It shows that, nano3 does not affect the synthesis method to produce graphene oxide. Highefficient synthesis of graphene oxide based on improved. Synthesis of graphene oxide using modified hummers method. An improved hummers method for ecofriendly synthesis of. Synthesis of graphene oxide by hummers method and its. Then, go will be reduced to graphene using various reducing agents. Conclusionthe innovative synthesis of graphene oxide for producing go nanoparticles has more significant advantages over hummers method. Characterization of high yield graphene oxide synthesized. The hummers method provides several advantages such as.
These methods allow not only the production of graphite oxide but also reduced graphene oxide, without undergoing chemical, thermal, or mechanical reduction steps. In this method, the experiment was synthesized without sodium nitrate nano3 and ice bath, but carried out at room temperature. The effectiveness of this oxidation process can be evaluated by the. Concentration of sulphuric acid is most important in hummers method. Here we reported an improved nano3free hummers method by partly replacing kmno4 with k2feo4 and controlling the amount of. 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. Highefficient synthesis of graphene oxide based on. Structural and physiochemical properties of the products were investigated with the help of ultravioletvisible spectroscopy uvvis, fourier transform infrared spectroscopy ftir, x. Graphite is oxidised using improved hummer s method soft chemistry synthetic route to produce graphene oxide go nanoparticles. Study of reduced graphene oxide preparation by hummers.
Dec 03, 2020 the aim of this study is to study the influence of different solvents on the structure and electrical properties of graphene oxide. Research article study of reduced graphene oxide preparation. It is commonly used by engineering and lab technicians as a reliable method of producing quantities of graphite oxide. Reduced graphene oxide synthesis via improved hummers. Here, graphene oxide go was prepared by oxidizing the purified natural flake graphite nfg by a modified hummers method.
E ect of graphene oxide synthesis method on properties and. The graphene oxide was prepared by graphite oxide exfoliating in distilled water with ultrasonic waves. Graphene oxide go has been initially prepared by a modified hummers method. 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. The publication preparation of graphitic oxide bywilliam s. The basic preparation methods were developed by brodie 3, staudenmaier 4, hoffmann 5, hummers 6, hummers and offemann 7, and tour 8,9. Either sodium chlorate in nitric acid similar to brodies method or potassium permanganate in sulfuric acid similar to hummers method treatment are possible. The protocol for running the reaction does not involve a large exotherm and produces no toxic gas.
We have found that excluding the nano3, increasing the amount of kmno4, and performing the reaction in a 9. During the oxidation process, graphite crystal was treated with strong oxidizing. Hummer s method of synthesis graphene oxide was synthesized by hummers method through oxidation of graphite. A series of preparation protocols emanated trying to optimize the synthesis of graphene oxide in order to obtain a less defective material, as source for graphene. Hummers method graphene oxide can be easily synthesized by modifi ed hummers method recently reported by marcano et al 22. Characterization of graphite oxide and reduced graphene oxide. Pdf synthesis of graphene oxide by modified hummers. To attack graphene layers, the oxidizing agent needs to. Characterization of high yield graphene oxide synthesized by. There are several modifications experimented on basic hummers approach in order to achieve modified graphene. Characterization of graphite oxide and reduced graphene. This method is commonly known as hummers method and involves the oxidation of graphite to form graphene oxide nanosheets go by using strong oxidizing agent such as potassium permanganate and potassium perchlorate. Pdf synthesis of graphene oxide go by modified hummers. Pdf synthesis of graphene oxide by modified hummers method.
This method includes all former developments but with key improvements. The results demonstrate that nio nano particles uniformly. Research article preparation and characterization of. Reduced graphene oxide synthesis via improved hummers method. Thermal analysis of the improved hummers synthesis of. The xrd spectroscopy obtained the fractional content of the 2h graphite phase of 71. Moreover, the new method yields a higher fraction of welloxidized hydrophilic carbon material. Hummer s method is widely used method for preparation of graphene. In hummer s method first graphite powder is mixed with acid and graphite oxide is formed. Research article preparation and characterization of graphene. Andrey krayev m graphene oxide production of graphene oxide. Graphite flakes 2 g and nano 3 2 g were mixed in 50 ml of h 2 so 4 98% in a ml volumetric flask kept under at ice bath 05c with continuous stirring. Pdf an innovative synthesis of graphene oxide by hummer.
In this research, go produced by the hummers, tour, and staudenmaier methods were characterized and embedded at various fractions into the. Nowadays, the hummers method of 1958 is still widely employed to delaminate and oxidize graphite because of the improved convenience in comparison with. Graphene oxide is graphite that has been oxidized to intersperse the carbon layers. Synthesis of graphite oxide with different surface oxygen.
Pdf the aim of this study is to study the influence of different solvents on the structure and electrical properties of graphene oxide. Currently, hummers method kmno4, nano3, h2so4 is the most common method used for preparing graphene oxide. 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. 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 extent and the obtained graphite oxides gtos could be fully. A simple approach to stepwise synthesis of graphene oxide. Jan 29, 2020 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, reduced graphene oxide, hummers method, lithium ion battery, anode support material. Synthesis of graphene oxide by modified hummers method. The synthetisation enables the production of large scale by increasing the kmno 4 ratio. Graphene oxide go was synthesized according to hummers method by using graphite flakes, sodium nitrate. An innovative synthesis of graphene oxide by hummer s method. Feb 09, 2012 graphene oxides gos with large sheets and more perfect aromatic structure were prepared by a novel modified hummers method. Pdf graphene oxide synthesized by using modified hummers.
Synthesis of graphene oxide nanosheets via modified. Then graphite oxide is converted into graphene oxide using sonication. Go was obtained from graphite flakes by using modified hummers method in which different from conventional hummers method. Nov 03, 2016 an improved hummers method for ecofriendly synthesis of graphene oxide. In this process, graphite is first oxidized to give go nanosheets using.
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. This method have several advantages that are we can produce graphene in the laboratory easily and the quantity of the output product is more. The classification of synthesis method is shown in fig below. These methods allow not only the production of graphite oxide but also reduced graphene oxide, without undergoing chemical, thermal, or. Graphite oxide was first prepared by oxford chemist benjamin c. Pdf highefficient synthesis of graphene oxide based on.
Effect of graphene oxide synthesis method on properties and. To achieve these, samples are taken after every preparation step and analyzed with tgdtams, ftir, xrd and semedx techniques. First, the concentration of the reactants and the reaction conditions were optimized to improve the efficiency of the oxidation process of graphite. Graphene oxide preparation by using modified hummer s method graphene oxide go was prepared from graphite flakes by using modified hummer s method. The tem imaging was further used to characterize and the prepared go has flakelike shapes. Brodie was exploring the structure of graphite by investigating the reactivity of graphite flake 1. Additionally changes proposed to the graphene oxide exfoliation process can improve the synthesis yield up to 70 %. Synthesis of graphene oxide go by modified hummers. Synthesis of graphene oxide graphene oxide was prepared using the simplified hummers method.
The synthesized nanocomposite was characterized by the xrd, raman, sem, tga and energy dispersive spectrometer analysis. Abstract graphene oxides gos with large sheets and more perfect aromatic structure were prepared by a novel modi. Method of solvent stripping did not destroy the structure of the graphene and presented no surface defects in the graphene sheet. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go. Briefl y, 3 g graphite fi ne powder was added into a mixture of concentrated h 2 so 4 h 3 po 4 540 ml. Safer modified hummers method for the synthesis of. It is also able to be revised in the creation of a onemoleculethick version of the substance known as graphene oxide. Synthesis, characterization, chemical reduction and. In this paper, a simple stepbystep synthetisation of go using modified hummers method is report. Graphene can be obtained in the form of reduced graphite oxide, sometimes also referred as graphene oxide.
However, the present synthesis methods depend on the. In 1957 hummers and offeman developed a safer, quicker, and more efficient process called hummers method, using a mixture of sulfuric acid h. Synthesis of graphene oxide by modified hummers method and. Gos was prepared following the staudenmaier method 24, and got was prepared by following the tour method 25 using 45 m. However, assist is found that all the approaches are similar to the fundamental approach of producing graphene using hummers method. Redox method is the most popular method to prepare graphene and graphite 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. Graphene oxide go was synthesized according to hummers method by using graphite flakes, sodium nitrate, hydrogen peroxide30%, sulphuric acid70%, potassium permanganate 99%.
Synthesis of graphene oxide nanosheets via modified hummers. Accepted manuscript safer modified hummers method for the. 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. Tem, ftir spectrum, xrd, uvvis spectrum and raman spectroscopy were employed to characterize the prepared go. The last two methods hummers offemann 6 and tour 8,9 methods deserve special. Without using nano3 still produce same characteristic of go. Go was obtained from graphite flakes by using modified hummers. Offeman in 1958 has attracted the scientific attention in recent years, which is reflected in 18000 citations recorded on scopus. In typical procedure, graphene oxide go was produced using modified hummers method from pure graphite powder.
Safer modified hummers method for the synthesis of graphene. Natural flake graphite nfg was procured from loba chemie india having a mean size of 60 mesh and purity of 98%. Study of reduced graphene oxide preparation by hummers method and related characterization. The described method is termedhummers method,ormodified hummers method,when graphiteispretreated. Higher the concentration of sulphuric acid, higher the chances of complete exfoliation of graphite into graphene oxide. Pdf synthesis of graphene oxide using modified hummers. Measuring synthesis yield in graphene oxide synthesis by.
Graphene oxide go based on coconut shell waste was successfully synthesized using a modi. In the original hummers method, 3 wt equiv of potassium. Graphite graphene oxide go has also been prepared by using a bottomup synthesis method tanglau method in which the sole source is glucose, the process is safer, simpler, and more environmentally friendly compared to traditionally topdown method, in which strong oxidizers are involved. Gopd composite is synthesized by ultrasonication, chemical treatment with potassium tetrachloropalladate k2pdcl4 and overnight heat treatment.
Graphene oxide go was chemically synthesized from natural flake graphite nfg using the simplified hummers method. Synthesis of graphene oxide go by modified hummers method. 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, nino326h2o and urea as raw materials. It consists of carrying out a reaction of graphite powder with kmno. Conclusion we applied improved hummeras method in our experiment as to produce graphene oxide, and different from conventional hummer method because synthesis graphene oxide without using nano3. Reduced graphene oxide synthesis via improved hummers method 1rafig alibeyli, 1ali ata and 1erdal topac 1gebze institute of technology, nanotechnology research center, gebze kocaeli abstract in this study, we focused on production of rgo1 by reduction of go 2. Nov 15, 2017 in this method basically, graphite is converted into graphene oxide first and then into graphene. Characterization of graphene oxidegraphene oxide go was prepared using modified hummer s method. Graphene oxide go supported palladium pd nanocomposites. 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 is highly desired for printing electronics, catalysis, energy storage, separation membranes, biomedicine, and composites.
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. Kmno4 9g was added at different proportions to a cooled 0oc then the solution of concentrated h. Highyield and stepwise synthesis of graphene oxide by. Pdf an innovative synthesis of graphene oxide by hummers. Nov 01, 20 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 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. Brodie in 1859, by treating graphite with a mixture of potassium chlorate and fuming nitric acid. The graphite oxide was prepared by oxidizing purified natural flake graphite via modified hummers method. The raw material graphite, graphite oxide, and reduced graphene oxide were characterized by xray.
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