• Title/Summary/Keyword: XRD분석

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Synthesis of Visible-working Pt-C-TiO2 Photocatalyst for the Degradation of Dye Wastewater (염료폐수 분해를 위한 가시광 감응형 Pt-C-TiO2 광촉매의 합성)

  • Hahn, Mi Sun;Yun, Chang Yeon;Yi, Jongheop
    • Clean Technology
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    • v.11 no.3
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    • pp.123-128
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    • 2005
  • Among various metal oxides semiconductors, $TiO_2$ is the most studied semiconductor for environmental clean-up applications due to its unique ability in photocatalyzing various organic contaminants, its chemical inertness, and nontoxicity. $TiO_2$, however, has a few drawbacks to be solved such as reactivity mainly working under ultraviolet irradiation (${\lambda}$ < 387 nm) and electron - hole recombination on $TiO_2$. In this study, to extend the absorption range of $TiO_2$ into the visible range and enhance electron - hole separation, we synthesized platinum (Pt) deposited $C-TiO_2$. The presence of Pt as an electron sink has been known to snhance the separation of photogenerated electron-hole pairs and induce the thermal decomposition. The characterization of as-synthesized $Pt-C-TiO_2$ was performed by Transmission Electron Microscopic (TEM), the Brunuer-Emmett-Teller (BET) method, X-ray Diffractometer (XRD), UV-vis spectrometer (UV-DRS), and X-ray Photoelectron Spectroscopy (XPS). In order to estimate the photocatalytic activity of the synthesized materials, the photoelectron Spectroscopy (XPS). In order to estimate the photocatalytic activity of the synthesized materials, the photodegradation experiment of an azo dye (Acid Red 44; $C_{10}H_7N=NC_{10}H_3(SO_3Na)_2OH$)was carried out by using an Xe arc lamp (300 W, Oriel). A 420 nm cut-off filter was used for visible light irradiation. From the results, Pt-deposited $C-TiO_2$ showed a far superior phothdegradation activity to Degussa P25, the commercial product under the irradiation of visible light and enhanced photocatalytic activity of visible-working $C-TiO_2$. This is a useful result into the application for the purification system of dye wastewater using visible energy of sun light.

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A Study on the Effect of O$_2$ annealing on Structural, Optical, and Electrical Characteristics of Undoped ZnO Thin Films Deposited by Magnetron Sputtering (산소 어닐링이 마그네 트론 스퍼터링으로 증착된 undoped ZnO박막의 구조적, 광학적, 전기적 특성에 미치는 영향에 대한 연구)

  • Yun, Eui-Jung;Park, Hyeong-Sik
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.46 no.7
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    • pp.7-14
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    • 2009
  • In this paper, the effects of annealing conditions on the structural ((002) intensity, FWHM, d-spacing, grain size, (002) peak position), optical (UV peak, UV peak position) and electrical properties (carrier concentrations, resistivity, mobility) of ZnO films were investigated. ZnO films were deposited onto SiO$_2$/si substrates by RF magnetron sputtering from a ZnO target. The substrate was not heated during deposition. ZnO films were annealed in temperature ranges of $500\sim650^{\circ}C$ in the O$_2$ flow for 5$\sim$20 min. The film average thicknesses were in the range of 291 nm. The surface morphologies and structures of the samples were characterize by SEM and XRD, respectively. The optical properties were evaluated by photoluminescence (PL) measurement at room temperature (RT) using a He-Cd 325 nm laser. As the annealing temperature and time vary, the following relations were also observed: (1) proportional relationships among UV intensity (002) intensity, and grain size exist, (2) UV intensity is inversely proportional to FWHM, (3) there is no special relationship between UV intensity and electron carrier concentrations, (4) d-spacing is inversely proportional to (002) peak position, (5) UV peak position in the range of 3.20$\sim$3.24 eV means that ZnO films have a n-type conductivity which was consistent with that obtained from the electrical property, (6) the optimal conditions for the best optical and structural characteristics were found to be oxygen fraction, (O$_2$/(O$_2$+Ar)) of 0.2, RF power of 240W, substrate temperature of RT, annealing condition of 600$^{\circ}C$ for 20 min, and sputtering pressure of 20 mTorr.

Lithium Extraction from Smectitic Clay Occurring in Lithium-bearing Boron Deposits in Turkey (터키 리튬 함유 붕소광상에서 산출하는 스멕타이틱-점토로부터의 리튬 추출)

  • Lee, Won-Jong;Yoon, Soh-joung;Chon, Chul-Min;Heo, Chul-Ho;Lee, Gill-Jae;Lee, Bum-Han;Cicek, Murat
    • Journal of the Mineralogical Society of Korea
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    • v.29 no.4
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    • pp.167-177
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    • 2016
  • Smectitic clays, occurring in Kırka and Bigadiç boron evaporite deposits formed in Miocene playa lake environment in Turkey, contain $LiO_2$ 0.02-0.21% and 0.16-0.30%, respectively, and boron tailings are also reported to contain $LiO_2$ 0.04-0.26%. Lithium in smectitic clays was identified to be retained in hectorite. The XRD results revealed that hectorite was contained in 25.7% and 79.7% of Kırka and Bigadiç deposit samples respectively. In this study, we selected a clay sample from each deposit with lithium content of ~0.18% and estimated extractable lithium by acid treatment and roasting method commercially applicable to lithium resources, such as lepidolite and hectorite. When 1 g of crushed clay (particle size less than $74{\mu}m$) was reacted with 200 mL of 0.25 M HCl solution, the amount of lithium dissolved increased with the increase of reaction time up to 10 hours for both samples. Reaction time longer than 10 hours did not significantly increased the amount of lithium dissolved. After 10 hours of reaction, 89% of lithium in the clay sample from the Kırka deposit was dissolved, while 71% of lithium was dissolved from the Bigadiç deposit tailing sample. 87% of lithium in the clay sample from the Kırka deposit was extracted and 82% of lithium was extracted from the Bigadiç deposit tailing sample by the roasting extraction method, where clays were leached after a thermal treatment at $1,100^{\circ}C$ for 2 hours with $CaCO_3$ and $CaSO_4$.

Characterisitics of Redox Reaction of the Magnetite Powder Prepared by Hydrothermal Synthesis (수열합성법으로 합성된 마그네타이트 분말에 대한 산화.환원 특성)

  • Park, Sung Youl;Kang, Min Pil;Rhee, Young Woo;Nam, Sung Chan
    • Korean Chemical Engineering Research
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    • v.43 no.6
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    • pp.751-755
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    • 2005
  • Carbon dioxide, included in the flue gas from the combustion of fossil fuel, was known as a representative green house gas and various removal and utilization technologies of it has been studied for the prevention of global warming. This study was performed as an effort to find out a method to reuse carbon dioxide separated from flue gas by magnetite powder. Magnetite powder was synthesized using various oxidizers and alkalinity controlled aqueous solutions of $FeSO_4{\cdot}7H_2O$ and NaOH at 50, 80, 90, $100^{\circ}C$ and analyzed by XRD and SEM. The analysis results showed that magnetite powder synthesized at higher alkalinity and temperature had crystalline spinel and cubic structure. The reduction by hydrogen and the oxidation by carbon dioxide of synthesized powder were studied by TGA. The results showed that magnetite powder synthesized at low alkalinity and temperature was non-cubical amorphous but crystalline and cubical at high alkalinity and temperature. Comparing magnetite powders synthesized using oxidants(air and oxygen) and nitrogen, magnetite powder using more oxygen containing oxidant synthesized more crystalline magnetite powder. The experimental results of redox reaction of the synthesized magnetite powder showed that the reduction by hydrogen and the oxidation by carbon dioxide were seldom observed below $400^{\circ}C$ and observed well at $500^{\circ}C$. Magnetite powder synthesized at $100^{\circ}C$ and alkalinity(molal concentration ratio of $FeSO_4{\cdot}7H_2O$ to NaOH) of 2.0 using $O_2$ showed the highest reduction of 27.15 wt% and oxidation of 26.73 wt%, especially at reaction temperature of $500^{\circ}C$.

Mineralogical Characteristics of Carbonate Rock-Hosted Naturally Occurring Asbestos from Asan, Muju, Jangsu Areas (국내 탄산염암 지역(아산, 무주, 장수)에서 산출되는 자연발생석면의 광물학적 특성)

  • Shin, Eunhea;Jeong, Hyeonyi;Baek, Jiyeon;Jeong, Hyewon;Park, Jaebong;Roh, Yul
    • Economic and Environmental Geology
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    • v.51 no.4
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    • pp.309-322
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    • 2018
  • Naturally occurring asbestos (NOA) occurs in rocks and soils as a result of natural weathering and human activities. It is proved that inhalation of asbestos fibers can lead to increase risk of developing several diseases such as lung cancer and malignant mesothelioma. The parent rocks of asbestos have been mainly associated with (ultra)mafic and carbonate rock. The previous studies on NOA were mainly limited to (ultra)mafic rock-hosted asbestos, but studies on carbonate rock-hosted asbestos are relatively rare in S. Korea. Therefore, this study was aimed to examine mineralogical characteristics of carbonate rock-hosted NOA at three sites including Muju and Jangsu, Jeonbuk province and Asan, Chungnam province. Types of rocks at the three sites mainly consisted of Precambrian metasedimentary rocks, carbonate rock, and Cretaceous and Jurassic granites. Asbestos-containing carbonate rock samples were obtained for mineralogical characterization. XRD, PLM, EPMA, SEM and EDS analyses were used to characterize mineralogical characteristics of the carbonate rock-hosted NOA. From the carbonate rock, fibrous minerals were occurred acicular and columnar forms in the three sites. Fibrous minerals were composed of mainly tremolite and associated minerals included possibly asbestos containing materials (ACM) such as talc, vermiculite, and sepiolite. The length and aspect ratios of tremolite were similar to the standard asbestiform (length >$5{\mu}m$, length:width = 3:1). These results indicate that both non-asbestiform and asbestiform tremolite with acicular forms occurred in carbonate rocks at three sites. Geological and geochemical characteristics and mineral assemblages indicate tremolite and associated minerals might be formed by hydrothermal alternation and/or hydrothermal veins of carbonate rocks due to intrusion of acidic igneous rocks.

EFFECT OF HYDROGEN PEROXIDE CONCENTRATION ON THE WHITENING AND PHYSICAL PROPERTIES OF HYDROXYAPATITE DISCS (Hydrogen Peroxide 농도와 적용시간이 Hydroxyapatite Discs의 미백과 물리적 성질에 미치는 영향)

  • Yang, Yeon-Mi;Lee, Doo-Cheol;Baik, Byeong-Ju;Kim, Jae-Gon;Shin, Jeong-Geun
    • Journal of the korean academy of Pediatric Dentistry
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    • v.34 no.1
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    • pp.1-12
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    • 2007
  • The purpose of this study was to evaluate the effect that various concentration and application time of hydrogen peroxide had on tooth whitening and physical properties. The hydroxyapatite (HA) discs of $12mm({\Phi}){\times}1.2mm(t)$ in dimensions were made by compression $(100kg/cm^2)$ and sintering (at $1350^{\circ}C$ for 2 hours) All specimens were polished sequentially with '240 through '2000 emery paper and one side of each specimen was polished finally with $0.3{\mu}m$ alumina paste. The discs were placed in sterile whole stimulated saliva overnight at $37^{\circ}C$ in order to form an in vitro pellicle layer. Then the discs were rinsed with distilled water and soaked into staining broth at $37^{\circ}C$ for 7 days. These stained specimens were bleached with hydrogen peroxide according to the change of concentration $(3{\sim}30%)$ and application time ($3{\sim}10$ days). The specimens were analyzed with a spectrophotometer, X-ray diffractometer (XRD), scanning electron microscope (SEM), surface roughness tester, microhardness tester and biaxial flexural strength. The results of present study can be summarized as follows : 1. The bleaching effect was increased with the increased concentration and the extended application time of hydrogen peroxide. 2. The surface roughness was significantly increased from the specimen bleached with 15% hydrogen peroxide for 10 days and with 30% for 7 and 10 days respectively (p<0.05). 3. The changes of crystal phase observed by XRD between before and after bleaching weren't shown of any difference, but microporous structure of surface observed by SEM was shown of increase with the increased concentration and the extended application. 4. The biaxial flexural strength was significantly decreased from bleaching of specimen with 30% hydrogen peroxide for 7 and 10 days respectively (p<0.05) 5. Microhardness was significantly decreased from bleaching with 15% hydrogen peroxide for 10 days and with 30% for 3, 7 and 10 days respectively (p<0.05). Although the tooth bleaching effect was greater when the high concentration was applied, further in vivo experiment will be needed to prove it's safety.

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Effect of the Preparation Method on the Activity of CeO2-promoted Co3O4 Catalysts for N2O Decomposition (촉매 제조방법에 따른 Co-CeO2 촉매의 N2O 분해 특성 연구)

  • Kim, Hye Jeong;Kim, Min-Jae;Lee, Seung-Jae;Ryu, In-Soo;Yi, Kwang Bok;Jeon, Sang Goo
    • Clean Technology
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    • v.24 no.3
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    • pp.198-205
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    • 2018
  • This study investigated the influence of catalyst preparation on the activity of $Co-CeO_2$ catalyst for $N_2O$ decomposition. $Co-CeO_2$ catalysts were synthesized by co-precipitation and incipient wetness impregnation. In order to estimate the performance of the as prepared catalysts, direct catalytic $N_2O$ decomposition test was carried out under $250{\sim}375^{\circ}C$. As a result, the catalyst prepared by co-precipitation (CoCe-CP) showed an enhanced performance on $N_2O$ decomposition reaction even in the presence of $O_2$ and/or $H_2O$, whereas the impregnation catalyst (CoCe-IM) did not. In order to investigate the difference in catalytic activity, characterization such as XRD, BET, TEM, $H_2-TPR$, $O_2-TPD$, and XPS was conducted. It is confirmed that the particle size and specific surface area were changed depending on the catalyst preparation method and the synthesis process influenced the physical properties of the catalysts. In addition, the improvement in the activity of the catalyst prepared by co-precipitation is due to the enhanced reduction from $Co^{3+}$ to $Co^{2+}$ and the improved oxygen desorption rate. However, it has been confirmed that the surface electron state and binding energy, which are related to $N_2O$ decomposition, do not change depending on the preparation method.

Preparation of TiCoxFe1-x(x=0.50~1.00) System Metal Membrane for Hydrogen Separation (수소분리용 TiCoxFe1-x(x=0.50~1.00)계 금속막 제조)

  • Jang, Kyu-young;Kang, Tae Beom
    • Membrane Journal
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    • v.25 no.2
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    • pp.191-201
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    • 2015
  • We have studied on the preparation of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloy, the characteristics of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloy by X-ray diffractometer (XRD), pressure composition temperature (PCT) curve, scanning electron microscopy (SEM) and the $H_2-N_2$ gas mixture separation of $TiCo_xFe_{1-x}$(x=0.50~1.00)- stainless steel (SS) composite membranes. The formation of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloys with cubic crystal same as TiCo was confirmed by X-ray diffractometer. $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloys showed the hysteresis at $120^{\circ}C$. As the Fe content of $TiCo_xFe_{1-x}$(x=0.50~1.00) system alloys increased, the hysteresis was increased both range x=0.90~1.00 and x=0.55~0.60, and the range x=0.55~0.90 gave decreased hysteresis. $TiCo_{0.55}Fe_{0.45}$ alloy was the one showed the lowest hysteresis among them. The lowest value of hydrogen permeation pressure of $TiCo_xFe_{1-x}$(x=0.50~1.00)-SS composite membrane was $TiCo_{0.55}Fe_{0.45}$-SS composite membrane with the value of 2.5 atm at $120^{\circ}C$; otherwise, $TiCo_{0.90}Fe_{0.10}$-SS composite had the highest pressure value among the membranes with the value of 10 atm. $TiCo_{0.55}Fe_{0.45}$-SS composite membrane was the best to separate the $H_2-N_2$ gas mixture excellently among the $TiCo_xFe_{1-x}$(x=0.50~1.00)-SS composite membranes since $TiCo_{0.55}Fe_{0.45}$ had the least hysteresis, and hydrogen permeation pressure was the lowest with value of 2.5 atm.

Pressure-load Calibration of Multi-anvil Press and the Thermal Gradient within the Sample Chamber (멀티 앤빌 프레스의 압력-부하 보정 작업과 시료 내의 온도구배 연구)

  • Kim, Eun Jeong;Lee, Sung Keun
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.3
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    • pp.161-172
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    • 2018
  • Multi-anvil press (MAP) is one of the high pressure apparatuses and often generates the pressure-conditions ranging from 5 to 25 GPa and temperature-conditions up to $2,300^{\circ}C$. The MAP is, therefore, suitable to explore the pressure-induced structural changes in diverse earth materials from Earth's mantle and the bottom of the mantle transition zone (~660 km). In this study, we present the experimental results for pressure-load calibration of the 1,100-ton multi-anvil press equipped in the authors' laboratory. The pressure-load calibration experiments were performed for the 14/8 step, 14/8 G2, 14/8 HT, and 18/12 assembly sets. The high pressure experiments using ${\alpha}$-quartz, wollastonitestructure of $CaGeO_3$, and forsterite as starting materials were analyzed by powder X-ray diffraction spectroscopy. The phase transition of each mineral indicates the specific pressure that is loaded to a sample at $1,200^{\circ}C$: a transition of ${\alpha}$-quartz to coesite at 3.1 GPa, that of garnet-structure of $CaGeO_3$ to perovskite-structure at 5.9 GPa, that of coesite to stishovite at 9.2 GPa, and that of forsterite to wadsleyite at 13.6 GPa. While the estimated pressure-load calibration curve is generally consistent with those obtained in other laboratories, the deviation up to 50 tons is observed at high pressure above 10 GPa. This is partly because of the loss of oil pressure at high pressure resulting from the differences in a sample chamber, and the frictional force between pressure medium and second anvil. We also report the ${\sim}200^{\circ}C/mm$ of thermal gradient in the vertical direction of the sample chamber of 14/8 HT assembly. The pressure-load calibration curve and the observed thermal gradient within the sample chamber can be applied to explain the structural changes and the relevant macroscopic properties of diverse crystalline and amorphous earth materials in the mantle.

High-temperature Thermal Decomposition of Cs-adsorbed CHA-Cs and CHA-PCFC-Cs Zeolite System, and Sr-adsorbed 4A-Sr and BaA-Sr Zeolite System (Cs-흡착 CHA-Cs 및 CHA-PCFC-Cs 제올라이트계와 Sr-흡착 4A-Sr 및 BaA-Sr 제올라이트계의 고온 열분해)

  • Lee, Eil-Hee;Kim, Ji-Min;Kim, Hyung-Ju;Kim, Ik-Soo;Chung, Dong-Yong;Kim, Kwang-Wook;Lee, Keun-Young;Seo, Bum-Kyoung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.16 no.1
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    • pp.49-58
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    • 2018
  • For the immobilization of high-radioactive nuclides such as Cs and Sr by high-temperature thermal decomposition, this study was carried out to investigate the phase transformation with calcined temperature by using TGA (thermogravimetric analysis) and XRD (X-ray diffraction) in the Cs-adsorbed CHA (chabazite zeolite of K type)-Cs and CHA-PCFC (potassium cobalt ferrocyanide)-Cs zeolite system, and Sr-adsorbed 4A-Sr and BaA-Sr zeolite system, respectively. In the case of CHA-Cs zeolite system, the structure of CHA-Cs remained at up to $900^{\circ}C$ and recrystallized to pollucite ($CsAlSi_2O_6$) at $1,100^{\circ}C$ after undergoing amorphous phase at $1,000^{\circ}C$. However, the CHA-CFC-Cs zeolite system retained the CHA-PCFC-Cs structure up to $700^{\circ}C$, but its structure collapsed in $900{\sim}1,000^{\circ}C$, and then transformed to amorphous phase, and recrystallized to pollucite at $1,100^{\circ}C$. In the case of 4A-Sr zeolite system, on the other hand, the structure of 4A-Sr maintained up to $700^{\circ}C$ and its phase transformed to amorphous at $800^{\circ}C$, and recrystallized to Sr-feldspar ($SrAl_2Si_2O_8$, hexagonal) at $900^{\circ}C$ and to $SrAl_2Si_2O_8$ (triclinic) at $1,100^{\circ}C$. However, the BaA-Sr zeolite system structure began to break down at below $500^{\circ}C$, and then transformed to amorphous phase in $500{\sim}900^{\circ}C$ and recrystallized to Ba/Sr-feldspar (coexistence of $Ba_{0.9}Sr_{0.1}Al_2Si_2O_8$ and $Ba_{0.5}Sr_{0.5}Al_2Si_2O_8$) at $1,100^{\circ}C$. All of the above zeolite systems recrystallized to mineral phase through the dehydration/(decomposition) ${\rightarrow}$ amorphous ${\rightarrow}$ recrystallization with increasing temperature. Although further study of the volatility and leachability of Cs and Sr in the high-temperature thermal decomposition process is required, Cs and Sr adsorbed in each zeolite system are mineralized as pollucite, Sr-feldspar and Ba/Sr-feldspar. Therefore, Cs and Sr seen to be able to completely immobilize in the calcining wasteform/(solidified wasteform).