• Title/Summary/Keyword: SURFACE CRYSTALLIZATION

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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.

The Crystallization and the Photoluminescence Characteristics of ZnO Thin Film Fabricated by Sol-gel Method (Sol-gel 법으로 제작된 ZnO 박막의 결정화 및 PL 특성에 관한 연구)

  • Choi Byeong Kyun;Chang Dong Hoon;Kang Seong Jun;Yoon Yung Sup
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.43 no.2 s.344
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    • pp.8-12
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    • 2006
  • We have fabricated ZnO thin film on $Pt/TiO-2/SiO_2/Si$ substrate by the sol-gel method and have investigated the effect of annealing temperature on the structural morphology and optical properties of ZnO thin films. The ZnO thin film annealed at $600^{\circ}C$ exhibits the highest c-axis orientation and its FWHM of X-ray peak is $0.4360^{\circ}C$. In the results of surface morphology investigation of ZnO thin film by using Am it is observed that ZnO thin film annealed at $600^{\circ}C$ exhibits the largest UV (ultraviolet) exciton emission at around 378nm and the smallest visible emission at around 510nm among these of ZnO thin films annealed at various temperatures. It is deduced that the ZnO thim film annealed at $600^{\circ}C$ is formed most stoichiometrically since the visible emission at around 510nm comes from oxygen vacancy or impurities.

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.

Effect of the Compatibilizer on Physical Properties of Polypropylene (PP)/Bamboo Fiber (BF) Composites (폴리프로필렌/대나무 섬유 복합체의 물성에 대한 상용화제의 영향)

  • Lee, Jong Won;Ku, Sun Gyo;Lee, Beom Hee;Lee, Ki-Woong;Kim, Cheol Woo;Kim, Ki Sung;Kim, Youn Cheol
    • Applied Chemistry for Engineering
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    • v.26 no.5
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    • pp.615-620
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    • 2015
  • Polypropylene (PP)/bamboo fiber (BF) composites were fabricated by twin screw extruder in order to investigate effects of the compatibilizer on physical properties of PP/BF composites. The content of BF changed from 10 to 25 wt% and that of the compatibilizer was fixed at 3 wt%. Maleic anhydride grafted PP (PP-g-MAH) was used to increase the compatibility between PP and BF as a compatibilizer. Chemical structures of the composites were confirmed by the existence of carbonyl group (C=O) stretching peak at $1,700cm^{-1}$ in FT-IR spectrum. Considering the degradation and mechanical properties, the optimum extrusion conditions were selected to be $210^{\circ}C$ and 100 rpm, respectively. There was no distinct changes in melting temperature of the composites, but the crystallization temperature increased by $10-20^{\circ}C$ owing to the heterogeneous nuclei of BF. It was checked that the optimum BF content was in the range of 15-20 wt% from the results of tensile and flexural properties of the composites. The effect of the compatibilizer on mechanical properties was confirmed by SEM images of fractured surface and contact angles.

A study on the characteristics of MEM structure of $SrBi_2Ta_2O_9$ thin films by RE magnetron sputtering (RF 마그네트론 스퍼터링법에 의한 MFM 구조의 $SrBi_2Ta_2O_9$ 박막 특성에 관한 연구)

  • 이후용;최훈상;최인훈
    • Journal of the Korean Vacuum Society
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    • v.9 no.2
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    • pp.136-143
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    • 2000
  • $SrBi_2Ta_2O_9;(SBT)$ films were deposited on p-type Si(100) at room temperature by rf magnetron sputtering method to confirm the possibility of application of $Pt/SBT/Pt/Ti/SiO_2/Si$ structure (MFM) for destructive read out ferroelectric RAM (random access memory). Their structural characteristics with the various annealing times and Ar/$O_2$ gas flow ratios in sputtering were observed by XRD (X-ray diffractometer) and the surface morphologies were observed by FE-SEM (field emission scanning electron microscopy), and their electrical properties were observed by P-V (polarization-voltage measurement) and I-V (current-voltage measurement). The Ar/$O_2$ gas flow ratios of sputtering gas were changed from 1 : 4 to 4 : 1 and SBT thin films were deposited at room temperature. The films show (105), (110) peaks of SBT by XRD measurement. SBT thin films deposited at room temperature were crystallized by furnace annealing at 80$0^{\circ}C$ in oxygen atmosphere during either one hour or two hours. Among their electrical properties, P-V curves showed shaped hysteresis curves, but the SBT thin films showed the asymmetric ferroelectric properties in P-V curves. When Ar/$O_2$ gas flow ratios are 1 : 1, 2: 1, the leakage current density values of SBT thin films are good, those values of 3 V, 5 V, and 7 V are respectively $3.11\times10^{-8} \textrm{A/cm}^2$, $5\times10^{-8}\textrm{A/cm}^2$, $7\times10^{-8}\textrm{A/cm}^2$.After two hours of annealing time, their electrical properties and crystallization are improved.

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Study on Fiber Laser Annealing of p-a-Si:H Deposition Layer for the Fabrication of Interdigitated Back Contact Solar Cells (IBC형 태양전지 제작을 위한 p-a-Si:H 증착층의 파이버 레이저 가공에 관한 연구)

  • Kim, Sung-Chul;Lee, Young-Seok;Han, Kyu-Min;Moon, In-Yong;Kwon, Tae-Young;Kyung, Do-Hyun;Kim, Young-Kuk;Heo, Jong-Kyu;Yoon, Ki-Chan;Yi, Jun-Sin
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.430-430
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    • 2008
  • Using multi plasma enhanced chemical vapor deposition system (Multi-PECVD), p-a-Si:H deposition layer as a $p^+$ region which was annealed by laser (Q-switched fiber laser, $\lambda$ = 1064 nm) on an n-type single crystalline Si (100) plane circle wafer was prepared as new doping method for single crystalline interdigitated back contact (IBC) solar cells. As lots of earlier studies implemented, most cases dealt with the excimer (excited dimer) laserannealing or crystallization of boron with the ultraviolet wavelength range and $10^{-9}$ sec pulse duration. In this study, the Q-switched fiber laser which has higher power, longer wavelength of infrared range ($\lambda$ = 1064 nm) and longer pulse duration of $10^{-8}$ sec than excimer laser was introduced for uniformly deposited p-a-Si:H layer to be annealed and to make sheet resistance expectable as an important process for IBC solar cell $p^+$ layer on a polished n-type Si circle wafer. A $525{\mu}m$ thick n-type Si semiconductor circle wafer of (100) plane which was dipped in a buffered hydrofluoric acid solution for 30 seconds was mounted on the Multi-PECVD system for p-a-Si:H deposition layer with the ratio of $SiH_4:H_2:B_2H_6$ = 30:120:30, at $200^{\circ}C$, 50 W power, 0.2 Torr pressure for 20 minutes. 15 mm $\times$ 15 mm size laser cut samples were annealed by fiber laser with different sets of power levels and frequencies. By comparing the results of lifetime measurement and sheet resistance relation, the laser condition set of 50 mm/s of mark speed, 160 kHz of period, 21 % of power level with continuous wave mode of scanner lens showed the features of small difference of lifetime and lowering sheet resistance than before the fiber laser treatment with not much surface damages. Diode level device was made to confirm these experimental results by measuring C-V, I-V characteristics. Uniform and expectable boron doped layer can play an important role to predict the efficiency during the fabricating process of IBC solar cells.

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Preparation of Al/RDX/AP Energetic Composites by Drowning-out/Agglomeration and Their Thermal Decomposition Characteristics (결정화/응집에 의한 구형 Al/RDX/AP 에너지 복합체 제조 및 그 열분해 특성)

  • Lee, Jeong-Hwan;Shim, Hong-Min;Kim, Jae-Kyeong;Kim, Hyoun-Soo;Koo, Kee-Kahb
    • Applied Chemistry for Engineering
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    • v.28 no.2
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    • pp.214-220
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    • 2017
  • The spherical Al/RDX/AP composites with an average size of $550{\mu}m$ were successfully prepared by drowning-out/agglomeration (D/A) process. The surface morphology and dispersion of Al particles of those composites were investigated using SEM and EDS (energy dispersive spectrometry). As a result of thermal analysis, the onset temperature of thermal decomposition of the Al/RDX/AP composites by the D/A process was found to decrease about $50^{\circ}C$ and their thermal stability was shown to be relatively enhanced due to the increase of activation energy compared to those of using the physical mixing method. In the first decomposition region of AP, Prout-Tompkins model was shown to describe well the thermal decomposition of both composites by the physical mixing and D/A process. On the other hand, in the second decomposition region of AP, the decomposition mechanisms of composites by the physical mixing and D/A process were explained by the zero-order and contracting volume model, respectively.

Annealing Characteristics of Electrodeposited Cu(In,Ga)Se2 Photovoltaic Thin Films (전해증착 Cu(In,Ga)Se2 태양전지 박막의 열처리 특성)

  • Chae, Su-Byung;Shin, Su-Jung;Choi, Jae-Ha;Kim, Myung-Han
    • Korean Journal of Materials Research
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    • v.20 no.12
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    • pp.661-668
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    • 2010
  • Cu(In,Ga)$Se_2$(CIGS) photovoltaic thin films were electrodeposited on Mo/glass substrates with an aqueous solution containing 2 mM $CuCl_2$, 8 mM $InCl_3$, 20 mM $GaCl_3$ and 8mM $H_2SeO_3$ at the electrodeposition potential of -0.6 to -1.0 V(SCE) and pH of 1.8. The best chemical composition of $Cu_{1.05}In_{0.8}Ga_{0.13}Se_2$ was found to be achieved at -0.7 V(SCE). The precursor Cu-In-Ga-Se films were annealed for crystallization to chalcopyrite structure at temperatures of 100-$500^{\circ}C$ under Ar gas atmosphere. The chemical compositions, microstructures, surface morphologies, and crystallographic structures of the annealed films were analyzed by EPMA, FE-SEM, AFM, and XRD, respectively. The precursor Cu-In-Ga-Se grains were grown sparsely on the Mo-back contact and also had very rough surfaces. However, after annealing treatment beginning at $200^{\circ}C$, the empty spaces between grains were removed and the grains showed well developed columnar shapes with smooth surfaces. The precursor Cu-In-Ga-Se films were also annealed at the temperature of $500^{\circ}C$ for 60 min under Se gas atmosphere to suppress the Se volatilization. The Se amount on the CIGS film after selenization annealing increased above the Se amount of the electrodeposited state and the $MoSe_2$ phase occurred, resulting from the diffusion of Se through the CIGS film and interaction with Mo back electrode. However, the selenization-annealed films showed higher crystallinity values than did the films annealed under Ar atmosphere with a chemical composition closer to that of the electrodeposited state.

Synthesis and Characterization of Zeolite 4A on Activated Carbon Supports (활성탄 지지체상에서 제올라이트 4A 합성 및 특성)

  • Park, Jeong-Hwan;Suh, Jeong-Kwon;Jeong, Soon-Yong;Lee, Jung-Min;Doh, Myung-Ki
    • Applied Chemistry for Engineering
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    • v.8 no.2
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    • pp.204-210
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    • 1997
  • Zeolite 4A-impregnated complex molecular sieve was prepared by hydrothermal reaction after aluminosilicate gel was penetrated into the pore of activated carbon granule. The crystals of zeolite 4A mainly were formed in the macropore of activated carbon, and their average diameter is $0.8{\mu}m$. The pore volume of activated carbon granule is $0.67m{\ell}/g$, and the pore volume of the sample including 21.6wt% of zeolite 4A crystal is $0.41m{\ell}/g$ decreasing the pore volume by 40% due to the crystallization of zeolite 4A crystals on the internal surface of activated carbon. The calcium ion exchange capacity of zeolite 4A-impregnated sample is 320mg $CaCO_3/g$ zeolite, and this value is almost the same as that of zeolite 4A powder. The crystal of zeolite 4A was not separated from the support of activated carbon granule in the course of ultrasonic dispersion. The adsorption isotherm of water on zeolite 4A-impregnated sample shows the intermediate shape between types, I and III. In addition, zeolite 4A-impregnated sample shows the hydrophilic and hydrophobic properties simultaneously.

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Preparation and Release Behavior of Atorvastatin Calcuim - Encapsulated Polyoxalate Microspheres (아토르바스타틴 칼슘을 함유한 폴리옥살레이트 미립구의 제조 및 방출거동)

  • Lee, Cheon Jung;Kim, Su Young;Lee, Hyun Gu;Yang, Jaewon;Park, Jin Young;Cha, Se Rom;Lim, Dong-Kwon;Lee, Dongwon;Khang, Gilson
    • Polymer(Korea)
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    • v.38 no.5
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    • pp.656-663
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    • 2014
  • Atorvastatin calcium-loaded polyoxalate (POX) microspheres were prepared by an emulsion solvent-evaporation/ extraction method of oil-in-oil-in-water ($O_1/O_2/W$) for sustained release. We investigated the release behavior according to initial drug ratio, molecular weight ($M_w$) and concentration of POX and concentration of emulsifier. The microsphere was characterized on the surface, the cross-section morphology and the behavior of atorvastatin calcium release for 10 days by scanning electron microscopy (SEM) and high performance liquid chromatography (HPLC). The analysis of crystallization was analyzed to use X-ray diffraction (XRD), differential scanning calorimeter (DSC) and Fourier transform infrared (FTIR). These results showed that the release behaviors can be controlled by preparation conditions.