• 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.

• 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.

• 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.

• Analytical Science and Technology
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• v.7 no.3
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• pp.315-320
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• 1994

Li-GICs as a high performance energy storager were synthesized as a function of the Li content by the admixture and add-pressure method. The characteristics of these prepared compounds have been determined from the studies by X-ray diffraction, UV-VIS spectrometry and CHN analysis. It follows from the results of X-ray diffraction that the lower-stage intercalation compounds are formed as the Li contents increase, however the mixed stages in these compounds are also observed. In the case of the $Li_{40wt%}$, the compound with the structure of stage 1 has been predominently, but the structure of only stage 1 is not obtained. The $d_{001}$ value of stage 1 was determined to be ca. $3.70{\AA}$. An analysis of spectrometric data shows that each of the compounds gives distingushible energy state spectra. It is seen from the spectra that the positions of $R_{min}$ values, with increase in the Li contents, are shifted in the region of higher energy state. Such a result can be attributed to the formation of stable stages. The results of CHN analysis allow us to find the mixing state related to chemical compositions of the intercalated compounds and the superiority to admixture and add-pressure method. From the results determined, it reveals that $Li_{10wt%}$-GIC and $Li_{20wt%}$-GIC can be utilized for an anode of rechargable battery.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.3 no.2
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• pp.167-175
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• 1993

Lithium-Carbon Intercalation Compounds(Li-CICs) have been synthesized from various carbon ma-terials by use of the modified stainless steel two-bulbs methods. These compounds had various colours by structural character of starting materials. The synthesized Li-CICs were identified to stage formation process by X-ray diffraction data. At these results, well-oriented natural graphite and graphite fiber are formed lower stages(Stage 1, Stage 2), but poor-oriented carbon fiber and petroleum cokes are also formed higher stages(Stage 3, Stage 4, Stage 5). And when we compared with measured d value and calculated d value, these values agreed with each other. But poor-oriented carbon materials are some difference from them. The stage stability and energy stage of Li-CICs were obtained by UV/VIS Spectrophotometric data. X-ray diffraction and UV/VIS Spectrophotometric data suggested that well-oriented carbon materials has distingushible curve between energy and reflectance. In these results, we know that many charge carriers between carbon layers are related to concentration of intercalants. And then, this paper also provides information on high efficiency energy storing materials at intercalation process of Li-CICs.

• Bulletin of the Korean Chemical Society
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• v.32 no.6
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• pp.2045-2050
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• 2011

Using first principles density functional theory the formation energies of various binary compounds of lithium graphite and its homologues were calculated. Lithium and graphite react to form $Li_1C_6$ (+141 mV) but not form $LiC_4$ (-143 mV), $LiC_3$ (-247 mV) and $LiC_2$ (-529 mV) because they are less stable than lithium metal itself. Properties of structure and reaction potentials of $C_5B$, $C_5N$ and $B_3N_3$ materials as iso-structural graphite were studied. Boron and nitrogen substituted graphite and boron-nitrogen material as a iso-electronic structured graphitic material have longer graphene layer spacing than that of graphite. The layer spacing of $Li_xC_6$, $Li_xC_5B$, $Li_xC_5N$ materials increased until to x=1, and then decreased until to x=2 and 3. Nevertheless $Li_xB_3N_3$ has opposite tendency of layer spacing variation. Among various lithium compositions of $Li_xC_5B$, $Li_xC_5N$ and $Li_xB_3N_3$, reaction potentials of $Li_xC_5B$ (x=1-3) and $Li_xC_5$ (x=1) from total energy analyses have positive values against lithium deposition.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.3
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• pp.435-441
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• 1998

Li-SGICs as a anode of lithium ion battery were synthesized by high-pressure method as a function of the Li-contents. The characteristics of these prepared compounds were determined from the studies with X-ray diffraction method and differential scanning calorimeter (DSC) analysis. From the results of X-ray diffraction, it was found that the lower stage intercalation compounds were formed with increase of Li-contents. The mixed stages in these compounds were also observed. In the case of the $Li_{30;wt%}$-SGIC, the compounds in the stage 1 structure were formed predominantly, but the structure of only pure stage 1, due to the structural defect of synthetic graphite, was not observed. The enthalpy and entropy changes of the compounds could be obtained from the differential scanning calorimetric analysis results. From the results, it was found that exothermic and endothermic reactions of Li-SGICs are related to thermal stability of lithium between artificial graphite layers.

• 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.10 no.3
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• pp.209-215
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• 1997

Li-AGICs as a anode of secondary battery were synthesized by high-pressure method as a function of the Li-contents. The characteristics of these prepared compounds were determined from the studies with X-ray diffraction method, UV/VIS spectrophotometric and differential scanning calorimeter(DSC) analysis. From the results of X-ray diffraction, it was found that the lower stage intercalation compounds were formed with increase of Li-contents. The mixed stages in these compounds were also observed. In the case of the $Li_{30wt%}$-AGIC, the compounds in the stage 1 structure were formed predominantly, but the structure of only pure stage 1 for structural defect of artificial graphite is not observed. According to UV/VIS spectrophotometric analysis, $Li_{30wt%}$-AGIC shows distinguishable energy state spectrum with the position of $R(%)_{min}$ values, but the characteristic spectra of almost all Li-AGICs are not observed. The enthalpy and entropy changes of the compounds can be obtained from the differential scanning calorimetric analysis results. From the results, it was found that exothermic and endothermic reactions of Li-AGICs are related to thermal stability of lithium between artificial graphite layers.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.4
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• pp.660-666
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• 1998

We discussed structure, energy state, characteristics of thermal stability, and electrochemical properties of Li-GFICs, Li-PCICs, and Li-AGICs during the intercalation process. According to X-ray diffraction patterns, we observed phase of stage 2 mainly from Li-GFICs, while stage 1 phase as well as stage 2 from Li-PCICs. For the structure of Li-AGICs, stage 1 phase was dominant, but it was not possible to obtain pure stage 1 compound probably due to structural characteristics of artificial graphite. We measured energy state of the compounds to stage stability, and revealed that Li-AGICs and Li-GFICs were in more stable state than Li-PCICs. Therefore, those two compounds could be excellent candidate for energy reserve material. From the study of thermal degradation, Li-GFICs showed strong exothermic reaction at around 300 and $400^{\circ}C$. In the study of thermal stability of Li-AGIC at various temperatures, we observed that lithium was not completely deintercalated and high stage was maintained even at high temperature. In the case of charge, discharge, and electrochemical studies, Li-GFICs showed the best results.