• Title/Summary/Keyword: Scanning transmission X-ray microscopy

Search Result 424, Processing Time 0.02 seconds

Ni0.5Zn0.4Cu0.1Fe2O4 Complex Ferrite Nanoparticles Synthesized by Chemical Coprecipitation Predicted by Thermodynamic Modeling

  • Kang, Bo-Sun;Park, Joo-Seok;Ahn, Jong-Pil;Kim, Kwang-Hyun;Tae, Ki-Sik;Lee, Hyun-Ju;Kim, Do-Kyung
    • Journal of the Korean Ceramic Society
    • /
    • v.50 no.3
    • /
    • pp.231-237
    • /
    • 2013
  • Thermodynamic modeling of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite system has been adopted as a rational approach to establish routes to better synthesis conditions for pure phase $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite. Quantitative analysis of the different reaction equilibria involved in the precipitation of $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ from aqueous solutions has been used to determine the optimum synthesis conditions. The spinel ferrites, such as magnetite and substitutes for magnetite, with the general formula $MFe_2O_4$, where M= $Fe^{2+}$, $Co^{2+}$, and $Ni^{2+}$ are prepared by coprecipitation of $Fe^{3+}$ and $M^{2+}$ ions with a stoichiometry of $M^{2+}/Fe^{3+}$= 0.5. The average particle size of the as synthesized $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$, measured by transmission electron microscopy (TEM), is 14.2 nm, with a standard deviation of 3.5 nm the size when calculated using X-ray diffraction (XRD) is 16 nm. When $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite is annealed at elevated temperature, larger grains are formed by the necking and mass transport between the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite nanoparticles. Thus, the grain sizes of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ gradually increase as heat treatment temperature increases. Based on the results of Thermogravimetric Analysis (TGA) and Differential Scanning Calorimeter (DSC) analysis, it is found that the hydroxyl groups on the surface of the as synthesized ferrite nanoparticles finally decompose to $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ crystal with heat treatment. The results of XRD and TEM confirmed the nanoscale dimensions and spinel structure of the samples.

Mineralogy and Biogeochemistry of Intertidal Flat Sediment, Muan, Chonnam, Korea (전남 무안 갯벌 퇴적물에 관한 광물학적 및 생지화학적 연구)

  • Park, Byung-No;Lee, Je-Hyun;Oh, Jong-Min;Lee, Seuug-Hee;Han, Ji-Hee;Kim, Yu-Mi;Seo, Hyun-Hee;Roh, Yul
    • Journal of the Mineralogical Society of Korea
    • /
    • v.20 no.1 s.51
    • /
    • pp.47-60
    • /
    • 2007
  • While sedimentological researches on Western coastal tidal flats of Korea have been much pelformed previously, mineralogical and biogeochemical studies are beginning to be studied. The objectives of this study were to investigate mineralogical characteritics of the inter-tidal flat sediments and to explore phase transformation of iron(oxyhydr)oxides and biomineralization by metal-reducing bacteria enriched from the inter-tidal flat sediments from Muan, Jeollanam-do, Korea. Inter-tidal flat sediment samples were collected in Chungkye-myun and Haeje-myun, Muan-gun, Jeollanam-do. Particle size analyses were performed using the pipette method and sedimentation method. The separates including sand, silt and clay fractions were examined by scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM), and X-ray diffiaction (XRD). After enriching the metal-.educing bacteria from the into,-tidal flat sediments, the bacteria were used to study phase transformation of the synthesized iron (oxyhydr)oxides and iron biomineralization using lactate or glucose as the electron donors and Fe(III)-containing iron oxides as the electron accepters. Mineralogical studies showed that the sediments of tidal flats in Chung]rye-myun and Haeje-myun consist of quartz, plagioclase, microcline, biotite, kaolinite and illite. Biogeochemical researches showed that the metal-reducing bacteria enriched from the inter-tidal flat sediments reduced reddish brown akaganeite and mineralized nanometer-sized black magnetite. The bacteria also reduced the reddish brown ferrihydrite into black amorphous phases and reduced the yellowish goethite into greenish with formation of nm-sized phases. These results indicate that microbial Fe(III) reduction may play one of important roles in iron and carbon biogeochemistry as well as iron biomineralization in subsurface environments.

Characterization of SiC nanowire Synthesized by Thermal CVD (열 화학기상증착법을 이용한 탄화규소 나노선의 합성 및 특성연구)

  • Jung, M.W.;Kim, M.K.;Song, W.;Jung, D.S.;Choi, W.C.;Park, C.J.
    • Journal of the Korean Vacuum Society
    • /
    • v.19 no.4
    • /
    • pp.307-313
    • /
    • 2010
  • One-dimensional cubic phase silicon carbide nanowires (${\beta}$-SiC NWs) were efficiently synthesized by thermal chemical vapor deposition (TCVD) with mixtures containing Si powders and nickel chloride hexahydrate $(NiCl_2{\cdot}6H_2O)$ in an alumina boat with a carbon source of methane $(CH_4)$ gas. SEM images are shown that the growth temperature (T) of $1,300^{\circ}C$ is not enough to synthesize the SiC NWs owing to insufficient thermal energy for melting down a Si powder and decomposing the methane gas. However, the SiC NWs could be synthesized at T>$1,300^{\circ}C$ and the most efficient temperature for growth of SiC NWs is T=$1,400^{\circ}C$. The synthesized SiC NWs have the diameter with an average range between 50~150 nm. Raman spectra clearly revealed that the synthesized SiC NWs are forming of a cubic phase (${\beta}$-SiC). Two distinct peaks at 795 and $970 cm^{-1}$ in Raman spectra of the synthesized SiC NWs at T=$1,400^{\circ}C$ represent the TO and LO mode of the bulk ${\beta}$-SiC, respectively. XRD spectra are also supported to the Raman spectra resulting in the strongest (111) peaks at $2{\Theta}=35.7^{\circ}$, which is the (111) plane peak position of 3C-SiC. Moreover, the gas flow rate of 300 sccm for methane is the optimal condition for synthesis of a large amount of ${\beta}$-SiC NW without producing the amorphous carbon structure shown at a high methane flow rate of 800 sccm. TEM images are shown two kinds of the synthesized ${\beta}$-SiC NWs structures. One is shown the defect-free ${\beta}$-SiC NWs with a (111) interplane distance of 0.25 nm, and the other is the stacking-faulted ${\beta}$-SiC NWs. Also, TEM images exhibited that two distinct SiC NWs are uniformly covered with $SiO_2$ layer with a thickness of less 2 nm.

Solvothermal Preparation of Nanocrystalline TiO2 Using Alcohol-water Mixed Solvent (알코올-물 혼합용액을 이용하는 Solvothermal 법에 의한 나노크기의 TiO2 제조)

  • Lee, Sang Geun;Park, Seong Soo;Hong, Seong Soo;Park, Jong Myung;Lee, Seung Ho;Kim, Dae Sung;Lee, Gun Dae
    • Applied Chemistry for Engineering
    • /
    • v.22 no.6
    • /
    • pp.685-690
    • /
    • 2011
  • In this study, a solvothermal reaction to prepare nanocrystalline titania was carried out using $TiCl_4$ and mixed solvents of alcohol and water. The effects of the type and the composition of alcohol on the crystal structure and agglomeration of final $TiO_2$ products were investigated. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) as well as scanning electron microscopy (SEM). In the solvothermal reaction using the n-butanol solutions with different volume ratios of n-butanol/water (100/0, 75/25, 50/50, 25/75, 0/100), the extent of agglomeration of obtained rutile $TiO_2$ was found to change with the volume ratio of n-butanol/water, and the n-butanol/water ratio of 75/25 revealed the best result for the preparation of well-dispersed nanocrystalline $TiO_2$ powders. The crystal phase of $TiO_2$ prepared through the solvothermal reaction changed with the type of alcohol in solvent (alcohol/water = 75/25). $TiO_2$ products obtained with the aqueous solutions of methanol, ethanol and isopropanol have an anatase phase, while that with n-butanol has a rutile phase. The results showed that, in the solvothermal reaction using both $TiCl_4$ as a starting material and the alcohol-water mixed solvents without any other additive, the enhancement of dispersion and control of crystal structure of $TiO_2$ products can be feasible by simply varying the composition and type of alcohol in the mixed solvents.