• Title/Summary/Keyword: x-ray diffraction(XRD)

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A Study on Desalination Methods for Application of Outdoor Iron Artefacts (옥외 철제문화재 적용을 위한 탈염처리 방법 연구)

  • Lee, Hye-Youn;Cho, Nam-Chul;Kim, Woo-Hyun
    • Journal of Conservation Science
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    • v.25 no.1
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    • pp.49-60
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    • 2009
  • Outdoor iron artefacts are easily corroded by salts, especially $Cl^-$ion, from environmental pollutants and acid rain because of their location, so that they need conservational treatments such as stabilization. However the conservation of outdoor iron artefacts are limited to be consolidated for the present and there are a few the studies for the desalinization. The general desalinization method is that objects are immersed in reagent such as alkaline corrosion inhibiting solutions targeting on buried iron artefacts, thus they are not available for outdoor iron artefacts. In this study, concerning those difficulties, the different desalting method is experimented that materials soaked in alkaline solutions attach to objects and they are packed by waterproof to avoid evaporation. This paper experiment burial iron artefacts at first in order to fine out an adaptable method for outdoor iron artefacts. The soaking materials are Korean traditional paper, gauze, cotton wipers, spill pads and the desalting regent is NaOH 0.1M. Additionally the exiting desalinization method which is to immerse objects in solution is performed to compare. The analyses are microscopes, SEM-EDS, X-ray diffraction, pH meter and Ion chromatography. The result is that spill pads show the best desalting effect out of other materials similar to immersing desalting method.

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Sulfate Resistance of Alkali-Activated Materials Mortar (알칼리 활성화 결합재 활용 모르타르의 황산염 침식 저항성)

  • Park, Kwang-Min;Cho, Young-Keun;Lee, Bong-Chun
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.20 no.2
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    • pp.94-101
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    • 2016
  • This paper presents an investigation into the durability alkali-activated materials(AAM) mortar and paste samples manufactured using fly-ash(FA) and ground granulated blast furnace slag(GGBFS) exposed to a sulfate environment with different GGBFS replace ratios(0, 30, 50 and 100%), sodium silicate modules($Ms[SiO_2/Na_2O]$ 1.0, 1.5 and 2.0) and initial curing temperatures($23^{\circ}C$ and $70^{\circ}C$). The tests involved immersions for a period of 6 months into 10% solutions of sodium sulfate and magnesium sulfate. The evolution of compressive strength, weight, length expansion and microstructural observation such as x-ray diffraction were studied. As a results, as higher GGBFS replace ratio or Ms shown higher compressive strengths on 28 days. In case of immersed in 10% sodium sulfate solution, the samples shows increase in long-term strength. However, for samples immersed in magnesium sulfate solutions, the general observation was that the compressive strength decreased after immersion. The most drastic reduction of compressive strength and expansion of weight and length occurred when GGBFS or Ms ratios were higher. Also, the XRD analysis of samples immersed in magnesium sulfate indicated that expansion of AAM caused by gypsum($CaSO_4{\cdot}2H_2O$); the gypsum increased up to 6 months continuously.

Effective of $Li_2CO_3$ and ZnBO for low temperature sintered $(Ba_{0.5},Sr_{0.5})TiO_3$ ceramics (BST 세라믹 저온소결에 $Li_2CO_3$와 ZnBO가 미치는 영향)

  • Kim, Se-Ho;You, Hee-Wook;Koo, Sang-Mo;Ha, Jae-Geun;Lee, Young-Hie;Koh, Jung-Hyuk
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.297-297
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    • 2007
  • The $(B_{0.5},Sr_{0.5})TiO_3$ ceramics, which added with low sintering materials $Li_2CO_3$ and ZnBO, was investigated for LTCC(low temperature co-fired ceramic) applications. To compare sintering temperature of $(B_{0.5},Sr_{0.5})TiO_3$ respectively, we added 1, 2, 3, 4, and 5wt% of $Li_2CO_3$ and ZnBO to $(B_{0.5},Sr_{0.5})TiO_3$. For confirming the sintering temperature, the respective specimens were sintered from $750^{\circ}C$ to $1200^{\circ}C$ by $50^{\circ}C$. The case of $Li_2CO_3$ greatly lowered the sintering temperature of $(B_{0.5},Sr_{0.5})TiO_3$ ($1350^{\circ}C$) below $900^{\circ}C$. The addition of ZnBO improved the loss tangent of $(B_{0.5},Sr_{0.5})TiO_3$. The crystalline structure of $LiCO_3$ doped $(B_{0.5},Sr_{0.5})TiO_3$ and ZnBO doped $(B_{0.5},Sr_{0.5})TiO_3$ was analyzed with the X-ray diffraction (XRD) analysis. The dielectric permittivity and loss tangent of $Li_2CO_3$ doped BST and ZnBO doped BST were measured with the HP 4284A precision. From the electrical characterization, we respectively obtained the dielectric permittivity 1361, loss tangent $6.94{\times}10^{-3}$ at $Li_2CO_3$ doped $(B_{0.5},Sr_{0.5})TiO_3$ (3wt%) and the dielectric constant 1180, loss tangent $3.70{\times}10^{-3}$ at ZnBO doped $(B_{0.5},Sr_{0.5})TiO_3$(5wt%).

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Effect of hydrogen in Ni-silicide with Iodine Catalyst Deposited Ni Film by using Atomic Layer Deposition

  • Gang, Hui-Seong;Ha, Jong-Bong;Kim, Gi-Won;Kim, Dong-Seok;Im, Gi-Sik;Kim, Seong-Nam;Lee, Gwang-Man;Lee, Jeong-Hui
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.234-234
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    • 2010
  • 최근 CMOS 소자 크기가 축소됨에 따라 소스와 드레인 영역에서의 접촉저항을 줄이기 위하여, 실리사이드 공정이 많이 연구되고 있다. 실리사이드 물질로서 NiSi는 낮은 저항률과 낮은 실리콘 소모, 낮은 공정온도, 등의 장점을 가지고 있다. 그러나, 실리사이드 형성으로 인한 나노소자의 소오스/드레인에서정션(junction) 누설전류의 증가는 큰 문제가 되므로 실리콘과 실리사이드 계면의 특성이 중요하다. 본 연구에서는 니켈을 이용한 실리사이드 형성시 계면 활성제인 에틸 요오드를 이용하여 실험을 진행하였다. 금속 유기 전구체인 MABONi을 사용하여 ALD 방식으로 증착 한 니켈 박막과 니켈 핵 형성시 계면활성제인 에틸요오드의 처리 방법에 따른 Ni-silicide 박막의 특성을 비교, 분석하였다. 먼저 자연산화막을 건식식각으로 제거한 뒤, 첫 번째 샘플에서는 10회의 주기로 초기 니켈을 증착한 뒤, 에틸요오드로 니켈의 표면 위를 처리하고, 다시 200회의 주기로 니켈을 증착하였으며, 두 번째는 첫 번째 방식에서 에틸요오드 주입 시 동시에 수소도 함께 주입하였다. 세 번째는 비교를 위해 에틸요오드 처리를 하지 않고 니켈 박막만을 증착 하였다. 이어서, 각 샘플을 급속 열처리 장비에서 $400^{\circ}C$부터 $900^{\circ}C$까지 각각 30sec간 열처리를 진행후, 반응하지 않은 잔여 니켈을 제거한 후, XRD(x-ray diffraction), AES(auger), 그리고 4-point probe 등을 이용하여 형성된 실리사이드의 특성을 분석하였다. 에틸요오드와 함께 수소를 주입한 경우 계면에서의 산소 불순물과 카본 성분이 효과적으로 제거되어 $400^{\circ}C$에서 $2.9{\Omega}/{\Box}$ 의 낮은 면저항을 가지는 NiSi가 형성되었고 모든 온도구간에서 다른 샘플에 비하여 가장 낮은 면저항 분포를 보였다. 이는 분해 흡착된 요오드에 의한 계면 특성 향상과 카본 성분이 포함된 잔여물들이 수소처리에 의해 효율적으로 제거되어 실리사이드의 특성이 향상되었기 때문이다. 계면활성제를 사용하지 않은 경우에는 $500^{\circ}C$에서 NiSi가 형성되었다. 반면에 에틸요오드로만 표면을 처리한 경우에는 니켈과 실리콘 계면에서의 카본 성분에 의하여 silicidation 이 충분히 일어나지 않았다. 이러한 결과는 향후 45nm 이하의 CMOS 공정상에서 소스와 드레인의 낮은 누설전류를 가지고, 접촉저항을 줄이기 위한 니켈 실리사이드 형성에 큰 도움을 줄 것으로 기대된다.

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Characteristics of Tremolite Asbestos from Abandoned Asbestos Mines in Boryeong Area, Chungnam (충남 보령지역의 폐석면 광산에서 산출하는 투각섬석 석면의 특성)

  • Yoon, Keun-Taek;Hwang, Jin-Yeon;Oh, Ji-Ho;Lee, Hyo-Min
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.1
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    • pp.73-84
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    • 2010
  • We studied the geological occurrence, associated minerals, mineralogical properties and formation process of tremolites from two abandoned asbestos mines, Jungang (Sinsuk) and Daebosuksan, located in Boryoung area, Chungnam. Morphologically different tremolites such as long fibrous, needle-like, bladed and prismatic forms coexisted. Fibrous tremolite, known for its high toxieity to human health, was systematically analyzed by polarized light microscopy and scanning electron microscopy. The average length of tremolite fibers was 31.2 ${\mu}m$ although the maximum length of some asbestos was 210.0 ${\mu}m$. The average width and aspect ratio were 1.6 ${\mu}m$ and 19.9, respectively. Tremolite showed inclined extinction in the range of 6.1~20.2$^{\cric}$. X-ray diffraction patterns were slightly different between fibrous (asbestiform) and prismatic (non-asbestiform) tremolites. EPMA analysis of tremolites in the study area indicated extremely high Mg content with very low Fe content, close to the composition of tremolite in end-member in the tremolite-actinolite solid solution series. The formational conditions of asbestiform and non-asbestiform tremolite appear to be different. Asbestiform tremolite was estimated to have been formed in later stage.

Effect of Microstructures and Sintering Additives on the Mechanical Properties of Si$_3$N$_4$ (질화규소의 기계적 특성에 미치는 미세구조 및 소결조제의 영향)

  • Park, Hye-Ryeon;Lee, O-Sang;Park, Hui-Dong;Lee, Jae-Do
    • Korean Journal of Materials Research
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    • v.2 no.5
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    • pp.330-336
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    • 1992
  • Four distinctive hot pressed and heat treated S${i_3}{N_4}$ceramics, S${i_3}{N_4}$-8%${Y_2}{O_3}$, S${i_3}{N_4}$-6% ${Y_2}{O_3}$-2% $A{l_2}{O_3}$, S${i_3}{N_4}$-4% ${Y_2}{O_3}$-3% $A{l_2}{O_3}$, 그리고 S${i_3}{N_4}$-1% MgO-1% Si$O_2$(in wt%), were prepared and characterized by X-ray diffraction, scanning electron microscopy, image analysis and mechanical tests. The fracture toughness of S${i_3}{N_4}$-8% ${Y_2}{O_3}$specimens containing large elongated grains showed the highest value of about 9.8MPa$m^{1/2}$. Two out of four S${i_3}{N_4}$, ceramics(S${i_3}{N_4}$-6% ${Y_2}{O_3}$-2% $A{l_2}{O_3}$and S${i_3}{N_4}$-4% ${Y_2}{O_3}$-3% $A{l_2}{O_3}$) heat treated at 200 $0^{\circ}C$retained the fracture strength of over 900MPa and fracture toughness of over 8.0MPa$m^{1/2}$. Large ${\beta}$-S${i_3}{N_4}$grains having a diameter larger than 1${\mu}$m appeared to contribute to increase in fracture toughness.

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Effect of Precipitator and Quantity on the Formation of Fe3(PO4)2 (Fe3(PO4)2 생성에 미치는 침전제와 첨가량의 영향)

  • An, Suk-Jin;Lee, Sun-Young;Oh, Kyoung-Hwan;Suhr, Dong-Soo
    • Korean Journal of Materials Research
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    • v.21 no.11
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    • pp.587-591
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    • 2011
  • The effect of the precipitator (NaOH, $NH_4OH$) and the amount of the precipitator (150, 200, 250, 300 ml) on the formation of $Fe_3(PO_4)_2$, which is the precursor used for cathode material $LiFePO_4$ in Li-ion rechargeable batteries was investigated by the co-precipitation method. A pure precursor of olivine $LiFePO_4$ was successfully prepared with coprecipitation from an aqueous solution containing trivalent iron ions. The acid solution was prepared by mixing 150 ml $FeSO_4$(1M) and 100 ml $H_3PO_4$(1M). The concentration of the NaOH and $NH_4OH$ solution was 1 M. The reaction temperature (25$^{\circ}C$) and reaction time (30 min) were fixed. Nitrogen gas (500 ml/min) was flowed during the reaction to prevent oxidation of $Fe^{2+}$. Single phase $Fe_3(PO_4)_2$ was formed when 150, 200, 250 and 300 ml NaOH solutions were added and 150, 200 ml $NH_4OH$ solutions were added. However, $Fe_3(PO_4)_2$ and $NH_4FePO_4$ were formed when 250 and 300 ml $NH_4OH$ was added. The morphology of the $Fe_3(PO_4)_2$ changed according to the pH. Plate-like lenticular shaped $Fe_3(PO_4)_2$ formed in the acidic solution below pH 5 and plate-like rhombus shaped $Fe_3(PO_4)_2$ formed around pH 9. For the $NH_4OH$, the pH value after 30 min reaction was higher with the same amount of additions of NaOH and $NH_4OH$. It is believed that the formation mechanism of $Fe_3(PO_4)_2$ is quite different between NaOH and $NH_4OH$. Further investigation on this mechanism is needed. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and the pH value was measured by pH-Meter.

Precipitation Hardening by Holding After Simulated Complete Firing in a Metal-Ceramic Alloy of Pd-Au-Ag-Sn System (금속-세라믹용 Pd-Au-Ag-Sn계 합금의 모의소성 후 계류에 따른 석출경화)

  • Kim, Min-Jung;Shin, Hye-Jung;Kwon, Yong-Hoon;Kim, Hyung-Il;Seol, Hyo-Joung
    • Korean Journal of Dental Materials
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    • v.43 no.4
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    • pp.343-349
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    • 2016
  • This experiment was carried out to examine whether the post-firing heat treatment is effective in increasing the hardness of metal-ceramic alloy of the Pd-Au-Ag-Sn system. Precipitation hardening by holding at $600^{\circ}C$ after simulated complete porcelain firing in a metal-ceramic alloy of the Pd-Au-Ag-Sn system was examined by observing the change in hardness, crystal structure, and microstructure using a hardness test, X-ray diffraction (XRD), and field emission scanning electron microscopy (FE-SEM). The hardness of the alloy increased apparently by holding the specimen at $600^{\circ}C$ for 30 min after simulated complete porcelain firing. The formation of fine grain interior precipitates during holding at $600^{\circ}C$ caused the formation of lattice strain in the grain interior, resulting in apparent hardening. The faster cooling rate (stage 0) during simulated complete porcelain firing resulted in more effective precipitation hardening during holding at $600^{\circ}C$. From the above results, an appropriate post-firing heat treatment, such as holding at $600^{\circ}C$ for 30 min after complete porcelain firing may increase the durability of metal-ceramic prostheses composed of Pd-Au-Ag-Sn alloy.

Effect of Hollow Sphere Size on Heat Shield Properties of hollow TiO2/polyacrylate Composites (중공구의 크기에 의한 hollow TiO2/polyacrylate 복합체의 열차단 특성)

  • Kim, Jong Seok
    • Applied Chemistry for Engineering
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    • v.32 no.6
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    • pp.690-694
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    • 2021
  • Carbon spheres (CS) were fabricated using glucose as a precursor in the hydrothermal method. Hollow TiO2 (H-TiO2) spheres with 200 nm, 500 nm, and 1,200 nm were synthesized by CS/TiO2 core-shell particles via a sol-gel and calcination method. H-TiO2 spheres with nano and micron sizes were characterized using FE-SEM, HR-TEM, and X-ray diffraction. The CIE color coordinate, solar reflectance, and heat shield temperatures of H-TiO2/polyacrylate (PA) composite film were investigated using a UV-Vis-NIR spectrometer and homemade heat insulation temperature measuring device. H-TiO2/PA composites exhibit excellent thermal insulation since the hollow structure filled with dry air has low thermal conductivity and near infrared light reflecting performance. The thermal insulation increased with increasing the hollow sphere (HS) size on H-TiO2/PA composites. The PA composite film mixed with H-TiO2 filled with 1200 nm HS reduced the heat shield temperature by 26 ℃ compared to that of the transparent glass counterpart.

Behavior of Oxidative Precipitation of High-Arsenic (III) Solution Utilizing Activated Carbon with Air Injection (공기와 활성탄 병용에 의한 용액 중 고농도 3가 비소의 산화-침전 거동 연구)

  • Kim, Rina;Kim, Gahee;Kim, Kwanho;You, Kwang-suk
    • Resources Recycling
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    • v.30 no.4
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    • pp.11-19
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    • 2021
  • Arsenic (As) oxidation followed by precipitation from a high-As(III)-containing leaching solution derived from a sulfidic ore was investigated in this study to remove aqueous As from the solution using activated carbon (AC) with air injection as an oxidant. To obtain the initial leaching solution, a domestic sulfidic ore was leached in a sulfuric acid solution at pH 1 and 50℃ for 95 h, and approximately 7 g/L of Fe and 3 g/L of As were leached out. To determine the effect of the oxidative reaction utilizing AC with air injection, the leaching solution was tested under the following five oxidative conditions at an initial pH of 1 and 90℃ for 72 h: air-only injection; air injection with 1, 5, and 10 w/v% of AC addition; and H2O2 addition. The tests in the presence of both air and AC revealed that the oxidation kinetics and As removal were improved by the reaction between the metallic species and the surface group formed on the AC surface. In addition, the greater the amount of AC added, the better was the reaction efficiency, removing 93-94% of As with more than 5 w/v% of AC addition. Finally, X-ray diffraction analysis confirmed that the precipitate formed from the oxidative reaction was scorodite (FeAsO4·2H2O).