• 한국세라믹학회지
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• 제22권6호
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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.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2010년도 하계학술대회 논문집
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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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• 한국초전도학회 2009년도 Korea Superconductivity Society Meeting 2009
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• pp.8-8
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• 2009

• Carbon letters
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• 제2권1호
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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.

• 한국세라믹학회지
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• 제25권4호
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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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• 제23권12호
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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.

• 한국결정성장학회지
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• 제8권1호
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• pp.83-90
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• 1998

Li, K과 Na-흑연 층간화합물의 stage 전이 특성을 탄소층사이에 존재하는 intercalants의 deintercalation 메카니즘을 고려하여 제시하였다. 온도와 압력을 조절하여 합성된 Li-GICs(graphite intercalation compounds)를 분위기하에서 자발적으로 분해시켰다. 이들 화합물을 XRD 분석한 결과 1, 2 stage의 d001-값이 각각 3.71, 7.06 $\AA$으로 나타났다. 분위기하에서 Li-GiCs를 deintercalation 반응을 시킨 6주 후에 잔유화합물이 형성됨을 알 수 있었다. 또한, two-bulb 법으로 K-GICs를 합성하였으며, K-GDICs(graphite deintercalation compounds)의 구조적 안정성과 stage 전이에 대하여 조사하였다. X-선회절 결과로부터 K-GDICs는 10주 동안 안정한 K-흑연 잔유 화합물을 형성하였다. 그리고 고온, 고압법을 이용하여 합성된 1, 2stage의 Na-GICs의 deintercalation 반응과 열적 안정성에 대한 온도 의존성에 대하여 논하였다. 열적 안정성과 관련하여 Na-GICs의 구조변화를 XRD에 의하여 확인하였다. 이들 과정에 따르면 stage 전이는 무질서한 stage를 가진 GDICs의 불규칙적인 deintercalation에 의하여 형성됨을 제시할 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제21권1호
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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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• 제2권1호
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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.

• 분석과학
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• 제8권2호
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• pp.131-138
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• 1995

가온 가압법으로 합성한 리튬-흑연섬유간화합물(Li-Graphite Fiber Intercalation Compounds, Li-GFICs)과 리튬-석유코크스층간화합물(Li-Petroleum Cokes Intercalation Compounds, Li-PCICs)을 공기 순환에 의하여 자발적으로 deintercalation시키고, 이 deintercalation의 분해 과정으로 나타나는 Li-GFDICs와 Li-PCICs의 구조를 전기적 성질에 미치는 영향에 대하여 논의하였다. 이에 대한 분석은 X-선 회절과 전기 비저항 측정에 의해 수행되었다. X-선 회절 분석에 의하면 Li-GFDICs의 경우 주로 2 stage가 형성되었고 Li-PCICs의 경우에는 1 stage와 2 stage가 주된 회절선으로 나타났다. 또한 deintercalatlon 반응 결과에 의하면 Li-GFDICs의 경우 5주 이후에, Li-GFDICs의 경우 3주 후에 deintercalation 반응이 각각 멈췄다. 전기 비저항 측정 결과에 의하면 Li-GFDICs의 경우 3주까지는 거의 변화가 없었고 그 후 완만한 상승곡선을 나타내었으며, Li-PCDICs의 경우에는 3주를 정점으로 하향곡선을 나타내었다. 따라서 본 연구결과에 의하면 기질로 사용된 흑연섬유와 석유 코크스의 경우 리튬의 원활한 intercalation-deintercalation 작용이 잘 이루어지므로 두 물질 모두 전지의 양극재로 사용될 수 있을 것으로 기대되어진다.