• Title/Summary/Keyword: pTEM

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X-선 회절분석을 이용한 일라이트-스멕타이트 기본입자의 적층성에 관한 연구

  • 강일모;문희수
    • Proceedings of the Mineralogical Society of Korea Conference
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    • 2003.05a
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    • pp.10-10
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    • 2003
  • 일라이트-스멕타이트 혼합층광물(I-S)은 열역학적으로 상호 대립적인 두 가지 모델로 이해되고 있다. 첫째, MacEwan 결정자 모델은 I-S를 5-20개의 스멕타이트와 일라이트 층으로 구성된 결정자로 해석한다. 이러한 모델은 분산과 재응집 과정을 기초로 하는 X-선 회절분석(XRD)에서 기인한 것으로 Reynolds의 XRD 모델과 동일하다. 둘째, 기본입자 모델은 I-S를 물리적으로 분리될 수 있는 최소 입자인 기본입자가 $c^{*-}$축 방향으로 응집된 응집체로 해석한다. 이러한 모델은 분산 과정을 기초로 하는 주사전자현미경(TEM) 관찰에서 기인한 모델이다. 강일모 등(2002)은 이 두 가지 모델을 비교함으로써 1< $N_{F}$<100/% $S_{XRD}$ ( $N_{F}$=평균 기본입자 층개수, %$S_{XRD}$=XRD 분석을 통하여 측정된 팽창성)을 도출하였다. 이 식은 기본입자모델과 Eberl & Srodon(1988)이 제시한 최대 팽창성(%$S_{MAX}$)을 동시에 해석할 수 있게 해준다. %$S_{MAX}$는 XRD 모델에서는 고려하지 않는 I-S 결정자 상$\cdot$하부에 존재하는 두 개의 0.5nm 규산염층을 하나의 스멕타이트 층으로 간주하여 얻어진 팽창성이다. Srodon et al.(1992)은 %$S_{MAX}$=100/ $N_{F}$을 제시하였으며, 강일모 등(2002)은 %$S_{MAX}$는 기하학적으로 기본입자가 무한적층을 하였을 때 관찰되는 %$S_{XRD}$와 동일함을 밝힌 바 있다. 만약, XRD 분석을 위한 시료 준비과정에서 I-S 결정자가 분산되었다가 재응집을 한다면, XRD에서 관찰되는 결과는 일차적으로 기본입자의 적층성에 영향을 받게 된다. 따라서, 기본 입자의 적층성은 XRD 분석을 이용하여 I-S 구조를 해석하는데 매우 중요한 요인이다. 본 연구는 기본입자의 적층성을 정량화하기 위해 %$S_{XRD}$=A/ $N_{F}$ (0$S_{MAX}$=100/ $N_{F}$로부터 얼마나 벗어나 있는가는 지시해 준다 금성산화산암복합체에서 산출되는 11개 I-S 시료와 14개의 Drits et al.(1998) 자료로부터 1nA=-0.14 $N_{F}$+4.7의 실험식을 도출할 수 있었으며, 기본입자의 적층성은 일차적으로 기본입자의 두께에 의해 영향을 받는 것으로 관찰되었다. Nadeau(1985)는 기본입자두께분포로부터 I-S 결정자의 팽창성을 측정하기 위하여 Ps=$\Sigma$p(N)/N을 제시하였다(Ps=스멕타이트 층 비율, N=기본 입자 층개수, p(N)=N의 확율). 그러나 위식은 실질적으로 %$S_{MAX}$를 제공해주기 때문에 %$S_{XRD}$를 유추하는데는 부적합하다. 본 연구는 이를 변형하여 Ps=$\Sigma$p(N)A(N)/N을 제시하였다(A(N)=N에 대한 A값). 위의 실험식을 사용하여 헝가리산 Zempleni 시료(15%$S_{XRD}$)의 기본입자분포로부터 %$S_{XRD}$를 계산한 결과, 16%$S_{XRD}$의 결과값을 얻을 수 있었다. 따라서, 본 연구에서 도출한 관계식들이 유효함을 확인할 수 있었다.계식들이 유효함을 확인할 수 있었다.

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Synthesis and magnetic properties of $Fe_3C$ fine particles ($Fe_3C$ 미립자의 제조와 자기적 특성)

  • Seo, Il-Gwon;Lee, Seung-Won;Gwon, Hyeok-Mu
    • Korean Journal of Materials Research
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    • v.3 no.6
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    • pp.652-660
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    • 1993
  • It was investigated to obtain the relationship between magnetic properties and conditions of forming $Fe_{3}C$ single phase from acicular goethite by heat treatment under the atmosphere of CO and $N_{2}$ mixed gas. X-ray analyses, TEM and VSM measurements were imployed for the characteristics of the carbide. Acicular goethite was sinthesized under proper process parameters. $Fe_{3}C$ single phase was obtained above $550^{\circ}C$, 60min. and $Fe_{5}C_2$ was formed with $Fe_{3}C$ below that temperature. The soturation magnetization of $Fe_{3}C$ single phase was about 100emu/g regardless of the reaction temperature. The coersive force and the ratio of Mr/Ms decreased respectively from 780 to 400 Oe. and from 0.35 to 0.13 with increasing reaction temperature.

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Preparation and Spectroscopic Characterization of Ilmenite-Type $CoTiO_3$ Nanoparticles

  • Zhou, Guo Wei;Lee, Don-Geun;Kim, Young-Hwan;Kim, Chang-Woo;Kang, Young-Soo
    • Bulletin of the Korean Chemical Society
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    • v.27 no.3
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    • pp.368-372
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    • 2006
  • The cobalt titanate, $CoTiO_3$ nanoparticles have been prepared by calcinations of precursor obtained from a mixture of $TiO_2$ and $Co(OH)_2$ in aqueous cetyltrimethylammonium bromide (CTAB) solution. The nanoparticles were investigated with X-ray powder diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and thermogravimetric/differential thermal analysis (TGA/DTA) to determine the crystallite size and the phase composition. The spectroscopic characterizations of these nanoparticles were also done with UV-Vis spectroscopy and FT-Raman spectroscopy. XRD patterns show that $CoTiO_3$ phase was formed at calcinations temperature above 600 ${^{\circ}C}$. UV-Vis absorption spectra indicate that the $CoTiO_3$ nanoparticles have significant red shift to the visible region (400-700 nm) with $\lambda_{max}$ = 500 nm compared to pure $TiO_2$ powder ($\lambda_{max}$ = 320 nm). The new absorption peaks (absorption at 696, 604, 520, 478,456, 383, 336, 267, 238, 208 $c m ^{-1}$), which were not appeared in FT-Raman spectra of P-25, also confirm the formation of Ti-O-Co bonds at above 600 ${^{\circ}C}$ and just not the mixtures of titanium dioxide with cobalt oxides.

Gold Nanoparticles Enhance the Anticancer Activity of Gallic Acid against Cholangiocarcinoma Cell Lines

  • Rattanata, Narintorn;Daduang, Sakda;Wongwattanakul, Molin;Leelayuwat, Chanvit;Limpaiboon, Temduang;Lekphrom, Ratsami;Sandee, Alisa;Boonsiri, Patcharee;Chio-Srichan, Sirinart;Daduang, Jureerut
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.16
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    • pp.7143-7147
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    • 2015
  • Gold nanoparticles (GNPs) were conjugated with gallic acid (GA) at various concentrations between 30 and $150{\mu}M$ and characterized using transmission electron microscopy (TEM) and UV-Vis spectroscopy (UV-VIS). The anticancer activities of the gallic acid-stabilized gold nanoparticles against well-differentiated (M213) and moderately differentiated (M214) adenocarcinomas were then determined using a neutral red assay. The GA mechanism of action was evaluated using Fourier transform infrared (FTIR) microspectroscopy. Distinctive features of the FTIR spectra between the control and GA-treated cells were confirmed by principal component analysis (PCA). The surface plasmon resonance spectra of the GNPs had a maximum absorption at 520 nm, whereas GNPs-GA shifted the maximum absorption values. In an in vitro study, the complexed GNPs-GA had an increased ability to inhibit the proliferation of cancer cells that was statistically significant (P<0.0001) in both M213 and M214 cells compared to GA alone, indicating that the anticancer activity of GA can be improved by conjugation with GNPs. Moreover, PCA revealed that exposure of the tested cells to GA resulted in significant changes in their cell membrane lipids and fatty acids, which may enhance the efficacy of this anticancer activity regarding apoptosis pathways.

Epitaxial Growth of Boron-doped Si Film using a Thin Large-grained Si Seed Layer for Thin-film Si Solar Cells

  • Kang, Seung Mo;Ahn, Kyung Min;Moon, Sun Hong;Ahn, Byung Tae
    • Current Photovoltaic Research
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    • v.2 no.1
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    • pp.1-7
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    • 2014
  • We developed a method of growing thin Si film at $600^{\circ}C$ by hot wire CVD using a very thin large-grained poly-Si seed layer for thin-film Si solar cells. The seed layer was prepared by crystallizing an amorphous Si film by vapor-induced crystallization using $AlCl_3$ vapor. The average grain size of the p-type epitaxial Si layer was about $20{\mu}m$ and crystallographic defects in the epitaxial layer were mainly low-angle grain boundaries and coincident-site lattice boundaries, which are special boundaries with less electrical activity. Moreover, with a decreasing in-situ boron doping time, the mis-orientation angle between grain boundaries and in-grain defects in epitaxial Si decreased. Due to fewer defects, the epitaxial Si film was high quality evidenced from Raman and TEM analysis. The highest mobility of $360cm^2/V{\cdot}s$ was achieved by decreasing the in-situ boron doping time. The performance of our preliminary thin-film solar cells with a single-side HIT structure and $CoSi_2$ back contact was poor. However, the result showed that the epitaxial Si film has considerable potential for improved performance with a reduced boron doping concentration.

Development of Wastewater Treatment System by Energy-Saving Photocatalyst Using Combination of Solar Light, UV Lamp and $TiO_2$ (태양광/자외선/이산화티타늄($TiO_2$)을 이용한 에너지 절약형 광촉매 반응 처리시스템 개발)

  • 김현용;양원호
    • Journal of Environmental Health Sciences
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    • v.29 no.1
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    • pp.51-61
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    • 2003
  • Pollution purification using titanium dioxide (TiO$_2$) photocatalyst has attracted a great deal of attention with increasing number of relent environmental problems. Currently, the application of TiO$_2$ photocatalyst has been focused on purification and treatment of waste water. However. the use of conventional TiO$_2$ powder photocatalyst results in disadvantage of stirring during the reaction and of separation after the reaction. And the usage of artificial UV lamp has made the cost of photocatalyst treatment system high. Consequently, we herein studied the pilot-scale design to aid in optimization of the energy-saving process for more through development and reactor design by solar light/UV lamp/ TiO$_2$system. In this study, we manufactured the TiO$_2$sol by sol-gel method. According to analysis by XRD, SEM and TEM, characterization of TiO$_2$ sol were nano-size (5-6 nm) and anatase type. Inorganic binder (SiO$_2$) was added to TiO$_2$ lot to be coated for support strongly, and support of ceramic bead was used to lower separation rate that of glass bead The influences were studied of various experimental parameters such as TiO$_2$ quantity, pH, flow rate. additives, pollutants concentration, climate condition and reflection plate by means of reaction time of the main chararteristics of the obtained materials. In water treatment system, variable realtor as solar light/ or UV lamp according to climate condition such as sunny and cloudy days treated the phenol and E-coli(Escherichia coli) effectively.

Modified Glassy Carbon Electrode with Silver Nanoparticles/Polyaniline/Reduced Graphene Oxide Nanocomposite for the Simultaneous Determination of Biocompounds in Biological Fluids

  • Ghanbari, Kh.;Moloudi, M.;Bonyadi, S.
    • Journal of Electrochemical Science and Technology
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    • v.10 no.4
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    • pp.361-372
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    • 2019
  • The silver nanoparticles/polyaniline/reduced graphene oxide nanocomposite modified glassy carbon electrode (Ag/PANI/RGO/GCE) was prepared by the electrochemical method. The Ag/PANI/RGO nanocomposite was characterized by transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, X-ray diffraction (XRD), and electrochemical impedance spectroscopy (ESI). Two electrochemical techniques namely differential pulse voltammetry (DPV) and cyclic voltammetry (CV) were used to the electrochemical behaviors investigation of ascorbic acid (AA), dopamine (DA), and uric acid (UA). The Ag/PANI/RGO/GCE exhibited remarkable electrocatalytic activity towards the oxidation reaction of AA, DA, and UA in Britton-Robinson (BR) solution (pH=4.0). Under the optimal conditions, the determinations of AA, DA, and UA were accomplished using DPV. AA-DA and DA-UA peak potential separations were 130 and 180 mV, respectively. For simultaneous detection, the linear response ranges were in the two concentration ranges of 0.05-0.8 mM and 2.0-16.0 mM with detection limit 0.412 μM (S/N = 3) for AA, 0.7-90.0 μM and 90.0-1000.0 μM with detection limit 0.023 μM (S/N = 3) for DA, and 0.8-70.0 μM and 70.0-1000.0 μM with detection limit 0.050 μM (S/N = 3) for UA. This modified electrode showed good sensitivity, selectivity, and stability with applied to determine AA, DA, and UA in human urine and drug.

Synthesis and Properties of Exfoliated Poly(methyl methacrylate-co-acrylonitrile)/Clay Nanocomposites via Emulsion Polymerization

  • Mingzhe Xu;Park, Yeong-Suk;Wang, Ki-Hyun;Kim, Jong-Hyun;Chung, In-Jae
    • Macromolecular Research
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    • v.11 no.6
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    • pp.410-417
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    • 2003
  • Poly(methyl methacrylate-co-acrylonitrile) [P(MMA-co-AN)]/Na-MMT nanocomposites were synthesized through emulsion polymerization with pristine Na-MMT. The nanocomposites were exfoliated up to 20 wt% content of pristine Na-MMT relative to the amount of MMA and AN, and exhibited enhanced storage moduli, E', relative to the neat copolymer. The exfoliated morphology of the nanocomposite was confirmed by XRD and TEM. 2-Acryla-mido-2-methyl-1-propane sulfonic acid (AMPS) widened the galleries between the clay layers before polymerization and facilitated the comonomers, penetration into the clay to create the exfoliated nanocomposites. The onset of the thermal decomposition of the nanocomposites shifted to a higher temperature as the clay content increased. By calculating areas of tan$\delta$ of the nanocomposites, we observed that the nanocomposites show more solid-like behavior as the clay content increases. The dynamic storage modulus and complex viscosity increased with clay content. The complex viscosity showed shear-thinning behavior as the clay content increased. The Young's moduli of the nano-composites are higher than that of the neat copolymer and they increase steadily as the silicate content increases, as a result of the exfoliated structure at high clay content.

Influence of particle size on sensing characteristics of hydrothermally treated nano-sized $SnO_2$ (수열합성법으로 제조한 나노 크기의 $SnO_2$ 입자 크기에 따른 반응 특성)

  • ;Anh-Hoa Bui
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.134-134
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    • 2003
  • SnO$_2$를 모물질로 하는 가스센서는 n형 산화물 반도체로서 공기중의 산소의 흡탈착 및 전자의 수수에 의해 전기전도도의 변화로 특정 가스를 감지한다. 지금까지 반도체식 가스센서의 모물질로 가장 많이 연구되어 왔지만 아직도 선택성, 안정성 등 여러 가지 문제를 안고 있다. 그리고 개선방안으로 귀금속 촉매의 첨가 및 입자의 크기의 조절 등이 흔히 연구되어 왔다. 따라서 본 연구에서는 순수한 SnO$_2$ 를 이용하여 소결 온도 및 입자 크기에 의한 영향을 CO가스 및 수분에 대한 감도, 반응 시간을 통해 알아보았다. 수열 합성 및 침전 법으로 나노 크기의 SnO$_2$ 분말을 합성하여 스크린 인쇄법으로 후막 가스센서를 제조하였다 침전법에서 SnCl$_4$에 암모니아수로 pH=10.5로 적정하여 SnO$_2$ 분말을 얻었다. 그리고 입자 크기를 조절하기 위해 수열 합성 시 autoclave 내의 수열처리 온도를 100, 150, 20$0^{\circ}C$로 조절하여 SnO$_2$ 분말을 제조하고 입자 크기와 성분분석을 위해 XRD, SEM, TEM, BET 측정을 하였다. 그 결과 침전법으로 제조한 입자의 크기는 20nm 정도였으며 수열 처리한 SnO$_2$ 입자는 10nm이하의 미세한 입자를 얻을 수 있었다. 수열 합성 시 온도가 높아질수록 더 작은 입자 크기를 얻을 수 있었고 600, 7()0, 80$0^{\circ}C$ 열처리 후 입자성장이 침전법에 의한 SnO$_2$ 분말보다 더 작게 일어났다. 이렇게 제조한 나노크기의 SnO$_2$ 분말을 이용하여 습도 및 CO 가스에 대한 그 특실을 평가하였다. CO 20ppm에 대하여 40%정도의 감도를 보였으며 입자가 작아질수록 높은 감도를 보이는 것을 확인 할 수 있었다. 반면 CO 가스와 반응 후 회복 시 입자 의기가 작아질수록 회복이 늦어짐을 알 수 있었다. 그리고 15$0^{\circ}C$에서 습도에 대한 반응 후 회복시간을 조사해보니 같은 결과를 얻을 수 있었다. 이것은 입자 필기가 작아질수록 많은 흡착 사이트를 제공함으로써 높은 감도를 가지지만 반면 다량의 흡착된 가스들이 탈착 하는데 더 많은 시간이 소요되었기 때문이다.

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Formation of Non-equilibrium Cu-Ta-Mo Alloy Powders by Mechanical Alloying (기계적 합금화법에 의한 비평형 Cu-Ta-Mo계 합금분말의 제조)

  • 이충효;이상진
    • Journal of Powder Materials
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    • v.6 no.4
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    • pp.314-319
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    • 1999
  • The solid state reaction by mechanical alloying(MA) generally proceeds by lowering the free energy as the result of a chemical reaction at the interface between the two adjacent layers. However, Lee et $al.^{1-5)}$ reported that a mixture of Cu and Ta, the combination of which is characterized by a positive heat of mixing of +2kJ/mol, could be amorphized by mechanical alloying. This implies that there exists an up-hill process to raise the free energy of a mixture of pure Cu and la to that of an amorphous phase. It is our aim to investigate to what extent the MA is capable of producing a non-equilibrium phase with increasing the heat of mixing. The system chosen was the ternary $Cu_{30}Ta_{ 70-x}Mo_ x$ (x=35, 10). The mechanical alloying was carried out using a Fritsch P-5 planetary mill under Ar gas atmosphere. The MA powders were characterized by the X-ray diffraction with Cu-K $\alpha$ radiation, thermal analysis, electron diffraction and TEM micrographs. In the case of x=35, where pure Cu powders were mixed with equal amount of pure Ta and Mo powders, we revealed the formation of bcc solid solution after 150 h milling but its gradual decomposition by releasing fcc-Cu when milling time exceeded 200 h. However, an amorphous phase was clearly formed when the Mo content was lowered to x=10. It is believed that the amorphization of ternary $Cu_{30}Ta_{60}Mo_{10}$ powders is essentially identical to the solid state amorphization process in binary $Cu_{30}Ta_{70}$ powders.

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