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Synthesis of Graphene.Pdf Materials Chemistry and Physics 206 (2018) 7e11 Contents lists available at ScienceDirect Materials Chemistry and Physics journal homepage: www.elsevier.com/locate/matchemphys Synthesis of graphene via ultra-sonic exfoliation of graphite oxide and its electrochemical characterization Hassnain Asgar a, K.M. Deen b, Usman Riaz a, Zia Ur Rahman c, Umair Hussain Shah a, * Waseem Haider a, c, a School of Engineering and Technology, Central Michigan University, Mt. Pleasant, MI 48859, USA b Department of Materials Engineering, University of British Columbia, Vancouver, BC V6T 1Z4, Canada c Science of Advanced Materials, Central Michigan University, Mt. Pleasant, MI 48859, USA highlights A relatively direct synthesis method for production of graphene is presented. IR, Raman and XRD analyses confirmed formation of graphene starting from graphite. XPS and TEM characterization validated the formation of graphene. Electrochemical response of GO and graphene was evaluated in de-aerated 0.5M KOH. Presence of functional groups in GO resulted in improved values of Rct and Ceff,p. abstract A direct method of producing graphene from graphite oxide (GO) via ultra-sonication is presented in this work. The synthesis of graphene was validated through IR, XRD, Raman, and XPS analyses. Moreover, the diffraction pattern obtained from TEM also validated the formation of graphene with char- acteristics (002) plane. The electrochemical behavior of GO and graphene was evaluated by electrochemical impedance spectroscopy and linear sweep voltammetry in 0.5M KOH solution. The relatively larger effective pseudocapacitance and broad current peak exhibited by GO in the LSV plots was related with the dominant adsorption of ‘Hads’ during reduction of water. It has been considered that large overpotential and relatively higher current response exhibited by GO compared to graphene was associated with the preferential adsorption of Hads in the presence of surface functional groups. © 2017 Elsevier B.V. All rights reserved. 1. Introduction processes [5e7]. But the large-scale use of graphene is still hin- dered due to extensive and time-consuming production methods. Graphene and its related materials have unique physicochem- In this work, a relatively direct and efficient route is presented to ical properties to support several electrochemical processes produce graphene from graphite and the effect of surface functional involving electro-catalysis [1], electrochemical sensing [2], super- groups on electrochemical properties has been investigated. capacitance [3] etc. It is well established that the heterogeneous electron transfer, required for these processes, from/to a graphene 2. Experimental sheet takes place on the edges and is affected by the attached functional groups. The presence of functional groups also facilitates Graphite powder (Asbury Carbon Inc.) was oxidized to graphite the adsorption/desorption of molecules on the graphene planes [4]. oxide (GO) using improved Hummer's method as explained in The production method for graphene greatly influences these Ref. [8]. After the reaction, GO was dried overnight at 80 C. To properties. A lot of work is going on with graphene as core interest produce graphene, GO was ultra-sonicated in DI water for 12 h and its production is being reported continuously via various ® using Branson M2800H ultrasonic bath operating at the frequency of 40 kHz. The powder from the suspension was obtained via centrifugation with a g-force of ~2285 using the Rotofix 32A ® Benchtop Centrifuge by Helmer Scientific. * Corresponding author. School of Engineering and Technology, Central Michigan University, Mt. Pleasant, MI 48859, USA. Infrared (IR) spectra of graphite, GO and graphene was acquired E-mail address: [email protected] (W. Haider). from FTIR-ATR spectrometer (NicoletTMiSTM 50) in Attenuated https://doi.org/10.1016/j.matchemphys.2017.11.062 0254-0584/© 2017 Elsevier B.V. All rights reserved. 8 H. Asgar et al. / Materials Chemistry and Physics 206 (2018) 7e11 Fig. 1. IR (a), XRD (b), and Raman (c) trends of graphite, graphite oxide, and graphene. Total Reflection (ATR) mode. X-ray diffraction (XRD) patterns 3. Results and discussion (Rigaku Mini Flex II) were obtained by using Cu Ka (l ¼ 1.54 Å) radiation source. For Raman spectra, the laser beam excitation of IR, XRD and Raman spectra of graphite, GO and graphene are 532 nm (Kaiser Optical Systems Inc.) was used. The XPS spectra shown in Fig. 1. Graphite exhibited an insensitive behavior in the (Thermo Scientific K-Alpha) of graphene were gathered by using Al infrared range (Fig. 1a). The transmittance peaks at 2325- À Ka irradiation source. The morphology and structure of graphene 1981 cm 1 could be associated with the diamond crystal used in À sheets were observed in transmission electron microscope (TEM) ATR mode [9]. A broad peak at 3405 cm 1 presented by GO could be (HT7700). attributed to the -OH bond stretching vibrations belonging to C-OH À For electrochemical studies, the working electrodes were and/or adsorbed moisture. Similarly, the peak at 1173 cm 1 could prepared by casting the paste made of an active material; GO be related to the stretching of C-O bond [10]. Graphene demon- and/or graphene (85 wt%), carbon black (5 wt%), binder; poly(- strated similar behavior as graphite in the IR range; no signatures vinylidene fluoride) (10 wt%) and curing agent; 1-methyl-2-pyr- for functional groups which could be removed during ultra-sonic rolidinone into the electrode cavity. The as-cast paste was cured cleavage of GO. The XRD patterns (Fig. 1b), represented the char- overnight at room temperature before electrochemical in- acteristic peak of graphite (2 <theta> ¼ 26.5) corresponding to vestigations. Electrodes containing GO and graphene are termed (002) plane. This peak was shifted to lower 2 <theta> values of as graphite oxide paste electrodes (GOPE) and graphene paste 10.8 and 23.9 in case of GO and graphene, respectively. In GO this electrodes (GrPE), respectively in the following discussion. Elec- corresponded to (001) plane which also suggests the successful trochemical analyses of GOPE and GrPE were carried out by using oxidation of graphite [11]. Whilst for graphene the peak at 23.9 Gamry-Potentiostat (R-3000) coupled with three-electrodes cell was related to the (002) plane of sp2 hybridized carbon atoms [12]. assembly in 0.5M KOH solution of pH 9.5 ± 0.5. GOPE/GrPE were The Raman spectra of graphite (Fig. 1c) showed a G band peak at À working electrodes, saturated calomel electrode (SCE) was the 1579 cm 1 which was affiliated with the stretching vibrations of in- reference, whereas, a platinum wire was used as a counter plane carbon atoms. In GO and graphene, the G band vibrations À electrode. Nitrogen gas was sparged for 30 min before each test originated at relatively higher wavenumbers 1597 cm 1 and À to eliminate the effect of dissolved oxygen. Electrochemical 1601 cm 1, respectively, compared to graphite. Another band, À impedance spectroscopy (EIS) was done with 5 mV AC potential known as D band, was also observed at 1359 cm 1 (GO) and À perturbation within 10 mHze100 kHz frequency range at 0 V DC 1352 cm 1 (graphene) which may be related with the defects or bias potential versus OCP. Linear sweep voltammetry (LSV) scans irregularities in the plane of carbon chains and/or may be due to the were obtained at sweep rates of 10, 5 and 2 mV/s in the reverse formation of grain boundaries [13]. XPS survey and high-resolution (cathodic) direction from 0 to À1.5 V vs. OCP. spectra of graphene are presented in Fig. 2a. All the peaks were Fig. 2. XPS high-resolution (inset; survey) spectra (a) and TEM micrograph (inset; diffraction pattern) (b) of graphene. H. Asgar et al. / Materials Chemistry and Physics 206 (2018) 7e11 9 Fig. 3. Nyquist plots (a), bode plots (b), and linear sweep voltammograms for GOPE (c) and GrPE (d) in de-aerated 0.5M KOH solution. calibrated in accordance with the C1s peak at 285.08 eV. The O1s [16]. The effective capacitance (Ceff) was calculated from the Hsu- peak was observed at 533.08 eV. In the high-resolution spectra, the Mansfeld model [17] which could be simulated with the normal peaks at 285.98 and 288.78 eV were attributed to the remaining/ distribution of time constants and originated from the additive unremoved epoxide (-C-O-C-) and carboxyl (-COOH) groups [14], effect of double layer and pseudocapacitance. From Table 1, the respectively. The spectra of C1s has depicted the same trend as Ceff,dl for the double layer in case of GOPE and GrPE was almost reported in the literature for reduced-GO/graphene [14,15]. similar, however, the effective pseudocapacitance (Ceff,p) related The morphology and diffraction pattern of graphene were with the adsorption of ionic species was relatively higher in GOPE. evaluated from TEM images. The sheets of graphene were observed To further confirm this behavior, the LSV curves (Fig. 3c and d) containing wrinkles (Fig. 2b), which could form due to the were obtained at three different sweep rates. The existence of increased surface energy and/or drying front of the suspension sweep rate dependent reduction peak and relatively larger current during sample preparation for microscopic analysis. The electron response at large overpotential was evident in the case of GOPE diffraction pattern of graphene (inset), also validated the existence compared to GrPE which represented large polarization under the of characteristic peak corresponding to (002) plane which was in same conditions without any reduction peak. confirmation with the XRD pattern. The impedance spectra of GOPE and GrPE are shown in Fig. 3a and b. The spectra were simulated with the equivalent circuit Table 1 fi model (ECM) (inset; Fig. 3a). The kinetic performance of the sam- Simulated electrochemical parameters calculated from the ECM tting to the experimental impedance spectra of GOPE and GrPE.
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