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Estudo e desenvolvimento de grafite como agente anti-chama para PVC / Study and development of graphite as fire retardant agent for PVC.Macedo, Nadia Guerra 02 August 2011 (has links)
O PVC é um dos principais polímeros termoplásticos da atualidade graças à sua grande versatilidade. Entretanto, uma de suas características é a baixa estabilidade térmica, sendo necessário o emprego de aditivos em sua estrutura. Uma das maiores preocupações mundiais é a segurança, sendo que muitos produtos levam proteção anti-chama em sua composição. Entre os vários agentes retardadores de chama a grafite aparece como um material promissor e pouco estudado. No presente trabalho foi estudada uma série de grafites com propriedades anti-chama oriundas de óxido de grafite \"flake\". O óxido de grafite foi submetido a vários tratamentos térmicos em atmosfera para a obtenção de grafites expandidas. O comportamento anti-chama dessas grafites foi testado adicionando-se 20% em peso no PVC. Membranas desses compósitos foram preparadas utilizando-se um \"doctor blade\". Os compósitos de grafites produzidas foram caracterizados por microscopia de varredura eletrônica e análise térmica. Isotermas de adsorção/dessorção de N2 também foram coletadas para determinação de área superficial específica e distribuição de poros. A grafite com melhores propriedades anti-chama foi aquela obtida em temperatura mais elevada, 900oC, ou seja, a grafite com mais elevada área superficial específica e com maior capacidade de produção de fuligem. / PVC is one of the most important thermoplastic polymers because of its versatility. However, like other polymers, for many technological uses, there is a need to enhance its thermal stability. Security is a global concern, so, the use of some fire retardants is required in polymer composites. Expanded graphite appears as a cleaner type of fire retardants, not well known yet. In the present work, expanded graphite obtained from the graphite oxide was studied. It were prepared PVC composite-membranes with 20 weight % of expanded graphite employing Doctor Blade. The samples were characterized by scanning electron microscope, thermogravimetric analysis and N2 adsorption/desorption isotherms were also collected for the determination of specific surface area and porous distribuition. The results show that the best fire retardant behaviour was achieved by the expanded graphite at 900oC, the graphite with the higher specific surface area and with the largest capacity of soot production.
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Thermal stability and mechanical property of polymer layered graphite oxide compositesCerezo, Frances Therese, francestherese_cerezo@hotmail.com January 2006 (has links)
Polymer composites formed from layered fillers with high surface volume ratio show enhanced reinforcement. Graphite oxide is a high modulus material that can be separated into thin layers with high surface area. The aim of this study is to prepare polymer layered graphite oxide composites using functionalised polyolefin to enhance compatibility with various forms of layered graphite oxide in varying concentration. Functionalised polyolefins reinforced with layered graphite oxides and expanded graphite oxides were prepared using solution blending and melt blending methods. Three different mixing methods with varying shear intensity were employed to prepare polymer layered graphite oxide composites. The crystalline structure, thermal and mechanical properties of the prepared polymer layered graphite oxide composites was studied. Oxidised graphite prepared from the Staudenmaier method and its exfoliated form were dispersed in poly(ethylene-co-methyl acrylate-co-acrylic acid) (EMAA) via solution blending to prepare EMAA layered composites. The thermal stability was determined using thermogravimetric analysis. The EMAA layered composites showed higher thermal stability in comparison with pure EMAA. The mechanical properties of these EMAA layered composites were determined through dynamic mechanical analysis. Shear modulus, yield stress and storage modulus of EMAA in the presence of graphite oxide fillers decreased. A solution blending method was used to prepare poly(propylene-grafted-maleic anhydride) layered expanded graphite oxide composites (PPMA-EGO). Two types of PPMA-EGO were prepared using different mixing methods - low and high shear were employed. The effects of preparative mixing methods on the PPMA-EGO properties were investigated. The mechanical properties of PPMA-EGO obtained from dynamic mechanical analysis indicated that EGO had a reinforcing effect on the elastic behaviour of PPMA-EGO. This is due to strong interfacial adhesion between PPMA and EGO as a result of hydrogen bonding. The elastic behaviour of PPMA-EGO was affected by the surface area of graphite flakes. Low sheared PPMA-EGO elastic behaviour was found to be higher compared with that of high sheared PPMA-EGO. A melt blending method was used to prepare PPMA-EGO with varying EGO concentration. The interconnected network structure of EGO in the PPMA-EGO was not observed as shown by its scanning electron microscopy images. Thermogravimetric analysis of PPMA-EGO indicates increased decomposition temperature of the PPMA matrix. Dynamic mechanical analysis showed enhanced storage modulus of PPMA-EGO. The maximum elastic modulus of PPMA-EGO was observed at 3 %wt of EGO. The electrical conductivity of PPMA-EGO was measured only for EGO concentrations above 2 %wt. The EGO concentration was found to be the most critical factor in the enhancement of the electrical conductivity of PPMA-EGO. Wide angle X-ray diffraction analysis of all polymer layered graphite oxide composites revealed no change in interlayer spacing of graphite layers, indicating the absence of EMAA intercalation in the graphite layers. The crystallisation temperature and crystallinity of all polymer layered graphite oxide composites were determined using differential scanning calorimetry. The results indicated that graphite oxide and expanded graphite oxides acted as nucleating agents in inducing the crystallisation of functionalised polyolefin in the layered composites. However, the degree of crystallinity of functionalised polyolefin decreased in the layered composites.
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Obtenção e caracterização de compósitos poliméricos com óxido de grafeno reduzido. / Obtention and characterization of polymer/reduced graphene oxide composites.Maria Anita de Paula Negreti 19 September 2016 (has links)
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.
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Comportamento reológico de compósitos reforçados com óxido de grafite em matriz de poli(metacrilato de metila). / Rheological behavior of graphite oxide reinforcement in poly(methyl methacrylate) matrix composites.Fernanda Cabrera Flores Valim 30 March 2015 (has links)
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.
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Estudo e desenvolvimento de grafite como agente anti-chama para PVC / Study and development of graphite as fire retardant agent for PVC.Nadia Guerra Macedo 02 August 2011 (has links)
O PVC é um dos principais polímeros termoplásticos da atualidade graças à sua grande versatilidade. Entretanto, uma de suas características é a baixa estabilidade térmica, sendo necessário o emprego de aditivos em sua estrutura. Uma das maiores preocupações mundiais é a segurança, sendo que muitos produtos levam proteção anti-chama em sua composição. Entre os vários agentes retardadores de chama a grafite aparece como um material promissor e pouco estudado. No presente trabalho foi estudada uma série de grafites com propriedades anti-chama oriundas de óxido de grafite \"flake\". O óxido de grafite foi submetido a vários tratamentos térmicos em atmosfera para a obtenção de grafites expandidas. O comportamento anti-chama dessas grafites foi testado adicionando-se 20% em peso no PVC. Membranas desses compósitos foram preparadas utilizando-se um \"doctor blade\". Os compósitos de grafites produzidas foram caracterizados por microscopia de varredura eletrônica e análise térmica. Isotermas de adsorção/dessorção de N2 também foram coletadas para determinação de área superficial específica e distribuição de poros. A grafite com melhores propriedades anti-chama foi aquela obtida em temperatura mais elevada, 900oC, ou seja, a grafite com mais elevada área superficial específica e com maior capacidade de produção de fuligem. / PVC is one of the most important thermoplastic polymers because of its versatility. However, like other polymers, for many technological uses, there is a need to enhance its thermal stability. Security is a global concern, so, the use of some fire retardants is required in polymer composites. Expanded graphite appears as a cleaner type of fire retardants, not well known yet. In the present work, expanded graphite obtained from the graphite oxide was studied. It were prepared PVC composite-membranes with 20 weight % of expanded graphite employing Doctor Blade. The samples were characterized by scanning electron microscope, thermogravimetric analysis and N2 adsorption/desorption isotherms were also collected for the determination of specific surface area and porous distribuition. The results show that the best fire retardant behaviour was achieved by the expanded graphite at 900oC, the graphite with the higher specific surface area and with the largest capacity of soot production.
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Characterisation of expandable graphite and its flame retardant abilities in flame retardant systems for polyethyleneKruger, Hermanus Joachim January 2017 (has links)
In the pursuit of lower cost intumescent flame retardant (IFR) systems, the compound expandable graphite (EG) was identified. This compound delivers high flame retardant performance but provides non-uniform thermal shielding when exposed to open flame from below due to negative gravitational effects. It was theorised that this may be remedied either through ion exchange of the interstratified ions with low glass transition ions or through use in binary systems with other compounds. Two classes of commercial EG were identified, namely a low and a high expansion onset temperature EG compound. Extensive characterisation of each EG compound was undertaken to assess its composition, expansion mechanisms and onset temperatures in order to identify compatible compounds for binary use. The susceptibility of each compound to ion exchange was also assessed. An industrial IFR ethylenediamine phosphate (EDAP) and a novel flame retardant were synthesised for assessment in binary use with EG. Coupled with the above study, this project developed two novel fire testing techniques as low cost alternatives to well-established fire testing methods such as cone calorimetry.
The first technique involved an open flame fire testing method which allowed vertical or horizontal testing. Digital and infrared (IR) video recording during operation facilitated comparison of multiple performance indicators further strengthening this method. The second technique allowed assessment of the mass loss resistance of each compound during laser pyrolysis. Characterisation of the EG compounds allowed development of structural models to describe each compound and explain the mechanisms of their expansion and gaseous release. Exhaustive ion exchange testing did not deliver favourable results, necessitating the pursuit of compounds for binary use with EG. A novel IFR was synthesised by neutralising 3,5-diaminobenzoic acid hydrochloride salt with ammonium dihydrogen phosphate. This compound, which melts at 257 °C, decomposes concurrently to release carbon dioxide gas which promotes intumescent charring. The flame retardant performance of this compound and EDAP as primary flame retardants and in combination with expandable graphite was evaluated. As a proof of concept, the novel compound was tested as a primary flame retardant using cone calorimetry after which its utility in binary systems with low temperature expandable graphite was tested. Substantial decreases in peak heat release rate (pHRR) and flame out time were achieved for all binary systems. This success led to testing of a number of combinations of low and high expansion onset EG and the other IFRs to identify the highest performing combination, which proved to be the 10-10 EDAP-EG system. Combinations of EG and the novel compound also showed excellent results. The novel fire testing techniques proved effective in identifying high performance combinations and showed comparable trends to those measured in cone calorimetry, at a greatly reduced cost and material requirement. IR analysis of open flame fire testing indicated increases in the temperatures required for ignition and burn through of the substrate. Observations, corroborated by optical video, showed that cohesive and uniform thermal shielding was achieved in all binary systems tested.
This study illustrates that systems of 10% EG combined with either 10% DABAP or 10% EDAP are both the most economical binary systems tested but are extremely high performance systems as well. Both of these systems delivered excellent results while being more economic than the widely used industrial system with a 25-30% EDAP loading. It is recommended that these compounds be considered for industrial use. Furthermore, the effective fire testing techniques developed in this study may be utilised in future fire testing to identify high performance compounds at a lower cost prior to further assessment through methods such as cone calorimetry. / Thesis (PhD)--University of Pretoria, 2017. / Chemical Engineering / PhD / Unrestricted
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Quantification of Graphene Oxide Structure Using an Improved ModelPradhan, Siddharth 23 October 2012 (has links)
No description available.
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Anglinių nanostruktūrų sintezė ir dangų gamyba / Synthesis and Coatings Production of Carbonaceous NanostructuresStankevičienė, Inga 17 October 2012 (has links)
Unikaliomis savybėmis pasižyminčios anglinės nanostruktūros panaudojamos dangų ir plėvelių gamyboje, kurios pritaikomos nanoelektronikoje, biotechnologijoje ir kitose srityse. Šio darbo tikslas buvo susintetinti daugiasienius anglinius nanovamzdelius ir grafito oksidą, pagaminti ir ištirti jų dangas. Mūsų laboratorijoje daugiasieniai angliniai nanovamzdeliai buvo susintetinti cheminio nusodinimo iš garų fazės metodu. Susintetinto produkto valymui nuo katalizatoriaus priemaišų pirmą kartą buvo panaudoti CCl4 garai. Ištyrus CCl4 garais paveiktą medžiagą buvo pagrįstas šio valymo metodo efektyvumas. Grafito oksidas buvo gautas oksiduojant grafitą Hummers'o metodu. Anglinių nanovamzdelių dangos ant skirtingų pagrindų buvo pagamintos cheminio nusodinimo iš garų fazės metodu bei suformuotos panaudojant medžiagos vandenines suspensijas. Grafito oksido su Kongo raudonojo dažo priedu dangos ir plėvelės buvo pagamintos laboratorijoje sukurtu filtravimo į tirpalą metodu. Anglinių nanovamzdelių ir jų dangų tyrimo rezultatai parodė, kad dangų morfologija priklauso nuo sintezės sąlygų, o paviršiaus savybes nulemia prisijungusių funkcinių grupių pobūdis ir kiekis. Ištyrus grafito oksido plėveles ir dangas buvo nustatyta, kad Kongo raudonojo dažo priedas skatina kompaktiškesnių nanokompozitų susidarymą ir stiprina dangų bei plėvelių patvarumą. / Films and coatings of carbonaceous nanostructures are employed in nanoelectronics, biotechnology and other fields. The aim of the research was to synthesize multi-walled carbon nanotubes and graphite oxide and fabricate coatings thereof. Consequently, multi-walled carbon nanotubes and their coatings were synthesized by the catalytic chemical vapour deposition method. As-grown carbon nanotubes inevitably contain remains of metal catalyst particles. A method developed in the laboratory using CCl4 was successfully applied to remove the residual catalyst from the batch of synthesized carbon nanotubes. Simultaneously, graphite oxide was synthesized from graphite powder by Hummer's method. Coatings and films of carbonaceous nanostructures were fabricated from carbon nanotubes and graphite oxide aqueous suspensions. The analysis of carbon nanotubes coatings revealed that their morphology depends on synthesis parameters. The surface properties of these coatings depend on the amount and nature of functional groups attached to carbon nanotube walls. The analysis of graphite oxide films indicated that Congo red dye addition leads to more compact structure of the nanocomposites due the interaction between functional groups of these particles.
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Synthesis and coatings production of carbonaceous nanostructures / Anglinių nanostruktūrų sintezė ir dangų gamybaStankevičienė, Inga 17 October 2012 (has links)
Films and coatings of carbonaceous nanostructures are employed in nanoelectronics, biotechnology and other fields. The aim of the research was to synthesize multi-walled carbon nanotubes and graphite oxide and fabricate coatings thereof. Consequently, multi-walled carbon nanotubes and their coatings were synthesized by the catalytic chemical vapour deposition method. As-grown carbon nanotubes inevitably contain remains of metal catalyst particles. A method developed in the laboratory using CCl4 was successfully applied to remove the residual catalyst from the batch of synthesized carbon nanotubes. Simultaneously, graphite oxide was synthesized from graphite powder by Hummer's method. Coatings and films of carbonaceous nanostructures were fabricated from carbon nanotubes and graphite oxide aqueous suspensions. The analysis of carbon nanotubes coatings revealed that their morphology depends on synthesis parameters. The surface properties of these coatings depend on the amount and nature of functional groups attached to carbon nanotube walls. The analysis of graphite oxide films indicated that Congo red dye addition leads to more compact structure of the nanocomposites due the interaction between functional groups of these particles. / Unikaliomis savybėmis pasižyminčios anglinės nanostruktūros panaudojamos dangų ir plėvelių gamyboje, kurios pritaikomos nanoelektronikoje, biotechnologijoje ir kitose srityse. Šio darbo tikslas buvo susintetinti daugiasienius anglinius nanovamzdelius ir grafito oksidą, pagaminti ir ištirti jų dangas. Mūsų laboratorijoje daugiasieniai angliniai nanovamzdeliai buvo susintetinti cheminio nusodinimo iš garų fazės metodu. Susintetinto produkto valymui nuo katalizatoriaus priemaišų pirmą kartą buvo panaudoti CCl4 garai. Ištyrus CCl4 garais paveiktą medžiagą buvo pagrįstas šio valymo metodo efektyvumas. Grafito oksidas buvo gautas oksiduojant grafitą Hummers'o metodu. Anglinių nanovamzdelių dangos ant skirtingų pagrindų buvo pagamintos cheminio nusodinimo iš garų fazės metodu bei suformuotos panaudojant medžiagos vandenines suspensijas. Grafito oksido su Kongo raudonojo dažo priedu dangos ir plėvelės buvo pagamintos laboratorijoje sukurtu filtravimo į tirpalą metodu. Anglinių nanovamzdelių ir jų dangų tyrimo rezultatai parodė, kad dangų morfologija priklauso nuo sintezės sąlygų, o paviršiaus savybes nulemia prisijungusių funkcinių grupių pobūdis ir kiekis. Ištyrus grafito oksido plėveles ir dangas buvo nustatyta, kad Kongo raudonojo dažo priedas skatina kompaktiškesnių nanokompozitų susidarymą ir stiprina dangų bei plėvelių patvarumą.
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Synthèse et caractérisation de nanocomposites conducteurs à base de « graphène » et de polysaccharides / Synthesis and characterization of conducting nanocomposites based « graphene » and polysaccharidesDhahri, Abdelwaheb 20 April 2017 (has links)
L'objectif principal de cette thèse a été d'expérimenter de nouvelles voies d'exfoliation des feuillets de graphène dans des matrices polysaccharides telles que la cellulose et le chitosane dopé avec des nanoparticules d'or (Au). Notre stratégie a été d'explorer de nouvelles voies de greffage de molécules et de macromolécules sur des feuillets d'oxyde de graphène (GO). Dans un premier temps, nous avons donc oxydé un graphite commercial par la méthode de Hummers qui est apriori la méthode la plus simple à mettre en oeuvre pour produire une suspension stable de feuillets d'oxyde de graphène totalement exfoliés dans l'eau. L'intérêt de cette oxydation est l'obtention de fonctions acide carboxylique et époxyde susceptibles d'être fonctionnalisées en deux étapes par l'éthylénediamine puis par un polysaccharide tel que la cellulose. En effet, afin d'améliorer la compatibilité du graphite oxydé avec des matrices organiques telle que la cellulose, l'idée est de lui greffer des chaînes polysaccharides. Ces résultats ont permis de mettre en évidence l'exfoliation partielle des feuillets de graphène après fonctionnalisation et l'obtention d'un taux de greffage massique d'environ 35% pour la cellulose. La conductivité électrique des nano-composites correspondants a aussi été étudiée par des mesures diélectriques à des températures variées. L'augmentation de la conductivité électrique après la fonctionnalisation du graphite oxydé a mis en évidence une solvo-thermoréduction simultanément à la fonctionnalisation. Enfin, le dopage de ce matériau par des particules d'or a permis d'obtenir une conductivité électrique de 1.60 10-4 S m-1. En ce qui concerne le matériau composite à base de chitosane, la démarche scientifique a été la même que pour l'analogue cellulose, le taux de greffage massique a été d'environ 68% et nous avons en plus testé son activité catalytique vis-à-vis de la conversion du 4-Nitrophénol en 4-Aminophénol et les résultats obtenus ont été très satisfaisants / The main objective of this thesis has been to experiment a new ways of exfoliation of graphene sheets in polysaccharide matrices such as cellulose and chitosan doped with gold nanoparticles (Au). Our strategy was to explore new routes for the grafting of molecules and macromolecules onto graphene oxide (GO). First, we have oxidized commercial graphite by the method of Hummers which is a priori the simplest method to implement to produce a stable suspension of graphene oxide sheets totally exfoliated in water. The advantage of this oxidation is the formation of carboxylic acid and epoxy functional groups onto the graphite surface that can be functionalized in two stages by ethylenediamine and then by a polysaccharide such as cellulose. Indeed, in order to improve the compatibility of graphite oxide with organic matrix such as cellulose, the idea is to graft it onto polysaccharide chains. These results made it possible to demonstrate the partial exfoliation of the graphene sheets after functionalization and to obtain a percentage of grafting of about 35wt% for cellulose. The electrical conductivity of the corresponding nanocomposites has also been studied by dielectric measurements at various temperatures. The increase of the electrical conductivity after the functionalization of graphite oxide showed a solvo-thermo reduction simultaneously with the functionalization. Finally, the doping of this material by gold particles made it possible to obtain an electrical conductivity of 1.60 10-4 S m-1. Concerning chitosan-based composite materials, the scientific approach was the same as cellulose substrate and we obtained a percentage of grafting of 68wt%. In addition, its catalytic activity for the conversion of 4-Nitrophenol to 4-Aminophenol was of high efficiency
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