몰리(Mo)가 증착된 유리를 사용하였다. 균일한 증착을 위해서 증착후 역전압을 걸어 주는 방법과 증착 후 플라즈마 처리를 하는 등의 여러 가지 방법을 사용했다. 전계방출 전류는 1$\times$10-7Torr이사에서 측정하였다. 1회 제작된 용액으로 반복해서 증착한 횟수에 따라 표면의 거치기, 입자의 분포, 전계방출 측정 결과 등의 차이가 관찰되었다. 발광이미지는 전압에 따라 변화하였고, 균일한 발광을 관찰하기 위해서 오랜 시간동안 aging 과정을 거쳐야 했다. 그리고 구 모양의 양극을 사용해서 위치를 변화시키며 시동 전기장을 관찰하여 위치에 따른 전계방출의 차이를 조사하여 발광의 균일성을 알 수 있었다.on microscopy로 분석하였으며 구조 분석은 X-선 회절분석, X-ray photoelectron spectroscopy 그리고Auger electron spectroscope로 하였다. 증착된 산화바나듐 박막의 전기화학적 특성을 분석하기 위하여 리튬 메탈을 anode로 하고 EC:DMC=1:1, 1M LiPF6 액체 전해질을 사용한 Half-Cell를 구성하여 200회 이상의 정전류 충 방전 시험을 행하였다. Half-Cell test 결과 박막의 결정성과 표면상태에 따라 매우 다른 전지 특성을 나타내었다.도상승율을 갖는 경우가 다른 베이킹 시나리오 모델에 비해 효과적이라 생각되며 초대 필요 공급열량은 200kW 정도로 산출되었다. 실질적인 수치를 얻기 위해 보다 고차원 모델로의 해석이 필요하리라 생각된다. 끝으로 장기적인 관점에서 KSTAR 장치의 베이킹 계획도 살펴본다.습파라미터와 더불어, 본 연구에서 새롭게 제시된 주기분할층의 파라미터들이 모형의 학습성과를 높이기 위해 함께 고려된다. 한편, 이러한 학습과정에서 추가적으로 고려해야 할 파라미터 갯수가 증가함에 따라서, 본 모델의 학습성과가 local minimum에 빠지는 문제점이 발생될 수 있다. 즉, 웨이블릿분석과 인공신경망모형을 모두 전역적으로 최적화시켜야 하는 문제가 발생한다. 본 연구에서는 이 문제를 해결하기 위해서, 최근 local minimum의 가능성을 최소화하여 전역적인 학습성과를 높여 주는 인공지능기법으로서 유전자알고리즘기법을 본 연구이 통합모델에 반영하였다. 이에 대한 실증사례 분석결과는 일일 환율예측문제를 적용하였을 경우, 기존의 방법론보다 더 나운 예측성과를 타나내었다.pective" to workflow architectural discussions. The vocabulary suggested

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Elevation of Properties of Al-Nb-Ar alloys Fabricated by Mechanical Alloying Metho (기계적합금화법을 이용한 고온 고강도 Al-Nb-Zr 합금 제조 및 특성 평가)

  • Kwon, Dae-Hwan;Ahn, In-Shup;Kim, Sang-Shik;Lee, Kwang-Min;Park, Min-Woo
    • Korean Journal of Materials Research
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    • v.10 no.7
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    • pp.499-504
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    • 2000
  • Recently there have been many investigations on the synthesis and properties of transition metal trialuminides based on Ti, Zr, V, Nb and Ta for use aircraft structure materials in an elevated environment. The effect of Zr additions on the formation behaviour of Al-Nb alloy was investigated. Al-1.3at.%(Nb+Zr) alloys with different Nb to Zr atomic 1:3, 1:1 and 3:1 were prepared by mechanical alloying(MA). The morphological changes and microstructural evolution of Al-Nb-Zr powders during MA were investigated by SEM, XRD and TEM. The intermetallic compound phase of $Nb_2Al\; and\; Al_3Zr_4$ was identified by X-ray diffraction. The intemetallic compound of $Al_3Zr,\; Al_3Nb$ and $Al_3Zr_4$ were formed by heat treatment for 1 hour at $500^{\circ}C$. The size of intermetallic compounds observed by TEM were approximately below 100nm, when they were heat treated after mechanically alloying for 30 hours.

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Physical and Electrochemical Properties of Gallium Oxide (β-Ga2O3) Nanorods as an Anode Active Material for Lithium Ion Batteries (리튬이온전지용 산화갈륨 (β-Ga2O3) 나노로드 (Nanorods) 음극 활물질의 물리적.전기화학적 특성)

  • Choi, Young-Jin;Ryu, Ho-Suk; Cho, Gyu-Bon;Cho, Kwon-Koo;Ryu, Kwang-Sun;Kim, Ki-Won
    • Journal of the Korean Electrochemical Society
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    • v.12 no.2
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    • pp.189-195
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    • 2009
  • $\beta-Ga_{2}O_{3}$ nanorods were synthesized by chemical vapor deposition method using nickel-oxide nanoparticle as a catalyst and gallium metal powder as a source material. The average diameter of nanorods was around 160 nm and the average length was $4{\mu}m$. Also, we confirmed that the synthesis of nanorods follows the vapor-solid growth mechanism. From the results of X-ray diffraction and HR-TEM observation, it can be found that the synthesized nanorods consisted of a typical core-shell structure with single-crystalline $\beta-Ga_{2}O_{3}$ core with a monoclinic crystal structure and an outer amorphous gallium oxide layer. Li/$\beta-Ga_{2}O_{3}$ nanorods cell delivered capacity of 867 mAh/g-$\beta-Ga_{2}O_{3}$ at first discharge. Although the Li/$\beta-Ga_{2}O_{3}$ nanorods cell showed low coulombic efficiency at first cycle, the cell exhibited stable cycle life property after fifth cycle.

A Study for Recoverability of Iron Resource in Red Mud (레드머드 내 철 자원 회수 가능성 고찰)

  • Kim, Bong-Ju;Kwon, Jang-Soon;Koh, Yong-Kwon;Park, Cheon-Young
    • Economic and Environmental Geology
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    • v.53 no.3
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    • pp.297-306
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    • 2020
  • The red mud generated from bauxite during the Bayer alumina production process has been regarded as an industrial waste due to the high alkaline property and high content of Na. Despite of its environmental problem, various studies for recovery of the valuable resources from red mud has been also carried out because of high content (25.7 wt.% as Fe2O3 in this study) of iron in red mud. In order to recover the iron resource in the red mud, microwave heating experiments were performed with adding of activated carbon and elemental sulfur to the red mud. Through the microwave heating the powdered red mud mixtures converted to porous and vitrified solid aggregates. The vitrified aggregates produced by microwave heating are composed of goethite, zero valent iron (Fe0), pyrrhotite and pyrite. And then, the microwave heating samples were dissolved in the aqua regia solution, and Fe precipitates were obtained as a Fe-chlorides by adding of NaCl salt in the aqua regia solution. The Fe recovery rates in the Fe-chloride precipitates showed differences depending on the experimental mixture conditions, and Fe grades of the end products are 49.0 wt.%, 58.0 wt.% and 59.5 wt.% under mixture conditions of red mud, red mud + activated carbon, and red mud + activated carbon + elemental S, respectively. The Fe content of 56.0 wt.% is generally known as the grade value of Fe in a iron ore for iron production, and the Fe grades of microwave heating samples with adding activated carbon and elemental S in this study are higher than the grade value of 56.0 wt.%.

Thermoelectric Properties of Al4C3-doped α-SiC (Al4C3 첨가 α-SiC의 열전변환특성)

  • 박영석;배철훈
    • Journal of the Korean Ceramic Society
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    • v.40 no.10
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    • pp.991-997
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    • 2003
  • The effect of A1$_4$C$_3$ additive on the thermoelectric properties of SiC ceramics were studied. Porous SiC ceramics with 47∼59% relative density were fabricated by sintering the pressed $\alpha$-SiC powder compacts with A1$_4$C$_3$at 2100∼220$0^{\circ}C$ for 3 h in Ar atmosphere. Crystalline phases of the sintered bodies were identified by powder X-Ray Diffraction (XRD) and their microstructures were observed with a Scanning Electron Microscope (SEM). In the case of A1$_4$C$_3$ addition, the phase transformation of 6H-SiC to 4H-SiC could be observed during sintering. The Seebeck coefficient and electrical conductivity were measured at 550∼95$0^{\circ}C$ in Ar atmosphere. In the case of undoped specimens, the Seebeck coefficients were positive (p-type semiconducting) possibly due to a dominant effect of the acceptor impurities (Al, Fe) contained in the starting powder and electrical conductivity increased as increasing sintering temperature. Electrical conductivity of A1$_4$C$_3$doped specimen is larger than that of undoped specimen under the same condition, which might be due to the reverse phase transformation and increasing of carrier density. And the Seebeck coefficient of A1$_4$C$_3$ doped specimen is also larger than that of undoped specimen. The density of specimen, the amount of addition and sintering atmosphere had significant effects on the thermoelectric property.

Electrochemical Properties of Spinel LiMn2O4 Prepared Through Different Synthesis Routes (스피넬형 양극활물질 LiMn2O4의 합성방법에 따른 전기화학적 특성 비교)

  • Lee, Ki-Soo;Bang, Hyun-Joo;Sun, Yang-Kook
    • Journal of the Korean Electrochemical Society
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    • v.10 no.1
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    • pp.48-51
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    • 2007
  • In order to investigate the effects of particle size and specific surface area(BET area) of spinel powder, $LiMn_2O_4$ were synthesized using metal oxide precursor by co-precipitation method(CoP) and solid state reaction (SSR) .X-ray diffraction(XRD) patterns revealed that the both prepared powder has a well developed spinel structure with Fd3m space group. The $LiMn_2O_4$ prepared by co-precipitation showed spherical morphology with narrow size distribution. However, the $LiMn_2O_4$ prepared by solid state reaction showed relatively smaller particles with irregular shape. The measured BET areas of the powers are $0.8m^2g^{-1}$ (CoP) and $3.6m^2g^{-1}$(SSR). The electrochemical performance of the Prepared $LiMn_2O_4$ powders was evaluated using coin type cells(CR2032) at elevated temperature ($55^{\circ}C$). The $LiMn_2O_4$ prepared by co-precipitation showed the better cycling performance(82.3%capacity retention at $50^{th}$ cycle) than that of the $LiMn_2O_4$(68.3%) prepared by solid state reaction at elevated temperature.