Yellampalli S. (ed.) Carbon Nanotubes - Synthesis, Characterization, Applications
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Carbon Nanotube-Based Thin Films: Synthesis and Properties
507
-0.2 0.0 0.2 0.4 0.6 0.8 1.0
-0.0012
-0.0008
-0.0004
0.0000
0.0004
1cycle
2cycle
3cycle
4cycle
5cycle
i/mA
E/V (vs. Ag/AgCl)
a
b
Fig. 12. CV traces of (a) SWNT SAM–ITO and (b) SWNT SAM–ITO endcapped by tetramer
aniline groups in an aqueous 1.0 M H
2
SO
4
solution. Scan rate = 0.05 V/s. Reproduced with
permission from Ref. [149]. Copyright 2009 Chemical Society of Japan.
Fig. 13. Tapping mode AFM images of (a) SAM–ITO and (b) tetramer aniline-terminated
ITO surface. Insert (c) shows the high-resolution image of an SWNT surface after being
endcapped by tetramer aniline. Reproduced with permission from Ref. [149]. Copyright
2009 Chemical Society of Japan.
Carbon Nanotubes - Synthesis, Characterization, Applications
508
Fig. 14. The XPS wide-scan spectra of: (a) pristine ITO, (c) SAM–ITO, (e) tetramer aniline-
terminated ITO surface, and (b), (d), and (f) their corresponding high resolution N 1s, S 2p,
C 1s, and Si 2p spectra, respectively. Reproduced with permission from Ref. [149].
Copyright 2009 Chemical Society of Japan.
However, the CV data recorded for tetramer aniline end-capped SAM–ITO (Figure 12b)
showed two reversible redox couples occurring at 0.50 and 0.40 V under the same
conditions, which were assigned to the oxidation and reduction of the tetramer aniline
between the leucoemeraldine and emeraldine oxidation states. Moreover, this was very
reproducible, indicating that the stability of the SAM–ITO was improved after being end-
capped by the tetramer aniline molecules.
From the AFM images in Figure 13, the SAM–ITO plate showed a monolayer with tube-like
particle topography, implying the successful incorporation of functionalized SWNTs onto
the ITO surface. The average length of the functionalized SWNTs is around 100 nm, with
average diameter of around 20 nm. The morphology of the obtained SWNT layer was
significantly changed after being end-capped using tetramer aniline groups (Figure 13b),
Carbon Nanotube-Based Thin Films: Synthesis and Properties
509
which showed a rougher SWNT surface compared with that of SWNT–ITO (see arrow label
in Figure 13c). From the AFM image shown in Figure 13b, the average length of the tetramer
aniline terminated SWNTs is around 200 nm with an average diameter of around 40 nm,
which showed a significant increase compared with that of the pure SWNT layer, because of
the presence of a tetramer aniline particle layer linked with functionalized SWNTs by
chemical bonds.
The XPS analysis showed the oxygen-containing defects on functionalized SWNT walls
were covered and protected by tetramer aniline groups after end-capping, as shown in
Figure 14. In addition to the intense and sharp features of the In 3d, Sn 3d, and O 1s peaks,
the spectrum of the bare ITO plate exhibited weak C 1s and Si 2p peaks, which correspond
to minor surface carbon contamination and the silicon from the glass, respectively (Figures
14a and 14b).[156] After attachment of the soluble functionalized SWNT, the peak intensity
of the In 3d, Sn 3d, and O 1s peaks decreased, and the Si 2p peaks increased, because of the
linked APTMS agent between the ITO layer and the functionalized SWNT (Figures 14c and
14d). In addition, the observed S 2p feature showed the presence of acid sulfonate (–SO
2
OH)
groups on the functionalized SWNTs. Aside from the C–C/ C–H peak at 285.3 eV, an
additional photoemission representing the higher binding energy bands indicated the
presence of carbon atoms bonded to other functional groups. The binding energy peak
occurring at 290 eV was attributed to C=O and O–C=O groups from the functionalized
SWNTs. The two-peak feature of O 1s peaks (denoted by asterisks in Figure 14c) shown in
the wide-scan spectra compared to that of the bare ITO plate, also offers evidence for
different chemical bonded states that correspond to COOH groups on the functionalized
SWNT surface. However, after end-capping the residual carboxyl acid groups by the
tetramer aniline terminated by amine groups, the intensity of the C 1s and O 1s features in
the higher binding energy bands was significantly decreased to form a shoulder peak, as
shown in Figures 14e and 14f. In addition, from the corresponding peak areas, the atomic
content of the C 1s and N 1s peaks was enhanced compared to that of the In 3d or Sn 3d
peaks. This is reasonable, considering that the enriched particle assembled by end-
terminated tetramer aniline molecules tightly covered the sidewalls of the soluble
functionalized SWNT via – interactions, where only the photoemission of the C 1s and N
1s peaks assigned to the tetramer aniline backbone was detected. This results in an increase
of the N 1s and C 1s peaks in the lower binding energy bands, and a decrease in the C 1s
and O 1s peaks in the higher binding energy bands.
As discussed above, the conjugate layer, assembled by the end-terminated tetramer aniline
molecules, tightly covered the sidewalls of the soluble functionalized SWNTs via covalent
bonding and – interactions, together with the doping effect between tetramer aniline and
the sulfonic groups on the SWNT surface, which made the SWNT layer more stable in the
CV scans in acidic aqueous solutions. It is expected that this stable electroactive SWNT layer
will find a wealth of applications in nanocomposite architectures.
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