• Title/Summary/Keyword: Powder Morphology

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Effect of Core Morphology on the Decomposition of CCI₄ over the Surface of Core/Shell Structured Fe₂O₃/MgO Composite Metal Oxides

  • 김해진;강진;박동곤;권호진;Kenneth J. Klabunde
    • Bulletin of the Korean Chemical Society
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    • v.18 no.8
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    • pp.831-840
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    • 1997
  • Core/shell structured composite metal oxides of Fe2O3/MgO were prepared by thermal decomposition of Fe(acac)3 adsorbed on the surface of MgO cores. The morphology of the composites conformed to that of the MgO used as the cores. Broad powder X-ray diffraction peaks shifted toward larger d, large BET surface area (∼350 m2/g), and the size of crystalline domains in nano range (4 nm), all corroborate to the nanocrystallinity of the Fe2O3/MgO composite which was prepared by using nanocrystalline MgO as the core. By use of microcrystalline MgO as the core, microcrystalline Fe2O3/MgO composite was prepared, and it had small BET surface area of less than 35 m2/g. AFM measurements on nanocrystalline Fe2O3/MgO showed a collection of spherical aggregates (∼80 nm dia) with a very rough surface. On the contrary, microcrystalline Fe2O3/MgO was a collection of plate-like flat crystallites with a smooth surface. The nitrogen adsorption-desorption behavior indicated that microcrystalline Fe2O3/MgO was nonporous, whereas nanocrystalline Fe2O3/MgO was mesoporous. Bimodal distribution of the pore size became unimodal as the layer of Fe2O3 was applied to nanocrystalline MgO. The macropores in a wide distribution which the nanocrystalline MgO had were absent in the nanocrystalline Fe2O3/MgO. The decomposition of CCl4 was largily enhanced by the overlayer of Fe2O3 on nanocrystalline MgO making the reaction between nanocrystalline Fe2O3/MgO and CCl4 be nearly stoichiometric. The reaction products were environmentally benign MgCl2 and CO2. Such an enhancement was not attainable with the microcrystalline samples. Even for the nanocrystalline MgO, the enhancement was not attained, if not with the Fe2O3 layer. Without the layer of Fe2O3, it was observed that the nanocrystalline domain of the MgO transformed into microcrystalline one as the decomposition of CCl4 proceeded on its surface. It appeared that the layer of Fe2O3 on the particles of nanocrystalline Fe2O3/MgO blocked the transformation of the nanocrystalline domain into microcrystalline one. Therefore, in order to attain stoichiometric reaction between CCl4 and Fe2O3/MgO core/shell structured composite metal oxide, the morphology of the core MgO has to be nanocrystalline, and also the nanocrystalline domains has to be sustained until the core was exhausted into MgCl2.

Preparation of $Pb(Sc_{1/2}Nb_{1/2})O_3$ powders by the molten salt synthesis method (용융염 합성법에 의한 $Pb(Sc_{1/2}Nb_{1/2})O_3$ 분말의 제조)

  • 박경봉
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.400-405
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    • 1997
  • Lead scandium niobate powders were prepared by a molten salt synthesis method using KCl as a flux. Variations in phase formation and particle morphology were investigated for the temperature range $700^{\circ}C$ to $850^{\circ}C$. Pure $Pb(Sc_{1/2}Nb_{1/2})O_3$ perovskite phase was formed at $850^{\circ}C$ after 2hrs and the average particle size of powder was below 0.5 $\mu\textrm{m}$. The results are discussed with respect to DTA, X-ray diffraction, and microstructural characterization data.

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Nickel Oxide Nano-Flake Films Synthesized by Chemical Bath Deposition for Electrochemical Capacitors (CBD(Chemical Bath Deposition) 법으로 제조된 전기화학식 캐패시터용 NiO 나노박편 필름)

  • Kim, Young-Ha;Park, Soo-Jin
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.163.2-163.2
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    • 2010
  • In this work, nano-flake shaped nickel oxide (NiO) films were synthesized by chemical bath deposition technique for electrochemical capacitors. The deposition was carried out for 1 and 2 h at room temperature using nickel foam as the substrate and the current collector. The structure and morphology of prepared NiO film were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). And, electrochemical properties were characterized by cyclic voltammetry, galvanostatic charge-discharge, and AC impedence measurement. It was found that the NiO film was constructed by many interconnected NiO nano-flakes which arranged vertically to the substrate, forming a net-like structure with large pores. The open macropores may facilitate the electrolyte penetration and ion migration, resulted in the utilization of nickel oxide due to the increased surface area for electrochemical reactions. Furthermore, it was found that the deposition onto nickel foam as substrate and curent collector led to decrease of the ion transfer resistance so that its specific capacitance of a NiO film had high value than NiO nano flake powder.

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Reinvestigation of Dion-Jacobson Phases CsCa2Nb2MO9 (M = Fe and Al)

  • Hong, Young-Sik
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.853-856
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    • 2006
  • Dion-Jacobson phases $CsCa_2Nb_2FeO_9$ and $CsCa_2Nb_2AlO_9$ were reinvestigated by the Rietveld analysis of powder X-ray diffraction (XRD) method, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). These nominal compounds, previously known as the oxygen-deficient layered perovskites with the sequences of $NbO_6-MO_4-NbO_6$ in tripled slab, in fact, were mixed phases of n = 3 Dion-Jacobson phases and impurities such as $Ca_2NbFeO_6$ and $Ca_3Al_2O_6$. The difference of morphology and chemical in-homogeneity between Dion-Jacobson phases and impurities could be clearly identified by scanning electron microscopy with energy-dispersive X-ray spectroscopy. The chemical composition of $CsCa_2Nb_2FeO_9$ was calculated into $Cs_{0.59}Ca_{2.64}Nb_{2.92}Fe_{0.81}$ in small agglomerate crystals and $Cs_{0.95}Ca_{1.97}Nb_{3.08}Fe_{0.15}$ in long plate-like crystals.

Synthesis of Nanocrystalline TiO2 by Sol-Gel Combustion Hybrid Method and Its Application to Dye Solar Cells

  • Han, Chi-Hwan;Lee, Hak-Soo;Han, Sang-Do
    • Bulletin of the Korean Chemical Society
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    • v.29 no.8
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    • pp.1495-1498
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    • 2008
  • $TiO_2$ nanopowders were synthesized by new sol-gel combustion hybrid method using acetylene black as a fuel. The dried gels exhibited autocatalytic combustion behaviour. $TiO_2$ nanopowders with an anatase structure and a narrow size distribution were obtained at 400-600 ${^{\circ}C}$. Their crystal structures were examined by powder Xray diffraction (XRD) and their morphology and crystal size were investigated by scanning electron microscopy (SEM). The crystal size of the nanopowders was found to be in the range of 15-20 nm. $TiO_2$ powders synthesized at 500 ${^{\circ}C}$ and 600 ${^{\circ}C}$ were applied to a dye solar cell. An efficiency of 5.2% for the conversion of solar energy to electricity ($J_{sc}$ = 11.79 mA/$cm^2$, $V_{oc}$ = 0.73 V, and FF = 0.58) was obtained for an AM 1.5 irradiation (100 mW/$cm^2$) using the $TiO_2$ nanopowder synthesized by the sol-gel combustion hybrid method at 500 ${^{\circ}C}$.

VLS growth of ZrO2 nanowhiskers using CVD method

  • Baek, Min-Gi;Park, Si-Jeong;Jeong, Jin-Hwan;Choe, Du-Jin
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.149-149
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    • 2016
  • Ceramic is widely known material due to its outstanding mechanical property. Besides, Zirconia(ZrO2) has a low thermal conductivity so it is advantage in a heat insulation. Because of these superior properties, ZrO2 is attracted to many fields using ultra high temperature for example vehicle engines, aerospace industry, turbine, nuclear system and so on. However brittle fracture is a disadvantage of the ZrO2. In order to overcome this problem, we can make the ceramic materials to the forms of ceramic nanoparticles, ceramic nanowhiskers and these forms can be used to an agent of composite materials. In this work, we selected Au catalyzed Vapor-Liquid-Solid mechanism to synthesize ZrO2 nanowhiskers. The ZrO2 whiskers are grown through Hot-wall Chemical Vapor Deposition(Hot wall CVD) using ZrCl4 as a powder source and Au film as a catalyst. This Hot wall CVD method is known to comparatively cost effective. The synthesis condition is a temperature of $1100^{\circ}C$, a pressure of 760torr(1atm) and carrier gas(Ar) flow of 500sccm. To observe the morphology of ZrO2 scanning electron microscopy is used and to identify the crystal structure x-ray diffraction is used.

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Transmission Electron Microscope Sampling Method for Three-Dimensional Structure Analysis of Two-Dimensional Soft Materials

  • Lee, Sang-Gil;Lee, Ji-Hyun;Yoo, Seung Jo;Datta, Suvo Jit;Hwang, In-Chul;Yoon, Kyung-Byung;Kim, Jin-Gyu
    • Applied Microscopy
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    • v.45 no.4
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    • pp.203-207
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    • 2015
  • Sample preparation is very important for crystal structure analysis of novel nanostructured materials in electron microscopy. Generally, a grid dispersion method has been used as transmission electron microscope (TEM) sampling method of nano-powder samples. However, it is difficult to obtain the cross-sectional information for the tabular-structured materials. In order to solve this problem, we have attempted a new sample preparation method using focused ion beam. Base on this approach, it was possible to successfully obtain the electron diffraction patterns and high-resolution TEM images of the cross-section of tabular structure. Finally, we were able to obtain three-dimensional crystallographic information of novel zeolite nano-crystal of the tabular morphology by applying the new sample preparation technique.

Synthesis and luminescence properties of lanthanum oxides/hydroxides nanorod bundles

  • Hussain, Sk. Khaja;Raju, G. Seeta Rama;Yu, Jae Su
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.171.2-171.2
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    • 2015
  • Nowadays, trivalent rare-earth ($RE^{3+}$) ions activated metal oxides have been proved to be excellent host materials due to their various applications. Facile wet-chemical technique have been considered as the best synthetic route due its intensive interest in the preparation of nanostructures. Europium ion doped lanthanum hydroxide ($La(OH)_3:Eu^{3+}$) phosphors were synthesized by the facile wet chemical method using the hexamethylenetetramine (HMTA) as a mediated surfactant. The thermal behavior for the $La(OH)_3:Eu^{3+}$ phosphors was investigated by thermogravimetric and differential thermal analysis method. The morphological studies were measured by scanning electron microscope and transmission electron microscope measurements, indicating three-dimensional (3D) flower-like $La(OH)_3:Eu^{3+}$ nanorod bundles. After subsequent annealing process, the lanthanum oxide ($La_2O_3:Eu^{3+}$) phosphor exhibited similar kind of morphology. The synthesized $La(OH)_3:Eu^{3+}$ and $La_2O_3:Eu^{3+}$ samples were characterized by X-ray powder diffraction and Fourier transform infrared spectroscopy. Furthermore, photoluminescence and cathodoluminescence properties were studied in details.

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An Investigation of Debris Configuration and Melt-Water Interaction in Steam Explosion Experiments using $ZrO_2$ (원자로 물질의 $ZrO_2$를 이용한 증기폭발 실험에서 용융물 거동 및 데브리의 분포)

  • Song, J.H.;Kim, H.D.;Hong, S.W.;Park, I.K.;Shin, Y.S.;Min, B.T.;Chang, Y.J.
    • Proceedings of the KSME Conference
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    • 2001.06e
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    • pp.57-62
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    • 2001
  • Korea Atomic Energy Research Institute (KAERI) launched an intermediate scale steam explosion experiment named Test for Real cOrium Interaction with water (TROI) using reactor material to investigate whether the corium would lead to energetic steam explosion when interacted with cold water at low pressure. The melt-water interaction is confined in a pressure vessel with the multi-dimensional fuel and water pool geometry. The cold crucible technology, where the mixture of powder in a water-cooled cage is heated by high frequency induction, is employed. In this paper, results of the first series of tests ($TROI-1{\sim}5$) were discussed. The ZrO2 jets with 5kg mass and 5cm diameter were poured into the 67cm deep water pool at $30{\sim}95^{\circ}C$. Either spontaneous steam explosions or quenching was observed. The morphology of debris and pressure wave profiles clearly indicates the each case.

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Carbon rich fly ash and their nanostructures

  • Salah, Numan;Habib, Sami S.;Khan, Zishan H.;Alshahrie, Ahmed;Memic, Adnan;Al-ghamdi, Attieh A.
    • Carbon letters
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    • v.19
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    • pp.23-31
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    • 2016
  • Carbon rich fly ash was recently reported to have compositions that are ideal for use as a precursor and catalyst for carbon nanotube growth. This fly ash powder is mostly composed of pure carbon, predominantly present as sp2. In this work, the effect of sonication time on the morphology and structural properties of carbon rich fly ash particles is reported. The obtained results show that ultrasound treatment is an effective tool for producing ultrafine particles/fragments with higher porosity, which might be suitable for the adsorption of gasses. Moreover, carbon nanoparticles (CNPs) of this fly ash were produced in parallel using the ball milling technique, and were evaluated as reinforcements for epoxy based composites. These CNPs have almost spherical shapes with particle sizes of around 30 nm. They were found to have strong C=O carbonyl group bonds, which might be generated during the ball milling process. The tensile testing results of a fly ash CNP reinforced epoxy composite showed significant improvements in the mechanical properties, mainly in the stiffness of the polymer. The stiffness value was increased by around 23% of that of neat epoxy. These CNPs with chemically active groups might also be useful for other applications.