Restoring the electrical conductivity of graphene oxide films by UV light induced. oxygen desorption

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1 Restoring the electrical conductivity of graphene oxide films by UV light induced oxygen desorption S. Bittolo Bon a, L. Valentini a* a) Dipartimento di Ingegneria Civile e Ambientale, Università di Perugia, UdR INSTM, Pentima 4, Terni - Italy. We report a chemical free method consisting of UV assisted deoxygenation of graphene oxide (GO) films. It was observed how for GO films annealed in air the oxygen species desorb from the GO surface upon exposure to UV light and how the surface resistivity of such deoxygenated GO films decreases with increasing the exposure to the UV light. The obtained results open a clean as well as facile route for the integration of GO based materials into optoelectronic devices. *Corresponding author. Tel: Fax: address: mic@unipg.it (L. Valentini) 1

2 The structure of graphene oxide (GO) sheets consists of basal plane of the sheet decorated with hydroxyl and epoxy functional groups; carbonyl groups are also present as carboxylic acids along the sheet edge but also as organic carbonyl defects within the sheet [1]. These functional groups provide a variety of surface-modification reactions, which can be used to develop functionalized GO based materials [2]. Although charge carrier transport observed in nearly ideal graphene are absent in GO, the easy processing and the versatile properties of GO make the reduction methods for such material attractive for fundamental research as well as for applications [3]. Chemical free methods for the reduction of graphene oxide has been recently obtained for example through photocatalytic action of TiO 2 [4]. Huang et al. [5] reported the flash reduction of graphene oxide films while Rao et al. [6] observed the light radiation reduction of GO solutions. However, these latter two works deal with the use of flash lamp energies that were around J/cm 2 and/or laser treatment of GO solutions, respectively. In this communication, we have shown that the annealing in air generated GO thin films active to UV treatment. We have found that upon exposure to the UV light, GO films decreased the electrical resistivity. The method reported here suggests that the deoxygenation of GO films could be obtained through a clean and dry method where no chemicals are required. The investigation presents an easy route for the preparation of GO based materials. Graphene oxide were purchased from Cheaptubes (thickness 1-5 nm by AFM see Supplementary Data). Water dispersion (1mg/1ml) was prepared and sonicated (750W, 60% amplitude) for 1 hr to yield a yellow suspension. Quartz substrates (20 mm X 20 mm; 1 mm thick) were cleaned by ethanol and acetone, rinsed with water, dried under nitrogen and taken inside a dry Ar glove box. Graphene oxide films were prepared by spreading the water solutions of the prepared graphene oxide sheets onto the substrates. The deposited films were then annealed at 100 C for 1 hour in vacuum (10-3 Torr) and air atmosphere, respectively. For UV irradiation, a pencil-type Hg calibration lamp (Oriel, 30 mw/cm 2 ) was used. The GO films were irradiated in vacuum 2

3 atmosphere (10-1 Torr) for 1 hour and 3 hours, respectively. Fourier transform infrared spectroscopy (FTIR), in the cm -1 range, was used to observe the surface modification of the GO functional groups. UV-Vis measurements of the deposited films were carried out with a Perkin- Elmer spectrometer Lambda 35; for all samples, a neat quartz slide was used as the reference. The morphologies of the prepared samples were investigated by atomic force microscopy (AFM) and field emission scanning electron microscopy (FESEM). The electrical characterization (four probe measurements) was performed using a computer controlled Keithley 4200 Source Measure Unit. For the four probe measurements, Al electrodes (1 mm 10 mm) having an average thickness of ~70 nm were thermally evaporated on the GO coated quartz substrates maintaining a spacing of 2 mm. The FESEM characterization performed on GO films before (Fig. 1a) and after UV irradiation (Fig. 1b and Fig. 1c) demonstrates that, upon UV exposure, the corrugation of the graphene sheets changes dramatically. Corrugation effects have been previously observed for chemically converted graphene produced by reduction of graphene oxide [1,7]. Simulations suggest that different chemical addends and their arrangements may result in significant wrinkling and even bending of graphene sheets [7]. The removal of the oxygen-containing functional groups from the basal plane of graphene flake upon UV irradiation could also contribute to the change in its corrugation [8]. In order to confirm this assumption the FTIR spectra of our GO films before and after UV irradiation have been reported in Fig. 2. The GO spectrum shows bands corresponding to the C=O stretching vibrations of the COOH groups at 1740 cm -1, the O-H deformations of the C-OH groups at cm -1, the C-O stretching vibrations at cm -1, and the epoxide groups at 1230 cm -1 [9]. These bands were attenuated in their intensity after the exposure for 1 hour and are completely absent from the spectrum of the GO exposed to the UV light for 3 hours, thus confirming the deoxygenation of our GO films. 3

4 The gradual red shift of the 305 nm peak of GO together with the increase of the absorption in the whole spectral region can be observed as a function of the UV irradiation time, as shown in Fig. 3. The red shift and the increase in absorption indicate deoxygenation of GO. The observed increase of the absorption was not due to a change of the layer thickness but suggests that the UV irradiation method can provide a way to tune the degree of deoxygenation of GO because the extent of the red shift is related to the degree of aromaticity in the graphene plane [3]. The high resistance of GO is due to the existence of oxygen-containing groups, which could introduce defects to graphene [3]. In contrast, deoxygenation could recover the GO conductivity to some extent. Recently, it has been shown that deoxygenation occurs in GO when it is heated above 100 C, [3] resulting in a thermal reduction. Then, the sheet electrical resistance of the prepared samples was investigated. As demonstrated by the values reported in Fig. 4, it is interesting to find that after irradiation of 1 hr the sheet resistance displays a distinct decrease. This finding suggests that the resistance of GO could be decreased via UV irradiation. During our experiments it was observed that environmental atmosphere during the annealing procedure affect the subsequent UV induced deoxygenation process. In particular it was found that the annealing in vacuum did not activate the deoygenation process leaving the GO an insulating material even after the UV exposition (see Supplementary Data). Analogously to what reported elsewhere [10] our results suggest that heated GO is reactive to ground state O 2 in air. This supports the heating induced GO activation mechanism and oxygen desorption under UV irradiation. On the contrary the heated GO in vacuum is too far from the reduction temperatures used for conventional thermal reduction processes of GO [3], leaving the GO unreduced, highly resistive and insensitive to the UV treatment. Chemical characterization of the graphene oxide after annealing in vacuum or in air are currently under investigation in our labs in order to give some information about the detailed oxygen groups after annealing, which may influence the interaction between the UV and graphene oxide. 4

5 Conclusions In summary, we have developed a facile chemical free deoxygenation of GO films by using UV light irradiation. We showed that in our UV treated GO films the electrical conductivity could be restored. Considering the accessibility of graphene oxide, this study provides a possibility that this method could be used in various fields such as optoelectronics devices. Acknowledgements We gratefully acknowledge Dr. Giovanni Pennelli (Dipartimento di Ingegneria dell'informazione: Elettronica, Informatica e Telecomunicazioni Università di Pisa) for the AFM analysis. 5

6 References [1] Lerf A, He H, Forster M, Klinowski J. Structure of graphite oxide revisited. J Phys Chem B 1998;102(23): [2] Stankovich S, Dikin DA, Piner RD, Nguyen ST, Ruoff RS. Synthesis and exfoliation of isocyanate-treated graphene oxide nanoplatelets. Carbon 2006;44(15): [3] Eda G, Chhowalla M. Chemically derived graphene oxide: towards large-area thin-film electronics and optoelectronics. Adv Mater 2010;22(22); [4] Akhavan O, Ghaderi E. Photocatalytic reduction of gra-phene oxide nanosheets on TiO 2 thin film for photoinac-tivation of bacteria in solar light irradiation. J Phys Chem C 2009;113(47): [5] Cote LJ, Cruz-Silva R, Huang J. Flash reduction and patterning of graphite oxide and its polymer composite. J Am Chem Soc 2009;131(31): [6] Kumar P, Subrahmanyam KS, Rao CNR. Graphene produced by radiation-induced reduction of graphene oxide. arxiv: v2. [7] Schniepp HC, Li JL, McAllister MJ, Sai H, Herrera-Alonso M, Adamson DH, et al. Functionalized single graphene sheets derived from splitting graphite oxide. J Phys Chem B 2006;110(33): [8] Paci JT, Belytschko T, Schatz GC. Computational studies of the structure, behavior upon heating, and mechanical properties of graphite oxide. J Phys Chem C 2007;111(49): [9] Abdelsayed V, Moussa S, Hassan HM, Aluri HS, Collinson MM, El-Shall MS. Photothermal deoxygenation of graphite oxide with laser excitation in solution and graphene-aided increase in water temperature. J Phys Chem Lett 2010;1(19): [10] Liu L, Ryu SM, Tomasik MR, Stolyarova E, Jung N, Hybertsen MS, et al. Graphene oxidation: Thickness-dependent etching and strong chemical doping. Nano Lett 2008;8(7):

7 Figure captions Figure 1. FESEM images of (a) GO, (b) GO UV irradiated for 1 hr and (c) GO UV irradiated for 3 hrs. Figure 2. FT-IR spectra showing the change of GO film absorbance as a function of irradiation time. Figure 3. UV-Vis spectra showing the change of GO film absorption as a function of irradiation time. Figure 4. Sheet resistance values of GO films as a function of irradiation time. 7

8 a) b) c) Figure 1. 8

9 Figure 2. 9

10 Figure 3. 10

11 Figure 4. 11

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