In this study, films of graphene oxide and chemically or thermally reduced graphene oxide were produced by a simple vacuum filtration method and submitted to a thorough characterization by x ray diffraction xrd, raman and infrared spectroscopies, fieldemission scanning electron microscopy, transmission electron microscopy, atomic force microscopy, confocal microscopy, and contact angle. Basics of xray diffraction introduction to powderpolycrystalline diffraction. Basic diffraction theory has numerous important applications in solidstate physics and physical metallurgy, and this graduatelevel text is the ideal introduction to the fundamentals of the discipline. In situ synchrotron xray diffraction characterization of. Indeed, it has a youngs modulus comparable to steel, on the order of 300 gpa. Immobilization of crvi from solution by a graphene oxide. In this study, films of graphene oxide and chemically or thermally reduced graphene oxide were produced by a simple vacuum filtration method and submitted to a thorough characterization by xray diffraction xrd, raman and infrared spectroscopies, fieldemission scanning electron microscopy, transmission electron microscopy, atomic force microscopy, confocal microscopy, and contact angle. Graphene oxide and reduced graphene oxide studied by the. Zinc oxide nanoparticles zno nps have received much attention for their implications in cancer therapy. In situ xray powder diffraction studies of the synthesis of.
Basics of x ray powder diffraction training to become an independent user of the x ray sef at the center for materials science and engineering at mit. Graphene oxide and reduced graphene oxide studied by the xrd. Johnsen and poul norby department of energy conversion and storage, technical university of denmark, frederiksborgvej. Recently, graphene oxide go, which was prepared by chemically oxidizing graphite to graphite oxide gto with strong oxidants and ultrasonic cleavage, has attracted much attention as a possible intermediate for manufacture of graphene in large volume.
Here we employ an in situ x ray diffraction xrd analysis to clarify the kinetics of go decomposition in different atmospheres and sample morphologies. In this study, gos were prepared by the newly modi. Schematic representation of graphene oxide synthesis from agro waste. Xray diffraction investigations of nanostructured zno. Development of nylon6graphene oxide go high performance nanocomposites abstract polymer nanocomposites have been gaining much attention in producing high strength materials due to the low cost and process ability of polymers. Positron annihilation lifetime spectroscopy pals is then used to extract information on the microenvironment in between the layers of graphene oxide. X ray photoelectron spectroscopy xps is employed to analyse extend of reduction of graphene oxide after the grafting of pss. Xray diffraction powder diffraction pattern of a crumpled not quite powdered origami shell, using cu k. Calculation of the spacing between graphene oxide sheets it can be calculated by the braggs law. Moreover, the diffraction pattern obtained from tem also validated the formation of graphene with characteristics 002 plane.
This observation is an example of xray wave interference roentgenstrahlinterferenzen, commonly known as xray diffraction xrd, and was direct evidence for the periodic atomic structure of crystals postulated for several centuries. Thermal decomposition of graphene oxide go has been extensively investigated in the past decade, but the detailed reaction kinetics remains elusive so far. Xray diffraction characterization of polymer intercalated graphite oxide. Characterization of xray irradiated graphene oxide coatings. Introduction graphene oxide go and reduced graphene oxide rgo, synthesised from go, has a future in fields ranging from electronics to energy technologies. Coatings using x ray diffraction, x ray photoelectron spectroscopy, and atomic force microscopy thomas n. This device is equipped with a ni filter, and generates monochromated cuk. It is proven that redox method is a promising way to synthesize go films on a large scale. Calculation of the spacing between graphene oxide sheets. Accelerated thermal decomposition of graphene oxide films.
X ray diffraction pattern of zinc oxide nanoparticles. Crystal structure of graphite, graphene and silicon dodd gray, adam mccaughan, bhaskar mookerji. Characterization of xray irradiated graphene oxide coatings using xray diffraction, xray photoelectron spectroscopy, and atomic force microscopy thomas n. Here we employ an in situ xray diffraction xrd analysis to clarify the kinetics of go decomposition in different atmospheres and sample morphologies. A graphene oxide gonanoscale zerovalent iron nzvibiochar composite go. Carbon bonded alumina filters coated by graphene oxide for. Development is rigorous throughout the book, the treatment is carried far enough to relate to experimentally observable quantities and stress is placed on modern applications to nonstructural. Crystal structure of graphite, graphene and silicon. Synthesis of graphene oxide go by modified hummers. In an effort to study an alternative approach to make graphene from graphene oxide go, exposure of go to highenergy x ray radiation has been performed. Graphene holds great promise for potential use in nextgeneration electronic and.
In the c 1s spectra of pssg the oxygen functionalities are considerably reduced, indicating the deoxygenation of graphene oxide figure s2. Graphene oxide has many carboxylic groups within its molecular structure, which is perfect for esterification and imidation, the derivatives graphene oxide gap, gso when reaction grapheme oxide with 2amino pyridine gap and 2hydroxy5sulfobenzoic acid gso. The bending modulus is found to be 1 kt,which is about two orders of magnitude lower than the bending rigidity of neat graphene. The go obtained from pure graphite was compared with graphite made from indonesian biomass coconut shell, rice husk, and.
Graphene oxide go was synthesized from graphite and also produced from waste materials, such as coconut shell, rice husk, and bagasse. Graphene oxide itself is a suitable material for the fabrication of membranes or foils 30. However, most common applications in the organic materials community have been restricted to either chemical identification or qualitative strain analysis. We offer a brief overview of the solventbased graphene production and summarize the current knowledge on the formation mechanism of graphite oxide that proceeds via graphite intercalation compounds.
The realspace and reciprocal crystalline structures are analyzed. Graphene oxides gos with large sheets and more perfect aromatic structure were prepared by a novel modified hummers method. Graphene oxide films obtained by vacuum filtration. By measuring the angles and intensities of these diffracted beams, a crystallographer can produce a threedimensional picture of the density of electrons within the.
Xray diffraction pattern of zinc oxide nanoparticles. Encapsulation of gfe2o3 decorated reduced graphene oxide in polyaniline coreshell. The peak in the x ray spectrum of a typical graphene oxide paper specimen corresponds to the layerto. X ray photoelectron spectroscopy xps and reflection electron energy loss spectroscopy reels.
Comprehensive characterizations of the properties of go films were conducted. Coatings using xray diffraction, xray photoelectron spectroscopy, and atomic force microscopy thomas n. The go obtained from pure graphite was compared with graphite made from indonesian biomass coconut shell, rice husk, and bagasse that had its silica content removed. Blanton and debasis majumdar eastman kodak company, kodak technology center, rochester, ny 146502106 usa abstract. The principles of xray diffraction 83 now the difference of optical path for the top and bottom wave is shown by the heavydrawn path lying between two parts of the wavefronts of the incident and reflected waves. How can we differentiate graphene and graphite using x ray. Graphene oxide go films with twodimensional structure were successfully prepared via the modified hummer method. Characterization of xray irradiated graphene oxide coatings using xray diffraction. The layering in our graphene oxide paper is evident from its xray diffraction pattern. Jan 22, 2019 a graphene oxide gonanoscale zerovalent iron nzvibiochar composite go. A xray diffraction analysis on graphene layers of assam coal. Subsequently reduced graphene oxide rgo having few layer graphene is extracted.
Xray diffraction characterization of polymer intercalated. Xray photoelectron spectroscopy xps and reflection electron energy loss spectroscopy reels. A xray diffraction analysis on graphene layers of assam. Two database versions are available the pdf i and the pdf ii. Oxidative stressmediated antibacterial activity of. Rgotio2, reduced graphene oxidetitanium dioxide nanocomposite. In situ xray powder diffraction studies of the synthesis. High quality of the synthesized go is corroborated using a host of characterization techniques including xray diffraction, optical. Xray diffraction xrd, xray photoelectron spectroscopy xps, and atomic force microscopy afm have been used to characterize go before and after irradiation.
Synthesis and characterization of novel nano derivatives. I boukhoubza 1,2, m khenfouch 2,3, m achehboune 1,2, b m mothudi 3, i zorkani 1 and a jorio 1. The sem images suggest that rgo having a thickness less than 10 nm could be synthesized by this process. The membership of the icdd consists of worldwide representation from. The peak in the xray spectrum of a typical graphene oxide paper specimen corresponds to the layerto. Synthesis and characterization of novel nano derivatives of. Xray diffraction patterns of a graphite and graphene. In xray diffraction pattern xrd, graphite shows a characteristic peak at 2.
Go retains the structure of graphite, but with a larger and irregular basal plane spacing. Hummers method, thermal reduction, graphene oxide, reduced graphene oxide, x ray diffraction, in situ 1. March, 2009 we analyze graphene and some of the carbon allotropes for which graphene sheets form the basis. Xray diffraction patterns of a graphite and graphene oxide and b reduced graphene oxide, titanium dioxide, and reduced graphene oxidetitanium dioxide nanocomposites. The international centre for diffraction data icdd. In this study, nylon6graphene oxide go nanocomposites were developed and characterized. Tem and dfm analyses showed that go sheets prepared in this study had single and double lamellar layer. March, 2009 we analyze graphene and some of the carbon allotropes for which graphene sheets form the. Oxidative stressmediated antibacterial activity of graphene oxide and reduced graphene oxide in pseudomonas aeruginosa sangiliyandi gurunathan, jae woong han, ahmed abdal dayem, vasuki eppakayala, jinhoi kimdepartment of animal biotechnology, konkuk university, seoul, south koreabackground. Basics of xray powder diffraction training to become an independent user.
Moreover, the diffraction pattern obtained from tem also validated the formation of. Preparation and characterization of graphene oxide paper. Natural flake graphite nfg was procured from loba chemie india having a mean size of 60 mesh and purity of 98%. Go can be reduced through several methods to obtain reduced graphene oxide rgo. Blanton and debasis majumdar eastman kodak company, kodak technology center, rochester, ny 146502106 usa abstract in an effort to study an alternative approach to make graphene from graphene oxide go, exposure of go to highenergy xray. Sep 20, 2018 this paper reports a facile and green method for conversion of graphene oxide go into graphene by lowtemperature heating 80 c in the presence of a glass wafer. Published under licence by iop publishing ltd journal of physics. In an effort to study an alternative approach to make graphene from graphene oxide go, exposure of go to highenergy xray radiation has been performed. Xray diffraction patterns of a graphite and graphene openi. The chemical composition and successful loading of both nutrients on go sheets were confirmed by xray photoelectron spectroscopy, thermogravimetric analysis, and xray diffraction xrd. However, the underlying molecular mechanisms behind the anticancer response of zno nps remain unclear. It has been reported that zno nps induce selective killing of cancer cells.
Accelerated thermal decomposition of graphene oxide films in. Xray diffraction pattern of graphite oxide show the performance about all factor that have indicated in ability to influenced the pattern of go. In situ xray diffraction studies of graphite oxidation. Xray diffraction characterization of polymer intercalated graphite oxide volume 27 issue 2 thomas n. Xray diffraction has been a standard technique for investigating structural properties of materials. A direct method of producing graphene from graphite oxide go via ultrasonication is presented in this work. Ruoff a, a department of mechanical engineering and the texas materials institute, the university of texas at austin, one university station c2200, austin, tx 787120292, usa b department of chemistry, inha university, incheon 402751, republic. The information is stored in an ascii format in a file called pdf1. Jul 26, 2007 the layering in our graphene oxide paper is evident from its x ray diffraction pattern. X ray diffraction xrd, x ray photoelectron spectroscopy xps, and atomic force microscopy afm have been used to characterize go before and after irradiation. Random layered graphene structural parameters of these coals were determined by using xray diffraction technique, which showed that the l a and l c are 6499 a and 2263 a for tirap2 and 5554 a and 2380 a for that of tirap1 coals respectively.
Moreover, its use for polymeric thin films has been challenging because of the low structure factor of carbon and the thin film nature of. The path difference between reflections on neighbouring planes is. Ruoff a, a department of mechanical engineering and the texas materials institute, the university of texas at austin, one university station c2200. The commercial and synthesised fewlayer graphene oxide, prepared using oxidation reactions, and fewlayer reduced graphene oxide samples were structurally and chemically investigated by the xray diffraction xrd, transmission electron microscopy tem and electron spectroscopy methods, i. Graphene oxide go has been initially prepared by a modified hummersmethod. Despite its very high stiffness, we show here that go is superflexible.
The pdf i database contains information on dspacing, chemical formula, relative intensity, rir quality information and routing digit. Xray crystallography xrc is the experimental science determining the atomic and molecular structure of a crystal, in which the crystalline structure causes a beam of incident xrays to diffract into many specific directions. Synthesis and structural characterization of separate graphene oxide and reduced graphene oxide nanosheets. Preparation and characterization of graphene oxide paper nature. Xray diffraction pattern of graphite oxide free download as pdf file. Jun 15, 2012 in situ x ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide. Blanton and debasis majumdar eastman kodak company, kodak technology center, rochester, ny 146502106 usa abstract in an effort to study an alternative approach to make graphene from graphene oxide go, exposure of go to highenergy x ray. Graphene oxide go, the main precursor of graphenebased materials made by solution processing, is known to be very stiff. 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. Subsequently reduced graphene oxide rgo having few layer graphene is extracted from go by the thermal reduction of go. Drude conductivity exhibited by chemically synthesized reduced graphene oxide daniyal younas, quratulain javed, sabeen fatima et al.
Characterization of xray irradiated graphene oxide. The figure below compares the xray diffraction patterns from 3 different forms of sio 2 these three phases of sio 2are chemically identical. 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. Characterization of xray irradiated graphene oxide coatings using xray diffraction, xray photoelectron spectroscopy, and atomic force microscopy tom blanton, debasis majumdar, steve brandt, jill fornalik eastman kodak company, corporate research and engineering, rochester, ny 146502106 usa graphene is a singlelayer planar sheet of sp2. Hydrazinereduction of graphite and graphene oxide sungjin park a,b, jinho an a, jeffrey r. Facile reduction of graphene oxide suspensions and films. In situ synchrotron xray diffraction characterization of the synthesis of graphene oxide and reduced graphene oxide graphene oxide go and reduced graphene oxide rgo synthesised from go, has a promising future in fields ranging from electronics to energy technologies1. In figure 6a, the xray diffraction xrd of grapheme oxide shows a large interlayer spacing equal to 8. Go may be synthesized by the modified hummers method2, where a. Potts a, aruna velamakanni a, shanthi murali a, rodney s. The principles of x ray diffraction 83 now the difference of optical path for the top and bottom wave is shown by the heavydrawn path lying between two parts of the wavefronts of the incident and reflected waves. Characterization of go the xray diffraction xrd pattern was obtained using a bruker d8 advance xray diffractometer berlin, germany. Majumdar, eastman kodak company, rochester, ny usa 146502106 graphite oxide go is generated by treating graphite with strong oxidizers.
The xrd peak 002, which is the major diffraction peak corresponding to the. Xray diffraction investigations of nanostructured zno coated with reduced graphene oxide. Xray diffraction investigations of nanostructured zno coated. In addition, the results of our in situ xray diffraction investigation. Convenient preparation of graphene oxide from expandable. The commercial and synthesised fewlayer graphene oxide, prepared using oxidation reactions, and fewlayer reduced graphene oxide samples were structurally and chemically investigated by the x ray diffraction xrd, transmission electron microscopy tem and electron spectroscopy methods, i. The socalled turbostatic structure of carbons in coal with randomly oriented stacking of the lamellae graphene produces intense peaks, which are the dominant features in its xray diffraction profiles. How can we differentiate graphene and graphite using x ray diffraction pattern and raman spectoscopy.
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