• Title/Summary/Keyword: 분말회절

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Preparation and Reactivity of Cu-Zn-Al Based Hybrid Catalysts for Direct Synthesis of Dimethyl Ether by Physical Mixing and Precipitation Methods (물리혼합 및 침전법에 의한 DME 직접 합성용 Cu-Zn-Al계 혼성촉매의 제조 및 반응특성)

  • Bang, Byoung Man;Park, No-Kuk;Han, Gi Bo;Yoon, Suk Hoon;Lee, Tae Jin
    • Korean Chemical Engineering Research
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    • v.45 no.6
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    • pp.566-572
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    • 2007
  • Two hybrid catalysts for the direct synthesis of DME were prepared and the catalytic activity of these catalysts were investigated. The hybrid catalyst for the direct synthesis of DME was composed as the catalytic active components of methanol synthesis and dehydration. The methanol synthesis catalyst was formed from the precursor contained Cu and Zn, the methanol dehydration catalyst was used ${\gamma}-Al_2O_3$. As PM-CZ+D and CP-CZA/D, Two hybrid catalysts were prepared by physical mixing method (PM-CZ+D) and precipitation method (CP-CZA/D), respectively. PM-CZ+D was prepared by physically mixing methanol synthesis catalyst and methanol dehydration catalyst, CP-CZA/D was prepared by depositing Cu-Zn or Cu-Zn-Al components on ${\gamma}-Al_2O_3$. The crystallinity and the surface morphology of synthesized catalyst were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM) to investigate the physical property of prepared catalyst. And BET surface area by $N_2$ adsorption and the surface area of Cu by $N_2O$ chemisorption were investigated about the hybrid catalysts. In addition, catalytic activity of these hybrid catalysts was examined with varying reaction conditions. At that time, the reaction temperature of $250{\sim}290^{\circ}C$, the reaction pressure of 50~70 atm, the $[H_2]/[CO]$ mole ratio of 0.5~2.0 and the space velocity of $1,500{\sim}6,000h^{-1}$ were investigated the catalytic activity. From these results, it was confirmed that the reactivity of CP-CZA/D was higher than that of PM-CZ+D. When the conditions of reaction temperature, pressure, $[H_2]/[CO]$ ratio and space velocity were $260^{\circ}C$, 50 atm and 1.0, $3,000h^{-1}$ respectively, CO conversion using CP-CZA/D hybrid catalyst was 72% and the CO conversion of CP-CZA/D was more than 20% compared with the CO conversion of PM-CZ+D. It was known that Cu surface area of CP-CZA/D hybrid catalyst was higher than that of hybrid PM-CZ+D catalyst using $N_2O$ chemisorption. It was assumed that the catalytic activity was improved because Cu particle of hybrid catalyst prepared by precipitation method was well dispersed.

Ti-Getter Effects on Magnetic Properties of Ti0.96Co0.02Fe0.02O2 (Ti-Getter가 Ti0.96Co0.02Fe0.02O2의 자기적 특성에 미치는 영향)

  • Nam, H.D.;Kim, S.J.;Baek, J.K.;Lee, S.R.;Park, Cheol-Su;Kim, E.C.
    • Journal of the Korean Magnetics Society
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    • v.18 no.3
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    • pp.109-114
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    • 2008
  • The samples were synthesized by using a solid state reaction. The X-ray diffraction pattern for $Ti_{0.96}Co_{0.02}Fe_{0.02}O_2$ showed a pure rutile phase with tetragonal structure, Mixtures of the proper proportions of the elements sealed in evacuated quartz ampoule were heated at $870{\sim}930^{\circ}C$ for one day and then slowly cooled down to room temperature at a rate of $10^{\circ}C$/h. In order to obtain single phase material, it was necessary to grind the sample after the first firing and to press the powders into pellets before annealing them for a second time in evacuated and sealed quartz ampoule. Magnetic properties have been investigated using the vibrating sample magnetometer (VSM). Room temperature magnetic hysteresis (M-H) curve showed an obvious ferromagnetic behavior and the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $1.5\;{\mu}_B$/CoFe. But the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $0.02\;{\mu}_B$/CoFe without Ti-getter. Size of particles is about $1\;{\mu}m$ using the transmission electron microscope (TEM). The ingredients of sample are distributed irregular in particles. Only Fe get shown on the surface of particles.

Characterization of SiC nanowire Synthesized by Thermal CVD (열 화학기상증착법을 이용한 탄화규소 나노선의 합성 및 특성연구)

  • Jung, M.W.;Kim, M.K.;Song, W.;Jung, D.S.;Choi, W.C.;Park, C.J.
    • Journal of the Korean Vacuum Society
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    • v.19 no.4
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    • pp.307-313
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    • 2010
  • One-dimensional cubic phase silicon carbide nanowires (${\beta}$-SiC NWs) were efficiently synthesized by thermal chemical vapor deposition (TCVD) with mixtures containing Si powders and nickel chloride hexahydrate $(NiCl_2{\cdot}6H_2O)$ in an alumina boat with a carbon source of methane $(CH_4)$ gas. SEM images are shown that the growth temperature (T) of $1,300^{\circ}C$ is not enough to synthesize the SiC NWs owing to insufficient thermal energy for melting down a Si powder and decomposing the methane gas. However, the SiC NWs could be synthesized at T>$1,300^{\circ}C$ and the most efficient temperature for growth of SiC NWs is T=$1,400^{\circ}C$. The synthesized SiC NWs have the diameter with an average range between 50~150 nm. Raman spectra clearly revealed that the synthesized SiC NWs are forming of a cubic phase (${\beta}$-SiC). Two distinct peaks at 795 and $970 cm^{-1}$ in Raman spectra of the synthesized SiC NWs at T=$1,400^{\circ}C$ represent the TO and LO mode of the bulk ${\beta}$-SiC, respectively. XRD spectra are also supported to the Raman spectra resulting in the strongest (111) peaks at $2{\Theta}=35.7^{\circ}$, which is the (111) plane peak position of 3C-SiC. Moreover, the gas flow rate of 300 sccm for methane is the optimal condition for synthesis of a large amount of ${\beta}$-SiC NW without producing the amorphous carbon structure shown at a high methane flow rate of 800 sccm. TEM images are shown two kinds of the synthesized ${\beta}$-SiC NWs structures. One is shown the defect-free ${\beta}$-SiC NWs with a (111) interplane distance of 0.25 nm, and the other is the stacking-faulted ${\beta}$-SiC NWs. Also, TEM images exhibited that two distinct SiC NWs are uniformly covered with $SiO_2$ layer with a thickness of less 2 nm.

Effects of acid-treatment conditions on the surface properties of the RBM treated titanium implants (산-처리 조건이 RBM처리한 티타늄 임플란트의 표면 특성에 주는 영향)

  • Lee, Han-Ah;Seok, Soohwang;Lee, Sang-Hyeok;Lim, Bum-Soon
    • Korean Journal of Dental Materials
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    • v.45 no.4
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    • pp.257-274
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    • 2018
  • The purpose of this study was to evaluate the effect of acid-treatment conditions on the surface properties of the RBM (Resorbable Blast Media) treated titanium. Disk typed cp-titanium specimens were prepared and RBM treatments was performed with calcium phosphate ceramic powder. Acid solution was mixed using HCl, $H_2SO_4$ and deionized water with 4 different volume fraction. The RBM treated titanium was acid treated with different acid solutions at 3 different temperatures and for 3 different periods. After acid-treatments, samples were cleaned with 1 % Solujet solution for 30 min and deionized water for 30 min using ultrasonic cleanser, then dried in the electrical oven ($37^{\circ}C$). Weight of samples before and after acid-treatment were measured using electric balance. Surface roughness was estimated using a confocal laser scanning microscopy, crystal phase in the surface of sample was analyzed using X-ray diffractometer. Surface morphology and components were evaluated using Scanning Electron Microscope (SEM) with Energy Dispersive X-ray spectroscopy (EDX) and X-ray Photoemission Spectroscopy (XPS). Values of the weight changes and surface roughness were statistically analyzed using Tukey-multiple comparison test (p=0.05). Weight change after acid treatments were significantly increased with increasing the concentration of $H_2SO_4$ and temperature of acid-solution. Acid-treatment conditions (concentration of $H_2SO_4$, temperature and time) did not produce consistent effects on the surface roughness, it showed the scattered results. From XRD analysis, formation of titanium hydrides in the titanium surface were observed in all specimens treated with acid-solutions. From XPS analysis, thin titanium oxide layer in the acid-treated specimens could be evaluated. Acid solution with $90^{\circ}C$ showed the strong effect on the titanium surface, it should be treated with caution to avoid the over-etching process.

Optimization for Ammonia Decomposition over Ruthenium Alumina Catalyst Coated on Metallic Monolith Using Response Surface Methodology (반응표면분석법을 이용한 루테늄 알루미나 메탈모노리스 코팅촉매의 암모니아 분해 최적화)

  • Choi, Jae Hyung;Lee, Sung-Chan;Lee, Junhyeok;Kim, Gyeong-Min;Lim, Dong-Ha
    • Clean Technology
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    • v.28 no.3
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    • pp.218-226
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    • 2022
  • As a result of the recent social transformation towards a hydrogen economy and carbon-neutrality, the demands for hydrogen energy have been increasing rapidly worldwide. As such, eco-friendly hydrogen production technologies that do not produce carbon dioxide (CO2) emissions are being focused on. Among them, ammonia (NH3) is an economical hydrogen carrier that can easily produce hydrogen (H2). In this study, Ru/Al2O3 catalyst coated onmetallic monolith for hydrogen production from ammonia was prepared by a dip-coating method using a catalyst slurry mixture composed of Ru/Al2O3 catalyst, inorganic binder (alumina sol) and organic binder (methyl cellulose). At the optimized 1:1:0.1 weight ratio of catalyst/inorganic binder/organic binder, the amount of catalyst coated on the metallic monolith after one cycle coating was about 61.6 g L-1. The uniform thickness (about 42 ㎛) and crystal structure of the catalyst coated on the metallic monolith surface were confirmed through scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. Also, a numerical optimization regression equation for NH3 conversion according to the independent variables of reaction temperature (400-600 ℃) and gas hourly space velocity (1,000-5,000 h-1) was calculated by response surface methodology (RSM). This model indicated a determination coefficient (R2) of 0.991 and had statistically significant predictors. This regression model could contribute to the commercial process design of hydrogen production by ammonia decomposition.

Janggunite, a New Mineral from the Janggun Mine, Bonghwa, Korea (경북(慶北) 봉화군(奉化郡) 장군광산산(將軍鑛山産) 신종광물(新種鑛物) 장군석(將軍石)에 대(對)한 광물학적(鑛物學的) 연구(硏究))

  • Kim, Soo Jin
    • Economic and Environmental Geology
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    • v.8 no.3
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    • pp.117-124
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    • 1975
  • Wet chemical analysis (for $MnO_2$, MnO, and $H_2O$(+)) and electron microprobe analysis (for $Fe_2O_3$ and PbO) give $MnO_2$ 74.91, MnO 11.33, $Fe_2O_3$ (total Fe) 4.19, PbO 0.03, $H_2O$ (+) 9.46, sum 99.92%. 'Available oxygen determined by oxalate titration method is allotted to $MnO_2$ from total Mn, and the remaining Mn is calculated as MnO. Traces of Ba, Ca, Mg, K, Cu, Zn, and Al were found. Li and Na were not found. The existence of (OH) is verified from the infrared absorption spectra. The analysis corresponds to the formula $Mn^{4+}{_{4.85}}(Mn^{2+}{_{0.90}}Fe^{3+}{_{0.30}})_{1.20}O_{8.09}(OH)_{5.91}$, on the basis of O=14, 'or ideally $Mn^{4+}{_{5-x}}(Mn^{2+},Fe^{3+})_{1+x}O_{8}(OH)_{6}$ ($x{\approx}0.2$). X-ray single crystal study could not be made because of the distortion of single crystals. But the x-ray powder pattern is satisfactorily indexed by an orthorhombic cell with a 9.324, b 14.05, c $7.956{\AA}$., Z=4. The indexed powder diffraction lines are 9.34(s) (100), 7.09(s) (020), 4.62(m) (200, 121), 4.17(m) (130), 3.547(s) (112), 3.212(vw) (041), 3.101(s) (300), 2.597(w) (013), 2.469(m) (331), 2.214(vw)(420), 2.098(vw) (260), 2.014 (vw) (402), 1.863(w) (500), 1.664(w) (314), 1.554(vw) (600), 1.525(m) (601), 1.405(m) (0.10.0). DTA curve shows the endothermic peaks at $250-370^{\circ}C$ and $955^{\circ}C$. The former is due to the dehydration: and oxidation forming$(Mn,\;Fe)_2O_3$(cubic, a $9.417{\AA}$), and the latter is interpreted as the formation of a hausmannite-type oxide (tetragonal, a 5.76, c $9.51{\AA}$) from $(Mn,\;Fe)_2O_3$. Infrared absorption spectral curve shows Mn-O stretching vibrations at $515cm^{-1}$ and $545cm^{-1}$, O-H bending vibration at $1025cm^{-1}$ and O-H stretching vibration at $3225cm^{-1}$. Opaque. Reflectance 13-15%. Bireflectance distinct in air and strong in oil. Reflection pleochroism changes from whitish to light grey. Between crossed nicols, color changes from yellowish brown with bluish tint to grey in air and yellowish brown to grey through bluish brown in oil. No internal reflections. Etching reactions: HCl(conc.) and $H_2SO_4+H_2O_2$-grey tarnish; $SnCl_2$(sat.)-dark color; $HNO_3$(conc.)-grey color; $H_2O_2$-tarnish with effervescence. It is black in color. Luster dull. Cleavage one direction perfect. Streak brownish black to dark brown. H. (Mohs) 2-3, very fragile. Specific gravity 3.59(obs.), 3.57(calc.). It occurs as radiating groups of flakes, flower-like aggregates, colloform bands, dendritic or arborescent masses composed of fine grains in the cementation zone of the supergene manganese oxide deposits of the Janggun mine, Bonghwa-gun, southeastern Korea. Associated minerals are calcite, nsutite, todorokite, and some undetermined manganese dioxide minerals. The name is for the mine, the first locality. The mineral and name were approved before publication by the Commission on New Minerals and Mineral Names, I.M.A.

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A Study on the Conservation State and Plans for Stone Cultural Properties in the Unjusa Temple, Korea (운주사 석조문화재의 보존상태와 보존방안에 대한 연구)

  • Sa-Duk, Kim;Chan-Hee, Lee;Seok-Won, Choi;Eun-Jeong, Shin
    • Korean Journal of Heritage: History & Science
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    • v.37
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    • pp.285-307
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    • 2004
  • Synthesize and examine petrological characteristic and geochemical characteristic by weathering formation of rock and progress of weathering laying stress on stone cultural properties of Unjusa temple of Chonnam Hwasun county site in this research. Examine closely weathering element that influence mechanical, chemical, mineralogical and physical weathering of rocks that accomplish stone cultural properties and these do quantification, wish to utilize by a basic knowledge for conservation scientific research of stone cultural properties by these result. Enforced component analysis of rock and mineralogical survey about 18 samples (pyroclastic tuff; 7, ash tuff; 4, granite ; 4, granitic gneiss; 3) all to search petrological characteristic and geochemical characteristic by weathering of Unjusa temple precinct stone cultural properties and recorded deterioration degree about each stone cultural properties observing naked eye. Major rock that constitution Unjusa temple one great geological features has strike of N30-40W and dip of 10-20NE being pyroclastic tuff. This pyroclastic tuff is ranging very extensively laying center on Unjusa temple and stone cultural properties of precinct is modeled by this pyroclastic tuff. Stone cultural propertieses of present Unjusa temple precinct are accomplishing structural imbalance with serious crack, and because weathering of rock with serious biological pollution is gone fairly, rubble break away and weathering and deterioration phenomenon such as fall off of a particle of mineral are appearing extremely. Also, a piece of iron and cement mortar of stone cultural properties everywhere are forming precipitate of reddish brown and light gray being oxidized. About these stone cultural properties, most stone cultural propertieses show SD(severe damage) to MD(moderate damage) as result that record Deterioration degree. X-ray diffraction analysis result samples of each rock are consisted of mineral of quartz, orthoclase,plagioclase, calcite, magnetite etc. Quartz and feldspar alterated extremely in a microscopic analysis, and biotite that show crystalline form of anhedral shows state that become chloritization that is secondary weathering mineral being weathered. Also, see that show iron precipitate of reddish brown to crack zone of tuff everywhere preview rock that weathering is gone deep. Tuffs that accomplish stone cultural properties of study area is illustrated to field of Subalkaline and Peraluminous, $SiO_2$(wt.%) extent of samples pyroclastic tuff 70.08-73.69, ash tuff extent of 70.26-78.42 show. In calculate Chemical Index of Alteration(CIA) and Weathering Potential Index(WPI) about major elements extent of CIA pyroclastic tuff 55.05-60.75, ash tuff 52.10-58.70, granite 49.49-51.06 granitic gneiss shows value of 53.25-67.14 and these have high value gneiss and tuffs. WPI previews that is see as thing which is illustrated being approximated in 0 lines and 0 lines low samples of tuffs and gneiss is receiving esaily weathering process as appear in CIA. As clay mineral of smectite, zeolite that is secondary weathering produce of rock as result that pick powdering of rock and clothing material of stone cultural properties observed by scanning electron micrographs (SEM). And roots of lichen and spore of hyphae that is weathering element are observed together. This rock deep organism being coating to add mechanical weathering process of stone cultural properties do, and is assumed that change the clay mineral is gone fairly in stone cultural properties with these. As the weathering of rocks is under a serious condition, the damage by the natural environment such as rain, wind, trees and the ground is accelerated. As a counter-measure, the first necessary thing is to build the ground environment about protecting water invasion by making the drainage and checking the surrounding environment. The second thing are building hardening and extirpation process that strengthens the rock, dealing biologically by reducing lichens, and sticking crevice part restoration using synthetic resin. Moreover, it is assumed to be desirable to build the protection facility that can block wind, sunlight, and rain which are the cause of the weathering, and that goes well with the surrounding environment.