Martin Luther Universität Halle-Wittenberg Institut für Geowissenschaften Mineralogie/Geochemie Prof. Dr. Dr. H. Pöllmann Von-Seckendorff-Platz 3, 06120 Halle, Tel: +49.345.5526111, Fax:+49.345.5527180, e-mail: [email protected] Investigation of Mechanisms and Kinetics of the Hydrothermal Synthesis of Novel Hydraulic Binding Materials Patrick Ullrich Main issue is the investigation of the hydrothermal synthesis of crystalline and nanocrystalline calcium-silicate-hydrates (C-S-H-phases) and especially the formation of -dicalcium-silicatehydrate (-C2SH). These materials are forming as precursor during the production of the novel hydraulic binding material Celitement (www.celitement.de). They are produced in the main process step, a hydrothermal synthesis in an autoclave at 200°C [Beuchle et al. 2008, Beuchle 2010]. The reactions taking place during the process in the autoclave should be investigated directly, so called: in situ. For this purpose, a micro-autoclave for use at the synchrotron radiation facility ANKA (KIT, Karlsruhe) has been developed. The experimental setup enables the conduction of a hydrothermal synthesis at the beamline SUL-X and at the same time, the determination of the phase composition in the reaction chamber by x-ray diffraction (XRD, E=16keV, beam cross section: 300m x 150m). The micro-autoclave has a reaction volume of 27l (path length: 1mm) and can be assembled with sapphire or diamond windows. Temperatures can be regulated by a temperature controller between 70°C and 200°C (+/-1°C). Abb. 1: Setup of the microautoclave at SUL-X. The in situ measurements enable the direct investigation of the processes during the reaction. Based on the results it is now possible to draw conclusions about reaction mechanisms and kinetics of the formation of C-S-H-phases. Abb. 2: Changes in the phase composition of a synthesis of SiO2 (quartz sand) and Ca(OH)2 in 3dimensional view. Literature: Beuchle, G. ; Garbev, K. ; Schweike, U. ; Stemmermann, P.: Einphasiges hydraulisches Bindemittel, Verfahren zu seiner Herstellung und mit diesem Bindemittel hergestellter Baustoff. 2008 Patentnummer: 10 2007 035 257 B3; 10 2007 035 258 B3; 10 2007 035 259 B3 Beuchle, G. ; Garbev, K. ; Schweike, U. ; Stemmermann, P.: Verfahren zur Herstellung eines belithaltigen Bindemittels.2010; Patentnummer: EP 1 915 325 B1
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