Magister Scientiae - MSc / It is well known that a lead pencil is made of graphite, a naturally form of carbon, this is important but not very exciting. The exciting part is that graphite contains stacked layers of graphene and each and every layer is one atom thick. Scientists believed that these graphene layers could not be isolated from graphite because they were thought to be thermodynamically unstable on their own and taking them out from the parent graphite crystal will lead them to collapse and not forming a layer. The question arose, how thin one could make graphite. Two scientists from University of Manchester answered this question by peeling layers from a graphite crystal by using sticky tape and then rubbing them onto a silicon dioxide surface. They managed to isolate just one atom thick layer from graphite for the first time using a method called micromechanical cleavage or scotch tape. In this thesis chemical method also known as Hummers method has been used to fabricate graphene oxide (GO) and reduced graphene oxide. GO was synthesized through the oxidation of graphite to graphene oxide in the presence of concentrated sulphuric acid, hydrochloric acid and potassium permanganate. A strong reducing agent known as hydrazine hydrate has also been used to reduce GO to rGO by removing oxygen functional groups, but unfortunately not all oxygen functional groups have been removed, that is why the final product is named rGO. GO and rGO solutions were then deposited on silicon substrates separately. Several characterization techniques in this work have been used to investigate the optical properties, the morphology, crystallography and vibrational properties of GO and rGO.

El grafeno es, por definición, una de las capas bidimensionales (2D) de espesor monoatómico que forman el grafito, cuando está aislada. Sus prometedoras propiedades (anómalo efecto Hall cuántico, alta movilidad portadora, alta concentración de portadores de carga, elevada resistencia mecánica) lo convierten en un foco de incesante estudio. Además del grafeno, existen diferentes materiales basados en grafeno, de los cuales el óxido de grafito o grafeno (G-O) es el que se obtiene con un método de síntesis que hasta el momento es el más viable industrialmente hablando [1, 2]. El G-O se obtiene por oxidación de un material grafítico y consiste en una capa de grafeno que contiene grupos funcionales oxigenados en el plano basal y en los bordes de plano. Los grupos funcionales y los defectos producidos hacen que el G-O pierda algunas de las propiedades características del grafeno, como su estructura electrónica conjugada, si bien algunas pueden recuperarse parcialmente mediante tratamientos de reducción, obteniéndose óxido de grafeno reducido, rG-O. Establecer un protocolo de síntesis adecuado requiere conocer en profundidad la estructura del óxido de grafeno, durante años estudiada, pero sobre la que aun existen dudas. En este trabajo se ha pretendido realizar un estudio exhaustivo de la estructura del óxido de grafeno, partiendo de la base de que dependerá de distintos factores relacionados con su síntesis, como el precursor o el método de oxidación. Este estudio ha consistido en probar cuatro métodos de obtención, que suponen el uso de distintos intercalantes, oxidantes y condiciones de reacción: método de Hummers-Offeman original (H2SO4/KMnO4/NaNO3) [3], de Hummers-Offeman modificado (H2SO4/KMnO4), de Brodie (HNO3/NaClO3) [4] y de Staudenmaier (HNO3/H2SO4/NaClO3) [5]. Las materias primas utilizadas para obtener G-O son nanofibras de carbono, tipo helical-ribbon [6], y grafito natural. También se ha estudiado la estructura real del óxido de grafeno en base a un modelo existente según el cual el G-O obtenido de la reacción es una estructura compleja formada por dos entes: las láminas de G-O y moléculas menores adheridas a ellas, debris [7]. Por último, se ha realizado la reducción de G-O mediante tratamientos basados en choques térmicos (a distintas temperaturas [8], en microondas [9] , y en presencia de disolventes [10]) o reactivos químicos (borohidruro de sodio [11], hidracina [12] y ácido hidriódico [13]). Mediante la producción por el método de Hummers-Offeman modificado se ha observado que partiendo de nanofibras de carbono se obtiene un mayor rendimiento de cristales de G-O monocapa que partiendo de grafito. Se da una mayor dificultad de incorporación de grupos oxigenados en el plano basal de las capas de grafito, es decir, es más efectiva la penetración de los reactivos en las nanofibras de carbono. Por otro lado, se ha demostrado la existencia de láminas de G-O y debris como estructura compleja, y que la formación de debris es mayor en el G-O procedente de nanofibras de carbono que en el procedente de grafito. En cuanto a los métodos de producción, el método de Hummers-Offeman, modificado u original, ha resultado ser el más efectivo en la formación de cristales de G-O de pocas capas. Se ha observado que el uso de NaNO3 en dicho método facilita la separación de capas y evita el posterior reapilamiento tras una exfoliación térmica, especialmente cuando se parte de grafito. Asimismo, este reactivo favorece la rotura de capas grafíticas y la penetración del KMnO4, dando lugar a una mayor formación de debris. Por último, se ha comprobado que los debris enmascaran la interpretación de los resultados de la reducción de G-O, pues durante los tratamientos térmicos o químicos, además de disminuir el contenido de oxígeno, se produce una eliminación de debris.

Det första musikinstrumentet som hittats är 35 000 år gammalt. Forskningen har visat att musikens funktion på den tid då skriftspråket fortfarande inte fanns, bör ha haft andra funktioner än vad musiken har idag. Samtidigt finns många likheter. Dessa kunskaper berikar vår förståelse för vår samtid. Dock visar denna studie att hälften av de musiklärare på högstadiet som deltagit, svarat att de inte nämner forntidens musik eller musikinstrument alls, eller bara i förbifarten. Orsaken till det skulle vara tidsbrist och egen brist på kunskap i ämnet. Läroplanen hjälper inte läraren att prioritera musikens ursprung och utveckling. / The first musical instrument found is 35 000 years old. Research has shown that music function at the time when the written language still not existed, should have had other functions than the music of today. While there are many similarities. This knowledge enriches our understanding of our times. However, this study shows that half of the music teachers in high school who participated, responded that they don´t mention the ancient music or musical instruments at all, or only in passing. The reason for this would be lack of time and their own lack of knowledge on the subject. The curriculum doesn´t help the teacher to give priority to the music's origin and evolution.

It is unclear whether all intercalation techniques truly lead to the insertion of atoms between the graphite layers, or also lead to other effects which contribute to expansion. The objective of this project is to better understand the effects caused by different intercalation methods. Three intercalation methods were explored to determine the method which incurs the least damage to the surface and microstructure of the graphite intercalated compounds, yet achieves the best intercalation and therefore expansion. All the main findings are summarised below:  The gas phase sample had virtually no mass loss at the point where expansion took place. Therefore the intercalation was very efficient, producing large expansion without significant mass loss.  The mass loss that only occurs at the sublimation of iron chloride (320 ºC) indicates the excessive "un-intercalated" or residual iron chloride.  After oxidation, before purification, the gas phase sample has 25 % residual mass; this also proves the presence of impurities and residual iron chloride in the exfoliated sample. For the Hummers and electrochemical samples, expansion and mass loss occur over a wide temperature range, this indicates that graphite oxide was formed rather than the theoretically expected "insertion of atoms between the sheets".  The mass losses before 200 ˚C of the samples of the Hummers and electrochemical methods are more evidence that graphite oxide and graphite surface complexes with oxygen were produced.  The Hummers and electrochemical intercalation methods show similar expansion and mass loss curves, therefore it can be concluded that the reaction mechanism for both these methods is alike.  The gas phase method yields the best expansion of 250 % using the TMA, whereas both the other methods deliver approximately 220 %.  Using microwave expansion the electrochemical intercalation method yields the best bulk volume expansion of 1500 %, with the gas phase sample delivering a volume expansion of 1450 %. The Hummers samples are extremely damaged. This is clear from the several and deep oxidation pits visible throughout the basal plane of these samples. The basal plane and the edges are even eroded before purification and oxidation. This intercalation technique employs oxidisers in the preparation method which additionally oxidises the samples. This explains why the Hummers method renders the most damage. The residual material on the gas phase sample acts as catalysts making the sample very reactive and consequently damaging the surface during oxidation. The partially oxidised purified gas phase sample visibly shows the pits and roughened edges. There are two “types” of intercalation. The first intercalation “type” is the actual insertion of atoms or molecules between the graphite layers, whereas the other “type” of intercalation is the production of graphite oxide. The compound comprises carbon, oxygen and hydrogen, obtained by treating graphite with strong oxidisers. The functional groups usually found in graphite oxide are carbonyl (C=O), hydroxyl (-OH), phenol amongst others and also some impurities of sulphur when sulphuric acid is used. Both these intercalation types lead to expansion. It is recommended that a more efficient method for removal of residual material in the gas phase samples be explored. It is also recommended that more research be done to determine the reaction mechanisms during the three different intercalation methods. The graphite surface complexes of the intercalated compounds and the evolved gases during expansion should be analysed. / Dissertation (MEng)--University of Pretoria, 2015. / tm2015 / Chemical Engineering / MEng / Unrestricted

Radionuclide liquid wastes generated from nuclear facilities can affect humans and the environment, thus substantial attention for their safe management has been received worldwide. Treatment of radionuclide liquid wastes is an important step in its management. In the present work, new composite nanomaterials, graphene oxide base nanomaterial (GO) are developed for treatment purpose. Graphene oxide (GO), one of the most graphene derivatives, its unique properties, such as chemical stability, hydrophilicity, large surface area and functional groups, make them able to form strong chemical bonds with radionuclides. GO was successfully synthesized via Hummers method, characterized by Raman spectroscopy, X-Ray Diffraction (XRD), UV/Vis Spectroscopy, Fourier transform infrared spectroscopy (FTIR) and Scanning electron microscopy (SEM) and applied as an adsorbent in removal of the metallic long-lived radionuclide 68Ge from of aqueous solution The method used for evaluation of nanomaterials retention properties was sorption experiment, being based on contact of solid material with tracer solution under defined boundary conditions (solid/solution ratio, solution composition etc.). Two sorption experimental methods were used in this study. Firstly, an aqueous solution of 68Ge radionuclide solution mixed with GO solution, the solution was filtered using syringe filter membrane unit and the aliquot was quantified by gamma spectrometry. Secondly, the 68Ge radionuclide was mixed with GO solid powder, suspension rotated in a mechanical shaker, centrifuged, an aliquot of 1.0 ml sample taken for gamma spectroscopy and the supernatant was put in an oven to dry overnight for characterization analysis. The results obtained from experiments were the evaluated, using sorption percentage equation and showed that the GO had much low sorption capacity for the pre-concentration of radionuclides from aqueous solutions. The function of the pH, the ionic strength and the reduction of GO will be investigated for future studies for the improvement of the research results. / Physics / M. Sc. (Physics)