Research article preparation and characterization of. Graphene oxide go has been initially prepared by a modified hummersmethod. Graphene oxide and reduced graphene oxide studied by the xrd. The preparation of graphite oxide and reduced graphene oxide. However, the generation of graphene layers from graphite is quite expensive, but can be achieved at lower cost via controlled oxidation of graphite. Xray photoelectron spectroscopy xps and reflection electron energy loss. The graphene oxide go was converted to reduced graphene oxide rgo by chemical reduction using ascorbic acid as the reducing agent. Surface functional groups of go layers and the oxidative debris od stacked on them were investigated after od was extracted. Multiscale patterning of graphene oxide and reduced graphene. 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.
Multiscale patterning of graphene oxide and reduced graphene oxide for. 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. Pdf graphene oxide and reduced graphene oxide studied by. Characterization of graphite oxide and reduced graphene oxide. Potts a, aruna velamakanni a, shanthi murali a, rodney s. The xray diffraction xrd pattern of graphene graphite oxide usually shows a characteristic diffraction peak at 2. 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. In graphene oxide and reduced graphene oxide prepared from the graphite the reels indicates 811 and 710 layers. 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. 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. Corrosion protection of carbon steel by polyurethane. A comparison of the raman spectra of singlelayer graphene and bulk graphite ab stacked can be seen in fig. The electrochemical test presented that ligningraphene oxide composites exhibited a typical cv curve and the specific capacitance reached 103fg at a. Recently, graphene and other graphenebased materials have become an essential part of composite science and technology.
Graphene synthesis via exfoliation of graphite by ultrasonication. Synthesis of graphene oxide go by modified hummers method. Xrd patterns of graphite, graphite oxide, reduced graph openi. The reduced graphene oxide was isolated from the reduced graphene oxide polyethyleneterephthalate composite and characterized by thermogravimetry, xray photoelectron spectroscopy and xray diffraction methods. Xrdhta, uv visible, ftir and sem interpretation of reduced.
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. Lattice structure our discussion of the crystal structure of graphite follows partially from d. 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. Xrd spectra of cofe 2 o 4 go confirm the polycrystalline nature of cofe 2 o 4 nanoparticles. 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.
Figure s3 a and figure s3 b show xps spectra of ti2p and o1s regions of gota, gote, and p25, respectively. Peak position, peak intensity and peak broadening of the raman spectra. Differential 5 number 10 average 50 m 100 particle diameter v. Ultravioletvisible spectra were recorded for aqueous solutions of graphite oxide by using uv1800, shimadzu spectrophotometer. 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. Combined effects of functional groups, lattice defects. 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. Analysis was performed successfully using fourier transform. Studies of reduced graphene oxide and graphite oxide in the. Facile reduction of graphene oxide suspensions and films using glass wafers.
Xrd pattern of rgo revealed the formation of layered sheet like structure which. 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. In this work graphene oxide was prepared by oxidizing graphite to form graphite oxide. Characterization of xray irradiated graphene oxide. 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. Over the span of years, improvements over various synthesis methods of graphene are constantly pursued to provide safer and more effective alternatives. The amount of graphite used for the synthesis of graphene oxide go is very important factor. Go was later reduced thermally to obtain reduced graphene oxide rgo. Jul 24, 2016 energy calibration of spectra atpixels by shifting intensity within spectra graphene oxidereduced graphene oxide stage map. Xrd patterns of the graphene, graphite oxide, and graphenemno2 composites. Currently, an improved method for the preparation of graphene. Polyurethane nanocomposites containing reduced graphene oxide. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go.
Characterization of graphite oxide and reduced graphene. Ir a, xrd b, and raman c trends of graphite, graphite oxide, and graphene. Polyurethane nanocomposites containing reduced graphene oxide, ftir, raman, and xrd studies article pdf available in journal of spectroscopy 20162. Polyurethane nanocomposites containing reduced graphene. The drift spectrum of go is shown in the figure 2a. Recently, graphene and other graphene based materials have become an essential part of composite science and technology. Ruoff a, a department of mechanical engineering and the texas materials institute, the university of texas at austin, one university station c2200. The reels results are consistent with those by the xrd indicating 8 flgoc and 4 layers flrgoc. 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. Xrd patterns of the graphene, graphite oxide, and graph. Initially graphite oxide was prepared by oxidizing the purified natural flake graphite nfg by the modified hummers method. 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. Figure s1 xrd patterns of graphene oxide and glass slide.
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. The reduction of graphene oxide into rgo is also confirmed by the xrd pattern of rgo 23. We conclude by comparing its calculated xrd spectra to experimental spectra of graphene and crystalline silicon. 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 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. Calculation of the spacing between graphene oxide sheets it can be calculated by the braggs law. Lattice strain estimated from xrd peaks are correlated to the observed raman shift. Preparation and characterization of graphene oxide reduced. A raman spectroscopic investigation of graphite oxide. Coexistence of interfacial stress and charge transfer in. 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. Graphene oxide go was synthesized from graphite and also produced from waste materials, such as coconut shell, rice husk, and bagasse. 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.
Combined effects of functional groups, lattice defects, and. Xrd patterns of the graphene, graphite oxide, and graph openi. The preparation of composite material of graphene oxide. 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.
The xray diffraction xrd patterns indicate that fullerenes had been successfully incorporated onto the surface of graphene and they worked as. Graphene oxide go layers are the individual sheets of conventional graphite oxide cgo. The go and rgo were characterized by uvvisible spectroscopy, ftir spectroscopy, and xray diffraction patterns. Nanocomposites a lot of research works have been reported on graphene or rgo andor go.
Crystal structure of graphite, graphene and silicon. 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. Synthesis of graphene oxide go by modified hummers. 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. The diffraction patterns were processed using fityk software. Research article preparation and characterization of graphene. Hydrazinereduction of graphite and graphene oxide sungjin park a,b, jinho an a, jeffrey r. 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. 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. Since a part of polymer could not be removed from reduced graphene oxide particles by trifluoroacetic acid, the hypothesis about. Graphene sheets that are now routinely obtained by the exfoliationreduction of graphite oxide exhibit raman spectra unlike traditional graphene systems. Uvvis absorption spectra suggests that the peak absorption in graphene decreases with high wavelengths. Natural flake graphite nfg was procured from loba chemie india having a mean size of 60 mesh and purity of 98%. Pdf synthesis and characterization of reduced graphene oxide.
Higher the concentration of graphite, lesser the penetration of oxidation. There is no obvious difference in ti 2p xps spectra and o1s xps spectra among gota, gote, and p25. 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. Having unique properties, graphene layers are a quite interesting nanomaterial for industrial applications. Note that the three composite samples are represented as graphenemno2a 5 min, graphenemno2b 10 min, and graphenemno2c 15 min. 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. Graphene oxide and reduced graphene oxide studied by the xrd, tem and electron spectroscopy methods article pdf available in journal of electron. 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. Graphene oxidereduced graphene oxide stage map in casaxps. Xray diffraction xrd, xray photoelectron spectroscopy xps, and atomic force microscopy afm have been used to characterize go before and after irradiation. Graphene oxide, stress, raman spectra, charge transfer and fermi level.
Doping nanoparticles doping nanoparticles onto graphene or go has been done for the following works brenner, 2012. A raman spectroscopic investigation of graphite oxide derived. Multiscale patterning of graphene oxide and reduced. This result confirms the formation of graphene oxide.
In graphene oxide xrd spectra, the major peak at 11. Energy calibration of spectra atpixels by shifting intensity within spectra graphene oxidereduced graphene oxide stage map. Thereafter, graphene oxide go was pre pared by the exfoliation of the graphite oxide in distilled water in an ultrasonicator. 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. Parameters such as reaction time, reaction temperature, and amount of concentration were varied to study the degree of oxidation of graphite to graphene oxide. Paper open access synthesis and characterization of.
One of the most structurally important materials, graphene oxide go, is prepared by the. There is a strong peak corresponding to interlayer distance of 0. Calculation of the spacing between graphene oxide sheets. Conclusions we performed a detailed analysis of the ir vibrational spectra of graphene oxide using. The structure, morphology and optical properties of synthesized nanocomposites are characterized with xrd, fesem, ftir and raman spectroscopies. Graphene oxide and reduced graphene oxide studied by the. Xrd results showed that lignin could completely block the restacking of go sheets. 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. The complete disappearance of peak at 10 and the formation of peak at 24. The origin of fluorescence from graphene oxide scientific. It is a surfacesensitive analytical technique that is useful to determine the chemical environment of atoms, in this case of carbon atoms in. 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.
Aug 18, 2019 graphene oxide is an excellent material to solve this problem 4,5,6. Xrd patterns of graphite, graphite oxide, reduced graph. Studies of reduced graphene oxide and graphite oxide in. 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. Sep 20, 2018 facile reduction of graphene oxide suspensions and films using glass wafers. The ftir spectra of cds rgo revealed peaks confirmed the presence of cds. Xrdhta, uv visible, ftir and sem interpretation of.
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