Resonance Raman Spectra of acid treated single-wall

carbon nanotubes

Greg Sonnenfeld
Department of Physics, New Mexico State University, Las Cruces New Mexico 88003

Resonance Raman spectroscopy was used to characterize the Raman spectra of nitric acid treated SWNT treated
nanotubes. The Stokes spectra of treated SWNT and pristine SWNT were taken at laser excitation levels of
488nm, 514nm and 785nm. Lorentzian fits of the dominate peaks were extrapolated via the Levenberg-
-1
Marquardt fitting algorithm between 500-3000 cm including the D, Gƒ, and D* modes. Comparisons
revealed a large increase in the D mode intensity, a broadening of the G+ peaks, a decrease in D* intensity, the
elimination of intermediate modes, and correlation between defects and the g2- and g2+ peaks.

The study of chemically treated carbon nanotubes is
essential for the advancement of nano-based
technology. Chemical treatments have been used for
purification as well as chemical functionalization.
Nitric acid treatment of single wall nanotubes (SWNT)
has been evaluated as a step in methods of removing
impurities7,11 and has been proposed in large scale
SWNT production process7. The effect of nitric acid
treatment on the phonon modes of SWNT and
impurities is therefore of interest.
Much previous work in Raman spectroscopy has been
used to characterize pristine SWNT. Regions of
interest in semiconductor SWNT nanotubes have been
identified as the Radial Breathing Mode (RBM)
occurring at ω ≈150-220 cm-1, the Defect Mode (D)
occurring at ω ≈ 350 cm-1, the High Energy Mode
(HEM) or G-band at ω ≈ 1550-1600 cm-1, and the D*
band ω ≈ 2700 cm-1.2
The RBM is inversely proportional to the diameter of
the nanotube with smaller diameters yielding larger
Raman shifts.2 The filters used in studies diminished
this band, so further discussion will be limited.
The D mode has been identified as a disorder induced
mode1,3,5,10 caused by defects in the nanotube structure.
It is a double resonance process similar to the defect
mode in graphite appearing under the same name. The
D* mode is a second harmonic of the D mode. Both the
D and D* modes are sensitive to chirality and diameter
and can be used to characterizing individual SWNT.
The D* mode will occasionally exhibit multiple peaks,
this is the result of interlayer coupling .1
The G- band is closely related to the ω ≈ 1582 cm-1
peak arising in 2-D graphite1. It is typically identified
by two sets of coupled peaks known as the G+ and the
G- modes. The G+ modes at ω ≈ 1590 cm-1 and ω ≈
1607 cm-1 have been identified as the phonon mode
(LO) along the length of the nanotube and is
independent of radius1,2. The G- mode is slightly more
complex and is dependant on tube radius. The radial
dependence of the G- mode has inferred that the
phonon mode is along the circumference of tubes
surface, thus being identified as the tangential phonon
mode (TO).1,2 The Raman shift of the G- phonon mode
has been experimental determined by comparison with
the RBM of individually measured nanotubes. The
diameter dependence is approximately
ω g− = ω g+ − c
d 2t (1)
where C = 47.7 cm-1 and wg+ 1591 cm-1, for a
semiconducting SWNT.2 For a tube diameter of ~1.3cm
peaks occur at ω ≈ 1549 cm-1 and ω ≈ 1567 cm-1. The
exact origin of the several G+ and G- peaks is a topic of
debate, with some believing they are defect induced6,
while others have concluded defect free, or “perfect”
SWNT should exhibit strong first order G-band
resonance features5.
Impurities also exist in raw SWNT, if nothing else, in
the form of graphite and amorphous carbon. Peaks of
this nature will be discussed as they arise.
Raman Spectroscopy Background
The following section a general review of Raman
Spectroscopy. For those already familiar with the
process, it may be skipped with out an interruption in
continuity.
Raman spectroscopy has long been an important tool
for analysis of the vibration modes of molecules.
Raman spectroscopy relies on the Raman Effect, the
inelastic scattering of light.
Photons incident on a material are usually scattered
via the elastic Rayleigh scattering where in the emitted
photon has the same energy as the incident photon.
Raman scattering is inelastic, emitting a photon with
energy shifted by some ∆E. This energy shift is the
result of a photon initially in a state Ei being raised to a
level Eexcited = Ei +Ephoton, then falling to a level Ej≠i. The
emitted photon thus carries an energy Eemitted = Ephoton
+∆E. It should be apparent that ∆E is the difference in
energy between Ej and Ei. This energy difference is
referred to as the Raman shift.
Raman shift is divided into two different shifts,
Stokes lines and anti-Stokes lines. Stokes lines occur
when an electron falls to an energy level higher than its
initial level producing a less energetic photon. Anti-
stokes lines occur when a photon falls to an energy
level lower than its initial level producing a more
energetic photon. Anti-stokes lines are often less
intense than stokes lines, as electrons have a higher
probability of occupying there lower energy states. It is
worth mentioning than, while stokes and anti-stokes
lines are often thought to be symmetric, asymmetries in
the peaks of Stokes and anti-Stokes lines have been
observed in materials such as single wall nanotubes [4].
Figure 1: Stokes and anti-Stokes transitions
It should be apparent that Raman spectroscopy is an
ideal method for characterizing the energy levels of
molecules or energy level differences between two
similar materials.
Resonance Raman spectroscopy (RRS) is an
enhanced method of Raman spectroscopy where a
material is driven near the resonance frequency of a
vibrational mode, yielded an intensity increase of
several orders of magnitude. RRS yields better results
for complex systems, or molecules that exhibit very low
Raman scattering intensities under non-resonant
conditions. The increase in intensity and sensitivity
observed in resonance Raman is thus well suited for
samples such as single wall nanotubes (SWNT) as
certain vibrational modes only exhibit significant
intensities when driven near resonance.
Experiment
Pristine SWNT were treated in a 3:1 solution of water
and nitric acid. Untreated SWNT served as a control for
comparison with the acid treated SWNT. Both
untreated and treated SWNT samples were prepared on
an intrinsic silicon slide. Spectra were taken on a
Rensihaw InVia Raman Spectrometer with laser lines
of 488nm, 514nm and 785nm at 20mW, 34mW and
380mW respectively. Spectral resolution was ~1.5 cm-1.
The system was calibrated to a reference of intrinsic
silicon and zero point corrected to its peak. The silicon
peak was approximately 0.5 cm-1 from nominal in each
calibration. Three measurements were taken of each
sample for each laser energy level with 5 accumulations
at 10 seconds at 5% power. The wave number range
spanned from 200 cm-1 to 3200 cm-1, the lower range
being imposed by a filter. The RBM was not available
for analysis. Peaks were extrapolated and averaged for
each laser energy level. Spectra were fitted by the
Levenberg-Marquardt algorithm, a recursive gradient
descent/LMS hybrid, to a sum of Lorentzian
distributions plus a linear component representing
background. The mean and variance of the mean were
taken over the three Lorentzian fits for each set of three
sample spectra per laser line. The systematic error from
the machine was added to the error.
Analysis and Discussion
An informative means of comparing the treated and
pristine SWNT samples is essential for producing
analyzable results.
The Lorentzian or Cauchy distribution,
1
Γ
Lx = 1
π
2
x−x o  + 12 Γ 2
2
(2)
has long been used to describe resonance behavior. The
Lorentzian (and to a lesser extend the Breit-Wigner-
Fano8 for certain metallic SWNT modes) is the model
most often used to fit resonance Raman spectra for
nanotubes1,2,3,4. It has been theorized by Woldeohannes,
John and Rupasov that the Lorentzian distribution
describes the resonance Raman spectra of general
photonic band-gap materials9.
Spectral data of our sample materials was fitted to a
sum of Lorentzian distributions and a linear term,
1
Γ
Iw = C 1 + C 2 w + ∑ ni=1 A i 1π 2
x−x o  + 12 Γ 2
2
(3)
the linear term representing background and
fluorescence, and a sum of Lorentzian representing our
phonon modes. Fitting was performed via the
Levenberg-Marquardt algorithm, a recursive gradient
descent/LMS hybrid. Weights were used proportional
to the square root of the number of counts, to minimize
contributions from areas with a poor signal to noise
ratio. The mean and variance on the mean were taken
over the three Lorentzian fits for each set of three
sample spectra per laser line. The systematic error from
the Spectrometer was then added to the error.
Piecewise fits were taken at the D peak, the G-peaks,
and the D* peak. Comparisons were made of the peak
position, gamma, and Lorentzian distribution
amplitude. Comparisons were normalized to the
488nm Untreated 488nm Treated
Peak Γ Peak % Integral % Peak Γ Peak % Integral % error
1528.7 ± 4.2 52.2 ± 2.8 5.1 ± 0.1 30.8 ± 2.8 1538.9 ± 4.6 21.3 ± 1.9 15.7 ± 2.1 9.6 ± 1.4
1559.4 ± 2.8 10.5 ± 0.5 25.5 ± 0.2 18.7 ± 0.8 1560.8 ± 2.4 12.4 ± 1.8 26.9 ± 0.8 20.5 ± 1.5
1587.3 ± 2.8 6.0 ± 0.4 45.0 ± 0.7 20.9 ± 1.3 1590.0 ± 3.2 9.2 ± 2.0 37.2 ± 2.4 28.5 ± 4.5
1594.3 ± 3.1 10.9 ± 0.7 24.4 ± 0.6 29.6 ± 0.7 1599.2 ± 4.7 16.4 ± 1.9 20.2 ± 0.6 41.5 ± 6.0

514nm Untreated 514nm Treated

1517.7 ± 1.6 54.7 ± 4.6 4.1 ± 0.5 43.7 ± 11.0
1548.5 ± 3.4 10.2 ± 3.4 25.8 ± 6.1 3.2 ± 2.0 1550.6 ± 4.6 25.6 ± 0.6 13.7 ± 1.1 17.6 ± 0.4
1568.1 ± 1.9 13.0 ± 1.0 17.3 ± 1.8 15.4 ± 1.8 1568.7 ± 1.7 13.8 ± 1.1 25.4 ± 1.0 19.9 ± 1.7
1592.1 ± 1.8 6.5 ± 0.4 34.6 ± 2.7 17.0 ± 2.1 1594.9 ± 2.6 9.2 ± 1.4 38.8 ± 1.8 17.9 ± 4.5
1599.2 ± 1.9 12.2 ± 0.5 18.2 ± 1.1 20.7 ± 5.1 1600.9 ± 3.3 15.8 ± 1.7 22.2 ± 0.2 44.6 ± 6.0

785nm untreated 785nm treated

1543.6 ± 1.6 18.0 ± 0.1 12.6 ± 0.1 14.0 ± 0.2 1541.3 ± 2.1 16.6 ± 1.4 18.5 ± 1.0 7.5 ± 0.5
1563.3 ± 1.6 6.5 ± 0.0 35.0 ± 0.2 11.0 ± 0.1 1565.9 ± 2.3 9.9 ± 0.3 30.7 ± 0.3 15.1 ± 0.6
1592.1 ± 1.5 6.6 ± 0.1 34.1 ± 0.1 31.8 ± 0.1 1593.4 ± 2.4 9.7 ± 0.1 31.4 ± 0.6 27.9 ± 0.3
1600.5 ± 1.5 12.3 ± 0.1 18.4 ± 0.1 43.2 ± 0.1 1600.8 ± 2.4 15.8 ± 0.5 19.4 ± 0.2 49.5 ± 0.6

Table I: Comparison of the G-modes of pristine and acid treated nanotubes. (a) Both G+ and G- peaks remain relatively unshifted for pristine and treated
SWNT. (b) Acid treated G+ peaks exhibit a very distinct increase in width, gamma increasing by ~3 and ~4 respective to G+ ~1590cm-1 and 1600cm-1. This
can cause an “apparent” shift in the combine G+ peak by a significant amount. (c) Pristine SWNT measured with the 514nm laser have a distinct broad peak
at ~1520cm-1 that account for < 40% of the counts in the region. Acid treated SWNT do not exhibit this peak.

pristine SWNT Acid Treated SWNT

G mode G mode
514nm 514nm

Fig 2. High energy mode of (a) Pristine SWNT fitted with a sum of Lorentzian measured with the 514nm laser line. A prominent peak appears at ~1517cm-1.
(b) Treated SWNT measured at the same wavelength do not exhibit this peak. The g+ peak increases significantly for acid treated SWNT.

integral of the Lorentzian fits under comparison. The
integral of the Lorentzian sum is simply the sum of the
distribution amplitudes Σ Ai, as the unscaled Lorentzian
is normalized. This method of normalization has an
advantage over normalizing over peak values as it is
invariant under shifts in the Lorentzian width.
G - High Energy Mode
The high energy mode, also known as the G-band,
was fitted with four Lorentzian distributions, two
corresponding to the G+ mode and two corresponding
to the g- mode. A fifth Lorentzian was added for the
analysis of the 514nm untreated SWNT measurement.
The results are presented in Table I.
The peaks of the G+ mode remained relatively
unshifted for all measured laser lines, but the width of
the two G+ fits exhibited a significant and consistent
increase among all treated SWNT measurements. G+
peaks were measured at ωg1+ ≈ 1592 cm-1 and ωg2+ ≈
1600 cm-1. The width parameter exhibiting an average
of Γ g1+ ≈ 6.4 cm-1 and Γ g2+ ≈ 11.8 cm-1 for untreated
SWNT and Γ g1+ ≈ 9.4 cm-1 and Γ g2+ ≈ 16.0 cm-1. This
corresponds to an increase in the gamma of ~3 cm-1 and
~4 cm-1 for the g1+ and g2+ modes. It is important to
note this broadening is observed regardless of energy
and on all samples. It now remains to postulate on what
is causing the broadening of the G+ modes. It could be
that the phonon band of both the g1+ and g2+ bands are
broadening due to a perturbation introduced by the
large number of defects.
An increase in amplitude is seen for g2+ relative to
peak g1+ for the 514nm and 785nm lines as
 488nm Untreated 488nm Treated
Peak Γ Integral % Peak Γ Integral %
1338.59 ± 2.8 35.17 ± 3.4 3.72 ± 0.1 1357.55 ± 3.56 57.84 ± 4.01 21.63 ± 3.59
G-band 96.28 G-band 78.37

514nm Untreated 514nm Treated

1333.16 ± 2.7 36.86 ± 1.3 4.95 ± 0.1 1352.01 ± 1.96 53.43 ± 0.83 28.91 ± 2.21
G-band 95.05 G-band 71.09

785nm untreated 785nm treated

1291.17 ± 1.6 17.06 ± 0.2 7.38 ± 0.1 1305.8 ± 2.74 32.94 ± 1.17 13 ± 1.51
1335 < 0.5% 1343.92 ± 2.59 46.59 ± 2.58 16.89 ± 2.02
G-band 92.62 G-band 70.11

Table II: D mode intensity and peaks relative to the overall G-band intensity for pristine and acid treated SWNT. (a) The D mode intensity of treated
SWNT exhibits an exceptionally large gain relative to the G-band of untreated tubes. Relative amplitude of the D mode increases 8 folds. (b) A positive
peak shift of ~18cm-1 is observed for treated tubes. (c) A broadening of the D mode is observed. (d) The 785nm laser line has a peak at ~1291cm-1 for
both pristine and treated tubes. Acid treatment doubles the amplitude and width of the ~1291cm-1 peak.

Fig 3. Defect induced mode of (a) Pristine SWNT fitted with a sum of Lorentzian measured with the 488nm laser line. (b) Treated SWNT measured at the
same wavelength. The D mode exhibits a large increase in intensity.

demonstrated in fig 1. It has been suggested that the
high energy mode is a defect induced mode6 and it has
been shown that acid treated MWCNT exhibit an
increase in the g2+ (or D’) peak3 with the introduction
of defects. Interestingly it seems that the g1+ amplitude
is decreased with respects to all other modes in the G-
band. This may be an indicator that the g1+ mode is not
enhanced by the introduction of defect, and that the g2+
peak is the product of structural disorder. This analysis
would be consistent with M. Souza et. al., who suggests
the HEM bands can be explained by a first-order single
resonance Raman peaks and defect-induced double
resonance features5. A similar effect is seen for the G-
peaks at 488nm and 785nm. The 514nm sample does
not exhibit this effect, but is likely skewed by a very
large and wide Lorentzian appearing at 1517 cm-1.
This brings us to our next item of interest, a ω ≈ 1517
cm-1 peak present only in the untreated SWNT sample
at 514nm. This peak contributes over 40% of the counts
in the region. Treatment of SWNT with nitric acid
completely eliminates this peak. This peak has not been
seen in the spectroscopy of individual SWNT2,12 [2, 12]
nor has it been characterized in graphite, amorphous
carbon, or diamond like carbon.13 It is uncertain
whether this peak is a property of nanotube bundles,
impurities interacting with nanotubes or impurities
independent nanotube presence.
D - Defect Induced Mode
The D-mode was fitted with a single Lorentzian and
normalized to the integral of the G-mode. Peaks were
observed at ω ≈ 1335 cm-1 for untreated SWNT and ω ≈
1350 cm-1 for treated SWNT. An additional Lorentzian
was added to describe an additional peak seen at ~1291
cm-1 for the 785nm laser line. The D-mode for the
785nm line had negligible amplitude.
In the past acid treatment has been used to introduce
defects in SWNT structures3,6. It comes as no surprise
that an increase in the amplitude of the D mode was
observed for treated SWNT. The amplitude of the D
mode was observed to increase an order of ~640% and
~800%, relative to the G-mode intensity, and a
broadening of the D-mode gamma was observed by ~22
cm-1 and ~17 cm-1, respectively to the 488nm and
 Fig 4: The count distribution of the D, G and D* mode normalized as a function of amplitude. This figure presents a normalization performed
on a single spectrum of acid treated SWNT at 785nm. The D peak amplitude is significantly higher than that of the untreated SWNT and the D*
peak significantly lower.
514nm excitation level. A positive peak shift of ~19 energy. A significant reduction in D* amplitude was
cm-1 was observed for using both laser lines. seen relative to the G and D modes amplitude for acid
The 785 nm line revealed an additional excitation treated SWNT.
mode at ~1291 cm-1 for untreated SWNT. This peak
exhibited a positive shift of ~16 cm-1 for treated SWNT. Comparison of D, G, D* amplitudes
The amplitude and gamma of this peak is Given the total counts observed in the G, D and D*
approximately doubled after treatment. This peak does modes, for each sample, one can compare the shift in
not seem to be directly correlated to the D mode of the intensity for each band as both a function of laser
carbon. It is more likely a different mode sensitive to energy and chemical treatment. Integrals of the
acid treatment. Overall, this peak can skew analysis of Lorentizan fits were taken of the three modes and there
the actually D mode amplitude if not accounted for. normalization is presented in table 4.

D* - Second Harmonic Defect Mode

The D* mode was fitted with a single Lorentzian for the 488nm
488nm, 514nm, and 785 laser lines. Peaks of the D* Pristine % Treated %
mode shifted as a function of laser energy for both D 2.1 ± 0.4 17.6 ± 3.8
untreated and treated SWNT. Peaks are presented in G 72.0 ± 5.2 67.0 ± 8.7
table III. D* 26.0 ± 1.7 15.5 ± 2.5
514nm
488nm Peak Γ
Pristine % Treated %
Pristine 2663.7 ± 3.5 39.1 ± 1.6
D 4.3 ± 0.7 31.0 ± 3.0
Treated 2683.1 ± 3.6 35.1 ± 0.8
G 85.3 ± 6.5 69.0 ± 7.0
D* 10.4 ± 2.1 <1% ± -
514nm Peak Γ
785nm
Pristine 2660.7 ± 4.3 30.0 ± 0.4
Pristine % Treated %
Treated 2679.4 ± 2.0 33.2 ± 1.3 D 2.7 ± 0.4 29.0 ± 0.7
G 80.1 ± 0.6 62.3 ± 1.3
785nm Peak Γ D* 17.2 ± 0.3 8.8 ± 0.5
Pristine 2573.1 ± 2.0 26.7 ± 0.3
Treated 2598.2 ± 2.7 32.3 ± 0.8
Table IV: Normalized distribution of the total counts for the D,
Table III: Peak and width of the D* mode for pristine and treated G and D* band at different excitation levels for pristine and acid
SWNT. treated SWNT. Acid treatment of nanotubes substantially
increases the D mode and substantially decrease the D* mode.
A positive peak shift of ~20 cm-1 was observed between The G mode is decreased slightly.
untreated and treated SWNT independent of laser
For untreated SWNT the majority of the distribution
was found at the G mode, with ~80% of the total counts
falling in this area. The D mode had low amplitude, ~2-
4%, indicating a low percentage of defects as expected
of pristine SWNT. The D* mode has a more varied
distribution with 10-26% of counts falling in this region
depending on excitation energy.
Treatment of the SWNT with nitric acid resulted in a
very significant increase in the D mode band and a very
drastic reduction in the D* band. For the 514nm line,
the D* mode was nearly eliminated. The G mode
exhibited a relative decrease of ~15% for all excitation
levels.
The absolute intensity change, with respects to the
control SWNT, is unknown as the density of SWNT in
each sample is not readily available. Performing RRS
on individual acid treated SWNT and comparing to
untreated SWNT with the same excitation parameters
would reveal in-depth information about the nature of
these increases. Such an experiment could provide key
evidence in the debate over whether the HEM mode is
primarily defect induced.
Conclusion
Analysis of SWNT with resonance Raman spectroscopy
revealed a great deal of information about chemical
functionalization occurring from treatment with nitric
acid.
Widening of the G+ peaks in the HEM mode was
seen for all samples, with ∆Γ g1+ ≈ 3 cm-1 and ∆Γ g2+ ≈
4 cm-1. A convincing shift in the peaks was not seen for
any of the HEM modes, with peaks averaging at ωg1+ ≈
1592 cm-1, ωg2+ ≈ 1600 cm-1. ωg1- ≈ 1550 cm-1, ωg2- ≈
1565 cm-1. The data suggested an amplitude increase of
both g2+ and g2- with acid treatment. This suggests a
correlation of the g2 peak with disorder. Whether this is
a real effect or an anomaly of the curve fit is uncertain.
The origin of a significant additional Lorentzian found
at ~1517cm-1 only for the 514nm excitation was not
identifiable. Acid treatment eliminated this peak.
The D mode amplitude increased drastically, on the
order of ~700%, in relation to the G mode, and the D*
mode decreased drastically relative to both the G and D
mode. The untreated SWNT D mode peak was
observed at approximately ωd ≈ 1333 cm-1 A shift of the
D mode peak was observed of ∆ωd ≈16 cm-1. The D*
mode peak for untreated SWNT was observed at
approximately ωd ≈2663 cm-1. A shift of the D* peak
was observed for treated SWNT of ∆ωd ≈16 cm-1.
Overall nitric acid treatment of SWNT presented a
great deal of information regarding the correlation
regarding disorder and the D, G, and D* modes of
SWNT. Because of the bulk nature of the
measurements, absolute intensities comparisons were
not easily obtainable. Further analysis on individually
treated SWNT should yield information on the absolute
correlation between the D, G, and D* modes and the
effects of disorder induction.
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