One of the major directions of research in the area of materials science is to impart multifunctionalities to materials. Carbon stands on the top of the list to provide various multifunctional materials. It exists in all dimensions, zero (fullerene), one (carbon nanotube, CNT), two (graphene) and three (graphite) dimensions are very well-known for their versatility in various studies. They are also used in various applications in nanoelectronics, polymer composites, hydrogen production and storage, intercalation materials, drug delivery, sensing, catalysis, photovoltaics etc. Electrical conductivity of carbon can be tuned from insulator (diamond) to semiconductor (graphene) to conductor (graphite) with varying band gap. The main reason for this versatility and varied properties is that carbon can be involved in different hybridizations. Graphene, a single layer of graphite has fascinated the world during the last several years culminating in a Nobel prize for Physics in 2010. The present study is an attempt to understand the physicochemical and electrochemical properties of graphite oxide and its reduced form. Graphene oxide (GO) possesses oxygen containing functional groups such as carbonyl, carboxyl and epoxy groups distributed very randomly in the extended graphene sheet which makes it ionically conducting and electrically insulating. The AFM images of single layer of graphite (graphene) obtained from micromechanical cleavage method and that of EGO are shown in figure 1. EGO is a layered material similar to graphite and can form very stable aqueous colloids over a wide pH range of 2-11. The stability of the colloid is due to electrostatic repulsive interactions between the functional groups. EGO behaves like a molecule due to its thickness (~1 nm) and like a particle due to its two dimensional nature (lateral size can vary from nm to few microns). It behaves as amphiphilic molecule having both hydrophilic and hydrophobic nature. Figure 1d shows the STM image of EGO which clearly indicates oxidized and unoxidized regions which will impart hydrophilic and hydrophobic regions respectively. Figure 1: AFM image of (a) graphene (b) EGO. STM image of (c) HOPG and (d) EGO. The present work is related to exploring EGO as a multifunctional material. Both hydrophilic and amphiphilic nature is explored for various studies. Reduced GO (rGO) is synthesized from EGO by assembling at different interfaces (solid-liquid and liquid-air) followed by reduction. Since EGO is hydrophilic, it is brought to the air-water interface with the help of a surfactant (CTAB) through electrostatic interactions. It is reduced chemically by hydrazine vapour to rGO and electrochemically by assembling EGO on gold through electrostatic interactions between EGO and amine groups of cystamine (figure 2). The reduction process is followed by AFM, UV-Visible and in-situ Raman spectroelectrochemistry. Figure 2: Schematic of EGO self assembly, cyclic voltammogram showing electrochemical reduction and schematic for in-situ Raman spectroelectrochemistry. The next section deals with composites of EGO and polymers. EGO/polyaniline (PANI) composite is formed by electrochemical polymerization under applied surface pressure. The in-situ electrochemical polymerization of aniline in the sub-phase of Langmuir-Blodgett trough under applied surface pressure in presence of EGO at the air-water interface leads to preferential orientation of PANI in the polaronic form. This is followed by electrochemistry and Raman spectroscopy. Figure 3 shows differential pulse voltammograms of EGO/PANI obtained under two different conditions. Externally polymerized sample shows three redox peaks at 0.086/0.064 V (A/A‟), 0.390/0.430 V (B/B‟) and 0.520/0.560 mV (C/C‟) which correspond to leucoemaraldine/emaraldine, quinone/hydroquinone and emaraldine/pernigraniline redox states respectively. The peak at C/C‟ vanishes when aniline is polymerized in-trough under applied surface pressure. This implies that oxidation of emaraldine to pernigraniline becomes difficult when sample is prepared in-trough. The Raman spectroscopy clearly reveals the preferential orientation of PANI in planar polaronic structure. Figure 3. Differential pulse voltammograms for EGO/PANI complex obtained through external polymerization (black) and in-trough polymerization (red). In the next part, EGO is used as a proton conducting material for polymer electrolyte membrane fuel cell (PEMFC). EGO possesses hydrophilic and hydrophobic regions similar to nafion (sulfonated tetrafluoroethylene based fluoropolymer-copolymer) and hence it can act as a good ionically conducting membrane. EGO is incorporated in poly(vinyl alcohol) (PVA) matrix and used in the present studies. The ionic conductivity increases from 10 μS cm-1 to 370 μS cm-1 when EGO content is increased from 1wt% to 7wt% in PVA matrix. Power densities of 25 and 90 mW cm-2 are obtained for PVA and PVA/EGO membranes in H2-O2 fuel cell at 40 0C respectively. In the next section, EGO is used as receptor for simultaneous electrochemical detection of heavy metal ions such as Cd, Pb, Cu and Hg with detection limit of 5 μM, 1 pM, 5 μM and 5 μM respectively. During the process it is observed that the EGO/PbO composite can give rise to detection limit of 10 nM for arsenic. Along with detection, EGO can also be used as an effective adsorbent for inorganics (metal ions) as well as organics (dye molecules). EGO behaves as good adsorbent for heavy metal ions and cationic dyes and rGO adsorbs anionic dyes effectively. Spectroscopic techniques are used to understand the interactions between adsorbent and adsorbates. The thesis is presented as follows: Chapter 1 gives general introduction about graphene and graphite oxide with particular emphasis on the latter one. Chapter 2 gives details on the experimental methods followed, along with schematics for various adsorption processes. Chapter 3 focuses on assembling EGO at interfaces (solid-liquid and liquid-air) followed by reduction with chemical and electrochemical methods. Chapter 4 explores EGO as an amphiphilic material where EGO is assembled at air-water interface with anilinium and subsequent electropolymerization to EGO/PANI composites. EGO/PVA composite is used as electrolyte for PEMFC. Chapter 5 explores EGO as receptor for heavy metal ion detection (Cd, Pb, Cu and Hg). Chapter 6 deals with EGO as adsorbent for adsorption of inorganics (metal ions) as well as organics (dye molecules). This is followed by summary and conclusions. The appendix section gives details on the studies on preparation of exfoliated graphite with various metal ion intercalation. The covalent functionalization of EGO with metal phthalocyanines and its assembly at air-water interface forms second part of the appendix. (For figures pl see the abstract pdf file)

This thesis proposes a modified structure model for graphite oxide (GO), an important precursor in graphene chemistry, develops a new strategy to convert GO back to graphene-like structure, and demonstrates its possible applications in both water purification and supercapacitor technologies. GO, a nontraditional compound first obtained from graphite oxidation over 150 years ago, is now becoming an important player in the production of graphene-based materials, which has high technological relevance. GO structure and reduction have been vigorously investigated, but its precise chemical structure still remains obscure, and the complete restoration of the sp2 carbon lattice has not yet been achieved. In our work, solid state 13C NMR (MAS) analysis offered a piece of evidence for five or six-membered ring lactol structure existing in GO that had never been assigned before, leading to a modified Lerf-Klinowski model for GO. A three-step reduction strategy, involving sodium borohydride (NaBH4), sulfuric acid, and high temperature thermal annealing, described in the thesis, successfully reduced GO back to chemically converted graphene (CCG) with the lowest heteroatom abundance among all those previously reported. In addition to the chemical significance of graphene/CCG production, GO and its derivatives were used as novel adsorbents in water purification. GO-coated sand showed higher retention than ordinary sand for both Rhodamine B and mercuric ion (Hg2+) contaminants in water. Further functionalization of GO with thiophenol resulted in better adsorption capacity toward Hg2+ than that of activated carbon. In addition, free-standing films of GO were treated and reduced with a CO2 laser beam into different conductive reduced GO (RGO) patterns, and directly used as supercapacitor devices which showed good cyclic stability and energy storage capacities comparable to that of existing thin film ultracapacitors. GO turned out to be a solid electrolyte with anisotropic proton conductivity similar to Nafion, while the large amount of trapped water in GO played an important role.

This thesis describes the transport properties observed in thermally treated graphite oxide (GO), which holds promise as an economical route to obtaining graphene. Graphene is a material consisting of a single atomic plane of carbon atoms and was first isolated as recently as 2004. Several isolation techniques have been investigated, including mechanical exfoliation, chemical vapor deposition, and the reduction (by various methods) of chemically synthesized graphite oxide. Two fundamental questions are pursued in this work. The first is concerned with the maximum electrical conductivity that can be achieved in atomically thin reduced graphite oxide samples (rGO). As produced, GO is insulating and of little use electronically. By heating and exposure to reducing atmospheres, however, the conductivity can be increased. Through the lithographic definition and fabrication of four-point contact structures atop microscopic samples of GO, the resistance of the sample can be monitored in situ as the reduction process takes place. It was discovered that the resistance of few-layer GO could be decreased by an order of magnitude when heated to 200 °C and subsequently cooled back to room temperature in forming gas. Final resistivities were on the order of 0.5 Ω-cm. An ambipolar field effect was observed in the thermally treated samples, with resistance decreasing by up to 16 % under a substrate bias of ±20 V. Mobilites were inferred to be on the order of 0.1 cm²/V-s. It was also found that the presence of forming gas during reduction decreased the resistance of the GO samples by roughly one half. The second question that this work begins to answer is concerned with the distance that electrons can travel in such thermally-reduced GO before spin-randomizing scattering. The answer can be elucidated with the aid of magnetoresistance measurements using ferromagnetic contacts to inject a spin-polarized current through the sample. The observation of the magnetoresistive effect with the contacts separated by a certain distance can be taken as evidence of a spin coherence length in the material of at least that distance. Though this experiment has not yet been carried out, progress has been made toward its possibility; specifically in the fabrication and characterization of independently switchable magnetic contacts. By exploiting magnetic shape anisotropy, contact pairs have been fabricated and demonstrated to differ in magnetic coercivity by up to 8 Oe. / Graduation date: 2011

Graphite oxide (GO), a carbon material prepared in one step from low cost commercial materials, and graphene oxide have been found to catalyze a wide range of reactions including oxidations, hydrations, and dehydrations, as well as cationic or oxidative polymerizations. Applicable in both small molecule and polymer chemistry, this single, metal-free catalyst shows remarkable breadth, including the combination of the aforementioned reactions in an auto-tandem fashion to form advanced substrates, such as chalcones, from simple starting materials. Some of these reactions, such as the selective oxidation of alcohols to aldehydes, have been shown to be dependent on the presence of molecular oxygen, suggesting that this may be the terminal oxidant. Aside from its eminently valuable reactivity, the use of GO as a catalyst also presents practical advantages, such as its heterogeneous nature, which facilitates separation of the catalyst from the desired product. The use of this simple material in synthetic chemistry, as well as others like it, is distinct from other forms of catalysis in that the active species is carbon-based, heterogeneous and metal-free (as confirmed by ICP-MS and other spectroscopic techniques). This has led us to propose the term “carbocatalyst” to describe such materials. With dwindling supplies of precious metals used in many common organic reactions, the use of inexpensive and widely available carbocatalysts in their place will ensure that commercial processes of fundamental importance can continue unabated. Moreover, as we have shown with just one material, carbons are capable of facilitating a broad range of reactions. / text

Made available in DSpace on 2016-12-08T17:19:22Z (GMT). No. of bitstreams: 1 Renata Hack.pdf: 4507234 bytes, checksum: a9a47eaf8a6524ae5f448abca5062a08 (MD5) Previous issue date: 2014-02-07 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / O grafite natural é uma fonte de baixo custo e é abundante para obtenção de grafeno. O método que se mostrou mais eficiente para a produção de grafeno em larga escala é o método Hummers modificado, que consiste na oxidação do grafite. Com isso, o objetivo principal deste trabalho foi produzir grafeno a partir do grafite natural pelo método de Hummers modificado, além de produzir nanocompósitos de matriz epoxídica reforçada com o grafeno produzido (GP) e o grafeno comercial (GC). Para a produção dos nanocompósitos foi utilizado à resina epoxídica à base de éter diglicidílico do bisfenol A (DGEBA). Foram obtidos nanocompósitos em concentrações de 0,75; 1,00 e 2,00% m/m de GC e GP, com e sem a utilização de solvente THF no processo de preparação. Os resultados obtidos indicaram um alto grau de oxidação do grafite, comprovando assim que o processo foi eficiente. As análises de Raman e FTIR realizadas no GC e GP mostraram que o GP possui as mesmas características do GC. A adição do GC e GP com e sem adição de THF elevou a estabilidade térmica dos nanocompósitos. A alta concentração de nanoreforços e a não utilização de solvente THF em alguns sistemas pode ter contribuído para a formação de aglomerados nestes nanocompósitos, decorrendo assim em uma diminuição do módulo de Young. Através da análise de impedância foi possível verificar que apenas os nanocompósitos com 2%m/m de GP sem THF apresentou percolação dielétrica. Verifica-se que a produção do grafeno a partir do grafite natural possui potencial para aplicação em nanocompósitos estruturais.

The topic of this thesis is the study of nitrogen functionalities in nitrogen-doped reduced graphene oxide using Raman spectroscopy. Specifically, the project set out to investigate if the Raman active nitrogen-related vibrational modes of graphene can be identified via isotope labelling. Previous studies have used Raman spectroscopy to characterise nitrogen doped graphene, but none has employed the method of isotope labelling to do so. The study was conducted by producing undoped, nitrogen-doped and nitrogen-15-doped reduced graphene oxide and comparing the differences in the first-order Raman spectrum of the samples. Results of this study are inconclusive. However, some indications linking the I band to nitrogen functionalities are found. Also, a hypothetical Raman band denoted I* possibly related to \spt{3} hybridised carbon is introduced in the same spectral area as I. This indication of a separation of the I band into two bands, each dependent on one of these factors could bring clarity to this poorly understood spectral area. As the results of this study are highly speculative, further research is needed to confirm them and the work presented here serves as a preliminary investigation.

In this study, the composite of aluminum metal-organic framework MIL-68(Al) and reduced graphene oxide (MA/RG) was synthesized via a one-step solvothermal method, and their performances for pnitrophenol (PNP) adsorption from aqueous solution were systematically investigated. The introduction of reduced graphene oxide (RG) into MIL-68(Al) (MA) significantly changes the morphologies of the MA and increases the surface area. The MA/RG-15% prepared at RG-to-MA mass ratio of 15% shows a PNP uptake rate 64% and 123% higher than MIL-68(Al) and reduced graphene oxide (RG), respectively. The hydrogen bond and pi-pi dispersion were considered to be the major driving force for the spontaneous and endothermic adsorption process for PNP removal. The adsorption kinetics, which was controlled by film-diffusion and intra-particle diffusion, was greatly influenced by solution pH, ionic strength, temperature and initial PNP concentration. The adsorption kinetics and isotherms can be well delineated using pseudo-second-order and Langmuir equations, respectively. The presence of phenol or isomeric nitrophenols in the solution had minimal influence on PNP adsorption by reusable MA/RG composite.

Graphene is a novel two dimensional material that is revolutionizing many areas of science and it is no surprise that a significant amount of effort is dedicated to its investigation. One of the major areas of graphene research is the development of procedures for large scale production. Among many recently developed methodologies, graphene oxide reduction stands out as a straightforward and scalable procedure for producing final material with properties similar to those of graphene. Laser reduction of graphite oxide is one of the novel approaches for producing multilayer graphene, and this work describes a viable approach in detail. It is determined that a material which is comprised of a combination of laser reduced graphite oxide-coupled to an unreduced graphite oxide layers beneath it, produces a broadband photosensitive material. The efficiency of light conversion into electrical current is greatly dependent upon the oxygen content of the underlying graphite oxide. Developing novel ways for reducing graphite oxide is an ongoing effort. This work also presents a new method for achieving complete reduction of graphite oxide for producing predominantly sp2 hybridized material. This approach is based on the irradiation of graphite oxide with a high flux 3 keV Ar ion beam in vacuum. It is determined that the angle of irradiation greatly influences the final surface morphology of reduced graphite oxide. Also, multilayer epitaxial graphene growth on silicon carbide in ultra-high vacuum was investigated with quadrupole mass spectrometry (QMS). Subliming molecular and atomic species were monitored as a function of temperature and heating time. The grown films were characterized with X-ray photoelectron spectroscopy coupled with Ar ion depth profiling.

O grafeno, uma das formas alotrópicas do carbono, tem ganho grande valorização no meio científico e industrial devido às suas propriedades excepcionais. Por apresentar condutividade elétrica correspondente a do cobre e condutividade térmica, dureza e resistência superiores a todos os outros materiais existentes, faz-se necessário à busca por melhores, mais eficientes e produtivos métodos de obtenção do mesmo. Um dos métodos mais utilizados atualmente, conhecido como método de Hummers, consiste na oxidação da grafita por tratamentos ácidos e posterior redução (química ou térmica). No entanto, o rendimento do processo, geralmente, não gera quantidade de material suficiente para preparo de compósitos poliméricos utilizando equipamentos tradicionais de mistura, como extrusoras. Os compósitos poliméricos com grafeno apresentam aumento na estabilidade térmica e dimensional de peças injetadas, quando comparado à mesma peça sem carga, podendo ser usado como retardante de chama e também, por garantir maior condutividade elétrica ao polímero, pode ser usado em touch screens e células solares flexíveis. Frente a estas possibilidades, faz-se necessário aperfeiçoar o método de Hummers, tornando-o mais eficaz e produtivo. Alguns parâmetros da cinética química da reação do óxido de grafite (GO), os métodos de remoção dos ácidos residuais do processo, as técnicas de redução dos grupos oxigenados e o método de obtenção do material seco para posterior incorporação no polímero foram avaliados neste trabalho. Três métodos de oxidação da grafita foram estudados e os materiais obtidos foram comparados ao GO comercial, e dois métodos de redução (química com NaBH4 e térmica à várias temperaturas e taxas de aquecimento) do GO foram testados. Os GOs e os óxidos de grafeno reduzidos (GORs) foram caracterizados com o auxílio das técnicas de espectroscopia Raman, espectroscopia vibracional de absorção no infravermelho (FTIR), análise termogravimétrica (TGA), microscopia eletrônica de varredura (MEV), espectrometria de raios X por energia dispersiva (EDS) e difração de raios-X (DRX). Os resultados mostraram que a cinética da reação de GO não é linear, pois foram obtidos óxidos com características diferentes, utilizando-se a mesma proporção de reagentes pelos métodos A e C. A filtração ou a diálise, utilizadas para remover os resíduos ácidos do tratamento, e a estufa ou a liofilização, utilizadas para obter os materiais secos, não interferiram nas propriedades finais dos GOs e dos GORs. Por fim, a redução química e o choque térmico a 700 °C se mostraram os métodos mais adequados para obter grafeno quimicamente modificado com boas propriedades e maior rendimento. Os compósitos obtidos através de um misturador interno foram caracterizados com ensaios mecânicos (tração e impacto), microscopia eletrônica de varredura (MEV), microscopia eletrônica de transmissão (MET) e calorimetria exploratória diferencial (DSC). Os resultados obtidos indicaram a má dispersão das cargas no polímero, o que pode ser confirmado pela presença de aglomerados nas análises morfológicas e pelas propriedades mecânicas inferiores dos compósitos. / The graphene, one of the carbon allotropes, has received a great valorization in the scientific and industrial areas due its exceptional properties. Its electrical conductivity corresponds to copper ones and its thermal conductivity, hardness and strength are superior to known existent material properties. For this reason, it is necessary to search for a more efficient and productive method of obtaining. One of the most used methods nowadays is the Hummers method, it is based on graphite oxidation via acid treatment and also on chemical and thermal reduction. However, the yield of the process generally does not generate sufficient amount of material for preparing polymer composites using traditional mixing equipment such as extruders. Polymeric composites graphene have increased thermal and dimensional stability of molded parts compared to the same part without load, can be used as a flame retardant and also to ensure higher electrical conductivity to the polymer, can be used in touch screens and flexible solar cells. Faced to these possibilities, it is necessary to search for improvements to Hummers method, making it more effective and productive. Evaluating the chemical kinetic from the reaction of graphite oxide (GO), the removal manners from the residual acids from the process, the reduction technician from the oxygenated functional groups and the obtention method of the dry material to posterior incorporation in to the polymer, were evaluated in this work. Three oxidation methods have been performed and compared to GO commercial, and three reduction methods (chemical with NaBH4 and thermal to 550 °C and 1000 °C) have been tested. The GOs and the graphene oxide reduced (GORs) were characterized by Raman Spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric Analysis (TGA), Scanning Electron Microscopic (SEM) and Energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The results showed that the reaction kinetic from the GO is not linear, because it has been obtained oxides with different characteristics, using the same reagents proportion in two methods (A and C). The filtration or the dialysis, used to remove the acids residues from the treatment, and the drying oven or the freeze drying, used to obtain the dry material, didn\'t interfere in the final properties of the GOs and GORs. Finally, the chemical reduction and the thermal shock at 700 ° C proved the most suitable methods for chemically modified graphene with good properties and increased yield. The composites obtained through an internal mixer were characterized with mechanical tests (tensile and impact), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). Results indicated poor dispersion of the fillers in the polymer, which can be confirmed by the presence of agglomerates in the morphological analysis and the inferior mechanical properties of the composites.

Neste trabalho, foram obtidos compósitos poliméricos de Óxido de Grafite (GO) incorporado em Poli(metaclilato de metila) (PMMA). A obtenção do Óxido de Grafite foi realizada por dois diferentes métodos: método de Hummers modificado e método de Staudenmaier. Em seguida, foi ainda adicionada uma etapa secundária de tratamento térmico à 1000 ºC nos GOs obtidos a fim de expandir as lamelas de grafite e remover os grupos funcionais aderidos durante o ataque ácido do grafite. As cargas obtidas foram caracterizadas com o auxílio das técnicas de Difração de Raios-X (DRX), Espectroscopia Raman, Espectroscopia Vibracional no Infravermelho (FTIR), Análise Termogravimétrica (TGA), Microscopia Eletrônica de Varredura (MEV), Microscopia Eletrônica de Transmissão (MET) e Microscopia de Força Atômica (AFM), constatando a formação do Óxido de Grafite por ambos os métodos, e ainda a expansão das folhas após o tratamento térmico. O estudo comparativo dos compósitos de matriz polimérica com 1, 3 e 5 % de concentração de GO antes do tratamento térmico e 1 e 3 % após o tratamento térmico foi realizado com o objetivo de entender a contribuição nas propriedades reológicas do polímero com a adição da carga de GO. Os compósitos poliméricos foram obtidos através de um misturador interno, variando-se o método de adição da carga na matriz polimérica via solvente ou via moinho - para estudar a melhor dispersão da carga na matriz. Os compósitos PMMA/GO foram caracterizados por Cromatografia de Permeação em Gel (GPC), Análise Termogravimétrica (TGA), Calorimetria Exploratória Diferencial (DSC), Microscopia Eletrônica de Varredura (MEV), Microscopia Eletrônica de Transmissão (MET); e por ensaios reológicos de Varredura de Deformação, Varredura de Tempo, e Cisalhamento Oscilatório de Pequenas Amplitudes (COPA). Os resultados reológicos apresentaram um aumento da viscosidade complexa tanto na Varredura de Tempo, quanto no COPA. De acordo com a metodologia adotada, ainda não foi possível verificar o aumento crescente da viscosidade complexa a baixas frequências. Este aumento de viscosidade indicaria que o Óxido de Grafite formou uma rede tridimensional, cuja percolação impede que as cadeias poliméricas relaxem completamente. / In this study, composites of graphite oxide (GO) in poly(methyl methacrylate) (PMMA) were obtained. Obtaining of graphite oxide was performed by two potential methods by literature: modified Hummers method and Staudenmaier method; Then, a secondary GOs obtained heat treatment step - at 1000° C - was added in order to expand the graphite flakes and remove functional groups attached during the acid attack of graphite. The reinforcement obtained by both methods were characterized by X-Ray Diffraction (XRD), Raman Spectroscopy, Infra Red Spectroscopy (FTIR), Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Atomic Force Microscopy (AFM), confirming the formation of Graphite Oxide by both methods, and also the expansion of the leaves after the heat treatment. Then, a comparative study of the polymer matrix composites with 1, 3 and 5 % concentration of oxides graphite before the heat treatment and 1 and 3 % after the heat treatment was performed in order to understand the contribution to the rheological properties of the polymer with the addition of GO reinforcement. The composites were obtained by internal mixer, varying the load adding method in the polymeric matrix - via mill and via solvent - to study the best dispersion of GO in the matrix. The samples were characterized by Gel Permeation Ghromatography (GPC), Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM); and rheological measurements of Deformation Scan, Time Sweep, and Small Amplitude Oscillatory Shear (SAOS). The rheological results showed an increase in complex viscosity at both Time Sweep, as in SAOS. However, it was not possible to verify the increase of complex viscosity at low frequencies, that would indicate that graphite oxide form a three-dimensional arrangement, which prevents the percolation of the polymer chains, letting them to relax completely.