• 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.

• Analytical Science and Technology
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• v.11 no.2
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• pp.92-95
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• 1998

K-SGICs(synthetic graphite intercalation compounds) were synthesized in a modified two-bulb pyrex tube. The pressure in the two-bulb tube was maintained at approximately $10^{-3}$ torr for the reaction of potassium and graphite. Deintercalation process of the K-SGlCs obtained by the modified method was heat-treated by keeping in liquid paraffin between $25^{\circ}C$ and $1400^{\circ}C$. The thermal stability and the temperature dependence of the K-SGICs were characterized using differential scanning calorimeter(DSC) analyzer. Enthalpy and entropy for K-SGIC formations were calculated by confirming the deintercalation and thermodynamic exothermic reactions depending on the various temperatures. The structure changes and thermal stability of K-SGICs during the deintercalation reaction of potassium ions and the interlayer spaces of the synthetic graphite were identified by X-ray diffraction(XRD).

• Analytical Science and Technology
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• v.9 no.1
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• pp.43-51
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• 1996

We have discussed on the deintercalation process of Li-EaGICs and Li-EGICs synthesized under pressure and temperature by spontaneous oxidation reaction of those compounds based on the results of X-ray diffraction, thermal analysis and electrical specific resistivity analysis. According to the results of the X-ray analysis for the intercalation process, we have found that the stage 1 for Li-EaGICs and Li-EGICs were not completly formed, but their lower stages were formed mainly. And from this results of the deintercalation process, we have found that the deintercalation process did not occur any more after 4 weeks, and the Li-EGDICs have more residual lithium metals than LiEaGDICs between the graphite interlayers. According to the thermal decomposition analysis, Li-two compounds had included very hard exothermic reaction. And we have found that these compounds did not occrurred deintercalation reaction above $400^{\circ}C$. According to the results of the electrical specific resistivity measurements, Li-EGDICs have relatively lower electrical specific resistivity than Li-EaGDICs, and Li-EaGDICs showed a formation of the ideal curve. From these results, we can suggest that Li-EaGDICs have a better properties as an anode material secondary than Li-EGICs.

• 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.

• 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.

• Journal of the Korean Ceramic Society
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• v.30 no.10
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• pp.797-802
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• 1993

Graphite fiber intercalated compound was deintercalated at $25^{\circ}C$, 65% of humidity and its deintercalated compound was discussed, based on the X-ray diffraction analysis, electrical resistivity measurement, and UV/VIS spectrometer measurements. During deintercalation, the structure was changed in orderlongrightarrowdisorderlongrightarroworder, and resistivity was decreased in the disorder state of the structure, which reflectance minimum of the UV/VIS spectrum ranged from 660 to 750nm (1.88~1.65eV).

• The Korean Journal of Ceramics
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• v.1 no.1
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• pp.40-44
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• 1995

Ethylammonium-layered aluminosilicates intercalates were prepared by ion exchange reaction between the layered silicates with different layer changes density of 0.32∼0.41 e per unit formula and ethylammonium chloride. A kinetic study on the thermal deintercalation of the ethylammonium-layered silicate intercalates was carried out by range of 350℃ to 480℃ (heating rate of 10℃/min). Based on the Ozawa's method, the activation energies of the thermal deintercalation reaction were estimated as 171.2∼133.0 kJ/mol, which increase linearly with the layer charge densities.

• 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.

• Journal of the Korean Electrochemical Society
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• v.5 no.4
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• pp.178-182
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• 2002

The electrochemical behavior of binder-free carbon anode, comprising of only artificial and natural graphite (AG and NG) particles, for intercalation and deintercalation of lithium ion $(Li^+)$ in aluminum chloride (AICI_3)-I-ethyl­3-methylimidazolium chloride (EMIC)-lithium chloride (LiCl)-thionyl chloride $(SOCI_2)$ room-temperature molten salt (RTMS) was studied. Binder-free carbon electrodes were fabricated using electrophoretic deposition (EPD) method. The binder-free carbon anodes provided a relatively flat charge and discharge potentials $(0\;to\;0.2V\;vs.\;Li/Li^+)$ and current capabilities $(250-340mAh{\cdot}g^{-1})$ for the intercalation and deintercalation of $Li^+$. Stability of the binder-free carbon anodes for intercalation and deintercalation of 50 cycles was confirmed.

• 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.