A comparison of the raman spectra of singlelayer graphene and bulk graphite ab stacked can be seen in fig. Studies of reduced graphene oxide and graphite oxide in. Raman spectroscopy has shown that william blythes graphene oxide is fully oxidised with an idig ratio of about 1, which is fairly typical for graphene oxide. It is a surfacesensitive analytical technique that is useful to determine the chemical environment of atoms, in this case of carbon atoms in. The uvinduced reduction of graphene oxide was monitored by various spectroscopic techniques, including optical absorption, xray photoelectron spectroscopy xps, raman, and xray diffraction xrd, while the. Research article preparation and characterization of graphene. The graphene oxide go was converted to reduced graphene oxide rgo by chemical reduction using ascorbic acid as the reducing agent.
The broad emission band appears between 400 and 800 nm analogous to previous reports on fluorescence spectra of go 6,10,11,12,14,17 and. A raman spectroscopic investigation of graphite oxide derived. The reduction of graphene oxide into rgo is also confirmed by the xrd pattern of rgo 23. Higher the concentration of graphite, lesser the penetration of oxidation. Graphene oxide go has been initially prepared by a modified hummersmethod. Facile reduction of graphene oxide suspensions and films using glass wafers. Differential 5 number 10 average 50 m 100 particle diameter v. The xray diffraction xrd patterns indicate that fullerenes had been successfully incorporated onto the surface of graphene and they worked as. The diffraction patterns were processed using fityk software. Thereafter, graphene oxide go was pre pared by the exfoliation of the graphite oxide in distilled water in an ultrasonicator. Research article preparation and characterization of. Go was later reduced thermally to obtain reduced graphene oxide rgo.
Though the extraction of graphene through hummers method is one of the oldest techniques yet it is one of the most suitable methods for the formation of bulk graphene. Ultravioletvisible spectra were recorded for aqueous solutions of graphite oxide by using uv1800, shimadzu spectrophotometer. Ir a, xrd b, and raman c trends of graphite, graphite oxide, and graphene. Combined effects of functional groups, lattice defects, and. Over the span of years, improvements over various synthesis methods of graphene are constantly pursued to provide safer and more effective alternatives. Having unique properties, graphene layers are a quite interesting nanomaterial for industrial applications. Jun 14, 2017 xray diffraction analysis of graphite, graphite oxide, and the reduced graphene oxide was carried out using rigaku ultima iv xray diffractometer with cu ka 1 radiation. Crystal structure of graphite, graphene and silicon. Hydrazinereduction of graphite and graphene oxide sungjin park a,b, jinho an a, jeffrey r. A new approach to synthesize graphene is oxidizing graphite powder with a mixture of h 2 so 4 h 3 po 4 acids and potassium permanganate. However, the generation of graphene layers from graphite is quite expensive, but can be achieved at lower cost via controlled oxidation of graphite. Multiscale patterning of graphene oxide and reduced graphene. Recently, graphene and other graphenebased materials have become an essential part of composite science and technology.
Currently, an improved method for the preparation of graphene. The preparation of graphite oxide and reduced graphene oxide. The electrochemical test presented that lignin graphene oxide composites exhibited a typical cv curve and the specific capacitance reached 103fg at a scan rate of 20mvs. The structure, morphology and optical properties of synthesized nanocomposites are characterized with xrd, fesem, ftir and raman spectroscopies. Xrd pattern of graphite, go and pssrgo xray photoelectron spectroscopy xps is employed to analyse extend of reduction of graphene oxide after the grafting of pss. Jul 24, 2016 energy calibration of spectra atpixels by shifting intensity within spectra graphene oxidereduced graphene oxide stage map. Combined effects of functional groups, lattice defects. In graphene oxide xrd spectra, the major peak at 11. The preparation of composite material of graphene oxide. Calculation of the spacing between graphene oxide sheets it can be calculated by the braggs law. Multiscale patterning of graphene oxide and reduced graphene oxide for. Figure s1 xrd patterns of graphene oxide and glass slide.
The intensity r atio between d peak and g peak in the raman spectra of graphene oxide and reduction of graphene oxide indicated that the. The reduced graphene oxide was isolated from the reduced graphene oxide polyethyleneterephthalate composite and characterized by thermogravimetry, xray photoelectron spectroscopy and xray diffraction methods. Graphene oxide, stress, raman spectra, charge transfer and fermi level. Parameters such as reaction time, reaction temperature, and amount of concentration were varied to study the degree of oxidation of graphite to graphene oxide. Nanocomposites a lot of research works have been reported on graphene or rgo andor go. The broad emission band appears between 400 and 800 nm analogous to previous reports on fluorescence spectra of go 6,10,11,12,14,17 and oxygenplasma treated graphene 20.
Graphene oxide go layers are the individual sheets of conventional graphite oxide cgo. Characterization of graphite oxide and reduced graphene oxide. Analysis was performed successfully using fourier transform. One of the most structurally important materials, graphene oxide go, is prepared by the. Ruoff a, a department of mechanical engineering and the texas materials institute, the university of texas at austin, one university station c2200. Pdf synthesis and characterization of reduced graphene oxide. Xrd patterns of graphite, graphite oxide, reduced graph openi.
Paper open access synthesis and characterization of. Xrd spectra of cofe 2 o 4 go confirm the polycrystalline nature of cofe 2 o 4 nanoparticles. Note that the three composite samples are represented as graphenemno2a 5 min, graphenemno2b 10 min, and graphenemno2c 15 min. Aug 18, 2019 graphene oxide is an excellent material to solve this problem 4,5,6. Xray diffraction analysis of graphite, graphite oxide, and the reduced graphene oxide was carried out using rigaku ultima iv xray diffractometer with cu ka 1 radiation. Xrd results showed that lignin could completely block the restacking of go sheets. Pdf graphene oxide and reduced graphene oxide studied by. Xray photoelectron spectroscopy xps and reflection electron energy loss spectroscopy reels.
Reduced graphene oxide is an excellent candidate for various electronic devices such as high performance gas sensors. Characterization of xray irradiated graphene oxide. In graphene oxide and reduced graphene oxide prepared from the graphite the reels indicates 811 and 710 layers. Doping nanoparticles doping nanoparticles onto graphene or go has been done for the following works brenner, 2012. The go obtained from pure graphite was compared with graphite made from indonesian biomass coconut shell, rice husk, and bagasse that had its silica content removed. Moreover, the raman spectroscopy rs, fourier transform infrared spectroscopy ftir, xray diffraction xrd and xray photoelectron microscopy xps were also applied for the characterization of the layers. Graphene oxide and reduced graphene oxide studied by the xrd. Sep 20, 2018 facile reduction of graphene oxide suspensions and films using glass wafers. The go and rgo were characterized by uvvisible spectroscopy, ftir spectroscopy, and xray diffraction patterns. At 210 nm, a peak can be noticed and one more peak around 226 nm with a little bit less intensity of absorption peak can be observed in uvvis spectra.
There is no obvious difference in ti 2p xps spectra and o1s xps spectra among gota, gote, and p25. Polyurethane nanocomposites containing reduced graphene. Peak position, peak intensity and peak broadening of the raman spectra. Initially graphite oxide was prepared by oxidizing the purified natural flake graphite nfg by the modified hummers method. Polyurethane nanocomposites containing reduced graphene oxide, ftir, raman, and xrd studies article pdf available in journal of spectroscopy 20162. Xrd patterns of the graphene, graphite oxide, and graph.
Xrd patterns of the graphene, graphite oxide, and graph openi. Energy calibration of spectra atpixels by shifting intensity within spectra graphene oxidereduced graphene oxide stage map. Graphene oxide and reduced graphene oxide studied by the xrd, tem and electron spectroscopy methods article pdf available in journal of electron spectroscopy and related phenomena 195 august. Xrd patterns of the graphene, graphite oxide, and graphenemno2 composites. We conclude by comparing its calculated xrd spectra to experimental spectra of graphene and crystalline silicon. Calculation of the spacing between graphene oxide sheets. The xray diffraction xrd pattern of graphene graphite oxide usually shows a characteristic diffraction peak at 2. Graphene oxidereduced graphene oxide stage map in casaxps. Graphene sheets that are now routinely obtained by the exfoliationreduction of graphite oxide exhibit raman spectra unlike traditional graphene systems. Recently, graphene and other graphene based materials have become an essential part of composite science and technology. Graphene synthesis via exfoliation of graphite by ultrasonication. The electrochemical test presented that ligningraphene oxide composites exhibited a typical cv curve and the specific capacitance reached 103fg at a.
Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go. Aksay, roberto car, and annabella selloni, department of chemistry and department of chemical and biological engineering, princeton university, princeton, new jersey 08544, united states. The general attributes of the raman spectra of these wrinkled graphene are first reaffirmed by evaluating the spectra of samples prepared by seven different exfoliationreduction methods. Corrosion protection of carbon steel by polyurethane. In an effort to study an alternative approach to make graphene from graphene oxide go, exposure of go to highenergy xray radiation has been performed. This result confirms the formation of graphene oxide. Xray photoelectron spectroscopy xps and reflection electron energy loss. Ruoff a, a department of mechanical engineering and the texas materials institute, the university of texas at austin, one university station c2200, austin, tx 787120292, usa b department of chemistry, inha university. Synthesis of graphene oxide go by modified hummers. The graphene oxide, prepared using a wet chemical method from the graphite, and the hydrazine reduced graphene oxide were synthesised and chemically and structurally investigated using surface sensitive electron spectroscopy methods, like xps and reflection electron energy loss spectroscopy reels. The broad, intense band centered at 3450 cm1 was assigned to oh stretching vibrations of the coh groups and the bands at 1737 cm1 were. Polyurethane nanocomposites containing reduced graphene oxide. Xray diffraction xrd, xray photoelectron spectroscopy xps, and atomic force microscopy afm have been used to characterize go before and after irradiation.
Since a part of polymer could not be removed from reduced graphene oxide particles by trifluoroacetic acid, the hypothesis about. The number of layers present has been estimated by comparing the area of the d and g peaks to the area of the silicon substrate peak ca 950 cm1. Surface functional groups of go layers and the oxidative debris od stacked on them were investigated after od was extracted. Uvvis absorption spectra suggests that the peak absorption in graphene decreases with high wavelengths. In this work graphene oxide was prepared by oxidizing graphite to form graphite oxide.
Conclusions we performed a detailed analysis of the ir vibrational spectra of graphene oxide using. There is a strong peak corresponding to interlayer distance of 0. The amount of graphite used for the synthesis of graphene oxide go is very important factor. The complete disappearance of peak at 10 and the formation of peak at 24.
Reduced graphene oxide as saturable absorbers for erdoped passively modelocked fiber laser grzegorz sobon, 1, jaroslaw sotor, 1 joanna jagiello,2 rafal kozinski,2 mariusz zdrojek, 3 marcin holdynski, 4 piotr paletko, 5 jakub boguslawski, 1 ludwika lipinska, 2 and krzysztof m. Xrdhta, uv visible, ftir and sem interpretation of. Lattice structure our discussion of the crystal structure of graphite follows partially from d. A raman spectroscopic investigation of graphite oxide. Figure s3 a and figure s3 b show xps spectra of ti2p and o1s regions of gota, gote, and p25, respectively. The drift spectrum of go is shown in the figure 2a. The commercial and synthesised fewlayer graphene oxide, prepared using oxidation reactions, and fewlayer reduced graphene oxide samples were structurally and chemically investigated by the xray diffraction xrd, transmission electron microscopy tem and electron spectroscopy methods, i. The purpose of this work is the structural analysis of graphene oxide go and by means of a new structural model to answer the questions arising from the lerfklinowski and the lee structural models. The reels results are consistent with those by the xrd indicating 8 flgoc and 4 layers flrgoc. Characterization of graphite oxide and reduced graphene. This observation is an example of xray wave interference roentgenstrahlinterferenzen, commonly known as xray diffraction xrd, and was direct evidence for the periodic atomic structure of crystals postulated for several centuries.
Graphene oxide and reduced graphene oxide studied by the. The origin of fluorescence from graphene oxide scientific. Graphene oxide and reduced graphene oxide studied by the xrd, tem and electron spectroscopy methods article pdf available in journal of electron. Graphene oxide go was synthesized from graphite and also produced from waste materials, such as coconut shell, rice husk, and bagasse. Synthesis of graphene oxide go by modified hummers method. Coexistence of interfacial stress and charge transfer in. Xrdhta, uv visible, ftir and sem interpretation of reduced. Studies of reduced graphene oxide and graphite oxide in the.
The broad diffraction of graphene in the range of 22 to 26 disappeared and this might be attributed to the assembled c60 clusters, which effectively prevented the restacking of the graphene layers. Xrd patterns of graphite, graphite oxide, reduced graph. Lattice strain estimated from xrd peaks are correlated to the observed raman shift. Their unique properties are not only restricted to graphene but also shared with derivative compounds like graphene oxide, reduced graphene oxide, functionalized graphene, and so forth. Potts a, aruna velamakanni a, shanthi murali a, rodney s. The inset shows the refined xrd patterns for the three samples with different microwave reaction times 5, 10, and 15 min. In the c 1s spectra of pssg the oxygen functionalities are considerably reduced, indicating the deoxygenation of graphene oxide figure s2. Preparation and characterization of graphene oxide reduced. Multiscale patterning of graphene oxide and reduced. Graphite oxides were obtained from scale, flake and synthetic graphites by two methods denoted a and b commercial graphite powders were ground in a planetary ball mill and sieved to a particle size spectra of graphene are presented in fig. Xrd pattern of rgo revealed the formation of layered sheet like structure which.