In the c 1s spectra of pssg the oxygen functionalities are considerably reduced, indicating the deoxygenation of graphene oxide figure s2. Synthesis, characterization and photocatalytic study of. In this work graphene oxide was prepared by oxidizing graphite to form graphite oxide. Pdf preparation and characterization of graphene oxide.
Pdf the commercial and synthesised fewlayer graphene oxide, prepared using oxidation. Since a part of polymer could not be removed from reduced graphene oxide particles by trifluoroacetic acid, the hypothesis about. Applications for singlelayer graphene oxide powder include chemical and bio sensors, supercapacitors, solar cells, and more. Surface functional groups of go layers and the oxidative debris od stacked on them were investigated after od was extracted. The development of novel membrane materials and membrane structures is an urgent demand to promote membranebased separation technology. 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. 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, incheon 402751, republic.
Synthesis of graphene oxide go by modified hummers method. Jan 24, 2019 graphene oxide go sheets have been used to construct various bulk forms of go and graphene based materials through solutionbased processing techniques. Natural flake graphite nfg was procured from loba chemie india having a mean size of 60 mesh and purity of 98%. Graphene oxide and reduced graphene oxide studied by the xrd. The go obtained from pure graphite was compared with graphite made from indonesian biomass coconut shell, rice husk, and. Synthesis and characterization of cuographene oxide composite. Xray diffraction patterns of graphite oxide go are theoretically simulated as a function of the displacements of carbon. The prepared nanocatalysts were tested for hydrodeoxygenation hdo of lignin monomer molecules vanillyl alcohol and. 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 reduced graphene oxide was isolated from the reduced graphene oxide polyethyleneterephthalate composite and characterized by thermogravimetry, xray photoelectron spectroscopy and xray diffraction methods. The 002 peak of graphene oxide go is shifted to 14. The composite was characterized by xray diffraction, ultravioletvisible diffuse reflectance spectroscopy, scanning electron microscopy sem and brunaueremmettteller. Singlelayer graphene oxide powder h method can be dispersed easily in a variety of solvents, making it highly popular among those in need of ultrastrong coatings for their equipment. Here we employ an in situ xray diffraction xrd analysis to clarify the kinetics of go decomposition in different atmospheres and sample morphologies.
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. 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. After chemical reduction by hydrazine, the sharp 002 peak of graphite oxide disappeared while another broad peak of around 24 shows up. Crystal structure of graphite, graphene and silicon dodd gray, adam mccaughan, bhaskar mookerji.
In this research, nb removal from water was studied via adsorption on graphene oxide go coated by polythiophene pt nanoparticles. It can be seen that the asprepared graphene shows a weak and broad diffraction peak at 2. Xrd patterns of graphite, graphite oxide, reduced graph openi. One of the most structurally important materials, graphene oxide go, is prepared by the. Xrd patterns obtained from the precursor graphite, go, rgo.
Thermal decomposition of graphene oxide go has been extensively investigated in the past decade, but the detailed reaction kinetics remains elusive so far. Xrd studies showed a disruption of the graphitic ab stacking order during the increase in oxidation levels. Graphene oxide as a substrate for a variety of chemical transformations, including its reduction to graphenelike materials, is also discussed. Xrd patterns of graphite, graphite oxide and reduced graphene oxide a. The xray diffraction xrd pattern of graphenegraphite oxide usually shows a characteristic diffraction peak at 2. 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. Characterization of reduced graphene oxide produced. Xrd patterns of the graphene, graphite oxide, and graph openi. Frontiers advances in microwaveassisted production of. Xrd patterns of graphite, graphite oxide, reduced graph. Graphene and graphene oxide graphene sheets can be obtained using a number of. 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. Xrd patterns recorded for flgoc, flrgoc and graphite.
Adsorption and removal characterization of nitrobenzene by. Parameters such as reaction time, reaction temperature, and amount of concentration were varied to study the degree of oxidation of graphite to graphene oxide. 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. Sep 03, 2014 xrd peak indexing, other calculations. Xray photoelectron spectroscopy xps and reflection electron energy loss spectroscopy reels. The preparation of composite material of graphene oxide. Particular emphasis is directed toward the synthesis of graphene oxide, as well as its structure. The realspace and reciprocal crystalline structures are analyzed. Surface functional groups of go layers and the oxidative debris od stacked on them were. Graphene oxide go was synthesized from graphite and also produced from waste materials, such as coconut shell, rice husk, and bagasse. The xrd peak 002, which is the major diffraction peak corresponding to the. Xray diffraction xrd is a versatile, nondestructive analytical technique which provides the.
The graphene oxide go was converted to reduced graphene oxide rgo by chemical reduction using ascorbic acid as the reducing agent. Xray diffraction pattern of graphite oxide iopscience. Graphene oxide go has been initially prepared by a modified hummersmethod. Xps and tem characterization validated the formation of graphene. Synthesis and characterization of reduced graphene oxide. Graphene oxide go with various degrees of oxidation was synthesized using a modified hummers method. Pdf graphene oxide and reduced graphene oxide studied by. Structural analysis of reduced graphene oxide by transmission. Potts a, aruna velamakanni a, shanthi murali a, rodney s. The chemical and structural analysis of graphene oxide.
Ultravioletvisible spectra were recorded for aqueous solutions of graphite oxide by using uv1800, shimadzu spectrophotometer. Characterization of graphite oxide and reduced graphene oxide. The formation of different types of oxygen containing functional groups in go, and their influences on its structure were analyzed using xray diffraction xrd, fourier transform infrared spectra, xray photoelectron spectra xps, zeta potential analysis and raman spectroscopy. 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. Research article preparation and characterization of graphene. Hydrazinereduction of graphite and graphene oxide sungjin park a,b, jinho an a, jeffrey r. The drift spectrum of go is shown in the figure 2a. Shalaby et al structural analysis of reduced graphene oxide by transmission electron microscopy. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go. Rukman, a atina khoiron nisa, a miftakhul jannatin, a benedictus piere, a abdullah, a mohamad zakki fahmi, a and heri septya kusuma c, graphene oxide go was synthesized from graphite and also produced from waste materials, such as coconut shell, rice husk, and bagasse.
The chemical and structural analysis of graphene oxide with. The elements present in graphite oxide and graphene oxide as well as their chemical state were identi. The xrd peak 002, which is the major diffraction peak corresponding to the interlayer distance in go samples, shifted from 11. A small characteristic diffraction peak of graphite oxide 001 at approximately 14 o still remained in the xrd pattern of rgo, besides. Research article preparation and characterization of graphene oxide jianguosong, 1 xinzhiwang, 1 andchangtangchang 2 college of environment and materials engineering, yantai university, qingquan road, laishan district, yantai, china. The first stage of measurements of the graphite oxides included analysis using the xrd method. Adsorption of basic magenta on graphene oxide modified. Accelerated thermal decomposition of graphene oxide films in. March, 2009 we analyze graphene and some of the carbon allotropes for which graphene sheets form the basis. The improved hummers synthesis of graphene oxide go from graphite is investigated to monitor how the functional groups form during the synthesis steps.
Reduced graphene oxide is an excellent candidate for various electronic devices such as high performance gas sensors. 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. Paper open access synthesis and characterization of. Recent developments of graphene oxidebased membranes. Improved pdru metal supported graphene oxide nanocatalysts. Binderfree graphene oxide doughs nature communications. Studies of reduced graphene oxide and graphite oxide in the. We present an in situ xray diffraction study of the synthesis of go and. The samples were characterized by xray diffraction xrd, raman spectroscopy, fourier transform infrared spectroscopy ftir, field effect. Synthesis of graphene oxide go by modified hummers. Design, synthesis, and characterization of graphene. Figure 1 shows the xrd patterns for graphene, graphite oxide, and graphenemno2 composites with different microwave reaction times 5, 10, and 15 min. Peak position, peak intensity and peak broadening of the raman spectra.
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. Thermal analysis of the improved hummers synthesis of. Studies of reduced graphene oxide and graphite oxide in. Synthesis and characterization of reduced graphene oxide rgo. Accelerated thermal decomposition of graphene oxide films. 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. Recently, graphene and other graphenebased materials have become an essential part of composite science and technology. No significant macroscopp,ic defects, wrinkles from the cu foil pmma xpsraman analysis analysis i i 006 raman mapping n ts r2r clt pmma or other functional groups on graphene in pmma or r2r i ty d g 0. Research article preparation and characterization of.
Sep 12, 2017 the development of novel membrane materials and membrane structures is an urgent demand to promote membranebased separation technology. Pdf graphene oxide and reduced graphene oxide studied by the. Graphene can be obtained in the form of reduced graphite oxide. The raw material graphite, graphite oxide, and reduced graphene oxide were characterized by xray diffraction. An xray diffraction pattern is a plot of the intensity of xrays scattered at different angles by a sample the detector moves in a circle around.
Thermal reduction of graphene oxide 75 where d 002 is the thickness of crystallite here, gp thickness, k is a constant dependent on the crystallite shape 0. Xray analysis by williamsonhall and sizestrain plot. In situ xray powder diffraction studies of the synthesis of graphene. Crystal structure of graphite, graphene and silicon. Currently, an improved method for the preparation of graphene oxide was the most common one. Graphene oxide as a substrate for a variety of chemical transformations, including its reduction to graphene like materials, is also discussed.
This paper shows a study of nanocomposite formed by adding reduced graphene oxide with high acidity and polystyrene. Graphene oxide go sheets have been used to construct various bulk forms of go and graphenebased materials through solutionbased processing techniques. Recently, graphene and other graphene based materials have become an essential part of composite science and technology. Xrdhta, uv visible, ftir and sem interpretation of. The adsorption of basic magenta on bagasse and graphene oxide. Ruoff a, a department of mechanical engineering and the texas materials institute, the university of texas at austin, one university station c2200. The go and rgo were characterized by uvvisible spectroscopy, ftir spectroscopy, and xray diffraction patterns. Evaluation and characterization of reduced graphene oxide. Study of reduced graphene oxide preparation by hummers. High quality cvd graphene of transferred by the clt technique 1 cl sem afm. Xrd patterns of the graphene, graphite oxide, and graph. The results from xrd analysis of the sample film formed has a bandwidth on the lower diffraction angle the results from xrd analysis of the sample film formed has a.
The interest and research in the material is due to the ability of these nanoparticles significantly altering the electrical and mechanical properties of the polymer, even addition of small levels. Xrd this is the basic analysis to know the crystal. Sep 20, 2018 this paper reports a facile and green method for conversion of graphene oxide go into graphene by lowtemperature heating 80 c in the presence of a glass wafer. The adsorbent was characterized using fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, and xray diffraction analyses. A relatively direct synthesis method for production of graphene is presented. Xray photoelectron microscopy was carried out using a phi 5000. By using hydrazine hydrate, the epoxy group in graphite oxide was reduced then the solution. To achieve these, samples are taken after every preparation step and analyzed with tgdtams, ftir, xrd and semedx techniques. Nitrobenzene nb has a wide range of usages as a chemical intermediate and also as a dye in printing applications. Xrdhta, uv visible, ftir and sem interpretation of reduced.
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. Graphene oxide go, as an emerging star nanobuilding material, has showed great potential in the membranebased separation field. Singlelayer graphene oxide powder h method graphene. Scheme of preparation of graphene oxidepolystyrene composite and b xrd pattern of grapene oxide and graphene oxidepolystyrene composite. 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. Study of oxygencontaining groups in a series of graphite oxides. Analysis was performed successfully using fourier transform. Facile reduction of graphene oxide suspensions and films. Xrd patterns are obtained from this analysis and compared with experimental results. Polyurethane nanocomposites containing reduced graphene oxide, ftir, raman, and xrd studies article pdf available in journal of spectroscopy 20162. Graphene oxide films obtained by vacuum filtration. Xray photoelectron microscopy was carried out using a. From xrd, it indicates the presence hexagonal of wurtzite structure for znonps. The prepared nanocatalysts were tested for hydrodeoxygenation hdo of lignin monomer molecules vanillyl alcohol and vanillin.
Polyurethane nanocomposites containing reduced graphene oxide. Aug 18, 2019 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. Graphene oxide and reduced graphene oxide studied by the. Development of nylon6graphene oxide go high performance nanocomposites abstract polymer nanocomposites have been gaining much attention in producing high strength materials due to the low cost and process ability of polymers.
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