• Title/Summary/Keyword: Intercalation Compounds

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Intercalation of Primary Diamines in the Layered Perovskite Oxides, $HSr_2Nb_3o_{10}$

  • 홍영식;김시중
    • Bulletin of the Korean Chemical Society
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    • v.17 no.8
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    • pp.730-735
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    • 1996
  • The layered perovskite oxide, KSr2Nb3O10, was synthesized. The interlayer potassium cations were readily exchanged by protons in hydrochloric acid solution to give the protonation compound, HSr2Nb3O10·0.5H2O. The intercalation compounds, [NH3(CH2)nNH3]xSr2Nb3O10, were also obtained by acid-base reactions between the protonation compound and organic bases, 1,n-alkyldiamines. The interlayer distances in the intercalation compounds were linearly increased with the increase of the number of carbon (Δc/Δn=1.05 Å) in 1,n-alkyldiamines. The intercalated alkyldiammonium ions formed a paraffin-like monolayer with average tilting angle (θ) of ca. 56°. The intercalation reactions occurred stoichiometrically. The thermal decomposition process of the intercalation compounds showed distinct three steps due to the desorption of hydrated water, the decomposition of organic moiety, and the decomposition of Sr-related compounds.

Mechanism of Intercalation Compounds in Graphite with Hydrogen Sulfate (I. Study of Intermediate Phase between 2 Stage and 1 Stage in Graphite Hydrogen Sulfate with Anodic Oxidation) (흑연에 황산을 Intercalation 시킬때의 Mechanism 규명 (I. 전기적 산화방법에 의한 Graphite Salts의 중간상에 관한 연구))

  • 고영신;한경석;이풍헌
    • Journal of the Korean Ceramic Society
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    • v.22 no.6
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    • pp.5-8
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    • 1985
  • Graphite has been oxidized to graphite hydrogen sulfate in concentrated $H_2SO_4$. Anodic oxidation and chemical oxidation of graphite in $H_2SO_4$ generally leads to the formation of intercalation compounds of the ionic salt type through incorporation of $H_2SO_4^-$ions and $H_2SO_4$ molecules into the graphite. Several other reactions also accur at various points of the charging cycle. But there is no satisfactory kinetics and mechanism of intercalationin graphite. We have studied them with anodic oxidation and chemical oxidation. We found six distinct phenomena between 2nd stage and 1st stage in chemical oxidation. We examined them in detail by the following in the measurements electrical oxidation. X-ray diffractions UV-Vis spectroscopy density measurements. We could obtained a equation for kinetic according to the reaction rate from this results and mechanism of intercalation between 2nd stage and 1st stage with hydrogen sulfate in graphite. Three thesis were written for the mechanism of intercalation compounds in graphite with hydrogen sulfate ; first thesis is anodic oxidation second thesis is chemical oxidation and definition of transit phase between 2nd etc the third thesis is the kinetic mechanism of intercalation compounds in graphite with Hydrogen sulfate. This thesis is the first paper among three thesis as anodic oxidation.

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The Study on the Intercalation-Deintercalation of Potassium-Carbon Fiber Intercalation Compounds (칼륨-탄소섬유층간화합물의 Intercalation-Deintercalation에 관한 연구)

  • Oh, Won-Chun;Cho, Sung-Jun;Choi, Young-Jai;Ko, Young-Shin
    • Analytical Science and Technology
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    • v.7 no.2
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    • pp.193-199
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    • 1994
  • We have synthesized K-CFICs by the modified two-bulb method. These synthesized compound were analysed with X-ray diffractometer and UV/VIS spectrophotometer. According to X-ray diffraction analysis, the intercalation of potassium between the carbon layers of carbon fiber was better then other intercalants. From obtained data for this deintercalation process, we can see that a number of potassiums were presented as a residue between the carbon layers and this residue compounds had a stability for a long term. Therefore, it is appear that these compounds have a capability as new useful material. From UV/VIS spectrometry data, we can suppose that spectrum of K-CFICs synthesized at $250^{\circ}C$ had only a $R_{min}$, and spectra of any other compounds were not appeared charecteristic peaks because potassium ions were little affect the energy levels of original carbon fiber.

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Deintercalation and Thermal Stability of Na-graphite Intercalation Compounds

  • Oh, Won-Chun
    • Carbon letters
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    • v.2 no.1
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    • pp.22-26
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    • 2001
  • Na alloyed graphite intercalation compounds with stage 1 and 2 were synthesized using the high temperature and pressure technique. Thermal stability and staging transitions of the compounds were investigated depending on heating rates. The thermal stability and temperature dependence of the deintercalation compounds were characterized using differential scanning calorimeter (DSC) analyzer. Enthalpy of formations were confirmed at temperatures between 25 and $500^{\circ}C$, depending on the various heating rates. The structure ions and interlayer spaces of the graphite were identified by X-ray diffraction (XRD). Diffractograms of stages with non-integral (00l) values were obtained in the thermal decomposition process, and stacking disorder defects and random stage modes were observed. The average value of the interlayer C-C bond lengths were found approximately $2.12{\AA}$ and $1.23{\AA}$ from the diffractions. Based on the stage transition, the degree of the deintercalaton has a inverse-linear relationship against the heating rate.

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Synthesis and Characterization of Lithium-Graphite Intercalation Compounds (리튬-흑연 층간 화합물의 합성 및 특성 분석)

  • Hong, Senug-Hyun;Kim, Tae-Young;Suh, Kwang-S.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.227-227
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    • 2010
  • The intercalation chemistry of graphite presents an attractive route to obtain few-layered graphene platelets based on the expanded interlayer spacing. We report that the lithium can be intercalated into the graphite in a controllable manner by adjusting the variables such as temperature, pressure, and reaction time. From the X-ray diffraction experiments, the lithium-graphite intercalaltion compounds (Li-GICs) can be produced as the first stage compounds ($LiC_6$), the second-stage compounds ($LiC_{12}$), and the mixtures, which is most likely to be dependent on the temperature and reaction time. Since these Li-GICs are expected to facilitate the exfoliation of graphite, we investigated the feasibility of Li-GICs as a effective precursors for the generation of single-or few-layered graphite nano-platelets.

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The relation of structural transition and electrical property by deintercalation of Li-Carbon intercalation compounds (I) : For the formation of Li-GFDICs and Li-PCDICs (리튬-탄소층간화합물의 Deintercalation에 따른 구조변이와 전기적 성질과의 관계(I) : Li-GFDICs와 Li-PCDICs의 생성에 대하여)

  • Oh, Won-Chun;Baek, Dae-Jin;Ko, Young-Shin
    • Analytical Science and Technology
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    • v.8 no.2
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    • pp.131-138
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    • 1995
  • We have discussed on the structural transition and its effect on the electrical property of Li-GFDICs and Li-PCDICs occuring during the deintercalation process of Li-Graphite Fiber Intercalation Compounds(Li-GFICs) and Li-Petroleum Cokes Intercalation Compounds(Li-PCDICs) synthesized under pressure and temperature by spontaneous oxidation by air circulation. The analytical results were obtained by X-ray diffraction and electrical specific resistivity measurements. According to X-ray analysis, we have found that the major stage of Li-GFICs was stage 2 and those of Li-PCICs were stage 1 and stage 2, respectively. And from this results of the deintercalation process, we have found that the deintercalation process did not occur any more after 5th week of Li-GFDICs and after 3rd week of Li-PCDICs. According to the results of the electrical specific resistivity measurements, Li-GFDICs showed little variation to 3rd week and rising in the steady curve after 4th week, while Li-PCDICs showed a rising in the steady curve to 3rd week and a declining curve after 3rd week. Therefore from these results, we can consider that graphite fiber and petroleum cokes as a substrate can be also used as an anode material of battery because they have good intercalation-deintercalation reactivity with lithium.

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Mechanism of Intercalation Compounds in Graphite with Hydrogen Sulfate (II. Study of Intermediate Phase between 2 stage and 1 stage in Graphite Hydrogen Sulfate) (흑연에 황산을 Intercalation 시킬 때의 Mechanism 규명 (II. 화학적 방법에 의한 Graphite Salts의 중간상에 관한 연구))

  • 고영신
    • Journal of the Korean Ceramic Society
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    • v.25 no.4
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    • pp.408-414
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    • 1988
  • This thesis is 2nd thesis from "Mechanism of Intercalation Compounds in Graphite with Hydrogen sulfate(J. Korea Cer. Soc. Vol. 22. No.6, 1985). We have oxidized natural Graphite flakes(0.1~0.2mm., Kropfm hl passau in Deutchland. S40) with a solution of CrO3 in H2SO4. Whilst persulfate ions were intercalated, too, below 7$^{\circ}C$, no evidence for intercalation of a peroxo compound was found at 22$^{\circ}C$. The reaction was interrupted after various times by filtering and washing with concentrated H2SO4. X-ray diffraction showed that the 2nd stage compound had already been formed after 2 minutes. We could only follow further oxidation to the blue stage compound which was completed after 35 minutes. We have found six distinct intermediate stage between 2nd stage and 1 stage. Experiments are described on the formation of intermediate stage color and X-ray diffraction analysis.ysis.

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Properties of Residue Compounds Obtained from H2SO4-Carbon Fiber Intercalated Compound (황산-탄소섬유 층간화합물에서 얻은 잔류화합물의 특성)

  • 김인기;최상흘;고영신
    • Journal of the Korean Ceramic Society
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    • v.30 no.12
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    • pp.1080-1088
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    • 1993
  • The residue compounds of sulfuric acid-carbon fiber system were obtained from P100, M40, TZ307, and T300 fibers. The fibers which easily formed intercalation compound had small change of d002 value, but, large change of diameter of fiber. It was considered that the cracks in carbon fiber were due to the this conflicting result. The resistivities of residue compound of carbon fibers were increased with the large change of diameter of fibers. It is thought that the reason of our results is increasing defects such as crack in fibers. From the UV reflection spectra, it was found that reflectances of residue compounds were all decreased and the residue compounds were more stable than intercalation compounds.

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7Li-NMR and Thermal Analysis for Lithium Inserted into Artificial Carbon Material

  • O, Won Chun
    • Bulletin of the Korean Chemical Society
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    • v.22 no.4
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    • pp.367-371
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    • 2001
  • Lithium inserted into artificial carbon has been synthesized as a function of the Li concentration. The characteristics of these prepared compounds were determined from the studies using X-ray diffraction(XRD), solid nuclear magnetic resonance (NM R) spectrophotometric and differential scanning calorimeter(DSC) analysis. X-ray diffraction showed that lower stage intercalation compounds were formed with increasing Li concentration. In the case of the AG3, most compounds formed were of the stage 1 structure. Pure stage 1 structural defects of artificial graphite were not observed. 7Li-NMR data showed that bands are shifted toward higher frequencies with increasing lithium concentration; this is because non-occupied electron shells of Li increased in charge carrier density. Line widths of the Li inserted carbon compounds decreased slowly because of nonhomogeneous local magnetic order and the random electron spin direction for located Li between graphene layers. The enthalpy and entropy changes of the compounds can be obtained from the differential scanning calorimetric analysis results. From these results, it was found that exothermic and endothermic reactions of lithium inserted into artificial carbon are related to the thermal stability of lithium between artificial carbon graphene layers.