• Title/Summary/Keyword: surface phase transition

Search Result 250, Processing Time 0.024 seconds

A Novel Acid-Base Catalyzed Sol-Gel Synthesis of Highly Active Mesoporous TiO2 Photocatalysts

  • Khan, Romana;Kim, Sun-Woo;Kim, Tae-Jeong;Lee, Hyo-Sun
    • Bulletin of the Korean Chemical Society
    • /
    • v.28 no.11
    • /
    • pp.1951-1957
    • /
    • 2007
  • A new synthetic strategy based on the acid-base catalyzed sol-gel method was developed for the preparation of a series of mesoporous TiO2 nanoparticles. A key feature of the method involves a gradual change in pH (0.8- 9) during the sol-gel transition, which guarantees easy introduction of mesoporosity without relying on the well-established sonochemical or template approach. In addition, this method leads to the exclusive formation of the anatase phase stable enough to the calcination temperature up to 600 oC. The physicochemical properties of the particles in the series were characterized by various spectroscopic and analytical techniques such as wide-angle XRD, SAXRD, BET surface area, FE-SEM, TEM, FT-IR, TGA, and XPS. The photocatalytic efficiency of these materials was investigated for the oxidation of toluene under UV-irradiation. All but T-ad in the series exhibited high photocatalytic activity pushing the reaction into completion within 3 h. The reaction followed the first order kinetics, and the rate reaches as high as 3.9 × 10?2/min which exceeds the one with the commercially available Degussa P-25 by a factor of 3.2. When comparison is made among the catalysts, the reactivity increases with increase in the calcination temperature which in turn increases the crystallinity of the anatase phase, thus revealing the following rate orders: T-3 < T-4 < T-5 < T-6.

Growth of Spinel CoMn2O4 Thin Films and Post-growth Annealing Effects on Their Physical Properties (CoMn2O4 스피넬 박막의 합성과 후열처리가 박막의 물리적 특성에 미치는 영향)

  • Kim, D.R.;Kim, J.K.;Yoon, S.W.;Song, J.H.
    • Journal of the Korean Magnetics Society
    • /
    • v.25 no.5
    • /
    • pp.144-148
    • /
    • 2015
  • We grew spinel structured $CoMn_2O_4$ thin films and have studied post-growth annealing effects on their physical properties. After post-growth annealing at $700^{\circ}C$ that is lower than the growth temperature ($720^{\circ}C$), crystal structure became cleared accompanying a change of surface structure. In the temperature dependences of magnetization, phase transitions were observed at ~100 K for both before and after post-growth treated samples which were not observed for the bulk. For both samples, ferromagnetic behaviors were observed above 100 K while it turned to ferrimagnetism at low temperature below 100 K. In particular, the ferrimagnetic behavior became strong after the post-growth treatment. These results indicate that the post-growth annealing process plays an important role in determining the physical properties of spinel $CoMn_2O_4$ thin film.

Change of Electrochemical Characteristics Due to the Fe Doping in Lithium Manganese Oxide Electrode

  • Ju Jeh Beck;Kang Tae Young;Cho Sung Jin;Sohn Tae Won
    • Journal of the Korean Electrochemical Society
    • /
    • v.7 no.3
    • /
    • pp.131-137
    • /
    • 2004
  • Sol-gel method which provides better electrochemical and physiochemical properties compared to the solid-state method was used to synthesize the material of $LiFe_yMn_{2-y}O_4$. Fe was substituted to increase the structural stability so that the effects of the substitution amount and sintering temperature were analyzed. XRD was used for the structural analysis of produced material, which in turn, showed the same cubic spinel structure as $LiMn_2O_4$ despite the substitution of $Fe^{3+}$. During the synthesis of $LiFe_yMn_{2-y}O_4$, as the sintering temperature and the doping amount of Fe(y=0.05, 0.1, 0.2)were increased, grain growth proceeded which in turn, showed a high crystalline and a large grain size, certain morphology with narrow specific surface area and large pore volume distribution was observed. In order to examine the ability for the practical use of the battery, charge-discharge tests were undertaken. When the substitution amount of $Fe^{3+}\;into\;LiMn_2O_4$ increased, the initial discharge capacity showed a tendency to decrease within the region of $3.0\~4.2V$ but when charge-discharge processes were repeated, other capacity maintenance properties turned out to be outstanding. In addition, when the sintering temperature was $800\~850^{\circ}C$, the initial capacity was small but showed very stable cycle performance. According to EVS(electrochemical voltage spectroscopy) test, $LiFe_yMn_{2-y}O_4(y=0,\;0.05,\;0.1,\;0.2)$ showed two plateau region and the typical peaks of manganese spinel structure when the substitution amount of $Fe^{3+}$ increased, the peak value at about 4.15V during the charge-discharge process showed a tendency to decrease. From the previous results, the local distortion due to the biphase within the region near 4.15V during the lithium extraction gave a phase transition to a more suitable single phase. When the transition was derived, the discharge capacity decreased. However the cycle performance showed an outstanding result.

HRTEM Observations on the Modulated Structure in Pseudo-brookite-type Compound, $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ (HRTEM에 의한 pseudo-brookite 형 화합물$(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$에서의 변조구조 관찰)

  • Lee, Hwack-Joo;Park, Hyun-Min;Cho, Yang-Koo;Ryu, Hyun;Nahm, Sahn;Bando, Y.
    • Applied Microscopy
    • /
    • v.29 no.1
    • /
    • pp.95-103
    • /
    • 1999
  • Microstructural observations on the pseudo-brookite $MgTi_2O_5$ and the similar type of $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ were carried out using a top-entry HRTEM working at 200 kV. The modulated structures were found in $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$, however, not in $MgTi_2O_5$. The electron diffraction patterns of sublattice in $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ are quite similar to those of pseudo-brookite $MgTi_2O_5$. but the complicated superlattice reflections are present in the diffraction patterns. Four types of modulations have been found. The periodicities for the modulated structure are found to be 3.63 nm, 0.79 nm and 0.64 nm along [220] direction, and 0.81 nm along [420] direction. The phase transition from the modulated structure to the unmodulated one was also observed in situ due to the electron beam irradiation reversibly. Further damage by the electron beam made the crystal to be fragmented into many small crystals with the formation of the voids at the kinks in ledged structure of the surface. The anisotropic arrangements of In and O atoms in $(In_{0.36}Zn_{1.09})Ti_2O_{5.64}$ might cause the compound to be unstable under the electron beam.

  • PDF

Firing Condition, Source Area and Quantitative Analysis of Plain Coarse Pottery from the Unjeonri Bronze Age Relic Site, Cheonan, Korea (천안 운전리 청동기 유적지에서 출토된 무문토기의 정량분석, 산지 및 소성조건)

  • Choi, Seok-Won;Lee, Chan-Hee;Oh, Kuy-Jin;Lee, Hyo-Min;Lee, Myeong-Seong
    • Korean Journal of Heritage: History & Science
    • /
    • v.36
    • /
    • pp.267-297
    • /
    • 2003
  • The plain coarse pottery from the Unjeonri Bronze Age relic sites in the Cheonan, Korea were studied on the basis of clay mineralogy, geochemistry and archaegeological interpretations. For the research, the potteries are utilized at the analysis for 6 pieces of plain coarse potteries. Color of the these potteries are mainly light brown, partly shows the yellowish brown to reddish brown. The interior, surface and inside of the pottery appear as different colors in any cases. Original source materials making the Unjeonri potteries are used of mainly sandy clay soil with extreme coarse grained irregularly quartz and feldspar. The magnetic susceptibility of the Unjeonri pottery range from 0.20 to 1.20. And the Unjeonri soil's magnetic susceptibility agree almost with 0.20 to 1.30. In the same magnetization of soil and pottery, the results revealed that the Unjeonri soil and low material of pottery are same produced by identical source materials. The Unjeonri potteries and soil are very similar patterns with all characteristics of soil mineralogy, geochemical evolution trend. The result seems to be same relationships between the behavior and enrichment patterns on the basis of a compatible and a incompatible elements. Consequently, the Unjeonri potteries suggest that made the soil to be distributed in the circumstance of the relic sites as the raw material are high in a greater part. In the Unjeonri soil, the kaolinite is common occurred minerals. However, in the Unjeonri pottery, the kaolinite was not detected in all broken pieces. The kaolinite was presumed to destroy crystal structure during the firing processes of over $550^{\circ}C$. The quartz is phase transition from ${\alpha}$-quartz to ${\beta}$-quartz at $573^{\circ}C$, but the Unjeonri pottery did not investigated any phase transition evidences of quartz. The chorite was detected within the mostly potteries and soils. As the results, the Unjeonri potteries can be interpreted by not experiencing a firing temperature over $800^{\circ}C$. The colloidal and cementing materials between the quartz and low materials during the heating did not exist in the internal part of the potteries. An any secondary compounds by heating does not appear within the crack to happen during the dry of the pottery. The hyphae group are kept as it is with the root tissue of an organic matters to live in the swampy land. In the syntheses of all results, the general firing condition to bake and make the Unjeonri pottery is presumed from $550^{\circ}C$ to $800^{\circ}C$. However, the firing condition making the Unjeonri pottery can be different firing temperature partially in one pottery. Even, the some part of the pottery does not take a direct influence on the fire.

Effect of composition on the structural and thermal properties of TiZrN thin film (TiZrN 박막의 조성이 구조적 특성 및 열적 특성에 미치는 영향)

  • Choi, Byoung Su;Um, Ji Hun;Seok, Min Jun;Lee, Byeong Woo;Kim, Jin Kon;Cho, Hyun
    • Journal of the Korean Crystal Growth and Crystal Technology
    • /
    • v.31 no.1
    • /
    • pp.37-42
    • /
    • 2021
  • The effect of chemical composition on the structural and thermal properties of TiZrN thin films was studied. As the Zr fraction in the deposited TixZr1-xN (x = 0.87, 0.82, 0.7, 0.6, and 0.28) increased, microstructural changes consisted of reduction in the grain size and a gradual transition from columnar structure to granular structure were observed. In addition, it was also confirmed that a gradual crystal phase transition from TiN to TiZrN has occurred as the Zr fraction increased up to 0.4. After heat treatment at 900℃, Ti0.82Zr0.18N and Ti0.7Zr0.3N layers were converted to a form in which rutile phase TiO2 and TiZrO4 oxides coexist, while Ti0.6Zr0.4N layer was converted to TiZrO4 oxide. Among the five compositions of TiZrN films, the Ti0.6Zr0.4N showed the best high temperature stability and produced a significant enhancement in the thermal oxidation resistance of Inconel 617 through suppressing the surface diffusion of Cr caused by thermal oxidation of the Inconel 617 substrate.

Surface Texture Changes due to the Oxidation of Pyrite by Acidithiobacillus Ferrooxidans (애시디싸이오바실러스 페로악시댄스에 의한 황철석 산화에 따른 표면 조직의 변화)

  • Yu, Jae-Young;Koh, Hyun-Jin;Song, Hong-Gyu
    • Journal of the Mineralogical Society of Korea
    • /
    • v.24 no.3
    • /
    • pp.235-244
    • /
    • 2011
  • A batch experiment of pyrite oxidation was performed and the surfaces of the reacted pyrite were regularly observed with the scanning electron microscope (SEM) together with the chemical compositions of the solution to help understand the oxidation mechanisms of pyrite by Acidithiobacillus ferrooxidans (Af). The dissolved Fe concentrations clearly indicated that Af experiences the lag and then exponential growth phase. An Af cell was observed to be attached to the surface of pyrite during the lag, implying that a direct leaching by the microbe really happens for the period. It is not certain, however, whether the main mechanism of pyrite oxidation during that time was the direct leaching or not, because there were just a few cells confirmed to be attached and most of the dissolved Fe was Fe(III). The dissolved Fe concentration stayed almost constant from the mid-lag phase to just before the onset of the exponential phase, suggesting that AI needs an adaptation time to switch its oxidation mechanism from one to the other whichever it is during that stage of growth. The moment of Af's cell division was observed by SEM on the surface of pyrite during the lag phase. The corrosion outline around the dividing cell was quite similar to the shape of the cell itself, which implies that the rate of the microbial oxidation is very uneven and the rate when the cell metabolizes should be much faster than that calculated from the concentration variation of the dissolved Fe. The number of etch holes by Af is much higher on the inoculated surfaces, indicating the average rate of pyrite oxidation is also much faster than that of abiotic oxidation. The microbial etch holes on pyrite surface are small and deep, which may influence the transition of the growth phases of Af from lag to exponential.

The Phase-Shift Method for the Langmuir Adsorption Isotherms of Electroadsorbed Hydrogens for the Cathodic H2 Evolution Reactions at the Poly-Pt Electrode Interfaces (다결정 Pt 전극계면에서 음극 H2 발생반응을 위한 전착된 수소의 Langmuir 흡착등온식에 관한 위상이동 방법)

  • Chun, Jang H.;Jeon, Sang K.;Lee, Jae H.
    • Journal of the Korean Electrochemical Society
    • /
    • v.5 no.3
    • /
    • pp.131-142
    • /
    • 2002
  • The Langmuir adsorption isotherms of the under-potentially deposited hydrogen (UPD H) and the over-potentially deposited hydrogen (OPD H) at the poly-Pt/0.5M $H_2SO_4$ and 0.5 M LiOH aqueous electrolyte interfaces have been studied using cyclic voltammetric and ac impedance techniques. The behavior of the phase shift $(0^{\circ}{\leq}{-\phi}{\leq}90^{\circ})$ for the optimum intermediate frequency corresponds well to that of the fractional surface coverage $(1{\geq}{\theta}{\geq}0)$ at the interfaces. The phase-shift method, i.e., the phase-shift profile $({-\phi}\;vs.\;E)$ for the optimum intermediate frequency, can be used as a new electrochemical method to determine the Langmuir adsorption isotherms $({\theta}\;vs.\;E)$ of the UPD H and the OPD H for the cathodic $H_2$ evolution reactions at the interfaces. At the poly-Pt/0.5M $H_2SO_4$ aqueous electrolyte interface, the equilibrium constant (K) and the standard free energy $({\Delta}G_{ads})$ of the OPD H are $2.1\times10^{-4}$ and 21.0kJ/mol, respectively. At the poly-Pt/0.5M LiOH aqueous electrolyte interface, K transits from 2.7(UPD H) to $6.2\times10^{-6}$ (OPD H) depending on the cathode potential (E) and vice versa. Similarly, ${\Delta}G_{ads}$ transits from -2.5kJ/mol (UPD H) to 29.7kJ/mol (OPD H) depending on I and vice versa. The transition of K and ${\Delta}G_{ads}$ is attributed to the two distinct adsorption sites of the UPD H and the OPD H on the poly-Pt surface. The UPD H and the OPD H on the poly-Pt surface are the independent processes depending on the H adsorption sites themselves rather than the sequential processes for the cathodic $H_2$ evolution reactions. The criterion of the UPD H and the OPD H is the H adsorption sites and processes rather than the $H_2$ evolution reactions and potentials. The poly-Pt wire electrode is more efficient and useful than the Pt(100) disc electrode for the cathodic $H_2$ evolution reactions in the aqueous electrolytes. The phase-shift method is well complementary to the thermodynamic method rather than conflicting.

Support Effect of Arc Plasma Deposited Pt Nanoparticles/TiO2 Substrate on Catalytic Activity of CO Oxidation

  • Qadir, Kamran;Kim, Sang Hoon;Kim, Sun Mi;Ha, Heonphil;Park, Jeong Young
    • Proceedings of the Korean Vacuum Society Conference
    • /
    • 2013.02a
    • /
    • pp.261-261
    • /
    • 2013
  • The smart design of nanocatalysts can improve the catalytic activity of transition metals on reducible oxide supports, such as titania, via strong metal-support interactions. In this work, we investigatedtwo-dimensional Pt nanoparticle/titania catalytic systems under the CO oxidation reaction. Arc plasma deposition (APD) and metal impregnation techniques were employed to achieve Pt nanoparticle deposition on titania supports, which were prepared by multitarget sputtering and sol-gel techniques. APD Pt nanoparticles with an average size of 2.7 nm were deposited on sputtered and sol-gel-prepared titania films to assess the role of the titania support on the catalytic activity of Pt under CO oxidation. In order to study the nature of the dispersed metallic phase and its effect on the activity of the catalytic CO oxidation reaction, Pt nanoparticles were deposited in varying surface coverages on sputtered titania films using arc plasma deposition. Our results show an enhanced activity of Pt nanoparticles when the nanoparticle/titania interfaces are exposed. APD Pt shows superior catalytic activity under CO oxidation, as compared to impregnated Pt nanoparticles, due to the catalytically active nature of the mild surface oxidation and the active Pt metal, suggesting that APD can be used for large-scale synthesis of active metal nanocatalysts.

  • PDF

Characterization of TiO2 Catalyst Modified with H2SO4 (황산으로 개질된 TiO2 촉매의 특성)

  • Pae, Young-Il;Park, Man-Young;Lee, Joon-Hee;Sohn, Jong-Rack
    • Applied Chemistry for Engineering
    • /
    • v.3 no.1
    • /
    • pp.46-52
    • /
    • 1992
  • $TiO_2/SO_4{^{2-}}$ was prepared by precipitation from the mixed solution of titanium chloride and hydrochloric acid followed by modification with sulfuric acid. The characterization of prepared catalyst was performed by using IR, XPS, XRD and DT-TGA. Infrared spectra of $TiO_2/SO_4{^{2-}}$ showed bidentate sulfate ion coordinated to the surface of $TiO_2$. The acid strength of modified catalyst was at least $H_0{\leq}-14.52$, showing the superacidic properties which are attributed to the double bond nature of S=O of the complex formed by the interaction of $TiO_2$ with sulfate ion. For $TiO_2/SO_4{^{2-}}$, the specific surface area increased and the transition from the amorphous to anatase phase occurred at a higher temperature, as compared with pure $TiO_2$.

  • PDF