Patent
Method of preparing graphene shell and graphene shell prepared using the method
| العنوان: | Method of preparing graphene shell and graphene shell prepared using the method |
|---|---|
| Patent Number: | 8,663,591 |
| تاريخ النشر: | March 04, 2014 |
| Appl. No: | 12/131703 |
| Application Filed: | June 02, 2008 |
| مستخلص: | Provided are a method of preparing a graphene shell and a graphene shell prepared using the method. A first heat treatment is performed on a mixture of an organic solvent and a graphitization catalyst so as to carburize the graphitization catalyst with carbon decomposed from the organic solvent. The graphitization catalyst is in the form of particles. A second heat treatment process is performed on the carburized graphitization catalyst in an inert or reductive gas atmosphere to thereby form graphene shells on surfaces of the carburized graphitization catalyst. |
| Inventors: | Yoon, Seon-mi (Yongin-si, KR); Choi, Jae-young (Yongin-si, KR); Shin, Hyeon-Jin (Yongin-si, KR) |
| Assignees: | Samsung Electronics Co., Ltd. (KR) |
| Claim: | 1. A method of preparing a graphene shell, comprising: performing a first heat treatment on a mixture of an organic solvent and a graphitization metal catalyst so as to carburize the graphitization metal catalyst with carbon decomposed from the organic solvent, the graphitization metal catalyst being in the form of particles; and forming graphene shells on surfaces of the carburized graphitization metal catalyst by performing a second heat treatment process on the carburized graphitization metal catalyst in an inert or reductive gas atmosphere; and wherein the graphitization metal catalyst comprises at least one metal selected from the group consisting of Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Ta, Ti, W, U, V, Zr, and an alloy thereof; and wherein the graphene shell has the same shape as the metal catalyst. |
| Claim: | 2. The method of claim 1 , wherein the organic solvent is a polar or non-polar organic solvent having a boiling point of about 60° C. to about 400° C. |
| Claim: | 3. The method of claim 1 , wherein the organic solvent comprises an alcohol based organic solvent, an ether based organic solvent, a ketone based organic solvent, an ester based organic solvent, an acid based organic solvent, or a mixture thereof. |
| Claim: | 4. The method of claim 1 , wherein the organic solvent is an alcohol based organic solvent or an ether based organic solvent, or a mixture thereof. |
| Claim: | 5. The method of claim 4 , wherein the alcohol based organic solvent is selected from the group consisting of monohydric alcohols and polyhydric alcohols. |
| Claim: | 6. The method of claim 5 , wherein the monohydric alcohol is selected from the group consisting of propanol, pentanol, hexanol, heptanol, and octanol. |
| Claim: | 7. The method of claim 5 , wherein the polyhydric alcohol is selected from the group consisting of propylene glycol, diethylene glycol, dipropylene glycol, triethylene glycol, tripropylene glycol, octylene glycol, tetraethylene glycol, neopentyl glycol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 2,3-butanediol, dimethyl-2,2-butanediol-1,2, and dimethyl-2,2-butanediol-1,3. |
| Claim: | 8. The method of claim 1 , wherein a base is added to the organic solvent. |
| Claim: | 9. The method of claim 8 , wherein the base includes an organic base. |
| Claim: | 10. The method of claim 8 , wherein the base is selected from the group consisting of tetramethyl ammonium hydroxide (TMAH), sodium hydroxide and potassium hydroxide. |
| Claim: | 11. The method of claim 8 , wherein the base is added to the organic solvent in a concentration of about 0.01M to about 5.0 M. |
| Claim: | 12. The method of claim 8 , wherein the base is added with water. |
| Claim: | 13. The method of claim 1 , wherein the graphitization metal catalyst is formed from a catalyst precursor in the organic solvent before or simultaneously with the first heat treatment process. |
| Claim: | 14. The method of claim 13 , wherein the catalyst precursor is a metal salt of the graphitization metal catalyst. |
| Claim: | 15. The method of claim 13 , wherein the mixture further includes a nucleating agent. |
| Claim: | 16. The method of claim 15 , wherein the nucleating agent includes at least one of K 2 PtCl 4 , H 2 PtCl 4 , PdCl 2 , and AgNO 3 . |
| Claim: | 17. The method of claim 1 , wherein the graphitization metal catalyst has a spherical shape, a cylindrical shape, or a polyhedral shape. |
| Claim: | 18. The method of claim 1 , wherein the first heat treatment process is performed in a temperature range of about 100° C. to about 400° C. for about 10 minutes to about 24 hours. |
| Claim: | 19. The method of claim 1 , wherein the first heat treatment process is performed while agitating the mixture. |
| Claim: | 20. The method of claim 1 , wherein the second heat treatment process is performed in a temperature range of about 400° C. to about 100° C. for about several seconds to about 10 hours. |
| Claim: | 21. The method of claim 1 , further comprising performing an acid treatment process to remove the graphitization metal catalyst from the graphene shells. |
| Claim: | 22. The method of claim 21 , further comprising performing a third heat treatment process on the graphene shells after the performing of the acid treatment process. |
| Claim: | 23. The method of claim 22 , wherein the third heat treatment process is performed at a temperature range of about 1000° C. to about 3000° C. for about several seconds to about 10 hours. |
| Claim: | 24. The method of claim 8 , wherein the base includes an inorganic base. |
| Claim: | 25. A method of preparing a graphene shell, comprising: performing a first heat treatment on a mixture of an organic solvent and a graphitization metal catalyst so as to carburize the graphitization metal catalyst with carbon decomposed from the organic solvent, the graphitization metal catalyst being in the form of particles; and forming graphene shells on surfaces of the carburized graphitization metal catalyst by performing a second heat treatment process on the carburized graphitization metal catalyst in an inert or reductive gas atmosphere without the presence of an external vapor carbon source; the graphitization metal catalyst comprises at least one metal selected from the group consisting of Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V, Zr, and an alloy thereof. |
| Claim: | 26. A method of preparing a graphene shell, consisting of: performing a first heat treatment on a mixture of an organic solvent and a graphitization metal catalyst so as to carburize the graphitization metal catalyst with carbon decomposed from the organic solvent, the graphitization metal catalyst being in the form of particles; and forming graphene shells on surfaces of the carburized graphitization metal catalyst by performing a second heat treatment process on the carburized graphitization metal catalyst in an inert gas atmosphere; the graphitization metal catalyst comprises at least one metal selected from the group consisting of Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Ta, Ti, W, U, V, Zr, and an alloy thereof. |
| Claim: | 27. The method of claim 26 , wherein a base is added to the organic solvent. |
| Claim: | 28. The method of claim 26 , wherein the graphitization metal catalyst is formed from a catalyst precursor in the organic solvent before or simultaneously with the first heat treatment process. |
| Claim: | 29. The method of claim 26 , further comprising performing an acid treatment process to remove the graphitization metal catalyst from the graphene shells. |
| Claim: | 30. The method of claim 21 , further comprising performing a third heat treatment process on the graphene shells after the performing of the acid treatment process. |
| Current U.S. Class: | 423/445R |
| Patent References Cited: | 7074380 July 2006 Iwaki et al. 7270795 September 2007 Kawakami et al. 7329398 February 2008 Kim 2002/0193040 December 2002 Zhou 2008/0159938 July 2008 Mauthner et al. 2006063449 March 2006 2006089370 April 2006 2006273707 October 2006 2007044614 April 2007 |
| Other References: | Choi et al., “Formation of Shell-Shaped Carbon Nanoparticles Above a Critical Laser Power in Irradiated Acetylene,” 2004, Adv. Mater., 16, No. 19, pp. 1721-1725. cited by examiner Altman et al., “Analysis of the mechanism of the critical transition in irradiated acetylene that leads to generation of shell-shaped carbon nanoparticles,” 2005, Carbon, 43, pp. 2693-2700. cited by examiner Yoon et al., “Graphitized Pitch-Based Carbons with Ordered Nanopores Synthesized by Using Colloidal Crystals as Templates,” 2005, J. Am. Chem. Soc., 127, pp. 4188-4189. cited by examiner Nature, vol. 418, pp. 964-967, Aug. 29, 2002. cited by applicant Japanese Office Action with English Translation for Application No. 2008-318431 dated Jul. 23, 2013. cited by applicant Korean Office Action with English Translation for Application No. 10-2007-0132681 dated Aug. 29, 2013. cited by applicant Yoon, et al., Graphitized Pitch-Based Carbons with Ordered Nanopores Synthesized by Using Colloidal Crystals as Templates, J. Am. Chem. Soc. vol. 127, No. 12, 2005, pp. 4188-4189. cited by applicant |
| Primary Examiner: | Saha, Bijay |
| Attorney, Agent or Firm: | Cantor Colburn LLP |
| رقم الانضمام: | edspgr.08663591 |
| قاعدة البيانات: | USPTO Patent Grants |
| الوصف غير متاح. |