• 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.

• 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.6 no.5
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• pp.479-487
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• 1993

Potassium-Graphite Fiber Intercalation Compounds(K-GFIC) have been prepared from well oriented pitch-based Graphite fiber by the transformed two-bulbs method with variation of reaction temperatures of graphite($T_g$ : $450^{\circ}C$, $400^{\circ}C$, $350^{\circ}C$, $300^{\circ}C$, $250^{\circ}C$). The stage transition process of K-GFICs was studied by X-ray diffraction methods, and we have observed peaks with d-values of (001) diffraction of $5.40{\AA}$ and $8.78({\pm}0.01){\AA}$, which are charecteristic for the stage 1 and stage 2, respectively. The stage stability and energy states of K-GFICs were studied by UV/VIS spectrophotometer. As a results, We found that the minimum values of reflactance of K-GFICs with pure stage was moved to higher energy pristine Graphite fiber's. But because of mixtured stage, we could not observe minimum reflectance in the visible region at high reaction temperatures($400^{\circ}C$, $450^{\circ}C$). From X-ray diffraction and UV/VIS sepctrophotometry data, we can suggest that K-GFICs with lower stage has many charge carriers existed between C atoms of graphite Layers. And then, these results also provides information on the electrical and other physical properties of K-GFICs.

• 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).

• 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.

• 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.3 no.1
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• pp.66-74
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• 1993

Potassium-Graphite Intercalation Compounds(K-GICs) have been prepared from purified natural graphite by transformed two-bulb method with variations of reaction temperature ($T_g:450^{\circ}C$, $400^{\circ}C$, $350^{\circ}C$, $300^{\circ}C$, $250^{\circ}C$).Prepared K-GICs were identified to stage transition process by X-ray diffraction data. At these results, d values of (00l) diffraction at 1 stage and 2 stage were corresponded to $5.35\AA$ and $8.73\AA$ respectively. The stage stability and energy states of K-GlCs were obtained by UV /VIS Spectrophotometric data. We found that the minimum value of reflectance was 2.67 eV(465nm) at $250^{\circ}C$and it's moved to higher energy than original graphite's. And X-ray diffraction and UV /VIS spectrophotometric datas suggest that K-GICs were formed lower stage and many charge carriers exist between C atoms of graphite. And then, these results also provide informations on the electrical and other physical properities of K-GICs.Especially, according to studied reports, d values differ from them of each author, but accurate values were established through this study.

• Journal of the Korean Ceramic Society
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• v.30 no.9
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• pp.768-774
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• 1993

Sulphuric acid was intercalated in mesophase pitch based graphite fiber (Thornel P100 of Amoco), PAN based graphite fiber (M40 of Thoray) and PAN based carbon fiber (T300 ofThoray, TZ307 of Taekwang in Korea) by 0.4wt% CrO3/H2SO4 solution. The degree of crystallization of fibers increased P100, M40, TZ307, T300 fiber in order and their d002 values were 3.384, 3.424, 3.470, 3.493$\AA$, respectively. After intercalation P100 fiber formed 1 stage compound whose d002 value was 3.994$\AA$(d001=7.988$\AA$). Other fibers showed (002) reflection belonging to their 1 stage comound and prinstine fiber.

• 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.