Optical Materials: Optical Properties of Chiral Single-Walled Carbon Nanotubes Thin Films
Optical Materials: Optical Properties of Chiral Single-Walled Carbon Nanotubes Thin Films
Optical Materials: Optical Properties of Chiral Single-Walled Carbon Nanotubes Thin Films
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Optical Materials
journal homepage: www.elsevier.com/locate/optmat
ARTICLEINFO ABSTRACT
This work contains experimental results of optical properties for thin films containing Single-Walled Carbon
Keywords:
Single-walled carbon nanotubes Nanotubes. Thin films concerning 0.5, 1 and 2 mg of low dimension chiral (10,6) Single-Walled Carbon
Absorbance Nanotubes dispersed in low concentration aqueous sodium dodecyl sulfate solution (2 mL) were successfully
Raman spectra fabricated by spin-coating technique on transparent substrates at ambient atmosphere. Optical properties of
Photoluminescence these thin films were examined using Transmission, Raman and Photoluminescence Spectroscopies. We find that
Decay time of photoluminescence investigated chiral Single-Walled Carbon Nanotubes show transmission and emission bands not only in infrared
Quantum yield range but also ultraviolet and visible range.
1. Introduction lattice that has the honeycomb structure. The pair of n and m indices
determines the chiral vector, chiral angle and diameter of the SWCNT.
Nanoscience and nanotechnology provides lots of new opportunities The chiral vector C of the graphene sheet can be described as:
not only for electronics or photovoltaics, but also for optics and its ⎯⎯→ ⎯⎯→ ⎯⎯ ⎯⎯→
C = n a1 + m a2 , where a1 and a2 are fundamental lattice vectors.
practical applications. A growing number of nanomaterials including The chiral angle θ and SWCNT diameter can be represented by the
organic and organometallic materials [1,2], and carbon allotropes [3,4] 3m
have been shown to possess extremely interesting optical properties. In relations: tan θ = 2n + m and d = a n2 + m2π + nm , where
⎯⎯
→ ⎯⎯
→
particular, carbon allotments discovered in recent decades become one a = a1 = a2 = 2.46 Å is carbon-carbon bond length [5]. If n= m,
of the most representative materials of nanotechnology, starting from SWCTs are named armchair nanotubes, if m = 0 - zigzag nanotubes and
carbon nanoparticles (graphite) and ending at fullerenes, carbon na- in any other case they are called chiral (as shown in Fig. 1).
notubes (CNTs) or the newest member from this family - recently dis- Also conductivity of the SWCNTs shows the dependence on these
covered graphene. Notably, recent studies on carbon nanotubes have two indices. For a given (n, m) nanotube, if n = m, the nanotube
implemented completely new fields of research in materials science, manifests metallic character; if n − m is a multiple of 3 and n ≠ m the
solid state physics, chemistry, but also optics. Theoretically, CNTs be- nanotube manifests quasi-metallic character with a very small band
long to the same family as fullerene structures, but their electrical and gap. Otherwise the nanotube exhibits conductivity characteristic for
optical properties may vary and strongly depend on the structure of the semiconductors [5–9]. The most useful quality to help in understanding
nanotube. the electronic structures of SWCNTs is the density of states (DOS). The
Carbon nanotubes can be considered as a product of folding gra- one-dimensionality of the SWCNT gives rise to 1D sub-bands instead of
phite layers to carbon cylinders that can have one or more walls. Thus, one wide electronic energy band in nanotube density of states, as shown
single-walled carbon nanotubes (SWCNTs) can be considered as wrap- in Fig. 2. Each SWCNT described by indices pair n and m has a unique
ping graphite's layer of the one atom thick, called graphene, into set of interband transition energies Eii indicating the energy differences
smooth and uniform cylinder. Most single-walled carbon nanotubes between the i-th conduction and valence bands. Optically allowed
have a diameter of around 1 nm and can be many million times longer. transitions can only occur between these mirror sub-bands: v1 - c1, v2 -
The way in which a graphene sheet is wrapped is described by a pair of c2, etc. These transitions (so-called van Hove singularities) are usually
indices (chiral indices): n and m. The integer's n and m indicate the sharp and strong. Dipole-forbidden crossover transitions: v1 – c2, v2 –
number of unit vectors along two directions in the graphene crystal c1, etc. are extremely week. Optically allowed transitions are a
∗
Corresponding author.
∗∗
Corresponding author.
E-MAIL ADDRESSES: azawa@fizyka.umk.pl (A. Zawadzka), [email protected] (P. Szroeder).
https://doi.org/10.1016/j.optmat.2019.109295
Received 31 December 2018; Received in revised form 31 July 2019; Accepted 4 August 2019
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also observed from the Kataura plot [3,18] and Rayleigh scattering
spectroscopy experiments [19].
In 2006 Ando demonstrated theoretically that the Coulomb inter-
action between the electron and hole pair is greatly enhanced in the 1-
nm cylindrical structure and, in fact, that the Coulomb interaction af-
fects the optical spectrum of SWNTs [20]. He showed that the attractive
Coulomb interaction between the optically-excited electron and hole
pair plays an important role in understanding the optically-excited
states in the solid. When the electron and hole are strongly confined in
the 1D system such as the SWNTs with only 1 nm diameter, the at-
tractive Coulomb interaction between the electron and hole is much
enhanced in comparison with 3D bulk materials. The enhanced Cou-
lomb interactions in 1D SWNTs can lead to the formation of tightly
bound electron–hole pairs (excitons) but also strengthen the intensity of
Fig. 1. Scheme of the SWCNT chiral vector.
the observed optical von Hove transitions.
Although SWNT has been studied for almost two decades, experi-
mental photoluminescence studies have mainly focused on the study of
isolated nanotubes, their aqueous solutions or solution of purified
SWNTs individually insulated inside surfactant micelles [21–23]. Pho-
toluminescence observed after illumination, regardless of the form of
the investigated material containing SWCNTs, occurred in the infrared
range of the spectrum. The ability of semiconductor material for lu-
minescence and its emission energy depends of course on internal band
structure, but also other external and internal factors. External factors
include above all, the surrounding environment and electric or mag-
netic fields [24–26]. Examples of internal factors include dopants, de-
fects, dislocations but also nearest neighbors interaction and surface
reconstructions (especially for thin films). These factors can empty or
fill existing bands and hence completely change the band structure. As a
result, the energy of photoluminescence emissions can be shifted or its
intensity may be change, causing to strengthen or even total destroy
[27,28]. The case of the SWNTs thin films is particularly interesting,
Fig. 2. Schematic of density of states for a semiconducting SWCNT. Allowed since for SWNTs all the constituent atoms are on the surface, and they
optical transitions are illustrated as vertical arrows. are therefore all exposed to the surrounding environment and nearest
neighbors interaction.
However, after several years of intensive experimental research,
characteristic feature of the SWCNTs and responsible for its many dis-
photoluminescence of the single-walled carbon nanotubes with a dia-
tinguished electronic and optical applications.
meter of about 1 nm and lower are still poorly tested experimentally.
The measurement of optical transitions allows, in principle, to de-
This is associated with the relatively low intensity of the observed
termine chiral indices and the bandgap energy of SWCNTs, which is
photoluminescence and its short decay time even in high concentration
proportional to the nanotube diameter. Therefore, a huge effort has
inside solutions. Therefore, thin films containing SWCNTs seem to be a
been made to measure photoluminescence (PL) of SWCNTs since their
good candidate for this type of research and we decided to fabricated
discovery [10–12]. Usually, observation of PL is a result of the isolation
and investigated them experimentally. Additionally, formation of the
of individual SWCNT that are prevented from assembling with other
thin film from the solution containing SWCNTs can give long ordered or
semiconducting and metallic carbon nanotubes. Energy transfer be-
disordered nanotubes. The degree of the thin film's ordering depends on
tween the semiconducting and metallic carbon nanotubes can occur
the external conditions applied during the film growth process, in-
and optically-excited carriers are non-radiatively quenched at the me-
cluding electric and magnetic field, gas flow or self-assembly process
tallic carbon nanotubes in the bundled samples [13]. Due to the in-
[29,30]. On the other hand, thin films with relatively high disordering
tensity of the observed PL, most publications concern on experimental
exhibit the strongest photoluminescence. Therefore, we decided to in-
research in the near-infrared (NIR) range of the emission and absorp-
vestigate optical properties of the disordered thin films containing
tion spectra [13–15]. The most popular explanation of the PL signal
SWCNTs with small diameter. The films were successfully grown on
from semiconducting SWCNTs is recombination of the optically-excited
quartz substrates by using spin-coating techniques. All investigated
free electron in the conduction band and free hole in the valence band.
films were randomly oriented and their thickness was equal several
In this one-electron approach without consideration of Coulomb in-
hundred nanometers.
teractions, the resonance features of the optical spectra are attributed to
the sharp electronic states corresponding to the von Hove singularity.
2. Experiment
Theoretical calculation for modeling electronic band structure of single-
wall carbon nanotube and their optical transition energies are based on
Solutions containing SWCNTs (Nanocyl, 70% purity) were prepared
the tight-binding (TB) model of π-bands of graphene with using the
by using 2 mL deionized water, 0.01 mg sodium dodecyl sulfate (SDS)
zone-folding approximation due to its simplicity and some qualitative
and 0.5 mg, 1 mg, 2 mg SWCNTs, respectively. SDS was used to prevent
agreement with experimental results [16,17]. The tight-binding model
process of SWCNTs aggregation. Prepared solution was subjected to
with the nearest-neighbor approximation delivers simple equation to
2jaγ0 ultrasonic bath for 6 h and then immediately after mixing, solutions of
calculate optical transitions of the semiconducting SWCNT: Eii = d ,
the SWCNTs were used to prepare thin films. The films were grown on
where A describe carbon-carbon bond length, d – SWCNT diameter, γ0 - quartz substrate by spin-coating technique in ambient atmosphere. The
nearest-neighbor hopping parameter and j - an integer. This inverse preparation of the quartz substrate consisted of four stages of the ty-
proportional trend of transition energies with SWCNT diameter was pical cleaning procedure. During the first stage, the substrate was
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d = (C/(ωG+ − ωG −))1/2 , where M 79.5 cm 1⋅nm and Fig. 5. Kataura plot relates to the nanotube diameter and its bandgap energies.
1− ⋅
CS 47.7 cm nm, we find that the diameter of the SWNTs is ranged
=
between 1.1 nm and 1.5 nm and coincide with the estimations derived
from the RBM band. Higher intensity of the GS peak in relation to the the solution used for their preparation. Broadening of the absorption
−
GM indicates that semiconducting nanotubes are predominant in the peak indicates the aggregation that occurs during the formation process
sample. Besides of the RBM and G mode, we observe the other bands of the spin-coated layer.
characteristic to carbon sp2 materials such as the M mode and the The effect of the solvent (especially its kind and polarity) on the
second order 2 M, as well as the disorder induced D band with its location of the absorption maximum is a phenomenon that occurs quite
overtones D’ and 2D. The position of that peaks shifts up with energy of frequently for many organic and inorganic materials [38,39]. De-
the laser excitation light. Different position of the G+ , G−M and GS we pending on the solvent, it can cause the spectra shift towards longer or
attribute to the different polarization of the laser incident light of the shorter wavelengths. In contrast, the widening of the absorption peak
length of 532 nm and 785 nm with respect to the nanotube orientation. indicates the aggregation that occurs during the formation process of
the spin-coated layer.
Transmission T(λ) spectra of the SWCNT thin films were in- Optical properties of carbon nanotubes derive from electron tran-
vestigated in the spectral range 200–2000 nm. Experimental data for all sitions for one-dimensional structure in the density of state. A typical
investigated thin films are recalculated to absolute values of the feature of one-dimensional structures is that their density of state is not
SWCNTs absorbance by elimination transmittance and reflectance of a continuous function of energy, but descends gradually and then in-
the quartz substrate covered SDS thin film. Experimentally determined creases in a discontinuous stream. The selection rules show that optical
absorbance spectra are presented in Fig. 4a and shown one wide ab- resonance transitions between van Hove singularities originating from
sorption band in UV region, located at the wavelength equal to 250 nm. bands numbered with the same indexes (v1 − c1, v2 − c2, etc.) are al-
Absorbance spectra for based solution are present at Fig. 4b. Detailed lowed. Energies correspond to these transition are named Εii. These
analysis of the spectra shows, that intensity of absorbance peak strongly energies are the quantities that characterize each individual nanotube
depend on the concentration of the carbon nanotubes on the substrate's with indices (n, m) with diameter d. Crossover transitions (c1 − v2,
surface (also the concentration of the based solution). As the con- c2 − v1, etc.) are dipole-forbidden and thus are extremely weak, but
centration increases, the intensity of the maximum absorbance also they were possibly observed. Energies between the Van Hove singula-
increases. The absorption of SDS in water solution observed in the rities depend on the SWCNT's structure. Thus by varying this structure,
range of 200–1100 nm does not show any absorption maxima and in the especially the diameter, one can tune the optoelectronic properties of
whole range was below the value of 0.1. This clearly indicates that the carbon nanotube.
observed maxima of absorbance come from thin films of single-walled The first attempt to link and provide the energy Eii values of the
carbon nanotubes. An extension of the absorption peak and its shift allowed optical transitions of nanotubes (n, m) with a diameter d for
towards shorter wavelength was observed for thin films in relation to optical spectroscopy was made by Kataura [3]. A typical picture of
Fig. 4. Absorbance spectra of SWNTs for thin films (a) and based solution used for its deposition (b).
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Fig. 6. 3D Photoluminescence spectra for SWCNT thin films: E33 (a) and E22(b) for concentration 2 mg/2 mL, E33 (c) and E22 (d) for concentration 1mg/2 mL, E33 (e)
and E22 (f) for concentration 0.5 mg/2 mL.
Kataura's plot is presented in Fig. 5. SWCNT semiconducting samples and specific structural indicators (n,
In the semiconductor SWCNT, the van Hove transition with the m) were assigned to each of these species [15,18,40]. In contrast, ex-
lowest energy (E11) corresponds to the absorption or photo- periments with the transitions E33 or higher are very rarely studied.
luminescence directly across the band gap. In the last 10 years, a dy- That is why we decided to experimentally examine transitions E33 and
namic development of experimental studies using spectrofluorometry to compare them with E22 for nanotubes with a diameter of about 1 nm. To
study transitions of E11 and E22 of a significant number of semi- explore optical properties a detailed study of photoluminescence was
conductor SWCNT species has been observed. The first and second van carried out at room temperature (RT) by using spectrofluorometer
Hove transient waves were observed for more than one hundred of FluroMax 4P Horiba. The temperature dependence of PL in the range
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Fig. 7. PL intensity for SWCNT thin films as a function of concentration for both investigated transitions: E33 (a) and E22 (b).
Fig. 8. PL decay-time for thin film prepared from 2 mg/2 mL concentration: E33 transition (a) and E22 transition (b).
Fig. 9. PL temperature dependence of transition in thin film (concentration 2 mg/2 mL): E33 transition (a) and E22 transition (b) at the excitation wavelength equal to
246 nm.
77–300 K was also examined. 3D Photoluminescence spectra of the for the higher one a typical sharp maxima is started to appear. The
SWCNTs thin film on quartz substrate recorded at RT are shown in maximum position for both E22 and E33 was independent on the con-
Fig. 6. centration of the solution used to prepare the film and was equal to
These PL spectra were measured in the emission wavelength range 388 nm and 775 nm, respectively. The intensity of the observed pho-
from 350 nm to 900 nm and excitation wavelength range from 230 nm toluminescence changed significantly. The strongest luminescence was
to 270 nm [41–43]. The highest intensity of the photoluminescence was observed for layers with the highest concentration of nanotubes. With
observed for the thin films prepared from the solution containing 2 mg/ the decrease of the concentration, the PL intensity also diminishes.
2 mL SWCNTs – the highest concentration. PL intensities for other Fig. 7 present PL intensity as a function of SWCNT concentration for
concentrations were significantly lower at RT. The photoluminescence both investigated transitions. A detailed analysis of the presented
spectra showed asymmetrical shape regardless the concentration but spectra shows that the intensity of the transition E33 is about 6 times
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Fig. 11. Temperature dependence of 3D Photoluminescence spectra for SWCNT thin films: E33 300 K (a) and E22 300 K (b), E33 77 K (c) and E22 77 K (d).
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Although a limited range of the PL temperature dependence same estimated as the order of 10−3. The blue shift of whole PL spectra as a
other trends can be also noticed. Namely, a significant decrease in PL function of the temperature for both investigated lines has been de-
intensity with increasing its measurement temperature. Both lines monstrated. PLQY have been experimentally and theoretically studied.
showed the same tendency, but this change is significantly greater for Our experimental results showed that single walled carbon nanotubes
E33 transition as shown in Fig. 10. Similar effects have been reported by thin films have possessed quite large PLQY compared to other semi-
Cronin et al. and Karaiskaj et al. for polymer wrapped nanotubes or conductors. So far, these effects have not been considered and experi-
frozen suspensions of nanotubes [47,48]. A strong enhancement of mentally tested by using spectrofluorometry. Low-temperature PL in-
photoluminescence intensity was observed when the excitation wave- vestigations have shown important features for physics of the SWCNT
length is from UV range and not so far from resonant with the third Van thin films and follow-up studies are clearly needed. The high stability of
Hove singularity, unambiguously confirming the origin of the photo- optical transitions as a function of temperature was very promising
luminescence. The observed course of decreasing intensity as a function from the point of view of optoelectronic applications.
of temperature growth is typical for semiconductor materials.
Fig. 11a–d present 3D Photoluminescence spectra of the highest con- Declaration of interests
centration SWCNT thin films for both observed transition at the tem-
perature equal to 77 K and 300 K (RT). From these images, in addition The authors declare that they have no known competing financial
to decreasing the PL intensity and shifting individual emission, one can interests or personal relationships that could have appeared to influ-
also observe a shift of individual excitation towards shorter wave- ence the work reported in this paper.
lengths. Similar effects have been reported by Lefebvre et al. for pillar-
suspended single-walled carbon nanotubes [49]. They showed that the Acknowledgements
atmospheric environment strongly affected the low-temperature lumi-
nescence and PL intensity was quenched at temperatures below ~40 K This research has been financed from the funds of the Polish
for nanotubes in high vacuum, while nanotubes in helium ambient National Science Centre (grant no. 2017/25/B/ST7/02124). The films
remain luminescent. used in this paper were obtained using Interdisciplinary Centre for
Experimental results of PL and its decay time were used to de- Modern Technologies facilities, NCU, Torun, Poland. The authors wish
termine photoluminescence quantum yield. Photoluminescence to thank the COST Action MP1403 Nanoscale Quantum Optics.
quantum yield is an intrinsic property of material which can be ex-
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