КОМПОЗИТ ГУМИНОВОЙ КИСЛОТЫ И ОКСИДА ГРАФЕНА: РЕЗУЛЬТАТЫ ВЫСОКОТЕМПЕРАТУРНОЙ ОБРАБОТКИ

Гуминовые кислоты (ГК) и углеродный наноматериал, полученный путем нагрева ГК при 900 °С в инертной атмосфере (УНГК), были изучены методами твердотельного ядерного магнитного резонанса (ЯМР), дифференциальной сканирующей калориметрии (ДСК), термогравиметрического анализа (ТГА), спектроскопии комбинационного рассеяния света и стандартной контактной порометрии (СКП). Масс-спектрометрия была также использована для анализа газов, выделяющихся при нагревании образцов. Были также получены композит ГК с оксидом графена (ГК-ОГ) и углеродный наноматериал, образующийся при карбонизации композита (ГК-ОГ) в инертной атмосфере при температуре 900 °С. Установлено, что при карбонизации образуются небольшие агломераты углерода с четко определенными краями, тогда как при карбонизации композита при тех же условиях образуются крупные агрегаты. Значения удельной поверхности для УНГК и УН (ГК-ОГ) составили 173 и 474 м2 /г соответственно. Удельная поверхность, соответствующая площади всех пор (Spore), равна только 3 м2 /г в случае УНГК, в случае УН (ГК-ОГ) Spore = 237 м2 /г.

гуминовые кислоты, оксид графена, композит, термическая обработка, пористость

1. Yu MF, Lourie O, Dyer MJ, Moloni K, Thomas FK, Ruoff RS. Strength and breaking mechanism of multiwalled carbon nanotubes under tensile load. Science, 2000; 287:637–40.

2. Zhou J, Lubineau G. Improving electrical conductivity in polycarbonate nanocomposites using highly conductive PEDOT/PSS coated MWCNTs. ACS Appl. Mater. Interfaces, 2013; 5: 6189–200.

3. Lubineau G, Rahaman A. A review of strategies for improving the degradation properties of laminated continuous-fiber/epoxy composites with carbon-based nano-reinforcements. Carbon, 2012; 50:2377–95.

4. Xu P, Gu T, Cao Z, Wei B, Yu J, Li F, Byun JH, Lu W, Li Q, Chou TW. Carbon nanotube fiber based stretchable wire-shaped supercapacitors. Adv. Energy Mater., 2013; 4:1300759.

5. Sun H, Xu Z, Gao C, Multifunctional, ultraflyweight, synergistically assembled carbon aerogels. Adv. Mater., 2013; 25:2554–60.

6. Ata S, Kobashi K, Yumura M, Hata K. Mechanically durable and highly conductive elastomeric composites from long single-walled carbon nanotubes mimicking the chain structure of polymers. Nano Lett., 2012; 12:2710–6.

7. Wu X, Wen T, Guo H, Yang S, Wang X, Xu A. Biomass-derived sponge-like carbonaceous hydrogels and aerogels for supercapacitors. ACS Nano, 2013; 7:3589–97.

8. Chen W, Rakhi RB, Hu L, Xie X, Cui Y, Alshareef HN. High performance nanostructured supercapacitors on a sponge. Nano Lett., 2011; 11:5165–72.

9. Wu ZY, Li C, Liang HW, Chen JF, Yu SH. Ultralight, flexible, and fire-resistant carbon nanofiber aerogels from bacterial cellulose. Angew. Chem., 2013; 125:2997–3001.

10. Tovmash AV, Polevov VN, Mamagulashvili VG, Chernyaeva GA, Shepelev AD. Fabrication of sorptionfiltering nonwoven material from ultrafine polyvinyl alcohol carbonized fibres by electrospinning. Fibre Chem., 2005; 37:187–91.

11. Sveningsson M, Morjan RE, Nerushev OA, Sato Y, Backstrom J, Campbell EB, et al. Raman spectroscopy and field emission properties of CVDgrown carbon-nanotube films. Appl. Phys. A Mater. Sci. Process, 2001; 73:409–18.

12. Morishita T, Soneda Y, Tsumura T, Inagaki M. Preparation of porous carbons from thermoplastic precursors and their performance for electric double layer capacitors. Carbon, 2006; 44:2360–7.

13. Qian H, Greenhalgh ES, Shaffer MSP, Bismarck A. Carbon nanotube-based hierarchical composites: a review. J. Mater. Chem., 2010; 20:4751-62.

14. Qian H, Bis marck A, Greenhalgh ES, Kalinka G, Shaffer MSP. Hierarchical composites reinforced with carbon nanotube grafted fibers: the potential assessed at the single fiber level. Chem. Mater., 2008; 20:1862–9.

15. Xu B, Wu F, Chen S, Cao G, Zhou Z. A simple method for preparing porous carbon by PVDC pyrolysis. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2008; 316:85–88.

16. Zussman E, Yarin AL, Bazilevsky AV, Avrahami R, Feldman M. Electrospun polyaniline/poly(methyl methacrylate)-derived turbostratic carbon micro- /nanotubes. Adv. Mater., 2006; 18:348–53.

17. Fatema UK, Uddin AJ, Uemura K, Gotoh Y, Fabrication of carbon fibers from electrospun poly(vinyl alcohol) nanofibers. Text Res. J., 2010; 81:659–72.

18. Huang W, Zhang H. Hierarchical porous carbon obtained from animal bone and evaluation in electric double-layer capacitors. Carbon, 2011;49: 838-43.

19. Wang Q, Cao Q, Wang X, Jing B, Kuang H, Zhou L. A high-capacity carbon prepared from renewable chicken feather biopolymer for supercapacitors. J. Power Sources, 2013; 225:101-7.

20. Yun Y, Cho S, Shim J, Kim B, Chang S, Jin H. Microporous carbon nanoplates from regenerated silk proteins for supercapacitors. Advanced Materials, 2013; 25:1993-8.

21. Zhang L, Zhang F, Yang X, Leng K, Huang Y, Chen Y. High-performance supercapacitor electrode materials prepared from various pollens. Small, 2013; 9:1342-7.

22. Chen X, Jeyaseelan S, Graham N. Physical and chemical properties study of the activated carbon made from sewage sludge. Waste Manage, 2002; 22:755-60.

23. Haykiri-Acma H, Yaman S, Kucukbayrak S. Gasification of biomass chars in steam–nitrogen mixture. Energy Convers Manage, 2005; 47:1004-1013.

24. Lanzetta M, Di Blasi C. Pyrolysis kinetics of wheat and corn straw. J. Anal. Appl. Pyrol., 1998; 44:181-92.

25. Minkova V, Razvigorova M, Bjornbom E, Zanzi R, Budinova T, Petrov N. Effect of water vapour and biomass nature on the yield and quality of the pyrolysis products from biomass. Fuel Proc. Technol., 2001; 70:53-61.

26. Minkova V, Marinov SP, Zanzi R, Bjornbom E, Budinova T, Stefanova M, Lakov L. Thermochemical treatment of biomass in a flow of steam or in a mixture of steam and carbon dioxide. Fuel Proc. Technol., 2000; 62:45-52.

27. Yang J, Liu Y, Chen X, Hu Z. Carbon electrode material with high densities of energy and power. Acta Physico-Chimica Sinica, 2008; 24:13-18.

28. Yun J, Jeong S, Shin S. High capacity disordered carbons obtained from coconut shells as anode materials for lithium batteries. J. Alloys Compounds, 2008; 448:141-7.

29. Kim Y, Lee B, Suezaki H, Chino T, Abe Y. Nanowires with a carbon nanotube core and silicon oxide sheath. Carbon, 2006; 44:1581-92.

30. Stevenson F J. Humus chemistry: genesis, composition, reactions. John Wiley & Sons, New York. 1994.

31. Baigorri R, Fuentes M, González-Gaitano G, García-Mina J. Complementary multi analytical approach to study the distinctive structural features of the main humic fractions in solution: gray humic acid, brown humic acid, and fulvic acid. J. Agricultural Food Chemistry, 2009; 57:3266-72.

32. Ghabbour EA, Davies G. Humic substances: structures, models and functions. Royal Society of Chemistry, Cambridge. 2001, ISBN 0-85404- 811-1.

33. Zhao L, Li Y, Zhao Y, Feng Y, Feng W, Yuan X. Carbon nanotubes grown on electrospun polyacrylonitrile-based carbon nanofibers via chemical vapor deposition. Appl. Phys. A, 2012; 106:863–9.

34. Dume´e L, Sears K, Mudie S, Kirby N, Skourtis C, Mcdonnell J, et al. Characterization of carbon nanotube webs and yarns with small angle X-ray scattering: revealing the yarn twist and inter-nanotube interactions and alignment. Carbon, 2013;63:562–6.

35. Geim AK, Novoselov KS. The rise of grapheme. Nature Materials, 2007; 6:183-91.

36. Chen D, Tang LH, Li J. H. Graphene-based materials in electrochemistry. Chemical Society Reviews, 2010; 39:3157–80.

37. Dreyer DR, Park S, Bielawski CW, Ruoff RS. The chemistry of graphene oxide. Chemical Society Reviews, 2010; 39:228-40.

38. Li XL; Wang HL; Robinson JT; Sanchez H; Diankov G; Dai HJ. Simultaneous Nitrogen Doping and Reduction of Graphene Oxide. J. Amer. Chem. Soc., 2009; 131:15939-44.

39. Nam B, Lee H-J, Goh H, Lee YB, Choi WS. Sandwich-like graphene nanocomposites armed with nanoneedles. J. Materials Chem., 2012; 22:3148-53.

40. Wang GX, Shen XP, Wang B, Yao J, Park J. Synthesis and characterization of hydrophilic and organophilic graphene nanosheets. Carbon, 2009; 47:1359-64.

41. Liu Q, Zhang H, Zhong H, Zhang S, Chen S. Ndoped graphene/carbon composite as non-precious metal electrocatalyst for oxygen reduction reaction. Electrochimica Acta, 2012; 81:313–20.

42. Ostrovsky VS, Virgil’ev YS, Kostikov VI, Shipkov NN. Artificial graphite. Moscow, Metallurgy 1986; 272.

43. Libra JA, Ro KS, Kammann C, Funke A, Berge ND, Neubauer Y, Titirici MM, Fühner C, Bens O, Kern J, Emmerich KH. Hydrothermal carbonization of biomass residuals: a comparative review of the chemistry, processes and applications of wet and dry pyrolysis. Biofuels, 2011; 2(1):89-124.

44. Groenli MG, Varhegyi G, Di Blasi C. Thermogravimetric analysis and devolatilization kinetics of wood. Ind. Eng. Chem. Res., 2002; 41:4201-8.

45. Becerril HA, Mao J, Liu Z, Stoltenberg RM, Bao Z, Chen Y. Evaluation of solution-processed reduced graphene oxide films as transparent conductors. ACS Nano, 2008; 2:463-70.

46. Shulga YM, Martynenko VM, Muradyan VE, Smirnov VA, Gutsev GL. Gaseous products of thermoand photo-reduction of graphite oxide. Chem. Phys. Lett., 2010; 498: 287-91.

47. Bissessur R, Liu PKY, White W, Scully SF. Encapsulation of polyanilines into graphite oxide. Langmuir, 2006; 22:1729-1734.

48. McAllister M J, Li J; Adamson D H, Schniepp HC, Abdala AA, Liu J, Herrera-Alonso M, Milius DL, Car R; Prud’homme RK, Aksay I. Single sheet functionalized graphene by oxidation and thermal expansion of graphite. Chem. Mater., 2007; 19:4396-404.

49. Stankovich S, Dikin DA, Piner RD, Kohlhaas KA, Kleinhammes A, Jia Y, Wu Y, Nguyen S T, Ruoff RS. Synthesis of graphene-based nanosheets via chemical reduction of exfoliated graphite oxide. Carbon, 2007; 45:1558-65.

50. Gomez-Navarro C, Weitz RT, Bittner AM, Scolari M, Mews A, Burghard M, Kern K. Electronic transport properties of individual chemically reduced graphene oxide sheets. Nano Lett., 2007; 7:3499-3503.

51. Cote LJ, Cruz-Silva R, Huang J. Flash reduction and patterning of graphite oxide and its polymer composite. J Am. Chem. Soc., 2009; 131:11027-32.

52. Zhu Y., Stoller MD, Cai W, Velamakanni A, Piner RD, Chen D, Ruoff RS. Exfoliation of Graphite Oxide in Propylene Carbonate and Thermal Reduction of the Resulting Graphene Oxide Platelets. ACS Nano, 2010; 4:1227.

53. Seung HH. Thermal Reduction of Graphene Oxide, Physics and Applications of Graphene - Experiments, (2011) Dr. Sergey Mikhailov (Ed.), ISBN: 978-953-307-217-3, InTech, DOI: 10.5772/14156. Available from: http://www.intechopen.com/books/physics-andapplications-of-graphene-experiments/thermalreduction-of-graphene-oxide

54. Zhu Y, Murali S, Stoller MD, Velamakanni A, Piner RD, Ruoff RS. Microwave assisted exfoliation and reduction of graphite oxide for ultracapacitors. Carbon, 2010; 48:2118-22.

55. Zhu Y, Murali S, Stoller MD, Ganesh KJ, Cai W, Ferreira PJ, Pirkle A, Wallace RM, Cychosz KA, Thommes M, Su D, Stach EA, Ruoff RS. Carbon-based supercapacitors produced by activation of graphene. Science, 2011; 332:1537-41.

56. Shulga YM, Baskakov SA, Knerelman EI, Davidova GI, Badamshina ER, Shulga NY, Skryleva EA, Agapov AL, Voylov DN, Sokolov AP, Martynenko VM. Carbon nanomaterial produced by microwave exfoliation of graphite oxide: new insights. RSC Adv., 2014; 4:587-92.

57. Paciolla MD, Davies G, Jansen SA. Generation of hydroxyl radicals from metal-loaded humic acids. Environ. Sci. Technol., 1999; 33:1814-8.

58. Gerse J, Kremo R, Csicsor J, Pintér L. Humic Substances in the Global Environment and Implications on Human Health, Ed. Senesi M. Amsterdam: Elsevier. 1994; 1297.

59. Petrosyan GP, Aranbaev MP, Grigoryan FA. Proceedings of the Fourth International Conference on Thermal Analysis. Ed. Buzás I. Budapest: 1974; 2:745.

60. Campanella L, Tomassetti M, Piccolo A. Thermochim. Acta, 1990; 170:67-80.

61. Peuravuori J, Paaso N, Pihlaja K. Kinetic study of the thermal degradation of lake aquatic humic matter by thermogravimetric analysis. Thermochim. Acta, 1999; 325:181-93.

62. Hummers WS, Offeman RE. Preparation of graphitic oxide. J. Am. Chem. Soc., 1958; 80:1339-9.

63. Volfkovich YM, Bagotzky VS. The method of standard porosimetry. J. Power Sources, 1994; 48:327-48.

64. Volfkovich YM, Bagotzky VS, Sosenkin VE, Blinov IA. The Standard Contact Porosimetry. Colloid and Surfaces A: Physicochemical and Engineering Aspects, 2001; 187-188: 349-65.

65. Barron PF, Wilson MA. The structure of freshwater humic substances as revealed by 13 C-NMR spectroscopy. Nature, 1981; 289:275-6.

66. Sullivan MJ, Maciel GE. Spin dynamics in the carbon-13 nuclear magnetic resonance spectrometric analysis of coal by cross polarization and magic-angle spinning. Anal. Chem., 1982; 54:1608-23.

67. Tekely P, Nicole D, Brondeau J, Delpuech JJ. Application of carbon-13 solid-state high-resolution NMR to the study of proton mobility. Separation of rigid and mobile components in coal structure. J. Phys. Chem., 1986; 90:5608-11.

68. Lukins PB, McKenzie DR, Vassallo AM, Hanna JV. 13C NMR and FTIR study of thermal annealing of amorphous hydrogenated carbon. Carbon, 1993; 31:569-75.

69. Sharma RK, Wooten JB, Baliga VL, Hajaligol MR. Characterization of chars from biomass-derived materials: pectin chars. Fuel, 2001; 80:1825-36.

70. Holtman KM, Chang HM, Jameel H, Kadla JFJ. Quantitative 13C NMR characterization of milled wood lignins isolated by different milling techniques. Wood Chem. Technol., 2006; 26: 21–34.

71. Cai W, Piner RD, Stadermann FJ, Park S, Shaibat MA, Ishii Y, Yang D, Velamakanni A, An SJ, Stoller M, An J, Chen D, Ruoff RS. Synthesis and solid-state NMR structural characterization of 13C-labeled graphite oxide. Science, 2008; 321:1815-7.

72. Crespilho FN, Zucolotto V, Siqueira JR, Constantino CJL, Nart FC, Olivera ON. Immobilization of Humic Acid in Nanostructured Layer-by-Layer Films for Sensing Applications. Environ. Sci. Technol., 2005; 39:5385-9.

73. Shin HS, Monsallier JM, Choppin GR. Spectroscopic and chemical characterizations of molecular size fractionated humic acid. Talanta 50; 1999:641-7.

74. Karthika P, Rajalakshmi N, Dhathathreyan KS. Functionalized exfoliated graphene oxide as supercapacitor electrodes. Soft Nanosci. Lett., 2012; 2:59-66.

75. Fu M, Jiao Q, Zhao Y, Li H. Vapor diffusion synthesis of CoFe2O4 hollow sphere/graphene composites as absorbing materials. J. Mater. Chem. A, 2014; 2:735-44.

76. Han B., Sun S., Ding S., Zhang L., Yu X., Ou J. Review of nanocarbon-engineered multifunctional cementitious composites. Composites: Part A, 2015; 70: 69–81.