The graphite oxide was prepared by oxidizing purified natural flake graphite via modified hummers method. Jan 31, 2015 the above video shows a step by step synthesis procedure of go. Highefficient synthesis of graphene oxide based on improved. Gro samples were analyzed by raman spectroscopy, sem, tem, elemental analysis, xray diffraction, n2 adsorptiondesorption, and thermogravimetric analysis. Photosynergetic electrochemical synthesis of graphene oxide. Structurally, graphene oxide can be visualized as a graphene sheet with its basal plane decorated by oxygencontaining. A read is counted each time someone views a publication summary such as the title, abstract, and list of authors, clicks on a figure, or views or downloads the fulltext. Us20180029887a1 method for the synthesis of graphene oxide.
As a novel twodimensional carbon material, graphene has fine potential applications in the fields of electron transfer agent and supercapacitor material for its excellent electronic and optical property. Here we propose a strategy of radical oxidation reaction for the highefficiency production of graphene oxide go. Hummers et al 25, 36 and nekahi et al 26, 37 used kmno 4. The invention also relates to a preparation method of graphene using graphene oxide obtained by method mentioned before. Pdf structure and synthesis of graphene oxide semantic. The hummers method is used for producing graphene by oxidising graphite to go by using suitable oxidising agents such as kmno4. The effect of temperature and type of peroxide on graphene. Synthesis of graphene oxide go by modified hummers. Jun 20, 2017 graphene oxide go is touted as a viable route for the largescale production and manipulation of graphene, a wonder material which has spawned a cornucopia of applications in high speed.
Here, the fact that two different synthetic methods for graphene oxide preparation lead to very similar types of graphene oxide with a preserved graphene lattice is demonstrated. Sep 25, 2017 the improved hummers synthesis of graphene oxide go from graphite is investigated to monitor how the functional groups form during the synthesis steps. Experimental method graphene oxide go has been initially prepared by a modified hummersmethod. Graphene oxide go has been initially prepared by a modified hummers method. Ftir spectrum showed similar spectrum for the 3day synthesized go and the 6day synthesized go. The structure of graphene oxide is reminiscent of graphene but the lattice is now distorted and. Characterization of high yield graphene oxide synthesized by. We report on an improved method for the synthesis of graphene oxide based on the modified hummers method proposed by marcano et al. Measuring synthesis yield in graphene oxide synthesis by. Massive production of graphene oxide from expanded graphite.
In the present study, a simple approach has been followed for the synthesis of graphene oxide go using modified hummers method in which graphite powder. Effect of reinforcement of reduced graphene oxide on. There are several modifications experimented on basic hummers approach in order to achieve modified graphene. Graphite was used as the raw material and kmno4 and h2so4 were used as chemical reagents. Hummers method has been used for 50 years to prepare graphene oxide go by oxidizing graphite using mn2o7. An improved method for the preparation of graphene oxide go is described. The aim of this study is to study the influence of different solvents on the structure and electrical properties of graphene oxide.
Hidden second oxidation step of hummers method chemistry. We have found that excluding the nano 3, increasing the amount of kmno 4, and performing the reaction in a 9. In a typical procedure, graphene oxide was synthesized from artificial graphite using a modified hummers method. Graphene oxide films obtained using the method disclosed herein were characterized using various analytical techniques. Synthesis of graphene oxide by modified hummers method and. The modified hummers method introduces a way to get a more stable go colloidal solution. Graphene oxide was synthesized by using modified hummers method and also graphenenio nanocomposite prepared by hydrothermal method with the use of graphene oxide solution, nino 326h 2 o and urea as raw materials. Gos was prepared following the staudenmaier method 24, and got was prepared by following the tour method 25 using 45 m. In this work, a new angle on hummers method is described.
The go was reduced hydrothermally using hydrazine hydrate as a reducing agent. Study of reduced graphene oxide preparation by hummers. Natural flake graphite nfg was procured from loba chemie india having a mean size of 60 mesh and purity of 98%. May 01, 2015 the hummers method is used for producing graphene by oxidising graphite to go by using suitable oxidising agents such as kmno4. E ect of graphene oxide synthesis method on properties and. We report on an improved method for the synthesis of graphene oxide based on the modified hummers method proposed by marcano et al different steps of the process were optimized. Pdf synthesis of graphene oxide using modified hummers. Scanning electron microscope, fourier transform infrared spectroscopy, uvvis. Researchers across multiple disciplines have paid enormous attention to it due to the unique physiochemical properties. The oxidation procedure before the addition of water, which has been respected as the main oxidation step of hummers method, is named step i oxidation, and the widely ignored. The effects of temperature and the type of peroxide used in improved hummers method for synthesis of graphene oxide were investigated. Concentration of sulphuric acid is most important in hummers method.
The improved hummers synthesis of graphene oxide go from graphite is investigated to monitor how the functional groups form during the synthesis steps. Higher the concentration of sulphuric acid, higher the chances of complete exfoliation of graphite into graphene oxide. Apr 30, 2019 here, the fact that two different synthetic methods for graphene oxide preparation lead to very similar types of graphene oxide with a preserved graphene lattice is demonstrated. The most common largescale preparation method is the oxidation of graphite to graphite oxide using concentrated acids in the presence of strong oxidants and consequent thermal exfoliation and reduction by thermal shock to produce. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go. Graphene oxide go films with twodimensional structure were successfully prepared via the modified hummer method. Currently, hummers method kmno 4, nano 3, h 2 so 4 is the most common method used for preparing graphene oxide. Compared with hummers method, electrochemical exfoliation of graphite is considered facile and.
Introduction quantifying the graphene oxide go synthesis by hummers method 1 or its derivatives including a mechanical exfoliation step 2 has expanded in the recent years. Comprehensive characterizations of the properties of go films were conducted. Then the mixture was washed and dried at ambient temperature. Here we reported an improved nano3free hummers method by partly replacing kmno4 with k2feo4 and controlling the amount of. Synthesis of graphene oxide graphene oxide was prepared using the simplified hummers method. However, assist is found that all the approaches are similar to the fundamental approach of producing graphene using hummers method. Synthesis of graphene oxide by modified hummers method. Characterization of high yield graphene oxide synthesized. Influence of different improved hummers method modifications. The two samples of go were analysed to investigate the functional groups, compositional, morphology, optical and structural properties. We started the synthesis of graphite oxide by using graphite powder bay carbon, spectroscope powders, bay city, michigan 48706, 100. Different samples of graphite oxide gro were prepared by modification of the improved hummers method reported in the literature. Graphenes prepared by staudenmaier, hofmann and hummers.
Safer modified hummers method for the synthesis of. Pdf an innovative synthesis of graphene oxide by hummer. In this paper, graphite oxide was prepared from natural flake graphite by hummers method through liquid oxidization, and the reduced graphene oxide was obtained by chemical reduction of graphene oxide using nh 3 h 2 o aqueous solution and hydrazine hydrate. Us9938150b2 preparation method of graphene as well as. Highefficient synthesis of graphene oxide based on. These analytical techniques confirmed the creation of single to few layer graphene oxide with relatively large lateral size distribution using the. Abstract graphene oxide go is one typical twodimension structured and oxygenated planar molecular material. Hummer used an alternative method for mass production of graphene oxide go. Graphene oxide is synthesized by chemical treatment of graphite using only h 2 so 4, kmno 4, h 2 o 2 andor h 2 o as reagents.
The synthesized nanocomposite was characterized by the xrd, raman, sem, tga and energy dispersive spectrometer analysis. An improved hummers method without using nano 3 can produce graphene oxide nearly the same to that prepared by conventional hummers method. Hummers graphene can be prepared using hummer hummers method 19 was reported by marcano methods for synthesis of grapheme there are various methods for synthesis of graphene as follows. In this method, the experiment was synthesized without sodium nitrate nano 3 and ice.
I have prepared graphene oxide using improved hummers method. Pdf the graphene oxide is synthesized from graphite powder using modified hummers method. Hummers method is a chemical process that can be used to generate graphite oxide through the addition of potassium permanganate to a solution of graphite, sodium nitrate, and sulfuric acid. However, the challenge is to synthesize graphene in a bulk quantity. Based on these work, hummers and offeman 15 developed an alternate oxidation method in 1958, often called hummers method, in which nano 3 and kmno 4 dissolved in concentrated h 2 so 4 was used to.
The oxidation procedure before the addition of water, which has been respected as the main oxidation step of hummers method, is named step i oxidation, and the widely ignored further oxidation step after the addition of water is. In this paper, graphite oxide was prepared from natural flake graphite by hummers method through liquid oxidization, and the reduced graphene oxide was obtained by chemical reduction of graphene oxide using nh 3 ch 2 o aqueous solution and hydrazine hydrate. Go plays important roles in the sustainable development of energy and the environment, taking advantages of oxygencontaining functional groups for good dispersibility and assembly. Graphene oxide go is touted as a viable route for the largescale production and manipulation of graphene, a wonder material which has spawned a cornucopia of. Synthesis of graphene oxide using modified hummers method. And currently, synthesis methods for mass production are seemingly. The raw material graphite, graphite oxide, and reduced graphene oxide were. For more details please logon to instanano nanotechnology at instanat synthesis of graphene oxide hummers method synthesis of go modified hummers method.
Synthesis of graphene oxide using modified hummers. The structures of pristine graphene a and a model of graphene oxide b. An improved hummers method for ecofriendly synthesis of. Synthesis of reduced graphene oxide rgo modified hummer s method was partially employed using natural graphite flakes as precursor for the synthesis of reduced graphene oxide 14. After that, the mixture was ulteriorly oxidized by. Effective synthesis of highly oxidized graphene oxide that. In this article, we are going to learn about the methods of graphene synthesis that are hummers method, chemical vapor deposition, chemical exfoliation of graphene, electrochemical exfoliation. Facile synthesis of reduced graphene oxide by modified. Currently, hummers method kmno 4, nano 3, h 2so 4 is the most common method used for preparing graphene oxide.
Graphite flakes was added into sulphuric acid and the mixture. The results demonstrate that nio nano particles uniformly. Recent developments of graphene oxidebased membranes. Graphene materials with different structures prepared from. There are several methods of synthesizing graphene and graphene oxide. Pdf an innovative synthesis of graphene oxide by hummers.
We have found that excluding the nano3, increasing the amount of kmno4, and performing the reaction in a 9. Aug 02, 2017 for more details please logon to instanano nanotechnology at instanat synthesis of graphene oxide hummers method synthesis of go modified hummers method. Largescale fabrication of graphene is highly important for industrial and academic applications of this material. Safer modified hummers method for the synthesis of graphene. First, the concentration of the reactants and the reaction conditions were optimized to improve the efficiency of the oxidation process of graphite. Jun 07, 2012 largescale fabrication of graphene is highly important for industrial and academic applications of this material. Graphene oxide go was chemically synthesized from natural flake graphite nfg using the simplified hummers method. Graphene oxide was synthesized by using modified hummers method and also graphenenio nanocomposite prepared by hydrothermal method with the use of graphene oxide solution, nino326h2o and urea as raw materials. Us20180029887a1 method for the synthesis of graphene. The functional groups of graphene oxide can vary depending on its method of production and its thermal andor storage history. Tem and dfm analyses showed that go sheets prepared in this study had single and double lamellar layer.
Graphene oxide go is of great interest due to its low cost, easy access, and widespread ability to convert to graphene. In this paper, graphite oxide was prepared from natural ake graphite by hummers method through liquid oxidization, and the reduced graphene oxide was obtained by chemical reduction of graphene oxide using nh 3 h 2 o aqueous solution and. Highquality preparation of graphene oxide via the hummers. Currently, hummers method kmno4, nano3, h2so4 is the most common method used for preparing graphene oxide. This paper describes the synthesis of graphene oxide go using modified hummers method. Theoretical calculations of the reduction of graphene oxide the model used for graphene oxide had the graphene decorated with hydroxyl and epoxide groups suggest that reduction below 6.
An innovative synthesis of graphene oxide by hummers method. Based on these work, hummers and offeman 15 developed an alternate oxidation method in 1958, often called hummers method, in which nano 3 and kmno 4 dissolved in concentrated h 2. The amounts of intercalator and oxidant along with the particle size of graphite are important factors that affect the structure and properties of go. Accepted manuscript safer modified hummers method for the. Schematic diagram of go preparation via hummersoffeman method 10. Thermal analysis of the improved hummers synthesis of. Characterization of graphite oxide and reduced graphene. Nowadays, the most widely used methods to prepare graphite oxide go andor graphene oxide gro is either the hummers 20 or the brodie 21 method. Abstract graphene oxides gos with large sheets and more perfect aromatic structure were prepared by a novel modi.
Additionally changes proposed to the graphene oxide exfoliation process can improve the synthesis yield up to 70 %. The go so produced is again then chemically reduced to get graphene. Graphene oxide was synthesized by using modified hummers method and also graphene nio nanocomposite prepared by hydrothermal method with the use of graphene oxide solution, nino 326h 2 o and urea as raw materials. Graphene oxide go has been initially prepared by a modified hummersmethod. The first route involved stirring the one pot mixture continuously for three days at ambient temperature while the second route involved stirring another one pot mixture for six days also at ambient temperature. The present invention relates to a preparation method of graphene oxide based on anthracite. He used kmno 4 and nano 3 for synthesis of go 2, 4, 7. The hummers method, in which concentrated sulfuric acid h2so4 acts as the intercalator and potassium permanganate serves as the oxidant, is a commonly used method to prepare graphene oxide go. Either sodium chlorate in nitric acid similar to brodies method or potassium permanganate in sulfuric acid similar to hummers method treatment are possible. Nov 15, 2017 in this method basically, graphite is converted into graphene oxide first and then into graphene.
Go was obtained from graphite flakes by using modified hummers method in which different from conventional hummers method. Research article study of reduced graphene oxide preparation. Hidden second oxidation step of hummers method chemistry of. However, models used to describe the structure of go are still in dispute and ongoing to update. It is commonly used by engineering and lab technicians as a reliable method of producing quantities of graphite oxide.
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