abstract: Ultra High Performance (UHP) cementitious binders are a class of cement-based materials with high strength and ductility, designed for use in precast bridge connections, bridge superstructures, high load-bearing structural members like columns, and in structural repair and strengthening. This dissertation aims to elucidate the chemo-mechanical relationships in complex UHP binders to facilitate better microstructure-based design of these materials and develop machine learning (ML) models to predict their scale-relevant properties from microstructural information.To establish the connection between micromechanical properties and constitutive materials, nanoindentation and scanning electron microscopy experiments are performed on several cementitious pastes. Following Bayesian statistical clustering, mixed reaction products with scattered nanomechanical properties are observed, attributable to the low degree of reaction of the constituent particles, enhanced particle packing, and very low water-to-binder ratio of UHP binders. Relating the phase chemistry to the micromechanical properties, the chemical intensity ratios of Ca/Si and Al/Si are found to be important parameters influencing the incorporation of Al into the C-S-H gel. ML algorithms for classification of cementitious phases are found to require only the intensities of Ca, Si, and Al as inputs to generate accurate predictions for more homogeneous cement pastes. When applied to more complex UHP systems, the overlapping chemical intensities in the three dominant phases – Ultra High Stiffness (UHS), unreacted cementitious replacements, and clinker – led to ML models misidentifying these three phases. Similarly, a reduced amount of data available on the hard and stiff UHS phases prevents accurate ML regression predictions of the microstructural phase stiffness using only chemical information. The use of generic virtual two-phase microstructures coupled with finite element analysis is also adopted to train MLs to predict composite mechanical properties. This approach applied to three different representations of composite materials produces accurate predictions, thus providing an avenue for image-based microstructural characterization of multi-phase composites such UHP binders. This thesis provides insights into the microstructure of the complex, heterogeneous UHP binders and the utilization of big-data methods such as ML to predict their properties. These results are expected to provide means for rational, first-principles design of UHP mixtures. / Dissertation/Thesis / Doctoral Dissertation Engineering 2020

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The diploma thesis is focused on evaluation of properties of fine aggregate by means of laboratory tests. Fine aggregate evaluation was performed using sieving test, laser diffraction, delta ring and ball test, bitumen number test, uncompacted void content of fine aggregate according to AASHTO T 304, voids of dry compacted filler (Rigden) test and particle density of filler. Laboratory research has led to the discovery of some properties of fine aggregate and their dependencies.

The work deals with the preparation and study of polyphosphate composites. Aluminum phosphates provide some unusual properties like high-heat resistance in terms of inorganic binders. The addition of chromium in the form of Cr2O3 or directly the bond with the aluminum-chromium-phosphate can improve the properties of this binder. Highly viscous Al2Cr(H2PO4)9 and Al3Cr(H2PO4)12 binders were prepared by dissolving Al(OH)3 and CrO3 in 85% phosphoric acid, and mixed with Al2O3 and Cr2O3 fillers. The composites were cured in the furnace at 150 °C for 24 h under pressure of 10 MPa. During the annealing at temperatures up to 1 500 °C changes in chemical structure of the cured composites were observed, leading to the understanding of the creation of crystalline phases and their eventual changes. The characterization of binders was mainly based on FT-IR, EDAX, TG-DTA and optical microscopy analyses.

The work studies the possibilities of the utilization of secondary raw materials produced by power industry. It addresses mainly the gypsum by-products and fluidized coal combustion ash. As for the secondary raw materials the content of sulphites is observed and the dependences of their transformation to sulphides via natural oxidation by air oxygen or by addition of adequate oxidant are studied. The work follows with describing the effect of sulphides contained in raw materials on the mechanical properties of composites prepared from several various matrices such as alumina or portland cement, lime or portland clinker. As for pure portland clinker the ability to retard the setting is also observed. The amount of contained sulphites is measured volumetrically via indirect titration of iodine surplus by sodium thiosulphate with the starch size as the indicator.

Tato diplomová práce zkoumá možnosti tvorby porézních struktur za použití partikulárních materiálů pojených anorganickými pojivy bez dodatečné tepelné úpravy vypalováním. Jako základní pojiva byly použity portlandský a hlinitanový cement a pojiva na bázi alkalicky aktivovaného metakaolinu (geopolymeru). Jako základní kamenivo byl použit karbid křemíku v různých frakcích podle velikosti částic. Byly taktéž použity další zrnité materiály, např. křemenný písek anebo odpadních materiálů (mleté sklo a porcelán) roztříděných do frakcí podle velikosti částic. Byl sledován vliv složení a množství kameniva na vytváření porézní struktury a tím i na mechanické vlastnosti, které byly testovány pomocí mechanických zkoušek. Pevnostní zkoušky byly provedeny na trámečcích 20 × 20 × 100 mm připravených z testovacích směsí. Granulometrické a fázové složení vstupních surovin bylo studováno metodou laserové granulometrie resp. RTG difrakce. Porézní struktura byla studována metodami rtuťové porozimetrie, dále pomocí světelné a rastrovací elektronové mikroskopie a taktéž pyknometrickou metodou. V rámci charakterizace přepážek (terčíky o průměru 90 mm) připravených z jednotlivých materiálů bylo provedeno stanovení efektivní permeability průtokem vzduchu. Dále byly provedeny testy vzlínavosti kapaliny v připravených materiálech. V závěru práce byly provedeny pokusy o filtraci jemných suspenzí přes uvedené přepážky.

The thesis deals with the development of self-leveling cement screed with compensated shrinkage. It is a ternary binder system with the majority of portland cement, that in the beginning of setting and hardening form an expandable folder ettringite. At first there was a background research of volume changes of hydrating cement composites and methods for measuring these changes. Various sort of expansion additives were also introduced, the main emphasis was on concepts of calculated formation of ettringite, which are typical for self-leveling underlayment. Background research included the issues of formation of ettringite, influences on it’s nucleation and it’s stability. The practical development of the screed began by measuring volume changes of different pastes on a ternary composition. Selected formulations suitable for use are verified together with additives to semi-application tests. After the final configuration of the screed mixture, there was a test in real application of an representative area. Individual formulations were tested in terms of long-term stability of ettringite in dry and moist environments.

This diploma thesis deals with influence of modifying additives on achieved properties of anhydrite binders. The first part is focused on funamentals of anhydrite binders. Ist second part introduces anhydrite under-layments and their standard requirements. The experimental part is dedicated to anhydrite binders modyfyied by plasticizers, while their final properties are compared.

This diploma thesis deals with the synthesis of an organosilica polymer which could be used as a binder for titanium dioxide photocatalytic layers. The main reason for incorporating the binder into the photocatalytic layers is not only the improving of the mechanical properties, but above all, the binder could help with production of low-temperature photocatalytic layers, that could be applied to heat-sensitive materials such as plastic materials. This could create layers on flexible materials that could be easily made into any shape. The work focuses on the synthesis of organosilica polymer from the organosilica precursor and subsequent characterization of the binder. Surface tension, viscosity, density, XRD, thermal analysis of silica binder solutions was performed. Titanium dioxide compositions with this binder were prepared, then they were printed and the layers were treated with UV and plasma. Treated layers were examined by FT-IR and a voltamperometric characterization was performed.

Grâce à leurs excellentes propriétés de dureté et de résistance à l’usure, les carbures cémentés sont les meilleurs candidats pour la réalisation d’outillage de coupe. Elaborés par la métallurgie des poudres, ils sont majoritairement composés de carbure de tungstène, choisis pour ses propriétés de dureté et d’un liant métallique à haute ductilité, le plus souvent le cobalt. Néanmoins, l’utilisation du cobalt comme liant est remis en question depuis quelques années par la commission européenne REACH à cause de sa toxicité. En conséquence, des liants alternatifs tels que les alliages de Fe et Ni sont étudiés. Malgré les différents travaux menés, il subsiste un manque de compréhension fondamental sur l’effet spécifique du liant sur le frittage et le grossissement de grains des carbures cémentés. Le but de cette étude est la compréhension de l’effet de la composition du liant sur le frittage et le grossissement de grains. Dans cet objectif, différent liants WC-20vol%M (M=Fe, Ni or Co) et différent taux de carbone sont considérés. Le frittage et le grossissement de grains seront étudiés à l’aide de caractérisations macroscopiques et microstructurales, puis les résultats discutés en comparaison avec la littérature. Comme il a été déjà observé dans le cas d’alliages WC-Co, le retrait au cours du frittage survient plus tôt dans le cas d’alliages riches en W qu’en C, quelque soit le liant considéré. Concernant l’effet de la nature du liant, le frittage en phase solide est décalé vers les hautes températures pour WC-Fe en comparaison avec WC-Co et WC-Ni. Dans cette étude le retrait est directement corrélé avec la capacité d’étalement du liant dans la porosité, comme le confirme l’analyse de la microstructure. Quant au grossissement de grain, il est inhibé pour un faible ratio C/W, quelque soit la nature du liant. Néanmoins, pour un ratio C/W élevé, celui-ci augmente, ainsi que la tendance au grossissement anormal, en particulier dans le cas du liant nickel. Les mécanismes de grossissement de grains sont discutés en lien avec les observations structurales des interfaces. / Thanks to their exceptional hardness and wear resistance, cemented carbides are the best candidates to make efficient cutting and drilling tools by the powder metallurgy route. Known as a very hard ceramic material, tungsten carbide is used as the major component of cemented carbides. A ductile metal binder is added as the matrix, which in most cases is cobalt. Nevertheless the use of cobalt as a binder is questioned by the new European regulation on chemicals (REACH). Therefore, new alternative binders are considered, especially Fe and Ni-alloys. Although a few studies exist for Fe-based and Ni-based WC cemented carbides, there is still a lack of fundamental understanding of the specific effect of the binder on sintering and grain growth. This work discusses the effect of binder composition on sintering and grain growth of cemented carbides. For this purpose, different binder compositions WC-20vol%M (M= Fe, Ni or Co) and different C/W ratio are considered. Sintering and grain growth behaviors are investigated using several macroscopic and microstructural characterizations, and results are discussed and compared to the literature. As already observed in previous works on WC-Co, shrinkage occurs earlier for W-rich than for C-rich alloys for the three binders. Regarding the influence of the binder nature, solid state sintering is delayed to higher temperature for WC-Fe in comparison to WC-Co and WC-Ni alloys. Shrinkage is directly related to the spreading efficiency of the binder into the porosity, as confirm by the microstructure analysis. Grain growth is inhibited for low C/W ratio whatever the binder nature. Nevertheless, for a high C/W ratio, grain growth is enhanced and the abnormal character of grain growth increases, especially in the case of a Ni binder. Grain growth mechanisms are discussed in relation with the observed structure of phase boundaries.