50
4 Cathodic Exfoliation of Graphite in Molten Salt Electrolytes
Fig. 4.11 Photographs of an
industrial-grade graphite rod
a before and b after being
used as the cathode during
the electrolysis of molten
LiCl–30 wt% SnCl 2 under
Ar atmosphere, using the
experimental setup exhibited
in Fig. 4.2a. The electrolysis
process was conducted in
molten LiCl at 770 °C for 2 h
at the constant current of 33
A, corresponding to an initial
cathode current density of
about 1 A cm −2 . No obvious
erosion of the electrode was
observed. Moreover, a Sn
disk could be observed at the
bottom of the cathode,
reproduced from Ref. [36],
copyright 2019, with
permission from Elsevier
length of two stainless steel electrical connectors. The graphite electrode used as the
cathode was eventually eroded, as shown in Fig. 4.12c, during which the SnCl 2 pellets were being added into the molten salt at varying intervals during the electrolysis
process. This figure displays the photographs of the graphite rod before and after
being used as cathode in the molten salt process for varying time periods of 20 min
and 2 h. At these intervals, total of 20 and 85 g SnCl 2 , respectively, had been added
to the melt. The mixture of solidified salt and Sn-filled carbon nanostructures inside
the graphite crucible is shown in Fig. 4.12c. About 20 g Sn–C hybrid material was
able to be attained after 2 h of electrolysis [34].
As depicted in Fig. 4.13a, the electrolytic product typically comprised of core–
shell tubular or spherical nanostructures with a typical dimension of less than 100 nm.
The central cavity of tubes and particles could be packed with Sn, as evidenced by
the energy-dispersive X-ray (EDX) analysis or preferentially the electron energy loss
spectroscopy (EELS) measurements, as shown in Fig. 4.13b. This figure illustrates a
STEM micrograph recorded on an incompletely filled carbon nanotube. Moreover,
as displayed EELS spectra were measured on the filled and empty area of the tube.
The spectrum measured at the hollow cavity of the CNT shows the presence of C
K-shell ionization edge at roughly 24 eV, while the spectra recorded on the filled
4 Cathodic Exfoliation of Graphite in Molten Salt Electrolytes
Fig. 4.11 Photographs of an
industrial-grade graphite rod
a before and b after being
used as the cathode during
the electrolysis of molten
LiCl–30 wt% SnCl 2 under
Ar atmosphere, using the
experimental setup exhibited
in Fig. 4.2a. The electrolysis
process was conducted in
molten LiCl at 770 °C for 2 h
at the constant current of 33
A, corresponding to an initial
cathode current density of
about 1 A cm −2 . No obvious
erosion of the electrode was
observed. Moreover, a Sn
disk could be observed at the
bottom of the cathode,
reproduced from Ref. [36],
copyright 2019, with
permission from Elsevier
length of two stainless steel electrical connectors. The graphite electrode used as the
cathode was eventually eroded, as shown in Fig. 4.12c, during which the SnCl 2 pellets were being added into the molten salt at varying intervals during the electrolysis
process. This figure displays the photographs of the graphite rod before and after
being used as cathode in the molten salt process for varying time periods of 20 min
and 2 h. At these intervals, total of 20 and 85 g SnCl 2 , respectively, had been added
to the melt. The mixture of solidified salt and Sn-filled carbon nanostructures inside
the graphite crucible is shown in Fig. 4.12c. About 20 g Sn–C hybrid material was
able to be attained after 2 h of electrolysis [34].
As depicted in Fig. 4.13a, the electrolytic product typically comprised of core–
shell tubular or spherical nanostructures with a typical dimension of less than 100 nm.
The central cavity of tubes and particles could be packed with Sn, as evidenced by
the energy-dispersive X-ray (EDX) analysis or preferentially the electron energy loss
spectroscopy (EELS) measurements, as shown in Fig. 4.13b. This figure illustrates a
STEM micrograph recorded on an incompletely filled carbon nanotube. Moreover,
as displayed EELS spectra were measured on the filled and empty area of the tube.
The spectrum measured at the hollow cavity of the CNT shows the presence of C
K-shell ionization edge at roughly 24 eV, while the spectra recorded on the filled