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"������]\��� �=BX?�N�O0�OX?�U�>��UX?�U�X?�:*:*X?:*:*:*:*:*&O&OX?:*:*:*�O:*:*:*:*���������������������������������������������������������������������U:*:*:*:*:*:*:*:*:*\(�:Laser bleaching of carbon nanotubes suspension in N,N-dimethylformamide
Konstantin G. Mikheev,*,[a] Gennady M. Mikheev,[a] Vladimir L. Kuznetsov,[b] Tatyana�N.�Mogileva,[a] Sergey�I.�Moseenkov,[b] and Mariya A. Shuvaeva[b]
[a]Institute of Mechanics of Ural Branch of Russian Academy of Sciences, 34 ul. T. Baramzinoy, 426067 Izhevsk, Russia [b]Boreskov Institute of Catalysis Siberian Branch of Russian Academy of Sciences, 5 Akad.�Lavrent�ev prosp.,�630090 Novosibirsk, Russia 
*Corresponding author: e-mail:  HYPERLINK "mailto:k.mikheev@udman.ru" k.mikheev@udman.ru

It is shown experimentally that the multiwall carbon nanotubes (MWNTs) suspension in N,N-dimethylformamide (DMF) irreversibly bleaches in a wide spectrum range under a pulsed nanosecond laser radiation at the wavelength of 532�nm. According to the data of the transmission electron microscopy�(TEM), the Raman spectroscopy and the reflection infrared spectrometry the bleaching is shown to be caused by MWNTs degradation, with the formation of new hydrocarbon chemical bonds which result from the laser-induced chemical reactions between MWNTs and DMF molecules.

Keywords: Carbon nanotubes, suspension, photochemical reactions, photo-induced bleaching
Introduction
Scientists have recently been studying light and nanocarbon materials interaction to acquire new knowledge to develop radically new devices for photonics and optoelectronics, e.�g. graphene mode-locked laser [1] and passive laser switches based on suspensions and films of single-wall carbon nanotubes�(SWNTs), permitting to obtain laser picosecond and subpicosecond pulses in the infrared region�[28]. One can also cite the study of the laser radiation interaction with nanographite films that resulted in creation of a quick-response photodetector which can operate in a wide spectral range�[9] at high temeperatures�[10]. A fundamentally new type of a polarization analyzer of laser radiation on the basis of this study has been designed and made [11], the principle of operation being the recording of the polarization-dependent surface photocurrents in nanographite films.
The study of laser radiation interaction with nanocarbon materials is also of interest from the point of view of production of new organic materials possessing different magnetic properties�[12,�13], magnetooptical light modulators developing�[13], improvement of optical limiters�based on nanocarbon materials�[14-17]. Research in this field is also useful as an approach to locally engineer the band gap and defect densities along the SWNTs�[18].
We have recently shown the semitransparent onion-like carbon�(OLC) suspension in N,N-dimethylformamide�(DMF) to irreversibly bleach under high light fluence at the wavelength of 1064�nm, with the bleached fraction possessing pronounced diamagnetic properties�[19]. We explained it by the laser-induced chemical reactions between OLC and DMF�(graphene shells hydration with formation of non-conducting fragments resembling condensed aromatic compounds) resulting in the transparent liquid formation. The photo-induced reactions between fullerenes and Hdonor molecules in presence of photosensitizers were previously observed�[20]. Besides, the reaction of SWNTs with hydrogen gas in the temperature range of 400550��C and under the hydrogen pressure of 50�bar was reported�[21]. The photo-induced chemical reactions of SWNTs with oxygen were also observed�[22]. In that study it is shown that laser radiation causes pronounced bleaching and decay of photoluminescence from SWNTs on either glass or mica substrates. To put it another way and to take into account the fact that MWNTs can absorb the electromagnetic radiation in the wide wave band�[23], it is logical to expect similar phenomena such as in the suspension of OLC in DMF to occur in the suspension of MWNTs in DMF under the laser radiation effect. In this paper we report on the study of the laser radiation interaction with this suspension.
Experimental Section
The MWNTs obtained by CVD technology in the reaction of the ethylene thermal catalytic decomposition on the Fe/Co catalysts were used in experiments. The MWNTs average diameter and length were 7-9�nm and 10-20��m respectively�(see Figure�1a,�b). The suspension of tubes in DMF with the MWNTs concentration of 0.015�g/l was dispersed ultrasonically�(22�kHz, 300�W). This suspension was stable for 24�hours.
The optical scheme of this experiment is presented in Figure 2a. Laser beam of the YAG:Nd3+laser� with a frequency converter into second harmonic�(the wavelength of 532�nm, the pulse duration of 17�ns) [24] passed through opened shutter (1) was focused by lens (2), with a focal distance of 100�mm, on an optical cuvette filled with the suspension under study(3). At closed shutter�(1), the region of interaction between laser radiation and suspension (3) was photographed by photocamera (4). The diameter of the focused beam waist was 70��m and the thickness of the cuvette was 1�mm.
To measure the transmission spectrum of the initial and bleached suspensions, the suspensions samples were placed in a 1.01-mm quartz cuvette. The measurements were made by the PerkinElmer LAMBDA 650 double-beam UV/Vis spectrophotometer.
The transmission electron microscope JEM 2012 (JEOL, Japan) with the accelerating voltage of 200�kV was used to obtain high resolution TEM images of the MWNTs and particles of the bleached suspension. The lattice plane resolution was 0.14�nm and the point resolution was 0.194�nm. 
The comparative analysis of the products contained in the initial and bleached suspensions has been carried out by the Raman spectrometer (Labram HR800, Horiba) at the wavelength of 632.8�nm and by the infrared reflectance spectrometer (FTIR 8000, Shimadzu). Thereto the films containing the solid fractions of the suspensions were produced on a quartz substrate by a simple exsiccation of a suspension layer deposited on the substrate.
Results and Discussion
The MWNT suspension was treated by pulsed laser radiation at different values of the input fluence W. The maximum value of the input fluence was below 2�J�cm-2. The bleaching was observed after the action of several pulses. The input fluence W of these pulses was above 0.8�J�cm-2. A typical image of the suspension bleached part is shown in Figure�2b. From this figure one can see that the bleached fraction of the suspension formed by the absorbed laser power, and therefore having a higher temperature, moves upward in the vertical direction.
To understand and analyze the bleaching mechanisms of the suspension, it was necessary to obtain the bleached fraction of the suspension in quantum satis. To this end the initial MWNTs suspension in DMF after its dispersion was injected into the optical cuvette and exposed to laser pulses for a long time, with the pulse repetition rate of 1�Hz, during 75(103�s. As a result initial semitransparent suspension was transformed into a practically transparent liquid.
The bleached fraction of the suspension had a yellowish shade. The optical density of initial (1�(blue line) and bleached (2�(green line) suspensions as functions of the light wavelength (() obtained relative to DMF are shown in Figure�3. From these measurements one can see that the bleaching phenomenon occurs over the whole range of the wave band from 200 to 900�nm, since the inequality (1(()((2(() is true. However, from the calculated dependence ((2/(1(()) which is shown in the inset in Figure�3 one can conclude that the degree of bleaching depends on the wavelength. Laser bleaching reveals itself strongly over the wave bands of 330(((900�nm and 200(((250�nm. The total bleaching was established to occur at the wavelength range of 615< �<900�nm. The bleaching at the wavelength range of 250(((330�nm is less pronounced since the (2/(1 ratio exceeds 0.5 over this wave band. It defines a weak yellowish shade of the bleached suspension obtained.
It was of interest to perform a comparative spectral analysis of materials contained in the initial and bleached suspensions using the Raman spectroscopy and the infrared reflectance spectrometry. The Raman spectrum of the initial MWNTs particles (prior to dispersion) was also obtained.
The study has shown that the Raman spectrum of the initial particles of MWNTs and samples of the MWNTs suspension practically does not differ in the frequency shifts region 10001800�cm-1. The scattering spectrum of the initial MWNTs consists of two peaks with the frequency shifts of 1594�cm1�(G�band) and 1335�cm-1�(D�band) (see Figure�4a). The presence of the D band, with the intensity being greater than that of the G band, is associated with the presence of impurities and a lot of defects in the MWNTs studied�[25].
From Figure�4b one can see that the Raman spectrum of the film obtained from the bleached fraction of the studied suspension differs considerably from that of the initial MWNTs (see Figure�4a) suspension and DMF (see Figure�4c). According to the reference data�[26] the scattering peaks of the bleached fraction with the frequency shifts of 1074 and 1460�cm-1 are due to the CH2 bonds, and the peak with the shift of 1138�cm-1 corresponds to the CH3 bonds. The esters (COOR) or aldehydes�(CHO) or carboxylic acids�(COOH) can cause a peak with the shift of 1739.9 cm-1. The peak with the shift of 1613.5�cm-1 can be conditioned by the NH2 group. The investigations carried out by the infrared spectrometer also confirm the presence of the chemical bonds in the bleached fraction of the suspension (see Figure�5). Thus, the peaks with the shifts of 2963�cm-1, 2933�cm-1, 2876�cm-1, 1468�cm-1 correspond to the CH3 bonds, the peaks with the shift of 1748�cm-1���to the lacto-group�(CH3COOCH3), the peaks with the shifts of 1163�cm-1 and 1059�cm-1���to the ethers�(ROCOR). It is difficult to interpret the peaks with the shifts of 816�cm-1, 713�cm-1, 650�cm-1, 541�cm-1. However, one can attribute the frequency range 720740�cm-1 to the methylene groups (-CH2-CH2-). The peaks with the shifts of 34003500�cm-1 and 1600�cm-1 were not observed in the infrared spectrum of bleached MWNTs suspension. These frequency ranges are typical for NH groups, so we can conclude that the dimethylformamide group is not present in the bleached MWNTs suspension. We should note that it was difficult to set off the effect of the background, so the peaks with the shifts of 2363�cm-1 and 2343�cm-1 correspond to CO2.
The TEM study of the bleached fraction of suspension has shown the bleached fraction to consist of an inhomogeneous mixture of different carbon formations (see Figure�1c,�d, e, f). It can be divided into graphite-like aggregates, polyhedral thin-walled formations and amorphized carbon-bearing remains of an organic solvent. A great amount of carbon is concentrated in large (several microns) graphite-like particles consisting of bundles of graphene layers, with the thickness of 520�nm. In addition, the polyhedral fragmented remains of carbon nanotubes with the length of 520�nm are observed. The graphene walls quantity of such fragments is 210. The formations remotely resembling the fragments of MWNTs are also present. The organic remains of the solvent localize on the graphite layers surface and cover the polyhedral formations. The film thickness ranges from 0.5�nm to 3�nm. These data indicate that the photochemical reactions between MWNTs and DMF in the suspension of MWNTs in DMF occur under the laser exposure, which results in the formation of new chemical bonds which are not present in the initial suspension. 
Conclusions
We have reported the phenomenon of the bleaching of MWNTs suspension in DMF under the powerful laser radiation effect at the wavelength of 532�nm, which reveals itself after several laser pulses. The suspension bleaches in the wide wave band from 200 to 900�nm. The bleaching results from the photochemical reactions between MWNTs and DMF, which leads to the formation of a new stable liquid fraction. It was verified by the analysis of the initial and bleached fractions of the suspension using the transmission electron microscopy, the infrared spectrometry and the Raman spectroscopy. Although presented results demonstrate that the powerful laser irradiation destroys the graphitic structure of the MWNTs we believe that there is a proper value of laser intensity for functionalizing the MWNTs by different groups of H-donor compounds. 
Acknowledgements
This work was supported by UB RAS grant !�11-1--248, RFFR grant !�12-02-31724 and by The Ministry of education and science of Russian Federation, project ! 8748 from 01.10.2012.
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[26]	J.�A.�Dean (1999) Lange�s handbook of chemistry. McGraw-Hill, Inc., New York.



Figure 1: TEM images of the (a,�b) initial MWNTs samples and (c,�d,�e,�f) particles of the bleached suspension. (c)�The tubes remains with amorphized external layers, (d)�a big graphite-like fragment, (e)�the fragments of nanotubes and capsules of multi-wall graphene-like layers, (f)�the remains of tubes walls (2-3 layers).
Figure 2: (a) The optical scheme of the experiment: (1) - shutter; (2) - focusing lens; (3) - optical cuvette with MWNT suspension in DMF; (4) - photo camera; (b) the image of the bleached part of the suspension: (1) suspension, (2) zone under irradiation (a focused laser beam was perpendicular to the image plane), (3) bleached suspension spreading upwards by virtue of thermal convection.
Figure 3: The optical density of (1 (1) initial and (2 (2) bleached suspensions as functions of the ( light wavelength�obtained relative to DMF. The suspensions were kept in quartz cuvettes with thickness of 1.01�mm. The (2/(1(() calculated dependence is shown in the inset.
Figure 4: The Raman spectra of the films exsiccated on the quartz substrate of (a)�the initial MWNTs suspension, (b)�bleached MWNTs suspension. (c)�The Raman spectrum of DMF.
Figure 5: The infrared spectrum of bleached MWNTs suspension.










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