Supporting Information:

Ex-MWNTs: Graphene Sheets and Ribbons Produced by

Lithium Intercalation and Exfoliation of Carbon Nanotubes
Abraham G. Cano-Márquez, Fernando J. Rodríguez-Macías, Jessica Campos-Delgado, Claudia
G. Espinosa-González, Ferdinando Tristán-López, Daniel Ramírez-González, David A. Cullen,
David J. Smith, Mauricio Terrones, and Yadira I. Vega-Cantú*

Nano Letters, DOI: 10.1021/nl803585s

Materials Characterization
AFM images were acquired with a JEOL JSPM-5200, TEM images with a Tecnai F20 and a JEOL
4000EX. We used a Bruker D8-Advance for the X-Ray difractograms, a Renishaw InVia microRaman
for Raman spectroscopy, and a Thermo Haake Caahn Versatherm HS for thermogravimetry. FTIR
spectra were collected with a ThermoNicolet 6700 spectrometer with a DTGS KBr detector, KBr beam
splitter, and an ATR attachment (ZnSe crystal).

Figure S1. Treating cut MWNTs in NH3 without lithium shows that Li must intercalate to obtain
ex-MWNTs. Exfoliation and unwrapping are not seen for this blank experiment after acid and thermal
treatments. SEM images such as (A) show only surface damage similar to the one seen on the starting
acid cut MWNTs. STEM images such as (B) clearly show that the MWNT do not unwrap, and catalytic
metal particles can still be seen in the center of the nanotubes.
Figure S2. (A) Height of steps for ex-MWNT of figure 7A (the correct aspect ratio is the one shown in
Figure 7A), the steps marked as 1, 2 and 3 would be about 75, 40, and 239 layers respectively. The
latter number corresponds to the maximum range of diameters for the MWNT used, suggesting that the
layered material observed here is formed by the superposition of more than one ex-MWNT. (B) Heights
of some graphene flakes seen on the ex-MWNTs surface. The region measured corresponds to the lower
left corner of Fig. 7B. The heights of the graphene layers are not completely uniform, 1 corresponds to
~9 graphene layers, 2 corresponds to ~24, and 3 to ~13 layers.

Figure S3. (A) Topography image of an ex-MWNT and the graphene flakes generated in the process,
(B) Phase Image, the contrast between regions is mostly a result of topography, indicating similar
surface properties as would be expected for graphene pieces and open MWNTs over HOPG.

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Figure S4. First-derivative from TGA analysis (flowing air, 10 ºC/min ramp): (A) As-synthesized
MWNT, (B) purified MWNT have a lower onset of burning since the purification treatment opens the
tips and may cause some wall damage, (C) cut-MWNT show a very low onset due to the presence of
oxidized carbon material, (D) ex-MWNT material, exfoliated by HCl and thermal treatments. The
observed shoulders may be due to functional groups, defects, and reactive sites. T0 is the temperature at
which the maximum oxidation rate occurs. %RM is the percentage of residual material after burning.

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Figure S5. FTIR spectra (1068 scans, resolution of 8) of: (a) As-synthesized MWNT, (b) purified
MWNT, (c) cut-MWNT, (d) ex-MWNT material, intercalated and acid treated, (e) ex-MWNT material
after acid and thermal treatments.

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