• Title/Summary/Keyword: Crystal impurity

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Separatipon of Oryzanol from the Refining By-Product of Rice Bran Oil (미강유 정제 부산물로부터 오리자놀 분리)

  • Kim, In-Hwan;Kim, Chul-Jin
    • Korean Journal of Food Science and Technology
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    • v.23 no.1
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    • pp.76-80
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    • 1991
  • To isolate oryzanol from the by-product of rice bran oil refinning, experiment of solvent fractional crystallization was carried out at various conditions with the dark oil obtained by acidifying the soap stock of micella refinning process and the pitch obtained from vacuum distillation of the dark oil. The impurity interfering the crystallization process such as waxes can be removed as precipitates by cooling the 1:1 mixtrue of acetone and dark oil to $0^{\circ}C$, From the dewaxed dark oil, oryzanol concentrate with 51.3% purity was obtained by fractional crystallization at$0^{\circ}C$ with the mixture of 8 part volume of hexane and 1 part of the dewaxed dark oil. The concentrate was recrystallized at room temperature with 20 part volume of methanol to yield oryzanol crystal of 98.3% purity. The optimum condition of vacuum distillation was temperature of $180^{\circ}C\;at\;0.2{\sim}0.4\;torr$ with 2% steam sparging. At this condition, the free fatty acid in the dark oil was removed as distillate without thermal deomposition to yield 82.3% of oryzanol as the pitch of 27.3% purity. After concentration from the pitch with 20 part volume of hexane to yield yellow powder of 75.4% purity, the yellow powder was recrystallized in methanol at room temperature to obtain the crystal containing 99.0% oryzanol. The overall oryzanol yield from the dark oil and the pitch was 9.5 and 28.5%, respectively. The change of the composition of sterols and triterpenoid alcohols in the compounds isolated during fractionation was analyzed by GC-MS.

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Development of environmentally friendly inorganic fluorescent pigments, A3V5O14 (A = K and Rb) and Cs2V4O11: Crystal structure, optical and color properties (친환경 무기 형광 안료 A3V5O14 (A = K and Rb) and Cs2V4O11 개발: 결정구조, 광학적 특성 및 착색 특성)

  • Jeong, Gyu Jin;Kim, Jin Ho;Lee, Younki;Hwang, Jonghee;Toda, Kenji;Bae, Byoungseo;Kim, Sun Woog
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.30 no.2
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    • pp.47-54
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    • 2020
  • To develop the bright-vivid red- and yellow-inorganic fluorescent pigments with high luminescence properties, A3V5O14 (A = K and Rb) and Cs2V4O11 inorganic pigments were synthesized by a water assisted solid state reaction (WASSR) method and a conventional solid state reaction method. Although impurity peaks corresponding to the AVO3 and AV3O8 (A = K, Rb, and Cs) were observed in all samples prepared, the trigonal structure A3V5O14 (A = K and Rb) and orthorhombic structure Cs2V4O11 were successfully obtained as a main phase. These inorganic pigments showed the broad absorption band (under 550 nm) originated from CT transitions of VO4 polyhedron, and the strong broad red- and green-emission bands due to 3T21A1 and 3T11A1 transitions of the [VO4]3- group. The A3V5O14 (A = K and Rb) and Cs2V4O11 pigments showed a bright-vivid red- and yellow-body color, where the a* values of the A3V5O14 (A = K and Rb) were +35.5 and +45.9, respectively, and b* value of Cs2V4O11 pigments was +50.3. The L* values of the A3V5O14 (A = K and Rb) and Cs2V4O11 inorganic pigments were over +45. These results indicate that the A3V5O14 (A = K and Rb) and Cs2V4O11 inorganic pigments could be an attractive candidate as a bright-vivid red- and yellow inorganic pigments.

Luminescence properties of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ red phosphor as the effect of Zn ion (Zn ion의 영향에 따른 $(Y,\;Zn)_2O_3$:$Eu^{3+}$ 적색 형광체의 발광특성)

  • Song, Y.H.;Moon, J.W.;Park, W.J.;Yoon, D.H.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.6
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    • pp.253-257
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    • 2008
  • To enhance the luminescence properties, the red phosphor composed of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ as doping concentration of Zn ion is synthesized at $1200^{\circ}C$ for 6 hrs in air atmosphere by conventional solid reaction method. As a result of the red phosphor $(Y,\;Zn)_2O_3$:$Eu^{3+}$ is measured X-ray diffraction (XRD), The main peak is nearly corresponded to the same as JCPDS card (No. 41-1105). When the doping concentration of Zn ion is more than 5 mol%, However, the ZnO peak is showed by XRD analysis. Therefore, when the doping concentration of Zn ion is less than 5 mol%, the Zn ion is well mixed in $Y_2O_3$ structure without the impurity phases. The photoluminescence (PL) properties is shown as this phosphor is excited in 254 nm region and the highest emission spectra of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ has shown in 612 nm region because of a typical energy transition ($^5D_0{\rightarrow}^7F_2$) of $Eu^{3+}$ ion. As the doping concentration of Zn ion is more than 10 mol%, the emission peak is suddenly decreased. when the highest emission peak as doping concentration of Zn ion is shown, the composition of this phosphor is $(Y_{0.95},\;Zn_{0.05})_2O_3$:$Eu^{3+}_{0.075}$ and the particle size analyzed by FE-SEM is confirmed from 0.4 to $3{\mu}m$.

Optimization of ZnO-based transparent conducting oxides for thin-film solar cells based on the correlations of structural, electrical, and optical properties (ZnO 박막의 구조적, 전기적, 광학적 특성간의 상관관계를 고려한 박막태양전지용 투명전극 최적화 연구)

  • Oh, Joon-Ho;Kim, Kyoung-Kook;Song, Jun-Hyuk;Seong, Tae-Yeon
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.11a
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    • pp.42.2-42.2
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    • 2010
  • Transparent conducting oxides (TCOs) are of significant importance for their applications in various devices, such as light-emitting diodes, thin-film solar cells, organic light-emitting diodes, liquid crystal displays, and so on. In order for TCOs to contribute to the performance improvement of these devices, TCOs should have high transmittance and good electrical properties simultaneously. Sn-doped $In_2O_3$ (ITO) is the most commonly used TCO. However, indium is toxic and scarce in nature. Thus, ZnO has attracted a lot of attention because of the possibility for replacing ITO. In particular, group III impurity-doped ZnO showed the optoelectronic properties comparable to those of ITO electrodes. Al-doped ZnO exhibited the best performance among various doped ZnO films because of the high substitutional doping efficiency. However, in order for the Al-doped ZnO to replace ITO in electronic devices, their electrical and optical properties should further significantly be improved. In this connection, different ways such as a variation of deposition conditions, different deposition techniques, and post-deposition annealing processes have been investigated so far. Among the deposition methods, RF magnetron sputtering has been extensively used because of the easiness in controlling deposition parameters and its fast deposition rate. In addition, when combined with post-deposition annealing in a reducing ambient, the optoelectronic properties of Al-doped ZnO films were found to be further improved. In this presentation, we deposited Al-doped ZnO (ZnO:$Al_2O_3$ = 98:2 wt%) thin films on the glass and sapphire substrates using RF magnetron sputtering as a function of substrate temperature. In addition, the ZnO samples were annealed in different conditions, e.g., rapid thermal annealing (RTA) at $900^{\circ}C$ in $N_2$ ambient for 1 min, tube-furnace annealing at $500^{\circ}C$ in $N_2:H_2$=9:1 gas flow for 1 hour, or RTA combined with tube-furnace annealing. It is found that the mobilities and carrier concentrations of the samples are dependent on growth temperature followed by one of three subsequent post-deposition annealing conditions.

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Applications of XPS and SIMS for the development of Si quantum dot solar cell

  • Kim, Gyeong-Jung;Hong, Seung-Hwi;Kim, Yong-Seong;Lee, U;Kim, Yeong-Heon;Seo, Se-Yeong;Jang, Jong-Sik;Sin, Dong-Hui;Choe, Seok-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.08a
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    • pp.297-297
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    • 2010
  • Precise control of the position and density of doping elements at the nanoscale is becoming a central issue for realizing state-of-the-art silicon-based optoelectronic devices. As dimensions are scaled down to take benefits from the quantum confinement effect, however, the presence of interfaces and the nature of materials adjacent to silicon turn out to be important and govern the physical properties. Utilization of visible light is a promising method to overcome the efficiency limit of the crystalline Si solar cells. Si quantum dots (QDs) have been proposed as an emission source of visible light, which is based on the quantum confinement effect. Light emission in the visible wavelength has been reported by controlling the size and density of Si QDs embedded within various types of insulating matrix. For the realization of all-Si QD solar cells with homojunctions, it is prerequisite not only to optimize the impurity doping for both p- and n-type Si QDs, but also to construct p-n homojunctions between them. In this study, XPS and SIMS were used for the development of p-type and n-type Si quantum dot solar cells. The stoichiometry of SiOx layers were controlled by in-situ XPS analysis and the concentration of B and P by SIMS for the activated doping in Si nano structures. Especially, it has been experimentally evidenced that boron atoms in silicon nanostructures confined in SiO2 matrix can segregate into the Si/$SiO_2$ interfaces and the Si bulk forming a distinct bimodal spatial distribution. By performing quantitative analysis and theoretical modelling, it has been found that boron incorporated into the four-fold Si crystal lattice can have electrical activity. Based on these findings, p-type Si quantum dot solar cell with the energy-conversion efficiency of 10.2% was realized from a [B-doped $SiO_{1.2}$(2 nm)/$SiO_2(2\;nm)]^{25}$ superlattice film with a B doping level of $4.0{\times}10^{20}\;atoms/cm^2$.

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Ferroelectric, Leakage Current Properties of BiFeO3/Pb(Zr0.52Ti0.48)O3 Multilayer Thin Films Prepared by Chemical Solution Deposition (Chemical Solution Deposition 방법을 이용한 BiFeO3/Pb(Zr0.52Ti0.48)O3 다층박막의 전기적 특성에 대한 연구)

  • Cha, J.O.;Ahn, J.S.;Lee, K.B.
    • Journal of the Korean Vacuum Society
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    • v.19 no.1
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    • pp.52-57
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    • 2010
  • $BiFeO_3/Pb(Zr_{0.52}Ti_{0.48})O_3$(BFO/PZT) multilayer thin films have been prepared on a Pt/Ti/$SiO_2$/Si(100) substrate by chemical solution deposition. BFO single layer, BFO/PZT bilayer and multilayer thin films were studied for comparison. X-ray diffraction analysis showed that the crystal structure of all films was multi-orientated perovskite phase without amorphous and impurity phase. The leakage current density at 500 kV/cm was reduced by approximately four and five orders of magnitude by bilayer and multilayer structure films, compared with BFO single layer film. The low leakage current density leads to saturated P-E hysteresis loops of bilayer and multilayer films. In BFO/PZT multlayer film, saturated remanent polarization of $44.3{\mu}C/cm^2$ was obtained at room temperature at 1 kHz with the coercive field($2E_c$) of 681.4 kV/cm.

Rietveld Refinement and Crystal Structure of K-Ba Substituted Synthetic Hollandite, ($K_{2x}Ba_{1-x}Cr_2Ti_6O_{16}$) (리트벨트법을 이용한 K-Ba 치환 합성 홀란다이트($K_{2x}Ba_{1-x}Cr_2Ti_6O_{16}$)의 결정구조 연구)

  • 최진범;김태현
    • Journal of the Mineralogical Society of Korea
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    • v.14 no.2
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    • pp.128-136
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    • 2001
  • The K-Ba complete solid solution of 7 synthetic hollandite-type minerals ($K_{2x}$ $Ba_{1-x}$ $Cr_2$/$Ti_{6}$ $O_{16}$ , x=0, 0.1, 0.3, 0.5, 0.7, 0.9, 1.0, respectively) are studied by the X-ray powder diffraction and Rietveld refinement to find structural transformation during substitution of $Ba^{2+}$ by $K^{+}$ in A site of the tunnel structure of hollandite. Rietveld indices indicate that $R_{wp}$ with respect to $R^{exp}$ ($R_{wp}$ $R_{exp}$ ) are in the range of 15.66%/20.90% and 14.74%/l9.37%, $R_{B}$ and S(Goodness of Fitness) are 6.45~8.97%, 1.45~1.63, respectively. Unit cell parameters of synthetic hollandites, space group 14/m, are a=10.1194(2)~10.0599(2)$\AA$, c=2.9572(6)~2.9512(7)$\AA$, and V=302.75~298.66$\AA^{3}$. Rutile formed as an impurity in those with more than 50% K contents in hollandite series. Substitution of Ba by K ion in a tunnel structure results in constant decrease of cell parameters, but is not sufficient enough to change the hollandite structure. Our data indicate that transformation of tetragonal 14/m to lower symmetry of monoclinic 12/m in hollandite structure may at least be affected by other cation substitution in same A site and/or by cation substitution in B site.

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A Study of the Photoluminescence of ZnO Thin Films Deposited by Radical Beam Assisted Molecular Beam Epitaxy (라디칼 빔 보조 분자선 증착법 (Radical Beam Assisted Molecular Beam Epitaxy) 법에 의해 성장된 ZnO 박막의 발광 특성에 관한 연구)

  • Suh, Hyo-Won;Byun, Dong-jin;Choi, Won-Kook
    • Korean Journal of Materials Research
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    • v.13 no.6
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    • pp.347-351
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    • 2003
  • II-Ⅵ ZnO compound semiconductor thin films were grown on $\alpha$-Al$_2$O$_3$(0001) single crystal substrate by radical beam assisted molecular beam epitaxy and the optical properties were investigated. Zn(6N) was evaporated using Knudsen cell and O radical was assisted at the partial pressure of 1$\times$10$^{4}$ Torr and radical beam source of 250-450 W RF power. In $\theta$-2$\theta$ x-ray diffraction analysis, ZnO thin film with 500 nm thickness showed only ZnO(0002)and ZnO(0004) peaks is believed to be well grown along c-axis orientation. Photoluminescence (PL) measurement using He-Cd ($\lambda$=325 nm) laser is obtained in the temperature range of 9 K-300 K. At 9 K and 300 K, only near band edge (NBE) is observed and the FWHM's of PL peak of the ZnO deposited at 450 RF power are 45 meV and 145 meV respectively. From no observation of any weak deep level peak even at room temperature PL, the ZnO grains are regarded to contain very low defect density and impurity to cause the deep-level defects. The peak position of free exciton showed slightly red-shift as temperature was increased, and from this result the binding energy of free exciton can be experimentally determined as much as $58\pm$0.5 meV, which is very closed to that of ZnO bulk. By van der Pauw 4-point probe measurement, the grown ZnO is proved to be n-type with the electron concentration($n_{e}$ ) $1.69$\times$10^{18}$$cm^3$, mobility($\mu$) $-12.3\textrm{cm}^2$/Vㆍs, and resistivity($\rho$) 0.30 $\Omega$$\cdot$cm.

Preparation of Al-doped NiO via Solvothermal Synthesis and its Crystal Structural and Electrical Properties (용매열 합성법을 통하여 알루미늄을 도핑한 니켈옥사이드의 제조와 그 결정구조적, 전기적 특성)

  • Hong, Sun-Ki;Ji, Mi-Jung;Lee, Min-Jin;Jung, Sung-Hun;Seol, Kwang-Hee;Choi, Byung-Hyun
    • Korean Journal of Materials Research
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    • v.22 no.11
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    • pp.631-635
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    • 2012
  • Nickel oxide was doped with a wide range of concentrations (mol%) of Aluminum (Al) by solvothermal synthesis; single-phased nano powder of nickel oxide was generated after calcination at$900^{\circ}C$. When the concentration of Al dopant was increased, the reduced intensity was confirmed through XRD analysis. Lattice parameters of the synthesized NiO powder were decreased after treatment of the dopant; parameters were increased when the concentration of Al was over the doping limit (5 mol% Al). The binding energy of $Ni^{2+}$ was chemically shifted to $Ni^{3+}$ by doping $Al^{3+}$ ion, as confirmed by the XPS analysis. The tilted structure of the synthesized NiO with 5 mol% Al dopant and the polycrystalline structure of the $Ni_{0.75}Al_{0.25}O$ were observed by HR-TEM analysis. The electrical conductivity of the newly synthesized NiO was highly improved by Al doping in the conductivity test. The electrical conductivity values of the commercial NiO and the synthesized NiO with 5 mol% Al dopant ($Ni_{0.95}Al_{0.05}O$) were 1,400 s/cm and 2,230 s/cm at $750^{\circ}C$, respectively. However, the electrical conductivity of the synthesized NiO with 10 mol% Al dopant ($Ni_{0.9}Al_{0.1}O$) decreased due to the scattering of free-electrons caused by the large number of impurity atoms; the electrical conductivity of $Ni_{0.9}Al_{0.1}O$ was 545 s/cm at $750^{\circ}C$.

Mineralization and Characterization of Boseung Kaolin in Gaya Area (가야 지역 보성 고령토의 광화작용 및 광물 특성)

  • Noh, Jin-Hwan
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.4
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    • pp.397-413
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    • 2008
  • In Gaya area, the Boseong kaolin deposits exhibit locally unusual occurrences such as downward enrichment of kaoin minerals, characteristic hydrothermal alterations (illite and stilbite), and phase relations among kaolin minerals in addition to the extensive weathering of anorthositic country rocks. This indicates that the kaolin deposits seem to be genetically formed as a mixed hydrothermal and residual model. The kaolin ores can be divided into five types on the basis of differences in occurrence, mineral composition and characters. These consist of two types of high-grade ores ranging above 80% in grade and low-grade ores as low as less than 80% including feldspar residuals or the peculiar impurity phase of illite-vermiculite-stilbite. Halloysite and kaolinite are mostly coexisted in the Boseong kaolin, and these kaolin minerals exhibit diverse appearances in crystallinity and morphology. Such a diversity in mineral phase and crystallinity seems to be originated from the complexity in genesis. In addition to these diverse characters of the kaolin, its applied-mineralogical characteristics such as chemical composition, thermal properties, whiteness, viscosity, and etc. made it disadvantageous in terms of ore quality.