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On the Difficulties and Pitfalls with the Analysis of Solid-State 13C NMR Spectra in Graphitic Materials

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Abstract

The difficulties and pitfalls with the interpretation of solid-state 13C nuclear magnetic resonance (NMR) spectra in graphitic materials are discussed in detail here, with special emphasis on the case of 13C-enriched samples, which have been used in several recent NMR studies. The issues with the spectral simulation and the interpretation of the spectral parameters obtained by some arbitrary models reported in the recent literature are examined and alternative methods to obtain informative experimental data and to analyze them in a more appropriate way are presented.

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References

  1. Y. Maniwa, M. Sato, K. Kume, M.E. Kozlov, M. Tokumoto, Carbon 34, 1287–1291 (1996)

    Article  Google Scholar 

  2. C. Goze-Bac, S. Latil, P. Lauginie, V. Jourdain, J. Conard, L. Duclaux, A. Rubio, P. Bernier, Carbon 40, 1825–1842 (2002)

    Article  Google Scholar 

  3. J.C.C. Freitas, A.G. Cunha, F.G. Emmerich, in Chemistry and Physics of Carbon, ed. by L.R. Radovic (CRC Press, Boca Raton, 2012), pp. 85–170

  4. M. Deschamps, S. Cadars, E. Gilbert, P. Azaïs, E. Raymundo-Pinero, F. Béguin, D. Massiot, Solid State Nucl. Magn. Reson. 42, 81–86 (2012)

    Article  Google Scholar 

  5. J.C.C. Freitas, F.G. Emmerich, G.R.C. Cernicchiaro, L.C. Sampaio, T.J. Bonagamba, Solid State Nucl. Magn. Reson. 20, 61–73 (2001)

    Article  Google Scholar 

  6. M.A. Vieira, G.R. Gonçalves, D.F. Cipriano, M.A. Schettino Jr., E.A. Silva Filho, A.G. Cunha, F.G. Emmerich, J.C.C. Freitas, Carbon 98, 496–503 (2016)

    Article  Google Scholar 

  7. A.M. Panich, A.I. Shames, N.A. Sergeev, M. Olszewski, J.K. McDonough, V.N. Mochalin, Y. Gogotsi, J. Phys. Condens. Matter 25, 245303 (2013)

    Article  ADS  Google Scholar 

  8. A.M. Panich, A.I. Shames, M.I. Tsindlekht, V.Y. Osipov, M. Patel, K. Savaram, H. He, J. Phys. Chem. C 120, 3042 (2016)

    Article  Google Scholar 

  9. S. Stankovich, D.A. Dikin, R.D. Piner, K.A. Kohlhaas, A. Kleinhammes, Y. Jia, Y. Wu, S.T. Nguyen, R.S. Ruoff, Carbon 45, 1558–1565 (2007)

    Article  Google Scholar 

  10. Y. Si, E.T. Samulski, Nano Lett. 8, 1679–1682 (2008)

    Article  ADS  Google Scholar 

  11. W. Gao, L.B. Alemany, L. Ci, P.M. Ajayan, Nat. Chem. 1, 403–408 (2009)

    Article  Google Scholar 

  12. A.M. Panich, A.I. Shames, A.E. Aleksenskii, A. Dideikin, Solid State Commun. 152, 466–468 (2012)

    Article  ADS  Google Scholar 

  13. N.A. Sergeev, A.M. Panich, S.D. Goren, Appl. Magn. Reson. 49, 999–1010 (2018)

    Article  Google Scholar 

  14. S. Hayashi, F. Hoshi, T. Ishikura, M. Yumura, S. Ohshima, Carbon 41, 3047–3056 (2003)

    Article  Google Scholar 

  15. W. Cai, R.D. Piner, F.J. Stadermann, S. Park, M.A. Shaibat, Y. Ishii, D. Yang, A. Velamakanni, S.J. An, M. Stoller, J. An, D. Chen, R.S. Ruoff, Science 321, 1815–1817 (2008)

    Article  ADS  Google Scholar 

  16. L.B. Casabianca, M.A. Shaibat, W.W. Cai, S. Park, R. Piner, R.S. Ruoff, Y. Ishi, J. Am. Chem. Soc. 132, 5672–5676 (2010)

    Article  Google Scholar 

  17. Y.V. Fedoseeva, A.V. Okotrub, V.O. Koroteev, Y.M. Borzdov, Y.N. Palyanov, Y.V. Shubin, E.A. Maksimovskiy, A.A. Makarova, W. Münchgesang, L.G. Bulusheva, A. Vyalikh, Carbon 141, 323–330 (2019)

    Article  Google Scholar 

  18. D.L. VanderHart, W.L. Earl, A.N. Garroway, J. Magn. Reson. 44, 361–401 (1981)

    ADS  Google Scholar 

  19. V.E. Zorin, S.P. Brown, P. Hodgkinson, J. Chem. Phys. 125, 144508 (2006)

    Article  ADS  Google Scholar 

  20. V.O. Koroteev, W. Münchgesang, Y.V. Shubin, Y.N. Palyanov, P.E. Plyusnin, D.A. Smirnov, K.A. Kovalenko, M. Bobnar, R. Gumeniuk, E. Brendler, D.C. Meyer, L.G. Bulusheva, A.V. Okotrub, A. Vyalikh, Carbon 124, 161–169 (2017)

    Article  Google Scholar 

  21. M.M. Golzan, P.B. Lukins, D.R. McKenzie, A.M. Vassallo, J.V. Hanna, Chem. Phys. 193, 167–172 (1995)

    Article  Google Scholar 

  22. F. Mauri, B.G. Pfrommer, S.G. Louie, Phys. Rev. Lett. 79, 2340–2343 (1997)

    Article  ADS  Google Scholar 

  23. T.M. Alam, T.A. Friedmann, P.A. Schultz, D. Sebastiani, Phys. Rev. B 67, 245309 (2003)

    Article  ADS  Google Scholar 

  24. E. Zurek, C.J. Pickard, J. Autschbach, J. Phys. Chem. C 112, 11744–11750 (2008)

    Article  Google Scholar 

  25. L.B. Casabianca, J. Phys. Chem. A 120, 7011–7019 (2016)

    Article  Google Scholar 

  26. P.A. Christy, A.J. Peter, C.W. Lee, Solid State Commun. 283, 22–26 (2018)

    Article  ADS  Google Scholar 

  27. G. Cho, B.K. Yen, C.A. Klug, J. Appl. Phys. 104, 013531 (2008)

    Article  ADS  Google Scholar 

  28. J. Mao, X. Cao, D.C. Olk, W. Chu, K. Schmidt-Rohr, Prog. Nucl. Magn. Reson. Spectrosc. 100, 17–51 (2017)

    Article  Google Scholar 

  29. J.Z. Hu, M.S. Solum, C.M.V. Taylor, R.J. Pugmire, D.M. Grant, Energy Fuels 15, 14–22 (2001)

    Article  Google Scholar 

  30. D. Massiot, F. Fayon, M. Capron, I. King, S. Le Calvé, B. Alonso, J.-O. Durand, B. Bujoli, Z. Gan, G. Hoatson, Magn. Reson. Chem. 40, 70–76 (2002)

    Article  Google Scholar 

  31. R.K. Harris, E.D. Becker, S.M.C. De Menezes, P. Granger, R.E. Hoffman, K.W. Zilm, Pure Appl. Chem. 80, 59–84 (2008)

    Article  Google Scholar 

  32. F.A.L. De Souza, A.R. Ambrozio, E.S. Souza, D.F. Cipriano, W.L. Scopel, J.C.C. Freitas, J. Phys. Chem. C 120, 27707–27716 (2016)

    Article  Google Scholar 

  33. P. Lauginie, A. Messaoudi, J. Conard, Synth. Met. 55–57, 3002–3007 (1993)

    Article  Google Scholar 

  34. N.K. Sethi, R.J. Pugmire, J.C. Facelli, D.M. Grant, Anal. Chem. 60, 1574–1579 (1988)

    Article  Google Scholar 

  35. H. Darmstadt, C. Roy, S. Kaliaguine, G. Xu, M. Auger, A. Tuel, V. Rmaswamy, Carbon 38, 1279–1287 (2000)

    Article  Google Scholar 

  36. J. Vähäkängas, S. Ikäläinen, P. Lantto, J. Vaara, Phys Chem Chem Phys 15, 4634–4641 (2013)

    Article  Google Scholar 

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Acknowledgements

The financial support from the Brazilian agencies CNPq (Grant 408001/2016-0), FAPES (Grant 73296872, TO 21/2016) and CAPES (Grant 88881.178317/2018-01) is gratefully acknowledged.

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Correspondence to Jair C. C. Freitas.

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Freitas, J.C.C. On the Difficulties and Pitfalls with the Analysis of Solid-State 13C NMR Spectra in Graphitic Materials. Appl Magn Reson 50, 1245–1252 (2019). https://doi.org/10.1007/s00723-019-01151-7

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  • DOI: https://doi.org/10.1007/s00723-019-01151-7

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