Study of reduced graphene oxide preparation by hummers. Graphite powder 5 g was gradually added to a mixture of concentrated hno 3 65 %, 25 ml and concentrated h 2 so 4 298 %, 50 ml. In low temperature reaction, the edge of graphite was oxidized and intercalated with. Pdf role of graphite precursor and sodium nitrate in.
Preparation and properties of polystyrene nanocomposites. The effectiveness of this oxidation process can be evaluated by the magnitude of carbonoxygen ratio of the obtained graphene. Analysis of oxidation degree of graphite oxide and chemical. It was showed that the graphite interlayer distance. Graphene oxide was synthesized by hummers method through oxidation of graphite. It is found that the more intense of oxidation reaction is, the more crack the expanded graphite is, and more completely the expansion of the nano graphite oxide will be. This yield is much higher than that 110 3% from larger graphite flakes with sizes of 10100. Synthesis of graphene oxide using modified hummers method. Preparation of polyvinylpyrrolidonedecorated hydrophilic. Comprehensive characterizations of the properties of go films were conducted. Sulfuric acid intercalated graphite oxide for graphene. The preparation of go can modified to produce certain functionalized go which has lower or higher conductivity properties than pristine graphene,14. Results showed exfoliation of graphite into graphene, with surfaces decorated with pvp. Beside to chemical production of graphenes from graphene oxide in multistep processes, for which.
Copper and nickel were used as catalysts in the cvdgraphene synthesis, ch4 and h2being used as precursor gases. Waterdispersible graphene was prepared by reacting graphite oxide and 6amino4hydroxy2naphthalenesulfonic acid ans. Herein, we report the synthesis of the graphite oxide with diverse surface oxygen content through three b, c, d different modi. Cancer natural graphite may contain small amounts of impurities of 0% 1% crystalline silica, which is listed as a group 1 carcinogen by iarc and as a suspected human carcinogen by acgih. The disappearance of the sharp peak can be attributed to the exfoliation of layered structures of graphite oxide. Highyield preparation of graphene oxide from small graphite flakes via an improved hummers method with a simple purification process. Preparation and characterization of nitrogen doped reduced.
Supporting information file swelling of graphene oxide membranes in alcohols. Since the extraordinary characteristics of graphite are known, several methods for its preparation have been developed. Inhalation of high concentrations of crystalline silica over prolonged. Preparation of semiconducting graphenebased carbon films from silylated graphite oxide and covalent attachment of dye molecules yoshiaki matsuo, taito mimura, and yosohiro sugie department of materialsscience and chemistry, graduate school of. Fabrication of the electrodes consisted on the hybrid materials being. Preparation and characterization of graphite oxide. For preparation of graphite oxide, 230 ml of 18m h 2 so 4 was taken in a beaker 5 l capacity and cooled to 5 oc using an ice bath.
The optimization of both the chemical vapor deposition cvd synthesis method to prepare graphene and the improved hummers method to prepare graphite oxide is reported. The graphene particles were then oxidized into graphene oxide go using the combination of strong oxidizing agents, thermal oxidizing, and. An economic and facile method for graphene oxide preparation from. Highyield preparation of graphene oxide from small. A controlled process to form reduced graphene oxide surfaces from graphene oxide with tunable surface chemistry and morphology.
Optimization of the synthesis procedures of graphene and. For this reason, it is necessary to characterize products from. In a typical protocol, 2 g of graphite flakes were mixed with 1. Pdf preparation and characterization of graphene oxide paper. Preparation and characterization of graphene oxide paper. Reactivitycontrolled preparation of ultralarge graphene oxide by chemical expansion of graphite lei dong, 1,2 zhongxin chen, 1 shan lin, ke wang, 1,2 chen ma, 1 hongbin lu. The reduced graphene oxide is of very bad quality compared to pristine graphene, nevertheless graphene oxide could be the desired product. For more details please logon to instanano nanotechnology at instanat synthesis of graphene oxide hummers method synthesis of go modified hummers method how to synthesized graphene. 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 preparation of graphene. Natural flake graphite nfg was procured from loba chemie india having a mean size of 60 mesh and purity of 98%. The catalytic microwave exfoliated graphite oxide cmego is of higher quality than the traditional microwave exfoliated graphite oxide, including a much higher exfoliation degree with thinner graphene sheets and higher specific surface area 886 m 2 g.
A lowcost nonexplosive synthesis of graphene oxide for. Pdf synthesis of graphite oxide with different surface oxygen. Graphite oxide can be described as group of layers graphene oxide 38. Ultrasonically assisted preparation of graphene by kathrin hielscher, hielscher ultrasonics gmbh. 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. Graphite oxide, formerly called graphitic oxide or graphitic acid, is a compound of carbon. Graphite oxide has attracted much interest as a possible route for preparation of natural graphite in the largescale production and manipulation of graphene as a material with extraordinary electronic properties. Graphite oxide was first prepared by oxford chemist benjamin c. Preparation of graphene oxide and reduction of go to prgo nanosheets. The field of nanotechnology has advanced following the discovery of a twodimensional material of sp2 hybridized carbon atoms, graphene in 2004 by geim and novoselov.
Reactivitycontrolled preparation of ultralarge graphene. The composition of the sample matrix can have a major effect on the analysis. Graphite oxide was acquired from the oxidation of graphite by improved hummers method and characterized by xray diffraction, scanning electron microscope, fourier transform infrared absorbance spectroscopy and thermogravimetric analysis. Graphite oxide can be exfoliated using any organic solvent to form go and produce different form dispersion with different longterm stability and thickness of single layer go. Graphite oxide, formerly called graphitic oxide or graphitic acid, is a compound of carbon, oxygen, and hydrogen in variable ratios, obtained by treating graphite with strong oxidizers. Brodie in 1859, by treating graphite with a mixture of.
Characterization of graphite oxide and reduced graphene oxide. Go and graphite oxide can be produced by similar in chemical process but different in its structure37. It is proven that redox method is a promising way to synthesize go films on a large scale. The following equation gives the reaction between kmno 4 and h 2 so 4. Analysis was performed successfully using fourier transform. Insitu synthesis and characterization of reduced graphene. Synthesis and fabrication of graphene and graphene oxide. Polystyrene psgo and psgraphene nanocomposites were prepared via melt blending. Pdf graphene oxide go can be regarded as one typical twodimension structured oxygenated planar molecular material. Preparation of amino functionalized graphene oxide go graphite oxide is prepared by following hummers method 17.
Exfoliated graphene sheets decorated with metal metal. The thermal exfoliation and reduction of graphite oxide go is the most commonly used strategy for largescale preparation of graphene, and the oxidation. Graphene oxide go has been initially prepared by a modified hummersmethod. Graphene oxide go films with twodimensional structure were successfully prepared via the modified hummer method. Graphite oxide is a layered material consisting of hydrophilic oxygenated graphene sheets graphene oxide sheets bearing oxygen functional groups on their basal planes and edges. Scheme of the preparation of graphite oxide and reduced graphene oxide from graphite.
In this study, graphite oxides gos with different oxidation degrees and graphene nanosheets were prepared by a modified hummers method and thermal exfoliation of the prepared go, respectively. Preparation of semiconducting graphenebased carbon. Graphene sheets were processed by in situ ballmilling graphite flakes in an ethanol solution of polyvinylpyrrolidone pvp. Role of graphite precursor and sodium nitrate in graphite oxide synthesis. Synthesis variables were optimized according to a thickness value, calculated using a homemade excelvba application. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go.
Synthesis of graphite oxide with different surface oxygen contents. To this reactant, a mixture of powdered flake graphite 10 g and nano 3 5 g was added gradually under constant. Characterization of graphite oxide and reduced graphene. Preparation and characterization of graphene oxide paper article pdf available in nature 4487152. C60rgo hybrids show characteristic peaks of c60 at 10. In 1859, brodie was first to prepared graphite oxide by the oxidation of graphite with fum. Pdf structure and synthesis of graphene oxide researchgate. Graphite oxide was synthesized from graphite by modified hummers method 27, 28. Reaction mechanism of solutionbased reduction of graphite oxide will be discussed, to begin with the mechanism of hummers, though kmno 4 is used as a kind of oxidizing agent. Pdf graphite oxide is synthesized via oxidation reaction using oxidant compounds that have lattice defects by the incorporation of unlike. An external file that holds a picture, illustration, etc. This new pvpfunctionalized graphene could be further dispersed in varieties of polar solvents, including ethanol, dimethylformamide, and water. Graphite, graphite oxide, graphene oxide, and reduced. Xray diffraction study showed that the basal reflection 002 peak of graphite oxide was absent in the ansfunctionalized.
Selective ionic transport through tunable subnanometer pores in singlelayer graphene membranes pdf. Here, raphene oxide g go was prepared by oxidizing the purified natural flake graphite nfgby a mo dified hummers method. Polyaniline was synthesized by chemical polymerization, and au nanoparticles npau were added afterward. Initially graphite oxide was prepared by oxidizing the purified natural flake graphite nfg by the modified hummers method. Synthesis of graphite oxide with different surface oxygen. This indicates that further work with solidstate nmr on clabelled graphite oxide is necessary, along with for example titration with fluorescent tags of carboxylic and other groups to identify their spatial distribution on individual graphene oxide platelets derived from graphite oxide as discussed further below. Supporting information file effects of molecule size and.
These methods allow not only the production of graphite oxide but also. Simple synthesis of large graphene oxide sheets via. Graphite oxide go was synthesized by a modified hummers method. The maximally oxidized bulk product is a yellow solid with c. The preparation of graphite oxide is one of essential steps for graphene by oxidation reduction method. Paper open access preparation of nanographite oxide. The broad peak may stem from the partial restacking of exfoliated graphene layers. Synthesis and characterization of reduced graphene oxide. The preparation of graphite oxide and reduced graphene oxide. In this work, synthesis and characterization of reduced graphene oxidepolyanilineau nanoparticles gopaninpau as a hybrid capacitor are presented. Xrd patterns of graphite, graphite oxide, reduced graph.
Tem and dfm analyses showed that go sheets prepared in this study had single and double lamellar layer. We demonstrated that natural graphite is wellpurified by acid. 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. Graphene graphite is composed of two dimensional sheets of sp2hybridized, hexagonally arranged carbon atoms the graphene that. Synthesis of graphene oxide go by modified hummers.
Xray diffraction results showed that gos and graphene were exfoliated in the ps composites. Thereafter, graphene oxide go was pre pared by the exfoliation of the graphite oxide in distilled water in an ultrasonicator. Also the obtained graphene oxide has to be reduced afterwards, using thermal treatments or chemicals again 7. Preparation of graphitic oxide journal of the american. In this activity students use natural graphite to duplicate the mechanical exfoliation technique used to separate graphene sheets from graphite. Purification and preparation of graphite oxide from. Borate inorganic crosslinked durable graphene oxide membrane preparation and membrane fouling control.
Graphite oxide was prepared by modified hummers method from purified natural graphite sample from west kalimantan. Surface functional groups of go layers and the oxidative debris od stacked on them were investigated after od was extracted. Materials prepared through different methods will have difference properties. How temperature influences purity volume 33 issue 23 iman sengupta, samarshi chakraborty, monikangkana talukdar, surjya k. Graphene has received so much attention due to its exceptional electronic, thermal, mechanical, and optical properties in addition to its large surface area and singleatom thickness. The graphite lattice is fully oxidized within a few seconds in our electrochemical oxidation reaction, and the graphene oxide obtained is similar to those achieved by the present methods. Graphite oxide is synthesized via oxidation reaction using oxidant compounds that have lattice defects by the incorporation of unlike functional groups. Go was later reduced thermally to obtain reduced graphene oxide.
Pdf preparation of waterdispersible graphene by facile. Ideally this would coincide with a trip to an electron microscope facility. Furthermore, exfoliation of graphite oxide would produce single layer sheet of graphite oxide which call go39. Reduced graphene oxides were obtained using hightemperature exfoliationreduction according to the following process. Voltammogram for graphite material is very similar to its oxide form. The graphite oxide was prepared from graphite powder by. Mechanical exfoliation to make graphene and visualization.
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