• 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.

• 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.

• 한국초전도학회:학술대회논문집
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• 2009.07a
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• pp.8-8
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• 2009

• 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.

• 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.

• Bulletin of the Korean Chemical Society
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• v.23 no.12
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• pp.1801-1805
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• 2002

The graphite intercalation compounds(GIC) were prepared by a dry process that led to the intercalation from the direct reaction of gaseous $SO_3$ with flake type graphite. The basal spacing of the GIC was increased from 8.3 ${\AA}$ to 12 in the gallery height. The ejection of interlayer $SO_3$ molecules by the heating for 1 minute at $950^{\circ}C$ resulted in an exfoliated graphite (EG) with surprisingly high expansion in the direction of c-axis. The expansion ratios of the exfoliated graphites were increased greatly between 220 times and 400 times compared to the original graphite particles, and the bulk density was range of 0.0053 to 0.01 $g/cm^3$, depending on reaction time. The pore size distribution of exfoliated graphite was in the range of $10-170{\mu}m$, which exhibites both mesoporosity and macroporosities. This result indicates that the direct reaction of graphite paricles with gaseous $SO_3$ can be proposed as an another route for the exfoliated graphite having excellent physical properties.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.1
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• pp.83-90
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• 1998

Stage transformation characteristics of Li, K and Na-graphite deintercalation compounds (GDICs) were studied under consideration of a deintercalation mechanism of the intercalants between carbon layers. Li-graphite intercalation compounds (GICs) synthesized by a controlling temperatures and pressures have been spontaneously decomposed in the atmosphere. By X-ray differaction analysis the $d_{001}$-values of stage 1 and 2 were identified to be 3.71 and 7.06 $\AA$, respectively. After 6 weeks, the deintercalation reaction of the Li-GICs ceased and only residual compounds could be observed. K-GICs were synthesized by the modified two-bulb method resulting in structural stabilities and stage transitions. By X-ray diffraction analysis the very stable K-graphite residue compounds were observed after 10 weeks. Na-GICs with stage 1 and 2 were synthesized using the high temperature and pressure technique. The temperature dependence of a deintercalation reaction and a thermal stability of Na-GICs were discussed. The structure changes of the Na-GDICs depending on heating rates were identified by X-ray diffraction. According to the deintercalation process, the stage transformations could be attributed to irregular deintercalations of the GDICs with disordered stage.

• Bulletin of the Korean Chemical Society
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• v.21 no.1
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• pp.101-104
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• 2000

Li-graphite intercalation compounds (GICs), synthesized at elevated temperature and pressure, were allowed to decompose spontaneously in the atmosphere. The decomposition processes were analyzed by of X-ray diffraction, DSC analysis, FT-IR measurements, UV/VIS spectrophotometry. The deintercalation reaction of the Li-GICs ceased after 6 weeks and only the residual compounds could be observed. A strong exothermic reaction was observed at 300 $^{\circ}C$ in thermal decomposition, and relatively stable decomposition curves were formed. A few endothermic curves have been observed at 1000 $^{\circ}C.$ After 6 weeks deintercalation reaction time of GICs, many exothermic and endothermic reactions were accompanied at the same time. In addition the reactions of the functional groups such as aromatic rings, nitrogen, $-CH_3$, $-CH_2$ etc. of GDIC obtained by the above reaction were confirmed by FT-IR spectrum. UV/VIS spectrophotometric measurement clearly shows the formation of a minimum energy value ($R_{min}$) for the compounds between Li-GICs as a starting material and Li-GDICs obtained until after 3 weeks of the deintercalation reaction, while they were no clear energy curves from 4 weeks of reaction time, because of the formation of the graphite structure, of high stages and of the Li compounds surrounding the graphite in the deintercalation reaction.

• Carbon letters
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• v.2 no.1
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• pp.55-60
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• 2001

Graphite intercalation compounds (GIC) were prepared by direct reaction of $SO_3$ gas with flake graphite. The intercalated $SO_3$ molecules were ejected by rapid heating to $950^{\circ}C$ under an oxidizing atmosphere for about 1 minute, resulting in surprisingly high expansion in the direction of c-axis. The characteristics of the micro-structure and pore size distribution were examined with a SEM and mercury intrusion porosimetry. The XRD analysis and spectroscopic analysis were used for the identification of the graphite and surface chemistry state. The pore size distribution of the exfoliated graphite (EG) was a range of $1{\sim}170{\mu}m$. The higher expanding temperature the higher expanded volume, so oil sorption capacities were 58.8 g of bunker-C oil and 34.7 g of diesel oil per 1 g of the the EG. The sorption equilibrium was achieved very rapidly within several minutes. As the treatment temperature increases, bulk density decreases.

• 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.