TY - THES A1 - Rößler, Christiane T1 - Hydratation, Fließfähigkeit und Festigkeitsentwicklung von Portlandzement – Einfluss von Fließmitteln, Alkalisulfaten und des Abbindereglers T1 - Hydration, fluidity and strength development in Portland cement – influence of superplasticizers, alkali sulphates and set regulator N2 - Eine zielführende Anwendung von Zusatzmitteln bei der Ausführung anspruchsvoller Betonbauten setzt einen hohen Kenntnisstand bezüglich der Wirkungsmechanismen und Interaktionen der einzelnen Betonkomponenten voraus. In der vorliegenden Arbeit wurden einige Aspekte der Zementhydratation in Abhängigkeit von der Fließmittelzugabe diskutiert. Im Ergebnis liefern die Teile eins und zwei der vorliegenden Arbeit einen Beitrag dazu, Veränderungen der Fließfähigkeit von Zementleim in Abhängigkeit der Zementhydratation und Fließmittelzugabe besser zu verstehen. Es konnte so z.B. gezeigt werden, dass Bildung langprismatischer Kristalle (z.B. Syngenit, Gips) die Fließfähigkeit von Zementleim und Beton vermindert. Infolge anhaltender Scherung von Zementleimen / Betonen mit langprismatischen Kristallen wird ein Zuwachs an Fließfähigkeit erzielt. Elektronenmikroskopische Untersuchungen zeigen, dass dies darauf zurückzuführen ist, dass die Kristalle in eine Vorzugsorientierung relativ zur Scherbewegung rotieren. Weiterhin wurde der Mechanismus einer so genannten Zement-Fließmittel-Inkompatibilität aufgezeigt. Durch diese Erweiterung des Kenntnisstandes zum Einfluss von Fließmitteln auf die Zementhydratation ist es möglich der Zement-Fließmittel-Inkompatibilität durch gezielte Auswahl des Zementes vorzubeugen. Dabei ist besonders darauf zu achten, dass der Zement ein ausgewogenes Verhältnis an zur Reaktion zur Verfügung stehendem C3A und Menge / Löslichkeit des Abbindereglers besitzt. Fließmittel verändern nicht nur die Verarbeitungseigenschaften sondern auch die Festigkeit und Dauerhaftigkeit von Zementstein und Beton. Im dritten Teil der vorliegenden Arbeit wird daher der Einfluss der Fließmittel und deren verflüssigender Wirkung auf die Festigkeitsentwicklung von Zementstein und C3S untersucht. Es konnte gezeigt werden, dass durch die dispergierende Wirkung der Fließmittel auch ohne Verminderung des Wasserzementwertes, eine Verdichtung des Zementsteingefüges erzielt werden kann. Es konnte weiterhin gezeigt werden, dass durch die Erhöhung der Partikelpackungsdichte am Anfang der Hydratation die Ausbildung der festigkeitsgebenden C-S-H Phasen verändert wird. Ein dichteres Verwachsen dieser nanostrukturierten C-S-H Phasen ermöglicht einen zusätzlichen Festigkeitszuwachs. N2 - The construction of sophisticated concrete buildings requires the pinpointed application of concrete additives. This requires a high level of knowledge concerning the interaction and mode of action of individual concrete components. The presented study aims to improve the understanding of the concrete components cement and superplasticizers. Main focus is laid on the influence of superplasticizers on cement hydration reactions and the consequences for cement and concrete performance characteristics (fluidity and strength). Results of parts one and two of the thesis reveal how the fluidity of cement paste is influenced by cement hydration and addition of superplasticizers. It is shown that the formation of long prismatic crystals like syngenite and gypsum decreases the fluidity of cement pastes and concrete. This decrease in fluidity is partly reversible if the suspension is continuously stirred. It was proven by scanning electron microscopy (SEM) that this gain in fluidity is caused by the rotation of long prismatic crystals into a preferred orientation. Furthermore the cause of a cement-superplasticizers-incompatibility was identified. The knowledge of this mechanism is essential for a successful selection of cement type in combination with superplasticizers. Results showed that for an effective selection of polycarboxylate-type superplasticizer and cement, it is essential that the ratio of aluminate clinker phases (C3A) to the amount / solubility of set regulator is appropriate. Superplasticizers improve not only the fluidity but also the compressive strength of cement and concrete. The third part of the thesis shows how the liquefying action of superplasticizers influences the strength development of cement and C3S pastes. Thus it was shown that a densification of the cement microstructure is achieved by the superplasticizers dispersing action. The increased particle packing density caused by superplasticizers in the suspension state of cement pastes increases the intergrowth of strength determining C-S-H phases. This leads to an increase in compressive strength without diminishing the water to cement ratio. KW - Zement KW - Hydratation KW - Mikrostruktur KW - Betonverflüssiger KW - Festigkeit KW - Fließverhalten KW - Alkalisulfate KW - Abbinderegler KW - C-S-H Phasen KW - Fließmittel KW - cement KW - hydration KW - microstructure KW - superplasticizer KW - strength KW - fluidity KW - C-S-H phases KW - set regulator Y1 - 2006 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:gbv:wim2-20070206-8425 N1 - ISBN 978-3-8325-1490-7, Logos Verlag Berlin, 2007 ER - TY - JOUR A1 - Kleiner, Florian A1 - Rößler, Christiane A1 - Vogt, Franziska A1 - Osburg, Andrea A1 - Ludwig, Horst-Michael T1 - Reconstruction of calcium silicate hydrates using multiple 2D and 3D imaging techniques: Light microscopy, μ-CT, SEM, FIB-nT combined with EDX JF - Journal of Microscopy N2 - This study demonstrates the application and combination of multiple imaging techniques [light microscopy, micro-X-ray computer tomography (μ-CT), scanning electron microscopy (SEM) and focussed ion beam – nano-tomography (FIB-nT)] to the analysis of the microstructure of hydrated alite across multiple scales. However, by comparing findings with mercury intrusion porosimetry (MIP), it becomes obvious that the imaged 3D volumes and 2D images do not sufficiently overlap at certain scales to allow a continuous quantification of the pore size distribution (PSD). This can be overcome by improving the resolution and increasing the measured volume. Furthermore, results show that the fibrous morphology of calcium-silicate-hydrates (C-S-H) phases is preserved during FIB-nT. This is a requirement for characterisation of nano-scale porosity. Finally, it was proven that the combination of FIB-nT with energy-dispersive X-ray spectroscopy (EDX) data facilitates the phase segmentation of a 11 × 11 × 7.7 μm3 volume of hydrated alite. KW - Zementklinker KW - Bildsegmentierung KW - Rasterelektronenmikroskopie KW - Computertomographie KW - tomography KW - focussed ion beam KW - cement microstructure KW - micro-CT Y1 - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:gbv:wim2-20220106-45458 UR - https://onlinelibrary.wiley.com/doi/10.1111/jmi.13081 VL - 2021 SP - 1 EP - 6 PB - John Wiley & Sons Ltd CY - Oxford ER - TY - CHAP A1 - Kleiner, Florian A1 - Rößler, Christiane T1 - Utilizing Modern FIB/SEM Technology and EDS for 3D Imaging of Hydrated Alite and its Pore Space T2 - ERICA-CASH II Final Converence N2 - The exploration of cementitious materials using scanning electron microscopes (SEM) is mainly done using fractured or polished surfaces. This leads to high-resolution 2D-images that can be combined using EDX and EBSD to unveil details of the microstructure and composition of materials. Nevertheless, this does not provide a quantitative insight into the three-dimensional fine structure of for example C-S-H phases. The focused ion beam (FIB) technology can cut a block of material in thin layers of less than 10 nm. This gives us a volume of 1000 μm³ with a voxel resolution of down to 4 x 4 x 10 nm³. The results can be combined with simultaneously acquired EDX data to improve image segmentation. Results of the investigation demonstrate that it is possible to obtain close-to-native 3D-visualisation of the spatial distribution of unreacted C3S, C-S-H and CH. Additionally, an optimized preparation method allows us to quantify the fine structure of C-S-H phases (length, aspect ratio, …) and the pore space. KW - Rasterelektronenmikroskop KW - Alit KW - SEM KW - Focussed Ion Beam KW - EDX KW - energy dispersive X-ray spectroscopy KW - alite Y1 - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:gbv:wim2-20210702-44555 ER - TY - JOUR A1 - Jiang, Mingze A1 - Rößler, Christiane A1 - Wellmann, Eva A1 - Klaver, Jop A1 - Kleiner, Florian A1 - Schmatz, Joyce T1 - Workflow for high-resolution phase segmentation of cement clinker fromcombined BSE image and EDX spectral data JF - Journal of Microscopy N2 - Burning of clinker is the most influencing step of cement quality during the production process. Appropriate characterisation for quality control and decision-making is therefore the critical point to maintain a stable production but also for the development of alternative cements. Scanning electron microscopy (SEM) in combination with energy dispersive X-ray spectroscopy (EDX) delivers spatially resolved phase and chemical information for cement clinker. This data can be used to quantify phase fractions and chemical composition of identified phases. The contribution aims to provide an overview of phase fraction quantification by semi-automatic phase segmentation using high-resolution backscattered electron (BSE) images and lower-resolved EDX element maps. Therefore, a tool for image analysis was developed that uses state-of-the-art algorithms for pixel-wise image segmentation and labelling in combination with a decision tree that allows searching for specific clinker phases. Results show that this tool can be applied to segment sub-micron scale clinker phases and to get a quantification of all phase fractions. In addition, statistical evaluation of the data is implemented within the tool to reveal whether the imaged area is representative for all clinker phases. KW - Zementklinker KW - Bildsegmentierung KW - Rasterelektronenmikroskopie KW - cement clinker KW - image segmentation KW - EDX KW - superpixel Y1 - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:gbv:wim2-20211215-45449 UR - https://onlinelibrary.wiley.com/doi/epdf/10.1111/jmi.13072 VL - 2021 SP - 1 EP - 7 PB - Wiley-Blackwell CY - Oxford ER -