Статья поступила в редакцию 19.10.14. Ред. per. № 2120
The article has entered in publishing office 19.10.14. Ed. reg. No. 2120
УДК 541.145+541.141.3
SYNTHESIS AND CHARACTERIZATION OF GRAPHENE-BASED
MATERIALS PRODUCED VIA THERMAL EXFOLIATION OF GRAPHENE OXIDE AND OF ClF3 INTERCALATED GRAPHITE
Oleksandr B. Bondarchuk1*, Anatoly S. Lobach2, Sergey A. Baskakov2, Natalia G. Spitsyna2, Aleksandr V. Ryzhkov3, Valery A. Kazakov4, Alexander Michtchenko5, Alexander L. Gusev6, Roman D. Mysyk1,
Yury M. Shulga27
'CIC energiGUNE, Parque Tecnológico c/ Albert Einstein 48, 01510 Miñano, Alava, Spain 2Institute of Problems of Chemical Physics RAS 1 Ac. Semenov Av., Moscow Region, Chernogolovka, 142432 Russian Federation 3National Research Center "Kurchatov Institute" 1 Kurchatov sq., Moscow, 123182 Russian Federation
4Keldysh Research Center 8 Onezhskaya, Moscow, 125438 Russian Federation
5
5Instituto Politecnico Nacional, SEPI-ESIME-Zacatenco
C.P. 07738, D.F., Mexico
Scientific and Technical Center" TATA"" LLC
Post Box Office 683, Sarov, Nizhny Novgorod, 607183 Russian Federation i-
i
ph./fax: (83130)6-31-07, e-mail: gusev@hydrogen.ru National University of Science and Technology MISIS 4 Leninsky pr., Moscow, 119049 Russian Federation
doi: 10.15518/isjaee. 2014.19.001
ti
Referred 21 October 2014 Received in revised from 24 October 2014 Accepted 27 October 2014
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Graphene-based materials GM1 and GM2 have been synthesized by explosive exfoliating two different precursors: graphite oxide and graphite intercalated with chlorine trifluoride respectively. Compositional and structural transformations of the precursors into final graphene-based materials have been followed by using combination of X-ray photoelectron spectroscopy, FTIR and Raman spectroscopy, and Scanning Electron Microscopy. Specific surface area, pore size and electrical conductivity of the synthesized materials have also been measured.
Comparative mass spectrometry analysis of the gas co-products emitted during synthesis has revealed that synthesis of GM1 from graphite oxide is more environmentally viable. However, synthesized GM2 materials possess higher electrical conductivity and are characterized by larger size of graphene sheets.
We have demonstrated that the graphene nanosheets can be produced from suspensions of the GM1 and GM2 materials in the aqueous solution of a surfactant dodecylbenzenesulfonate.
The potential applications areas for the synthesized materials have been discussed.
Key words: Graphen-based materials, XPS, Raman spectroscopy.
International Scientific Journal for JM, n r- ——, №19(159) Международный научный журнал
Alternative Energy and Ecology -tSi- Г^)М,С\ H г-> ?ni4 «Альтернативная энергетика и экология»
©ScientificTechnical Centre «ТАТА», 2014 "^T^ —J<-— —'—> © Научно-технический центр «ТАТА», 2014
Бондарчук Александр
Борисович Oleksandr Bondarchuk
Сведения об авторе: кандидат физико-математических наук, заведующий лабораторией научно-исследовательского центра CIC energiGUNE, Миняно, Испания.
Образование: инженер-физик, радиофизический факультет Киевского университета им. Т.Г. Шевченко.
Область научных интересов: физика поверхности, рентгеновская спектроскопия, сканирующая зондовая микроскопия Публикации: около 40.
Information about the author: PhD
(physics), Head of Surface Science Laboratory of research center CIC energiGUNE, Minano, Spain.
Education: engineer-physicist, Faculty of Radiophysics, Taras Shevchenko National University of Kyiv, Ukraine.
Area of researches: surface science, X-ray photoelectron spectroscopy, scanning probe microscopy.
Publications: about 40.
Лобач Анатолий
Степанович Lobach Anatoly Stepanovich
Сведения об авторе: кандидат химических наук, старший научный сотрудник Института проблем химической физики РАН.
Образование: инженер-технолог, Московский химико-технологический институт им. Д.И. Менделеева.
Область научных интересов: химия углеродных наноматериалов, композиционные наноматериалы.
Публикации: более 100 работ в рецензируемых журналах; индекс Хирша 18.
Information about the author: Ph.D. (Chemistry), Senior research scientist of Institute of Problems of Chemical Physics Russian Academy of Science.
Education: engineer-technologist, Moscow D. Mendeleev Institute of Chemical Technology.
Area of researches: chemistry of carbon nanomaterials, composite nanomaterials.
Publications: more 100 peer-reviewed articles; h-index is 18.
M, - С -'м1
с о
Баскаков Сергей
Алексеевич Baskakov Sergey Alekseevich
Сведения об авторе: кандидат химических наук, старший научный сотрудник Института проблем химической физики РАН.
Образование: химик, Ивановский
государственный университет, биолого-химический факультет.
Область научных интересов: углеродные наноматериалы, композиционные материалы на основе графена, суперконденсаторы.
Публикации: автор более 30 научных работ в рецензируемых журналах.
Information about the author: Ph.D. (Chemistry), Senior research scientist of Institute of Problems of Chemical Physics Russian Academy of Science.
Education: chemist, Ivanovo State University, Faculty of Biology and Chemistry
Area of researches: carbon nanomaterials, composite materials based on graphene, supercapacitors.
Publications: more than 30 scientific publications.
МысыкРоман Дмитривич Roman Mysyk
Сведения об авторе: кандидат химических наук, заведующий группой суперкондесаторов научно-исследовательского центра С1С energiGUNE, Миняно, Испания.
Образование: инженер-химик, факультет экологии и химической технологии, Донецкий технический университет.
Область научных интересов: углеродные наноматериалы, суперкондесаторы (ионисторы).
Публикации: около 30 научных работ.
Information about the author:
Candidate of Science (PhD in Chemistry), Leader of Capacitor Group, research center CIC energiGUNE, Minano, Spain.
Education: engineer-chemist, Faculty of Ecology and Chemical Technology, Donetsk Technical University, Ukraine.
Area of researches: carbon nanomaterials, supercapacitors.
Publications: about 30 scientific publications.
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1. Introduction
Porous materials possessing low density in combination with high electrical conductivity and high specific surface area are demanded for various applications, particularly as electrode materials for the electrical energy storage devices. Graphene foam could be an idea candidate for this role. Graphene foam is synthesized by high temperature treatment of metal foam in atmosphere of hydrocarbons - CVD deposition, after which the metal is processed away [1-12]. The result is 3D mesh but constructed of graphene. Unfortunately, large scale production of graphene foam in this way is hindered by high production cost. Therefore several others strategies have been explored recently. Among them are explosive exfoliation of graphite oxide (GO) [13-15] or thermal exfoliation of graphite intercalated by reactive molecules [16-18]. The materials produced in these ways are believed to have properties similar to graphene foam.
In this work we have carried out a comparative study of the graphene-based materials synthesized by using explosive exfoliation of two different precursors: GO and graphite intercalated with ClF3. Special attention in this study has been given to identification of the potentially hazardous gaseous substances generated during explosive exfoliation of the precursors.
Q.
2. Experimental
c
Graphite oxide was prepared using modified Hammerss method [19]. The details of the preparation procedure can be found elsewhere [20]. The suspensions were made by mixing up GO (100 mg) with water (100mg) in a glass vial. GO films with thickness of 200300 wm were prepared by precipitating top layer of water suspension on a cover glass and then the GO films were mechanically removed from the support.
Samples of GO film with area about 1 cm2 were introduced into a deep glass bottle, to collect the explosion products the open part of the bottle was covered with a filter (cotton tissue). Then the bottle was heated up in a microwave oven (2450 MHz, 900 W) until the content of the bottle has exploded. The heating was stopped immediately with the onset of explosion The material prepared in the above described wa will be referred as graphene-based material of type 1 or GM1.
Graphene-based material of 2d type (GM2) was synthesized in several steps. Intercalation of highly oriented pyrolytic graphite (HOPG) at room temperature with liquid ClF3 was the first step. In the second step the product of graphite intercalation (PIG) underwent fast heating until onset of explosion. The intercalation procedure was similar to the one described elsewhere [21]. A 110 mg HOPG sample was put in a PTFE reactor and further treated with ClF3 gas. The pressure of ClF3 was gradually increased from 0 to 15 bar over 4 hours and then it was dwelling at the maximum pressure for
another 2 hours. In the next step the gas was condensed at -196 °C, and the sample was held in liquid ClF3 at room temperature for 8 days. Produced PIG is a layered material with golden colour, its volume is ~70-100 times of the initially pristine HOPG sample. Weight of the intercalated sample increased up to 190 mg. PIG sample was exfoliated by sealing it off in a long quartz ampoule which then was introduced for 10-20 s into a muffle furnace heated up to + 750 °C. Thermally stimulated explosion rendered PIG into black powder - GM2 sample. Weight of the GM2 yield was about ~70 mass % of the HOPG load.
GM suspensions were prepared by ultrasonic-assisted dispersion of the material in an aqueous surfactant solution, dodecylbenzenesulfonate (0.5 % w/v), using an ultrasonic dispenser UZDN-1 (frequency 35 kHz, power 500 W, treatment time 30 min), which was followed by ultracentrifugation (10000 g, 30 min). Optical absorption spectra of the suspensions were recorded using a UV-Vis-NIR Scanning Spectrophotometer (Shimadzu UV-3101PC) in the wavelength range from 200 to 1400 nm.
For ident
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