I am looking for a technique that can produce graphene directly onto glass substrates. Structural and electronic properties of graphene oxide and. Multifunctional oxides for integrated manufacturing of. Facile and effective synthesis of reduced graphene oxide. An innovative synthesis of graphene oxide by hummer s method. Green synthesis of graphene oxide by seconds timescale. The chemical reduction of graphene oxide can provide large quantities of reduced graphene oxide for potential application in electronics and composite materials. Preparation of a leaflike bivo4reduced graphene oxide. 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. Here we reported an improved nano3 free hummers method by partly replacing kmno4. 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 the present communication, we report on nmr study of mndecorated graphene oxide go produced by the hummers method 1. Simultaneous nitrogendoping and reduction of graphene oxide. A new environmentally friendly onestep method for producing multilayer preferably 79 layers nitrogendoped graphene nmlg with a slight amount of oxygencontaining defects was developed.
The approach is based on the electrochemical exfoliation of graphite electrode in the presence of azide ions under the conditions of electrolysis with pulse changing of the electrode polarization. Preparation of graphene oxide by modifying the hummers. A number of fundamental and process challenges exists for efficient graphene based tces, in particular, environmentally and thermally stable doping, interfacial band engineering for efficient. The thermal properties and morphology of graphene and graphene oxide have been investigated. Robinson, hernan sanchez, georgi diankov, hongjie dai department of chemistry, stanford university, stanford, california 94305 email. 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. Effective synthesis of highly oxidized graphene oxide that. What is the simplest method to synthesise graphene oxide.
Different samples of graphite oxide gro were prepared by modification of the improved hummers method reported in the literature. Here we synthesize and explore the biological applications of nano graphene oxide ngo, i. Synthesis of graphene oxide by the modified hummers method and measuring the synthesis yield were investigated. The graphite oxide was prepared by oxidizing purified natural flake graphite via modified hummers method. 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. 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. 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. 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. Massive production of graphene oxide from expanded graphite ling sun, bunshi fugetsu1 graduate school of environmental science, hokkaido university, sapporo 0600810, japan abstract.
Photosynergetic electrochemical synthesis of graphene oxide. Twentyfive milligrams of the graphite oxide paperlike film was placed in a beaker, and 50 ml deionized water was then added. Concentration of sulphuric acid is most important in hummers method. Onestep electrochemical preparation of multilayer graphene. As an important precursor and derivate of graphene, graphene oxide go has received wide attention in recent years.
Tailorable synthesis of highly oxidized graphene oxides via. Nov 07, 2016 researchers from brown university have developed a method of using graphene templates to make metal oxide films with intricate surface textures. Synthesis of graphene oxide go by modified hummers method. Researchers use graphene templates to make new metaloxide. You can produce graphene oxide by modified hummers method followed by. Gro samples were analyzed by raman spectroscopy, sem, tem, elemental analysis, xray diffraction, n2 adsorptiondesorption, and thermogravimetric analysis. Massive production of graphene oxide from expanded graphite. What is the best method for the synthesis of graphene. The simple method of preparation, easy scalability, cost effectiveness and high electrical conductivity 1.
Nanoscale tunable reduction of graphene oxide for graphene. A lowcost method for preliminary separation of reduced. Herein we report a rapid, chemical free and low temperature method for high throughput production of graphene by exfoliation of graphite oxide using focused solar radiation. Chapter 2 synthesis, characterization and models of.
This chapter describes the synthesis of graphene oxide by hummer s method and graphene through chemical reduction. In this study we report a green approach to the synthesis of graphene, bioreduced by crude polysaccharide. 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. Pdf an innovative synthesis of graphene oxide by hummer. Graphene oxide was synthesized from graphite flakes using modified hummers method. In hummer s method first graphite powder is mixed with acid and graphite oxide.
The improved hummers synthesis of graphene oxide go from graphite is investigated to monitor how the functional groups form during the synthesis steps. Synthesis of graphene oxide go by modified hummers. Compared with hummers method, electrochemical exfoliation of graphite is considered facile and. It is also known as graphene oxide when used to form unimolecular sheets. Simultaneous nitrogen doping and reduction of graphene oxide. Synthesis of graphene oxidetio nanocomposite as an adsorbent. There are two main processes described in the literature for producing graphite oxide, the hummers 19 and brodie 20 methods. 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. Graphene oxide go was chemically synthesized from natural flake graphite nfg using the simplified hummers method. E ect of graphene oxide synthesis method on properties and. An improved hummers method without using nano 3 can produce graphene oxide nearly the same to that prepared by conventional hummers method. Graphene can be obtained in the form of reduced graphite oxide, sometimes. It shows that, nano3 does not affect the synthesis method to produce graphene oxide. First, the concentration of the reactants and the reaction conditions were optimized to improve the efficiency of the oxidation process of graphite.
Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go. Doping of cnts with heteroatoms other than nitrogen for example, boron or oxygen enhances the catalytic activity for the. Based on the results, a comprehensive method to measure graphene oxide synthesis yield was proposed, which will allow comparison of future literature results. Without using nano3 still produce same characteristic of go. 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. Nonaqueous approach to the preparation of reduced graphene. Top down method for synthesis of highly conducting graphene.
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. Xray diffraction results show the presence of graphene and nickel on the prepared samples. Nickel nanoparticles were dispersed uniformly in a graphene oxide solution, using a laser ablation technique with different ablation times that ranged from 5 to 20 minutes. However detailed structure is still not understood due to strong disorder and irregular packing of layers. Graphene oxide go was made by a modified hummers method using expandable graphite flake graftech as starting material. Mdsric 2018 proceedings, 2930 august, 2018 wahpakistan 1 preparation of graphene oxide by modifying the hummer s method farmanullah khan1, zaheer ahmad1, tariq mahmood2, faisal nawaz1, shazia naheed 1, faiza asghar, muhammad ajmal1 1department of chemistry, university of wah, wah cantt, 47040 pakistan.
Graphene oxide is a graphene derivative showing wide applications, but it suffers from harsh synthetic conditions and long reaction time. The amount of nano3 and kmno4 was varied to produce sheet like structure. Several analytical methods were employed to characterize the composition and morphology. We report on a means to tune the topographical and electrical properties of reduced go rgo with nanoscopic resolution by local thermal reduction of go with a heated atomic force microscope tip. The raw material graphite, graphite oxide, and reduced graphene oxide were. Synthesis of reduced graphene oxide rgoni composite by a.
Hummer s method is one of the easiest and economical methods to synthesize huge amount of reduced graphene oxide rgo sheets. Heat treating stacked graphene oxide nanosheets to generate. Oct 03, 2017 graphene is singleatomthick sheet of carbon that has gained global attention as an innovative material. Using multifunctional oxide films, we report on the development of an integration strategy for scalable manufacturing of graphene based transparent conducting electrodes tces for organic electronics.
Synthesis of graphene oxide using modified hummers method. A number of techniques for preparing graphene sheets. We prepared a unique leaflike bivo 4 reduced graphene oxide bivo 4 rgo composite with prominent adsorption performance and photocatalytic ability by a singlestep method. This yield is much higher than that 110 3% from larger graphite flakes with sizes of 10100. The aim of this study is to study the influence of different solvents on the structure and electrical properties of graphene oxide. Natural flake graphite nfg was procured from loba chemie india. It adopts potassium permanganate and graphite powder in concentrated acid by oxidation reaction, get brown material at the edges in the plane and.
A reduced graphene oxidenickel rgoni composite has been succesfully synthesized using a combination of marcanos method for synthesizing graphene oxide go, subsequently followed by a facile microwave assisted reduction method. Graphene oxide go has been initially prepared by a modified hummersmethod. Reduced graphene oxide as catalyst for hydrogenation of. A team of scientists from kumamoto university, japan, has found out that we can generate pressure by simply mounting graphene oxide nanosheets one over the other, where graphene oxide is highly identical to graphene. Highefficient synthesis of graphene oxide based on improved. Copper nanoparticles stabilized by reduced graphene oxide for. Graphenes prepared by staudenmaier, hofmann and hummers. Gos was prepared following the staudenmaier method 24, and got was prepared by following the tour method 25 using 45 m. Highyield preparation of graphene oxide from small graphite flakes via an improved hummers method with a simple purification process. A method of preparing a reduced graphene oxide foam, the method comprising the steps of. It is also able to be revised in the creation of a onemoleculethick version of the substance known as graphene oxide.
Evidence of graphitic ab stacking order of graphite oxides. Thermal analysis of the improved hummers synthesis of. In this study we report a green approach to the synthesis of graphene, bio reduced by crude polysaccharide. Either sodium chlorate in nitric acid similar to brodies method orpotassium permanganate in sulfuric acid similartohummers method treatment are possi. The results indicate that the nickel nanoparticle sizes inside the graphene oxide decreased, and the volume fraction for the nickel nanoparticles in the graphene oxide increased with an increasing ablation time.
Research on adsorption performance of graphene oxide and. Synthesis of graphene oxide by hummers method and its. Currently, hummers method kmno4, nano3,h 2so4 is the most common method used for preparing graphene oxide. To achieve these, samples are taken after every preparation step and analyzed with tgdtams, ftir, xrd and semedx techniques. Preparation of graphene oxide stabilized nickel nanoparticles. Synthesis of reduced graphene oxide rgo via chemical reduction article pdf available in aip conference proceedings 16611 may 2015 with 4,443 reads how we measure reads. The synthesis of the graphene oxides graphite oxide go was synthesized by a modified hummers method. Higher the concentration of sulphuric acid, higher the chances of complete exfoliation of graphite into graphene oxide. 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. Tem and dfm analyses showed that go sheets prepared in this study had single and double lamellar layer. University of hyogo chemical modification of graphene oxide.
The first synthesis and thus discovery of go was described. First principles nmr signatures of graphene oxide ning lu, ying huang, haibei li, zhenyu li. Graphene oxide synthesized by using modified hummers. Massive production of graphene oxide from expanded graphite arxiv. Synthesis of graphene, various methods, mechanism, advantages and drawbacks, preparation of ndoped graphene. We have found that excluding the nano 3, increasing the amount of kmno 4, and performing the reaction in a 9.
It is proven that redox method is a promising way to synthesize go films on a large scale. Measuring synthesis yield in graphene oxide synthesis by. There are several methods of synthesizing graphene and graphene oxide. Go was obtained from graphite flakes by using modified hummers method in which different from conventional hummers method. Synthesis of graphene oxide using modified hummers. Hummers is relatively good, and the preparation process is relatively safe. 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. Hummer s method is widely used method for preparation of graphene. Synthesis of graphene oxide graphene oxide was prepared using the simplified hummers method. Comprehensive characterizations of the properties of go films were conducted. Pdf synthesis of reduced graphene oxide rgo via chemical. Nioh2 composites present high electrochemical properties, with specific capacitance of 1215 f g. Structural and optical properties of graphene oxide prepared by.
University of hyogo chemical modification of graphene oxide yoshiaki matsuo department of materials science and chemistry, university of hyogo 2167 shosha, himeji, hyogo 6712201, japan. 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. Improved synthesis of graphene oxide research nebraska. Currently, hummers method kmno 4, nano 3, h 2 so 4 is the most common method used for preparing graphene oxide. Graphene paper prepared by new proprietary method involving high pressure and high temperature treat ment in the reduction process show new possibilities. Safer modified hummers method for the synthesis of. Though the extraction of graphene through hummers method is one of the oldest techniques yet it is one of the most suitable methods for the formation of bulk graphene. 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. Go plays important roles in the sustainable development of energy and the environment, taking advantages of oxygencontaining functional groups for good dispersibility and assembly. It is also able to be revised in the creation of a onemoleculethick version of the. Synthesis of graphene oxide by modified hummers method.
We want to prepare graphene or reduced graphene oxide. Currently, hummers method kmno4, nano3, h2so4 is the most common method used for preparing graphene oxide. In this research, go produced by the hummers, tour, and staudenmaier methods were characterized and embedded at various fractions into the. Highyield preparation of graphene oxide from small graphite. The synthesized nanocomposite was characterized by the xrd, raman, sem, tga and energy dispersive spectrometer analysis. In a deviation from the conventional hummers method, a spontaneous expansion approach was introduced with expanded graphite as the precursors. Us9938150b2 preparation method of graphene as well as. Colloidal dispersions of graphene oxide sheets in water at a concentration of 5 mgml were obtained. A lowtemperature method to produce highly reduced graphene oxide. Controllable sizeselective method to prepare graphene. Complete graphite oxide was produced by hummers method see supplementary materials, and used as the starting material for the preparation of graphene oxide go colloids. It is the most common preparation method of the graphene oxide at present. We developed a simple chemical method to obtain bulk quantities of ndoped, reduced graphene oxide go sheets through thermal annealing of go in ammonia. Here, the fact that two different synthetic methods for graphene oxide preparation lead to very similartypes of graphene oxide with apreserved graphene lattice is demonstrated.
Starting from the same graphene oxide, chemical crgo, hydrothermal. Over the span of years, improvements over various synthesis methods of graphene are constantly pursued to provide safer and more effective alternatives. The synthesis of graphene from graphite flakes is represented in figure 2. 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. One can suggest that similar impurities occur in the precursor graphene oxide. Brodiestaudenmaier hummers and freewater based approaches are reported and where it is considered the in. Staudenmeiers process is extremely hazardous and has a low yield. These results are in near concord with results reported earlier graphene at different diffraction peaks varies from 32 to 84 nm as calculated from scherrers formula. Go was obtained from graphite flakes by using modified hummers. Pdf synthesis of graphene oxide using modified hummers. 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. Synthesis and characterization of graphene oxide using. It is commonly used by engineering and lab technicians as a reliable method of producing quantities of graphite oxide. Characterization of high yield graphene oxide synthesized.
The synthesis of go comprises three consecutive steps, namely peroxidation. Expandable graphite flake 1 g was ground with nacl 50 g for 10 min. Copper nanoparticles passivated with polyallylamine. The result shows that graphene oxide and reduced graphene oxide have successfully been synthesized.
This method have several advantages that are we can produce graphene in the laboratory easily and the quantity of the output product is more. Green conversion of graphene oxide to graphene nanosheets and. Simultaneous nitrogendoping and reduction of graphene oxide xiaolin li, hailiang wang, joshua t. Xray photoelectron spectroscopy xps study of go sheets annealed at various reaction temperatures reveals that ndoping occurs at a temperature as low as 300 c, while the highest doping level of. Structural and physiochemical properties of the products were investigated with the help of ultravioletvisible spectroscopy uvvis, fourier transform infrared spectroscopy ftir, x. 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. Graphene oxide as a substrate for a variety of chemical transformations, including its reduction to graphene like materials, is also discussed. After sonication, 400 ml go solution 5 mgml was transformed in situ into graphene under stirring by adding 2 ml hydrazine hydrate 50% and 5 ml ammonia solution 25% into the solution according to a modified wallaces method. The graphene oxide was prepared by graphite oxide exfoliating in distilled water with ultrasonic waves. Jun 11, 2010 the reduced form of graphene oxide go is an attractive alternative to graphene for producing largescale flexible conductors and for creating devices that require an electronic gap.
In the hummers method, the oxidation of graphite to graphite oxide is accomplished by treating graphite with essentially a waterfree mixture of. Particular emphasis is directed toward the synthesis of graphene oxide, as well as its structure. Slideshare uses cookies to improve functionality and performance, and to provide you with relevant advertising. Nacl was dissolved in water and removed by filtration. An improved method for the preparation of graphene oxide go is described. Twodimensional graphene offers interesting electronic, thermal, and mechanical properties that are currently being explored for advanced electronics, membranes, and composites. Synthesis of graphene oxidetio 2 nanocomposite graphene oxide 6 0 mg was dispersed in 30 ml of water by magnetic stirring for 1 h. Graphene oxide go was synthesized from graphite powder by improved hummers method as reported in previous studies 27. Hummer s method of synthesis graphene oxide was synthesized by hummers method through oxidation of graphite. Nanographene oxide for cellular imaging and drug delivery.
Either sodium chlorate in nitric acid similar to brodies method or potassium permanganate in sulfuric acid similar to hummers method treatment are possible. 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. Graphite was used as the raw material and kmno4 and h2so4 were used as chemical reagents. Effect of graphene oxide synthesis method on properties. Graphene oxide go films with twodimensional structure were successfully prepared via the modified hummer method. I suggest using this article because this method yields good. Graphene oxide go has been initially prepared by a modified hummers method. Graphene oxide synthesis graphene oxide go was prepared chemically via modi. We demonstrated onestep method to fabricate two different sizes of graphene quantum dots gqds through chemical cutting from graphene oxide go, which had many advantages in terms of simple process, low cost, and large scale in manufacturing with higher production yield comparing to the reported methods. Highefficient synthesis of graphene oxide based on. The interlayer spacings of graphite, graphite oxide and graphene oxide. An improved hummers method for ecofriendly synthesis of. Sigmaaldrich offers a number of graphene oxide products. Jun 15, 2017 university of illinois at chicago scientists have discovered a new chemical method that enables graphene to be incorporated into a wide range of applications while maintaining its ultrafast.
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