Chemische Zusammensetzung und Mikrostruktur polymerabgeleiteter Gläser und Keramiken im System Si–C–O. Teil 2: Charakterisierung der Gefügeausbildung mittels hochauflösender Durchstrahlungselektronenmikroskopie und Feinbereichsbeugung

Chemical Composition and Microstructure of Polymer‐Derived Glasses and Ceramics in the Si–C–O System. Part 2: Characterization of microstructure formation by means of high‐resolution transmission electron microscopy and selected area diffraction Liquid or solid silicone resins represent the economically most interesting class of organic precursors for the pyrolytic production of glass and ceramics materials on silicon basis. As dense, dimensionally stable components can be cost‐effectively achieved by admixing reactive filler powders, chemical composition and microstructure development of the polymer‐derived residues must be exactly known during thermal decomposition. Thus, in the present work, glasses and ceramics produced by pyrolysis of the model precursor polymethylsiloxane at temperatures from 525 to 1550 °C are investigated. In part 1, by means of analytical electron microscopy, the bonding state of silicon was determined on a nanometre scale and the phase separation of the metastable Si–C–O matrix into SiO₂, C and SiC was proved. The in‐situ crystallization could be considerably accelerated by adding fine‐grained powder of inert fillers, such as Al₂O₃ or SiC, which permits effective process control. In part 2, the microstructure is characterized by high‐resolution transmission electron microscopy and selected area diffraction. Turbostratic carbon and cubic β‐SiC precipitate as crystallization products. Theses phases are embedded in an amorphous matrix. Inert fillers reduce the crystallization temperature by several hundred °C. In this case, the polymer‐derived Si–C–O material acts as a binding agent between the powder particles. Reaction layer formation does not occur. On the investigated pyrolysis conditions, no crystallization of SiO₂ was observed.     

Partikelform und Porosität von biogenen Pyrolysekoksen

Char particles from pyrolyzed biomass vary in particle size and shape. On average, the particles are more elongated the larger their size. The average size‐specific elongation is almost alike for all investigated samples, i.e. independent from their source material and process. The particle collectives cannot be characterized accurately with classical particle size distributions, which assume spherical particle shape. Accounting for their shape, they can be described more accurately with particle size distributions that are based on an ellipsoid model. The high bulk porosity is mainly attributed to the spaces between particles.     

Graphene oxide nanoflakes from various agrowastes

Nowadays, the synthesis of graphene/ graphene oxide from graphite precursor using oxidizing agents is the most common procedure, but the direct synthesis of graphene or graphene oxide from a non-graphitic carbonaceous material without using inert atmosphere is really a great challenge. Besides, the chemistry behind the development of graphitic structure from a non-graphitic material during the thermal heating is still not clearly understood. In this research work, three agrowaste materials viz. rice husk, sugarcane bagasse and newspaper were selected and subjected to pyrolysis in presence of trace amount of air. The continued heating at the optimum temperature has resulted in aromatization and condensation along with the oxidation within the cellulosic structure of the agrowaste, which finally resulted in the formation of graphene oxide nanoflakes directly. The mechanism of formation of graphene oxide from these agrowaste materials was studied, which suggested that any carbonaceous waste materials can be converted to graphene oxide by optimizing the thermal heating conditions.     

Chemische Zusammensetzung und Mikrostruktur polymerabgeleiteter Gläser und Keramiken im System Si–C–O. Teil 1: Phasenidentifikation mittels Si‐L2,3‐Ionisationskanten‐Elektronenenergieverlustspektroskopie nach dem Fingerprint‐Verfahren und energiegefilterter Durchstrahlungselektronenmikroskopie

Chemical Composition and Microstructure of Polymer‐Derived Glasses and Ceramics in the Si–C–O System. Part 1: Phase identification by means of Si‐L_2,3‐ionisation edge electron energy‐loss spectroscopy according to the fingerprinting technique and energy‐filtered transmission electron microscopy Polymer or precursor ceramics represent a novel class of high‐performance materials that are produced by controlled pyrolysis of organometal compounds. Shrinkage and porosity resulting from thermal decomposition can be compensated by adding chemically reactive filler powders. This technique permits manufacturing of dense ceramic bulk components true to size by cost‐effective near‐net‐shape forming of cross‐linked green compacts. For process control, definition of the course of the reaction of the active fillers and thus the exact knowledge of the chemical composition and the microstructure development of the solid residues during pyrolysis of the polymer precursor is required. Due to both the great technical importance of the final ceramic products and their economical availability, in the present work, thermal decomposition of a silicone resin (polymethylsiloxane) at temperatures between 525 and 1550 °C was characterized nanochemically and microstructurally. In part 1, the results of the quantitative phase identification by means of analytical electron microscopy are reported. The bonding state of silicon was determined by fine structure analysis (Si‐L_2,3‐ionisation edge) of the electron energy‐loss spectrum and has proved to be always mainly oxidic. By means of energy‐filtered transmission electron microscopy, elemental distributions in the nanometre range were recorded. The phase separation of the polymer‐derived Si–C–O matrix into SiO₂, C and SiC could be proved definitely. The characterization of structure formation by high‐resolution imaging and diffraction methods follows in part 2.