Highefficient synthesis of graphene oxide based on improved hummers method. Initially graphite oxide was prepared by oxidizing the purified natural flake graphite nfg by the modified hummers method. Graphene due to its high specific surface area is considered to be a potential adsorbent for air and water purification systems. Synthesis of graphene oxide go by modified hummers. Highefficient synthesis of graphene oxide based on. Hummers method has been used for 50 years to prepare graphene oxide go by oxidizing graphite using mn2o7. Another approach to the production of graphene is sonication and reduction of graphene oxide go. In this study, graphene was synthesized using the recently developed improved hummers method to achieve a high oxidation rate and thermal treatment of the synthesized graphene was done to increase its pore size and make it more capable for applications in. In this method basically, graphite is converted into graphene oxide first and then into graphene. Graphene oxide go can also be synthesised by several methods.
Hummer s method is one of the easiest and economical methods to synthesize huge amount of reduced graphene oxide rgo sheets. It adopts potassium permanganate and graphite powder in concentrated acid by oxidation reaction, get brown material at the edges in the plane and. Schematic diagram of go preparation via hummersoffeman method 10. Graphene is a very huge and ultimate material for composite with metals, semiconductors and non metals in recent years, due to its has a unique atomthick with twodimensional 2d structure, excellent physical properties like high conductivity and. Higher the concentration of sulphuric acid, higher the chances of complete exfoliation of graphite into graphene oxide. Go was obtained from graphite flakes by using modified hummers method in which different from conventional hummer s method.
Concentration of sulphuric acid is most important in hummers method. A green method to fast prepare singlelayer graphene oxide. Nano express open access controllable sizeselective method to prepare graphene quantum dots from graphene oxide tianju fan1, wenjin zeng1, wei tang1, chunqiu yuan1, songzhao tong1, kaiyu cai1, yidong liu2, wei huang1,2, yong min1,3 and arthur j epstein3 abstract we demonstrated onestep method to fabricate two different sizes of graphene quantum dots gqds through. Hummer s method of synthesis graphene oxide was synthesized by hummers method through oxidation of graphite. Graphene oxide go is of great interest due to its low cost, easy access, and widespread ability to convert to graphene. Go was later reduced thermally to obtain reduced graphene oxide. Jm tour and coworkers studied the formation mechanism of graphene oxide by a modified hummers method using a single graphite flake. In hummer s method first graphite powder is mixed with acid and graphite oxide. Measuring synthesis yield in graphene oxide synthesis by modified hummers method erkka j. In the following some of these methods will be presented and discussed. Massive production of graphene oxide from expanded graphite. Insitu chemical reductioncoprecipitation method to prepare sfrgo using des.
Graphene produced through oxidation of graphite to graphene oxide go, exfoliation of resulting go and reduction of exfoliated graphene oxide rgo is the most popular method hummer s method. Study of reduced graphene oxide preparation by hummers. Synthesis of graphene oxide by hummers method and its. 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. 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. Hidden second oxidation step of hummers method chemistry. Nanoparticle hybrid materials for bioapplications perry t. Go was obtained from graphite flakes by using modified hummers method in which different from conventional hummers method. Graphene oxide as a substrate for a variety of chemical transformations, including its reduction to graphene like materials, is also discussed. 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. 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. Facile hydrothermal method to prepare graphene quantum. We showed that while staudenmaier and hofmann methods methods that do not use potassium permanganate as oxidant generated thermally reduced graphenes with comparable electrochemical properties, the graphene prepared by the hummers method which uses permanganate as oxidant showed higher heterogeneous electron transfer rates and lower. But at the end, it tuned black instead of yellowish color.
Preparation of graphene selected topics in physics. At present, a conventionallymodified hummers method is the primary method for preparing go. Basic protocol 1 and alternate protocol describe two different modified hummer s methods for highyield synthesis and exfoliation of graphene oxide go from bulk graphite. However, the challenge is to synthesize graphene in a bulk quantity. Synthesis of fewlayered, highpurity graphene oxide. Endotoxinfree preparation of graphene oxide and graphene. Thereafter, graphene oxide go was pre pared by the exfoliation of the graphite oxide in distilled water in an ultrasonicator. Hummers is relatively good, and the preparation process is relatively safe. Preparation and characterization of graphene oxide hindawi. Graphite is commonly chosen as the starting material due to its. However, assist is found that all the approaches are similar to the fundamental approach of producing graphene using hummers method. This protocol outlines two main methods for preparation of endotoxinfree a graphene oxide, and b graphene dispersions for biological and medical applications. I am sure there must be a lot of places where i might have done wrong but not. This method have several advantages that are we can produce graphene in the laboratory easily and the quantity of the output product is more.
This chapter describes the synthesis of graphene oxide by hummer s method and graphene through chemical reduction. 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 oxidize graphite into graphite oxide within a. These analytical techniques confirmed the creation of single to few layer graphene oxide with relatively large lateral size distribution using the. Highefficient synthesis of graphene oxide based on improved. Briefly, 300 ml of concentrated sulfuric acid and 6 g of sodium nitrate were mixed gently under continuous stirring in a 1 l beaker. Measuring synthesis yield in graphene oxide synthesis by.
Design, synthesis, and characterization of graphene. Go was prepared by oxidizing the purified natural flake graphite nfg by a mod ified hummers method. Graphene materials with different structures prepared from. Particular emphasis is directed toward the synthesis of graphene oxide, as well as its structure. Pdf synthesis of graphene oxide using modified hummers. Prepared go powders were then dissolved into different solvents, namely acetone and ethanol. A novel chemical reductioncoprecipitation method to. Preparation and characterization of reduced graphene oxide. A highly responsive methanol sensor based on graphene.
Research on adsorption performance of graphene oxide and. Based on the preparation of anthracite, the invention could reduce production costs effectively comparing to traditional preparation methods of graphene and graphene oxide, and make the reaction more fast and complete, facilitating the achievement of large scale industrial production. The graphite oxide was prepared by oxidizing purified natural flake graphite via modified hummers method. Graphenes prepared by staudenmaier, hofmann and hummers. Staudenmaier 19, 20, hofmann 21, hummers 22 and tour 23 have all. 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. Complete removal of the hydrogen peroxide after reaction was achieved by catalytic dialysis with manganese oxide. Go was obtained from graphite flakes by using modified hummers. The process started with the chemical oxidation of commercial graphite powder into graphite oxide by modified hummer s method, followed by the exfoliation of graphite oxide in distilled water using the ultrasound frequency from a laboratory ultrasonic bath. Go was prepared from natural flake graphite through onepot synthesis based on new modified hummers method. An innovative synthesis of graphene oxide by hummer s method. This method often yields of multilayers graphene rgo in flake types which having lateral length in the range of several hundred nano meters to.
Synthesis of graphene oxide by modified hummers method. Natural flake graphite nfg was procured from loba chemie india. Synthesis of graphene oxide using modified hummers. In this method, the experiment was synthesized without sodium nitrate nano3 and ice bath, but carried out at room temperature. Graphene based materialpolyindole composites were prepared by in situ polymerization. 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. The synthesized nanocomposite was characterized by the xrd, raman, sem, tga and energy dispersive spectrometer analysis. All three methods involve oxidation of chemical methods for the production of graphenes sungjin park1 and rodney s. Graphene oxide go films with twodimensional structure were successfully prepared via the modified hummer method. Us20180029887a1 method for the synthesis of graphene. Graphene oxide synthesized by using modified hummers approach. Pdf an innovative synthesis of graphene oxide by hummer. In this work, a new angle on hummers method is described. Synthesis of porous graphene powder through improved.
The thermal properties and morphology of graphene and graphene oxide have been investigated. Effect of graphene oxide synthesis method on properties. Graphene oxide go was prepared from graphite powder using modified hummer s method, followed by reduction of exfoliated go with hydrazine hydrate. The hummers method is used for producing graphene by oxidising graphite to go by using suitable oxidising agents such as kmno4. I tried to prepare graphene oxide using hummer s method. Structurally, graphene oxide can be visualized as a graphene sheet with its basal plane decorated by oxygencontaining. Graphene oxide go has been initially prepared by a modified hummersmethod. On the other hand, the hummers and tour methods produce go with larger sheet size, and are more effective in enhancing the mechanical. Synthesis of graphene oxide go by modified hummers method and its thermal reduction to obtain reduced graphene oxide rgo syed nasimul alam, nidhi sharma, lailesh kumar department of metallurgical and materials engineering, national institute of technology rourkela, rourkela, india abstract. 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. Staudenmeiers process is extremely hazardous and has a low yield.
Either sodium chlorate in nitric acid similar to brodies method or potassium permanganate in sulfuric acid similar to hummers method treatment are possible. Synthesis of graphene oxide go via hummer s method instanano duration. Graphene oxide films obtained using the method disclosed herein were characterized using various analytical techniques. Controllable sizeselective method to prepare graphene. Oxidationconditions determine the structure of graphene oxide. The go so produced is again then chemically reduced to get graphene. The result shows that graphene oxide and reduced graphene oxide have successfully been synthesized. 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. Synthesis of graphene oxide using modified hummers method. There are several modifications experimented on basic hummers approach in order to achieve modified graphene. Graphite oxide go is usually synthesized through the oxidation of graphite using oxidants including concentrated sulfuric acid, nitric acid and potassium permanganate based on brodie method, staudenmaier method, 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 further oxidation step after the addition of water is. Institute for advanced materials, devices, and nanotechnology. Hummer s method is widely used method for preparation of graphene. A simple approach to stepwise synthesis of graphene oxide. The natural graphite powder was oxidized to synthesize go by the use of formerly published modified hummer s method. 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.
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. This research studied the synthesis of graphene oxide and graphene via a lowcost manufacturing method. A simple technique to prepare graphene quantum dots gqds by the hydrothermal reaction of graphene oxide go sheets with hydrogen peroxide is presented. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go. The aim of this study is to study the influence of different solvents on the structure and electrical properties of graphene oxide. Green synthesis of graphene oxide by seconds timescale. 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 graphene oxide was prepared by the optimized improved hummers method. Synthesis of graphene oxide go by modified hummers method. It is the most common preparation method of the graphene oxide at present. Us9938150b2 preparation method of graphene as well as.
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