First, the concentration of the reactants and the reaction conditions were optimized to improve the efficiency of the oxidation process of graphite. The effects of temperature and the type of peroxide used in improved hummers method for synthesis of graphene oxide were investigated. Either sodium chlorate in nitric acid similar to brodies method or potassium permanganate in sulfuric acid similar to hummers method treatment are possible. 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. We report on an improved method for the synthesis of graphene oxide based on the modified hummers method proposed by marcano et al. Graphene materials with different structures prepared from. For more details please logon to instanano nanotechnology at instanat synthesis of graphene oxide hummers method synthesis of go modified hummers method. The raw material graphite, graphite oxide, and reduced graphene oxide were. Us9938150b2 preparation method of graphene as well as. Pdf an innovative synthesis of graphene oxide by hummer. Measuring synthesis yield in graphene oxide synthesis by. Massive production of graphene oxide from expanded graphite.
This paper describes the synthesis of graphene oxide go using modified hummers method. 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. At present, a conventionallymodified hummers method is the primary method for preparing go. He used kmno 4 and nano 3 for synthesis of go 2, 4, 7.
We started the synthesis of graphite oxide by using graphite powder bay carbon, spectroscope powders, bay city, michigan 48706, 100. We demonstrated that the graphite did not need to be oxidized to such a deep degree as described in hummers method because the space distance increased little when the oxidation proceeded to a certain. 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. Graphite is commonly chosen as the starting material due to its.
The two samples of go were analysed to investigate the functional groups, compositional, morphology, optical and structural properties. Graphene oxide is the oxidized form of graphene produced by oxidizing crystal graphite with a mixture of sulfuric acid, sodium nitrate, and potassium permanganate the hummers method. Abstract graphene oxides gos with large sheets and more perfect aromatic structure were prepared by a novel modi. 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. May 01, 2015 the hummers method is used for producing graphene by oxidising graphite to go by using suitable oxidising agents such as kmno4. 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. The present invention relates to a preparation method of graphene oxide based on anthracite. 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. 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 graphite oxide was prepared by oxidizing purified natural flake graphite via modified hummers method. Jun 07, 2012 largescale fabrication of graphene is highly important for industrial and academic applications of this material.
Schematic diagram of go preparation via hummersoffeman method 10. Synthesis of graphene oxide using modified hummers method. Currently, hummers method kmno4, nano3, h2so4 is the most common method used for preparing graphene oxide. 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. Graphenes prepared by staudenmaier, hofmann and hummers. Characterization of high yield graphene oxide synthesized. Hummer used an alternative method for mass production of graphene oxide go. The aim of this study is to study the influence of different solvents on the structure and electrical properties of graphene oxide. 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. Study of reduced graphene oxide preparation by hummers. The go was reduced hydrothermally using hydrazine hydrate as a reducing agent. Highefficient synthesis of graphene oxide based on. 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.
Synthesis of graphene oxide by hummers method and its. To achieve these, samples are taken after every preparation step and analyzed with tgdtams, ftir, xrd and semedx techniques. Research article study of reduced graphene oxide preparation. The effect of temperature and type of peroxide on graphene.
There are several methods of synthesizing graphene and graphene oxide. Synthesis of graphene oxide graphene oxide was prepared using the simplified hummers method. Facile synthesis of reduced graphene oxide by modified. Characterization of high yield graphene oxide synthesized by. Researchers across multiple disciplines have paid enormous attention to it due to the unique physiochemical properties. Scanning electron microscope, fourier transform infrared spectroscopy, uvvis. Graphene oxide go is of great interest due to its low cost, easy access, and widespread ability to convert to graphene. Graphene oxide go was chemically synthesized from natural flake graphite nfg using the simplified hummers method.
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. However, models used to describe the structure of go are still in dispute and ongoing to update. Safer modified hummers method for the synthesis of graphene. Currently, hummers method kmno 4, nano 3, h 2 so 4 is the most common method used for preparing graphene oxide. Graphene oxide go has been initially prepared by a modified hummers method. Gos was prepared following the staudenmaier method 24, and got was prepared by following the tour method 25 using 45 m. In this method, the experiment was synthesized without sodium nitrate nano 3 and ice. Characterization of graphite oxide and reduced graphene. Graphite was used as the raw material and kmno4 and h2so4 were used as chemical reagents. Effect of reinforcement of reduced graphene oxide on. An improved hummers method without using nano 3 can produce graphene oxide nearly the same to that prepared by conventional hummers method. Synthesis of graphene oxide by modified hummers method and. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go.
I have prepared graphene oxide using improved hummers method. Synthesis of graphene oxide by modified hummers method. Graphene oxide films obtained using the method disclosed herein were characterized using various analytical techniques. Different samples of graphite oxide gro were prepared by modification of the improved hummers method reported in the literature. Here we propose a strategy of radical oxidation reaction for the highefficiency production of graphene oxide go. Compared with hummers method, electrochemical exfoliation of graphite is considered facile and. Gro samples were analyzed by raman spectroscopy, sem, tem, elemental analysis, xray diffraction, n2 adsorptiondesorption, and thermogravimetric analysis. Go plays important roles in the sustainable development of energy and the environment, taking advantages of oxygencontaining functional groups for good dispersibility and assembly. 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. 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. Synthesis of graphene oxide using modified hummers. We have found that excluding the nano 3, increasing the amount of kmno 4, and performing the reaction in a 9. After that, the mixture was ulteriorly oxidized by.
The results demonstrate that nio nano particles uniformly. Graphene oxide synthesized by using modified hummers approach. 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. Accepted manuscript safer modified hummers method for the. However, assist is found that all the approaches are similar to the fundamental approach of producing graphene using hummers method. Currently, hummers method kmno 4, nano 3, h 2so 4 is the most common method used for preparing graphene oxide. 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. Experimental method graphene oxide go has been initially prepared by a modified hummersmethod. Influence of different improved hummers method modifications. 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. 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. 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.
The invention also relates to a preparation method of graphene using graphene oxide obtained by method mentioned before. The amounts of intercalator and oxidant along with the particle size of graphite are important factors that affect the structure and properties of go. Us20180029887a1 method for the synthesis of graphene oxide. Pdf structure and synthesis of graphene oxide semantic. The modified hummers method introduces a way to get a more stable go colloidal solution. An innovative synthesis of graphene oxide by hummers method. Safer modified hummers method for the synthesis of.
The synthesized nanocomposite was characterized by the xrd, raman, sem, tga and energy dispersive spectrometer analysis. Recent developments of graphene oxidebased membranes. Synthesis of graphene oxide go by modified hummers. 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.
The structures of pristine graphene a and a model of graphene oxide b. Natural flake graphite nfg was procured from loba chemie india having a mean size of 60 mesh and purity of 98%. Here we reported an improved nano3free hummers method by partly replacing kmno4 with k2feo4 and controlling the amount of. Hummers method has been used for 50 years to prepare graphene oxide go by oxidizing graphite using mn2o7.
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. 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. Graphite flakes was added into sulphuric acid and the mixture. 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. The hummers method is used for producing graphene by oxidising graphite to go by using suitable oxidising agents such as kmno4. Us20180029887a1 method for the synthesis of graphene. Hidden second oxidation step of hummers method chemistry.
The improved hummers synthesis of graphene oxide go from graphite is investigated to monitor how the functional groups form during the synthesis steps. Hummers et al 25, 36 and nekahi et al 26, 37 used kmno 4. Thermal analysis of the improved hummers synthesis of. Graphene oxide was synthesized using the simplified hummers method by oxidizing for three days and six days. Structurally, graphene oxide can be visualized as a graphene sheet with its basal plane decorated by oxygencontaining. Additionally changes proposed to the graphene oxide exfoliation process can improve the synthesis yield up to 70 %. 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. Then the mixture was washed and dried at ambient temperature. 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. And currently, synthesis methods for mass production are seemingly. However, the challenge is to synthesize graphene in a bulk quantity. An improved method for the preparation of graphene oxide go is described.
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. In a typical procedure, graphene oxide was synthesized from artificial graphite using a modified hummers method. We have found that excluding the nano3, increasing the amount of kmno4, and performing the reaction in a 9. 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. Pdf synthesis of graphene oxide using modified hummers. Go was obtained from graphite flakes by using modified hummers method in which different from conventional hummers method. Higher the concentration of sulphuric acid, higher the chances of complete exfoliation of graphite into graphene oxide. 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. 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. Jan 31, 2015 the above video shows a step by step synthesis procedure of go. The go so produced is again then chemically reduced to get graphene. These analytical techniques confirmed the creation of single to few layer graphene oxide with relatively large lateral size distribution using the.
Pdf the graphene oxide is synthesized from graphite powder using modified hummers method. 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. Concentration of sulphuric acid is most important in hummers method. Tem and dfm analyses showed that go sheets prepared in this study had single and double lamellar layer. Hidden second oxidation step of hummers method chemistry of. E ect of graphene oxide synthesis method on properties and. Pdf an innovative synthesis of graphene oxide by hummers. Largescale fabrication of graphene is highly important for industrial and academic applications of this material. In this work, a new angle on hummers method is described. 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. Graphene oxide go has been initially prepared by a modified hummersmethod. Abstract graphene oxide go is one typical twodimension structured and oxygenated planar molecular material.
Comprehensive characterizations of the properties of go films were conducted. An improved hummers method for ecofriendly synthesis of. The functional groups of graphene oxide can vary depending on its method of production and its thermal andor storage history. Nov 15, 2017 in this method basically, graphite is converted into graphene oxide first and then into graphene.
Effective synthesis of highly oxidized graphene oxide that. Highquality preparation of graphene oxide via the hummers. Photosynergetic electrochemical synthesis of graphene oxide. The reduction step can also be completed through several methods, such as the environmentally methods of. There are several modifications experimented on basic hummers approach in order to achieve modified graphene. It is commonly used by engineering and lab technicians as a reliable method of producing quantities of graphite oxide. Highefficient synthesis of graphene oxide based on improved. 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. A number of techniques for preparing graphene sheets. 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. Graphene oxide go films with twodimensional structure were successfully prepared via the modified hummer method. It is proven that redox method is a promising way to synthesize go films on a large scale.
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