TY - JOUR

T1 - Multiscale characterization of 13C-enriched fine-grained graphitic materials for chemical and electrochemical applications

AU - Koroteev, V. O.

AU - Münchgesang, W.

AU - Shubin, Yu V.

AU - Palyanov, Yu N.

AU - Plyusnin, P. E.

AU - Smirnov, D. A.

AU - Kovalenko, K. A.

AU - Bobnar, M.

AU - Gumeniuk, R.

AU - Brendler, E.

AU - Meyer, D. C.

AU - Bulusheva, L. G.

AU - Okotrub, A. V.

AU - Vyalikh, A.

N1 - Funding Information: We thank Dr. E. I. Zhmurikov for providing the pristine sample of 13 C carbon material, Mr. S.I. Kozhemyachenko for the measurements of Raman spectra, Mr. A.V. Ishchenko for the HRTEM measurements, and Dr. M. Avdeev and Dr. A. Knop-Gericke for fruitful discussion. We are also grateful to the bilateral Program “Russian-German Laboratory at BESSY II” for the assistance in XPS and NEXAFS measurements. Financial support of the Ministry of Education and Science of the Russian Federation (agreement № RFMEFI61614X0007 ) and the Bundesministerium für Bildung und Forschung (grant № 05K14OFA ) in the framework of joint Russian-German research project “SYnchrotron and NEutron STudies for Energy Storage (SyNeSteSia)” is greatly acknowledged. V.O.K. thanks the German-Russian Interdisciplinary Science Center (Grant # C-2016a-2 ). Publisher Copyright: © 2017 Elsevier Ltd

PY - 2017/11/1

Y1 - 2017/11/1

N2 - 13C-enriched fine-grained graphitic material has been studied towards its potential for chemical and electrochemical applications. The structural and morphological modification of the material as results of pressure-assisted thermal treatment and gaseous BrF3 and/or Br2 room-temperature treatments has been investigated using a combination of the characterization tools: electron microscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron and near edge X-ray absorption fine structure spectroscopy, solid state nuclear magnetic resonance (NMR) spectroscopy and magnetic susceptibility measurements. It has been found that the starting material represents graphitized carbon with oxygen containing defects. The evidence of distorted sp2 hybridization of carbon was found in the Raman and the 13C NMR spectra. Under high pressure and temperature, some initially open graphitic edges are coupled that causes decreasing specific surface area and mean in-plane size of crystallites, and, generally, a higher degree of disorder. The Br2 treatment improves the material structure due to removal of tiny graphitic flakes and oxygenated carbon groups. The use of BrF3 results, in addition, in partial fluorination of graphitic material. Electrochemical characteristics along with a high degree of 13C isotope enrichment enable the application of these graphitic materials in operando studies using methods sensitive to 13C isotope, such as NMR.

AB - 13C-enriched fine-grained graphitic material has been studied towards its potential for chemical and electrochemical applications. The structural and morphological modification of the material as results of pressure-assisted thermal treatment and gaseous BrF3 and/or Br2 room-temperature treatments has been investigated using a combination of the characterization tools: electron microscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron and near edge X-ray absorption fine structure spectroscopy, solid state nuclear magnetic resonance (NMR) spectroscopy and magnetic susceptibility measurements. It has been found that the starting material represents graphitized carbon with oxygen containing defects. The evidence of distorted sp2 hybridization of carbon was found in the Raman and the 13C NMR spectra. Under high pressure and temperature, some initially open graphitic edges are coupled that causes decreasing specific surface area and mean in-plane size of crystallites, and, generally, a higher degree of disorder. The Br2 treatment improves the material structure due to removal of tiny graphitic flakes and oxygenated carbon groups. The use of BrF3 results, in addition, in partial fluorination of graphitic material. Electrochemical characteristics along with a high degree of 13C isotope enrichment enable the application of these graphitic materials in operando studies using methods sensitive to 13C isotope, such as NMR.

KW - SOLID-STATE NMR

KW - RAMAN-SPECTRA

KW - ION BATTERIES

KW - CARBON

KW - TEMPERATURE

KW - STORAGE

KW - PERFORMANCE

KW - DESIGN

KW - LAYERS

KW - CELLS

UR - http://www.scopus.com/inward/record.url?scp=85028339397&partnerID=8YFLogxK

U2 - 10.1016/j.carbon.2017.08.038

DO - 10.1016/j.carbon.2017.08.038

M3 - Article

AN - SCOPUS:85028339397

VL - 124

SP - 161

EP - 169

JO - Carbon

JF - Carbon

SN - 0008-6223

ER -