• Title/Summary/Keyword: X-선 구조분석

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Synthesis and Characterization of Zeolite Using Water Treatment Sludge (정수슬러지를 이용한 제올라이트의 합성 및 특성연구)

  • Ko, Hyun Jin;Ko, Yong Sig
    • Clean Technology
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    • v.26 no.4
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    • pp.263-269
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    • 2020
  • Zeolite was synthesized hydrothermally using the water-treatment sludge, and the effects of various synthesis parameters like reaction temperature, reaction time, and Na2O/SiO2 molar ratio on the crystallization of zeolite were investigated. Crystal structure, physical property, and thermal stability of zeolite crystals were characterized by X-ray powder diffraction, FTIR spectroscopy, BET nitrogen adsorption, and TGA measurements. The removal efficiencies of nitrogen in ammonia, heavy metal ions, and TOC were calculated to evaluate zeolite's adsorption capacity. The primary chemical composition of water-treatment sludge was 28.79% Al2O3 and 27.06% SiO2. The zeolites were synthesized by merely employing the water-treatment sludge as silica and alumina sources without additional chemicals. Zeolite crystals synthesized through the water-treatment sludge were confirmed as an A-type zeolite structure. Zeolite A had the highest crystallinity obtained from a gel with the molar composition 2.1Na2O-Al2O3-1.6SiO2-65H2O after 5 h at a temperature of 90 ℃. The specific surface area of zeolite obtained was 55 ㎡ g-1, which was higher than commercial zeolite A. The removal efficiency of nitrogen in ammonia was 68% after 3 h of reaction time, while the removal efficiencies of Pb2+ and Cd2+ ions were 99.1% and 99.3%, respectively. These results indicate active ion exchange between Pb2+ or Cd2+ ion and Na+ ion in the zeolite framework. The adsorption experiments on the different zeolite addition conditions were performed for 3 h with 300 ppm humic acid. Based on the results, TOC's highest efficiency was 83% when 5 g of zeolite was added.

Scientific Analysis and Conservation Treatment on the Buddhist Scriptures of Paper Relics Excavated from Sum Tolgoi, Mongolia (몽골 숨 톨고이 출토 지류 유물의 과학적 분석 및 보존처리)

  • Bae, Su Bin;Yang, Min Jeong;Kwon, Yun Mi;Yoo, Ji Hyun;Jeong, Hee Won
    • Journal of Conservation Science
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    • v.37 no.6
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    • pp.723-737
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    • 2021
  • This study analyzed the composition and structure of materials with Buddhist paper scriptures excavated from architectural sites in 'Sum Tolgoi' of the 17th century and carried out conservation treatment base on the result of the analysis. The scriptures were covered in dust and foreign sub stances, and were so crumpled that it was impossible to identify the form. The damage, loss, and discoloration have been identified. Buddhist scriptures written in Tibetan used indigo and ink sticks on paper as a result of UV-Vis analysis, and ink sticks as black character materials from scriptures written ancient Mongolian. SEM-EDS and Micro-XRF analyses revealed that the outlines were drawn with red lines using a mix of Minium (Pb3O4) and Cinnabar (HgS), or Cinnabar (HgS) alone, and the contents of the scriptures were written with silver paint. Silver chloride (AgCl) and Calcium (Ca) were identified in the silver paint component of the characters, while Calcium and Orpiment (As2S3) were identified in the yellow lines. Concerning the paper ground, Buddhist scriptures written in ancient Mongolian were characterized by herbal plant fiber and bast fiber, and those written in Tibetan, by bast fiber. Radiocarbon dating indicates that the paper for the scriptures was produced between the 15th and 17th centuries. Conservation treatment of the scriptures was carried out based on the experiment on the production of pre-coated paper and how to coat that to prevent the second damage due to the deformation and fragility of the excavated paper. The scriptures were preserved and mounted, and a neutral box was made to identify the contents of the scriptures recorded on both sides after the treatment. This conservation treatment is the result of a study that applied new conservation treatment materials and methods according to the principle of conservation treatment reversibility.

Particle Size Analysis of Nano-sized Talc Prepared by Mechanical Milling Using High-energy Ball Mill (고에너지 볼 밀을 이용한 나노 활석의 형성 및 입도 분석)

  • Kim, Jin Woo;Lee, Bum Han;Kim, Jin Cheul;Kim, Hyun Na
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.1
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    • pp.47-55
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    • 2018
  • Talc, hydrous magnesium phyllosilicate, is one of the most popular industrial minerals due to their chemical stability and adsorptivity. While micro-sized talc has long been used as a filler and coating, nano-sized talc recently is attracting attention as additives for improving the stability of nanocomposites. In this study, we produced the nano-sized talc powder by mechanical method using high energy ball mill and investigated the changes in particle size and crystallinity with increasing milling time up to 720 minutes. X-ray diffraction results show that the peak width of talc gradually as the milling proceeded, and after 720 minutes of pulverization, the talc showed an amorphous-like X-ray diffraction pattern. Lase diffraction particle size analysis presents that particle size of talc which was ${\sim}12{\mu}m$ decreased to ${\sim}0.45{\mu}m$ as the milling progressed, but no significant reduction of particle size was observed even after grinding for 120 minutes or more. BET specific surface area, however, steadily increases up to the milling time of 720 minutes, indicating that the particle size and morphology change steadily as the milling progressed. Scanning electron microscope and transmission electron microscope images shows that layered particles of about 100 to 300 nm was aggregated as micro-sized particles after pulverization for 720 minutes. As the grinding time increases, the particle size and morphology of talc continuously change, but the nano-sized talc particles form micro sized agglomerates. These results suggest that there is a critical size along the a, b axes in which the size of plates is reduced even though the grinding proceeds, and the reduction of plate thickness along the c axis leads the increase in specific surface area with further grinding. This study could enhance the understanding of the mechanism of the formation of nano-sized talc by mechanical grinding.

Evaluation of titanium surface properties by $Nd:YVO_4$ laser irradiation: pilot study ($Nd:YVO_4$ 레이저 조사에 따른 티타늄의 표면특성 평가: 예비 연구)

  • Kim, Ae-Ra;Park, Ji-Yoon;Kim, Yeon;Jun, Sei-Won;Seo, Yoon-Jeong;Park, Sang-Won
    • The Journal of Korean Academy of Prosthodontics
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    • v.51 no.3
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    • pp.167-174
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    • 2013
  • Purpose: This study was conducted to evaluate the roughness and surface alternations of three differently blasted titanium discs treated by $Nd:YVO_4$ Laser irradiation in different conditions. Materials and methods: Thirty commercially pure titanium discs were prepared and divided into three groups. Each group was consisted of 10 samples and blasted by $ZrO_2$ (zirconium dioxide), $Al_2O_3$ (aluminum oxide), and RBM (resorbable blasted media). All the samples were degreased by ultrasonic cleaner afterward. Nine different conditions were established by changing scanning speed (100, 300, 500 mm/s) and repetition rate (5, 15, 35 kHz) of $Nd:YVO_4$ Laser (Laser Pro D-20, Laserval $Korea^{(R)}$, Seoul, South Korea). After laser irradiation, a scanning electron microscope, X-ray diffraction analysis, energy dispersive X-ray spectroscopic analysis, and surface roughness analysis were used to assess the roughness and surface alternations of the samples. Results: According to a scanning electron microscope (SEM), titanium discs treated with laser irradiation showed characteristic patterns in contrast to the control which showed irregular patterns. According to the X-ray diffraction analysis, only $Al_2O_3$ group showed its own peak. The oxidation tendency and surface roughness of titanium were similar to the control in the energy dispersive X-ray spectroscopic analysis. The surface roughness was inversely proportional to the scanning speed, whereas proportional to the repetition rate of $Nd:YVO_4$. Conclusion: The surface microstructures and roughness of the test discs were modified by the radiation of $Nd:YVO_4$ laser. Therefore, laser irradiation could be considered one of the methods to modify implant surfaces for the enhancement of osseointegration.

Preparation of Polypropylene/Clay Nanocomposites Using Aminosilane Treated Clay (아미노실란 개질 클레이를 사용한 폴리프로필렌 클레이 나노복합재료)

  • Hong Chae-Hwan;Bae Jin-Woo;Lee Yong-Bum;Lee Choon-Soo;Jho Jae-Young;Nam Byeong-Uk
    • Polymer(Korea)
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    • v.30 no.4
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    • pp.318-325
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    • 2006
  • Polypropylene-clay nanocomposites were studied by the modification of clay with amino silanes to introduce covalent bonds in nanocomposites, and prepared by melt-compounding with polypropylene, clay modified with amino silanes and maleic anhydride grafted polypropylene. The . .structure and surface properties of modified clay were determined by x-ray diffraction, infrared spectrum, and solid-state $^{29}Si$ nuclear magnetic resonance spectrum. The modification of clay with aminosilanes led to the increase of the silicate interlayers to about $19.8{\AA}$, the weakening effects of hydroxy group at $3650cm^{-1}$ and the signal of amine groups at -69 ppm proved that the modification had taken place.

RF-Magnetron Sputtering법에 의해 성막된 $Ga_2O_3$가 혼합된 ZnO박막의 전기적 및 광학적 특성

  • Kim, Mi-Seon;Bae, Gang;Son, Seon-Yeong;Hong, U-Pyo;Kim, Hwa-Min;Lee, Jong-Yeong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.120-120
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    • 2010
  • 최근 투명전도성 산화물(Transparent Conductive Oxide, TCO) 박막은 액정 표시소자(LCD), 플라즈마 디스플레이 패널(PDP), 압전소자 및 태양전지의 투명소자로 사용되어지고 있다. 현재 가장 널리 사용되어지고 있는 투명전극물질인 인듐주석산화물(indium tin oxide, ITO)은 낮은 비저항과 높은 투과율을 가지고 있지만, 높은 원자재의 가격 및 수소플라즈마 처리시 In과 Sn이 환원되어 전기적, 광학적으로 불안정한 문제점들이 지적되고 있다. 이러한 문제점들을 해결하기 위해 최근 적외선 및 가시광선 영역에서 높은 투과도 및 전기 전도성과 수소플라즈마에 대한 화학적 안정성을 갖는 ZnO를 기반으로 3족 원소를 첨가한 새로운 투명 전도막에 대한 연구가 활발하다. 본 연구에서는 RF-Magnetron Sputtering법을 이용하여 $Ga_2O_3$ 혼합비에 따라 제작된 ZnO(GZO) 박막들의 전기적, 광학적, 구조적인 특성들을 분석하였다. 측정결과, $Ga_2O_3$의 첨가량이 7 wt.%인 GZO 박막이 가시광선영역에서 80%이상의 높은 투과율과 $50.5\;\Omega/\Box$의 가장 낮은 면저항을 나타내었다. 이는 Ga원소가 다른 3족 원소와 격자결합을 비교할 때, 이온의 크기가 Zn원소와 비슷하여 최적화된 혼합율을 가지는 경우 격자결합을 최소화시켜 캐리어 밀도의 증가로 인해 높은 전도성을 가지며, 고온에서도 전기적 특성 및 내구성이 향상되기 때문이다. 또한 기판온도에 따른 열처리 특성으로서 기판의 온도를 $100^{\circ}{\sim}400^{\circ}C$까지 변화를 주어 실험하였다. X-선 회절패턴 분석결과 기판온도가 증가함에 따라 ZnO (002) 방향이 감소하는 반면 ZnO(103) 방향이 증가하였으며, 기판온도가 $300^{\circ}C$ 일 때 $17.1\;\Omega/\Box$의로 가장 낮은 면저항이 나타났다. 이는 SEM 이미지를 분석한 결과, 실온에서 제작된 박막과 비교해 300 에서 증착된 GZO 박막이 결정립의 크기가 크고 밀도도 조밀해져 전하의 이동도가 향상되었기 때문이다.

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Fixation Mechanism and Leachability of Heavy Metal for Sludge Solidified by Silica Fume and Cement (실리카흄을 이용한 중금속함유 유기성 슬러지 시멘트 고화체의 용출특성과 고정화기작에 관한 연구)

  • Jun, Kwan-Soo;Hwang, Byung-Gi
    • Applied Chemistry for Engineering
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    • v.16 no.2
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    • pp.180-186
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    • 2005
  • This paper discusses the development of mixtures for silica fume as a stabilization/solidification agent and a binder for industrial wastewater residue containing organic and heavy metal contaminants. The UCS (unconfined compressive strength) gradually increased to 66.7% as the silica fume content increased to 15%. The leaching of TOC (total organic carbon) and chromium decreased as more OPC (Ordinary Portland Cement) was substituted with the silica fume. When a mixture had 5% silica fume, it retained about 85% TOC, and chromium leached out 0.76 mg-Cr/g-Cr in acidic solution. Also, microstructural studies of the solidified analysis showed that the silica fume caused an inhibition to the ettringite formation which did not contrilbute to setting but coated the cement particles and retarded the setting reactions. The results indicated that the incorporation of silica fume into the cement matrix minimized the detrimental effects of organic materials on the cement hydration reaction and the contaminant leachability.

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.

Neutron Diffraction and Mössbauer Studies of Superexchange Interaction on Al Substituted Co-ferrite (Al이 치환된 Co 페라이트에 관한 뫼스바우어 분광법 및 중성자 회절 연구)

  • Kim, Sam-Jin;Myoung, Bo-Ra;Kim, Chul-Sung;Baek, Kyung-Seon
    • Journal of the Korean Magnetics Society
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    • v.16 no.6
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    • pp.287-292
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    • 2006
  • Al substituted $CoAl_{0.5}Fe_{1.5}O_{4}$ has been studied with x-ray and neutron diffraction, $M\"{o}ssbauer$ spectroscopy and magnetization measurements. $CoAl_{0.5}Fe_{1.5}O_{4}$ revealed a cubic spinel structure of ferrinmagnetic long range ordering at room temperature, with magnetic moments of $Fe^{3+}(A)(-2.29{\mu}_{B}),\;Fe^{3+}(B)(3.81\;{\mu}_{B}),\;Co^{2+}(B)(2.66{\mu}_{B})$, respectively. The temperature dependence of the magnetic hyperfine field in $^{57}Fe$ nuclei at the tetrahedral (A) and octahedral (B) sites was analyzed based on the $N\'{e}el$ theory of magnetism. In the sample of $CoAl_{0.5}Fe_{1.5}O_{4}$, the interaction A-B interaction and intrasublattice A-A superexchange interaction were antiferromagnetic with strengths of $J_{A-B}=-19.3{\pm}0.2k_{B}\;and\;J_{A-A}=-21.6{\pm}0.2k_{B}$, respectively, while the intrasublattice B-B superexchange interaction was found to be ferromagnetic with a strength of $J_{B-B}=3.8{\pm}0.2k_{B}$.

Effects of Nitrogen Addition on Thermal Stability of Ta-Al Alloy Films (Ta-Al 합금박막의 열적안정성에 미치는 질소첨가 효과)

  • Jo, Won-Gi;Kim, Tae-Yeong;Gang, Nam-Seok;Kim, Ju-Han;An, Dong-Hun
    • Korean Journal of Materials Research
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    • v.7 no.10
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    • pp.877-883
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    • 1997
  • Ar 및 Ar과 $N_{2}$ 분위기하에서 rf 마그네트론 스퍼터링방법으로 Ta-AI과 Ta-AI-N합금막을 제조하였다. Ta-7.9at.% AI계열, Ta-26.7 at% AI게열과 Ta-45.4at.%AI계열에 Ar에 대한 질서유량비로 26%까지 질소를 첨가하여 Ta-AI-N박막을 증착한후, 300-$600^{\circ}C$온도 구산에서 열처리 전후의 구조 및 전기적 특성과 열적안정성을 통하여 레지스터의 적용가능성을 조사하였다. 구조 및 조성 분석은 X-선 회절과 Rutherford Backscattering Spectrometry(RBS)로 관찰하였고 열적안정성은 4단자법(four point probe method)을 이용한 저항변화를 통하여 측정하였다. 순수 Ta에 AI을 첨가하면 확장된 $\beta$($\beta$-Ta)N 합금박막에서 가장 열적안정성이 우수하게 나타났던 질소첨가 범위는 Ta $N_{hcp}$또는 TaN/ sub fcc/또는 Ta $N_{fcc}$와 비정질과의 혼합상순으로 상천이를 나타내었다. Ta-AI-N 합금박막에서 가장 열적안정성이 우수하게 나타났던 질서첨가 범위는 Ta-26.7at. % AI계열의 경우 19-36at.% $N_{2}$구간이었고, Ta-45.5at.% AI계열의 경우는 30-45at.%구간이었다. Ta-AI합금박막은 질소가 첨가되지 않아도 열처리 온도 및 시간에 따라 약 10% 이내의 비교적 작은 저항변화를 보여 열적안정성이 우수하지만 질소를 첨가하여 Ta-AI-N합금박막을 형성시킬경우, 증착된 상태에서 이미 큰 비저항을 나타내었고 열처리 동안 3%이내의 매우 작은 저항변화를 나타내었기 때문에 레지스터용 재료로써 열적안정성에 대한 잠재력이 크다.

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