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Micromechanical Analysis of Blended Cement-Based Composites

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Micromechanical Analysis of Blended Cement-Based Composites Doctoral thesis Micromechanical analysis of blended cement-based composites carried out for the purpose of obtaining the academic double degree of a \Doctor of Philosophy" (Ph.D.) from CTU in Prague, Faculty of Civil Engineering, and \Doktor der technischen Wissenschaften" (Dr.techn.) from TU Wien { Vienna University of Technology, Department of Civil Engineering Dissertation Mikromechanische Analyse von Kompositmaterialien aus Mischzementen ausgef¨uhrtzum Zwecke der Erlangung des akademischen Doppelgrades eines \Doctor of Philosophy" (Ph.D.) eingereicht an der Tschechischen Technischen Universit¨atin Prag, Fakult¨atf¨urBauingenieurwesen, und eines Doktors der technischen Wissenschaft (Dr.techn.) eingereicht an der Technischen Universit¨at Wien, Fakult¨atf¨urBauingenieurwesen Ing. Michal Hlobil Matrikelnummer: 1229375 Supervisor: doc. Ing. V´ıt Smilauer,ˇ Ph.D. Department of Mechanics, Czech Technical University in Prague Supervisor: Assoc. Prof. Dipl.-Ing. Dr. techn. Bernhard Pichler Institut f¨urMechanik der Werkstoffe und Strukturen, Technische Universit¨at Wien i Acknowledgment It has been a great privilege to work under the dual supervision of both doc. Ing. V´ıt Smilauer,ˇ Ph.D. during my stay in Prague as well as Assoc. Prof. Dipl.-Ing. Dr. techn. Bernhard Pichler during my stay in Vienna. I thank doc. Smilauerˇ for his skilled guidance, sharing his knowledge on numerical mechanics and for his tremendous support throughout my studies. I am grateful to Assoc. Prof. Pichler for his continuing encouragement, for introducing me into continuum micromechanics and for his patience and advices that helped me a lot in my personal development. I would like to acknowledge the support from the industrial-academic nanoscience research network for sustainable cement and concrete `NANOCEM' (http://www.nanocem.org), provided within the framework of Core Project 10 entitled \Micromechanical analysis of blended cement-based composites", which enabled my employment at the Czech Technical University in Prague as well as my stays at the Lafarge Centre de Recherche in Lyon and at TU Wien { Vienna University of Technology. I also gratefully acknowledge CTU grants SGS15/030/OHK1/1T/11 and SGS16/037/OHK1/1T/11. I wish to thank to two industrial advisors from NANOCEM, namely to Klaus- Alexander Rieder from GCPAP and to Gilles Chanvillard (in memoriam) from LafargeHolcim, who supervised my project, offered advice and contributed to a fruitful project development in an encouraging atmosphere. I appreciated stim- ulating discussions on NANOCEM events, which further helped me to focus on questions and topics, which are important for the cement industry. I cannot forget to thank the team at Lafarge Centre de Recherche for their support during my internship, namely Pipat Termkhajornkit for his patience in introduc- ing me into microstructural phase assemblages of cement pastes, Fabienne Begaud for her help with mechanical testing, QuocHuy Vu for his advice and Svatopluk Dobrusk´yfor help, not only at the research center. The team at TU Wien both at Karlsplatz as well as in the Rella Halle deserves my thanks for creating a stimulating atmosphere and helpful discussions. Namely I wish to thank to Markus K¨onigsberger for his help and support with continuum micromechanics and to Wolfgang D¨ornerfor his help with mechanical testing. Thanks to the staff in the department of Mechanics at the Czech Technical Uni- ii versity in Prague for creating a calm and friendly atmosphere, especially Petr Hlav´aˇcek, Wilson Ricardo Leal da Silva, and Fernando Suarez for discussions not only on cement or Python. For that constant help I wish to thank my parents and my sister. And very special thank goes to my wife Ad´elafor her strong support not only during my studies. iii Abstract In order to reduce CO2 emissions associated with the production of building ma- terials, the cement and concrete industry has developed new binders by blending ordinary Portland cement with supplementary cementitious materials such as the industrial waste products blast furnace slag and fly ash, and/or with finely ground inert materials such as limestone and quartz. This is setting the scene for the present thesis which is motivated by the fact that the new binders exhibit different hardening characteristics compared to their predecessors that were produced with ordinary Portland cement alone. In order to improve the predictability of prop- erties of blended cementitious materials, a combined experimental-computational approach is used. In the experimental part, a comprehensive test database is elaborated by combin- ing state-of-the-art microstructural characterization techniques and mechanical testing. Microstructural characterization combines methods including thermo- gravimetric analysis, X-ray diffraction with Rietveld analysis, and scanning elec- tron microscopy, in order to determine the microstructural phase assemblages of the initial raw products as well as 1, 3, 7, 28, and 91 days after mixing with water. This allows for resolving phase volume evolutions at the specified times. Mechanical testing, in turn, includes characterization of stiffness and strength. The early-age evolution of static unloading modulus is determined with a test protocol including cyclic loading-unloading tests which are hourly repeated from 24 hours after production up to material ages of 8 days. Dynamic stiffness is determined based on measurements of ultrasonic pulse velocities of longitudinal and shear waves, evaluated on the basis of elastic wave propagation in isotropic media. The uniaxial compressive strength evolution is determined both on pastes and mortars, crushed 1, 3, 7, 28, and 91 days after production. The tensile split- ting strength, in turn, is determined 1, 3, 28, and 91 days after production. All the measured data is then stored in a newly established database \CemBase" along with additional data collected from the literature. At the end of this thesis \CemBase" contained information on 399 entries out of which approx. 20 % were measured during the experimental campaign and approx. 80 % were collected from available literature. The computational part focuses on multiscale strength homogenization in the iv frameworks of two complementary modeling methods: multiscale Finite Element- based homogenization and continuum micromechanics. Finite Element-based ho- mogenization uses nonlinear fracture mechanics with an isotropic damage model to establish a link between nanoscopic calcium-silicate-hydrates and the uniaxial compressive strength of cement pastes, emphasizing the nonuniform distribution of C-S-H around clinker grains. The model focuses on the special role of C-S-H as the main material phase contributing to the macroscopic mechanical prop- erties as well as introduces the C-S-H/space ratio as the main microstructural descriptor. In addition, the model identifies key factors influencing the compres- sive strength of cement pastes. Continuum micromechanics, in turn, is used for elasto-brittle modeling of both compressive and tensile strength. The method accounts for key features of cementitious microstructures in terms of their hierar- chical organization, quasi-homogeneous material phases, their volume fractions, characteristic shapes, and mutual interaction. The compressive strength model considers that the macroscopic strength is reached once stress peaks in micron- sized needle-shaped hydrates reach their strength. The latter is described based on a Mohr-Coulomb failure criterion including the angle of internal friction and the cohesion of low-density calcium-silicate-hydrates, as quantified by limit state analysis of nanoindentation tests. The model accounts for stress concentrations in the immediate vicinity of sand grains, and it uses strain energy-related stress av- erages for the scale transition from cement paste down to needle-shaped hydrates. It is found that microfillers effectively reinforce the hydrate foam, and that hy- dration of supplementary cementitious materials has a strengthening effect which is not only related to the increase of hydrate volume and the corresponding de- crease of capillary porosity, but also to an increase of the cohesion of low-density calcium-silicate-hydrates. The tensile strength model, in turn, is based on up- scaling elasticity and fracture energy from nanoscopic calcium-silicate-hydrates { as quantified by molecular dynamics simulations { all the way up to the uniaxial tensile strength of mortars and concretes. The model considers that cementi- tious materials suffer from pre-existing cracks which are only somewhat smaller than the maximum aggregate size, and that the tensile strength of the material is reached once these cracks start to propagate. Summarizing, the three devel- oped models define a new state-of-the-art regarding multiscale homogenization of strength properties of cementitious materials. v Abstrakt Za ´uˇcelem sn´ıˇzen´ı emis´ı CO2 vznikaj´ıc´ıch pˇri v´yrobˇe betonu pˇristoupil ce- ment´aˇrsk´ypr˚umysl k v´yvinu alternativn´ıch pojiv, kter´evzniknou sm´ıch´an´ım Portlandsk´ehocementu s doplˇnkov´ymicementov´ymipˇr´ımˇesmijako napˇr.struska a pop´ılek,pˇr´ıpadnˇedalˇs´ımiinertn´ımimateri´alyjako napˇr.mikromlet´ykˇremen anebo v´apenec. Motivac´ıpro tuto disertaˇcn´ıpr´acibyla skuteˇcnost,ˇzesmˇesn´e cementy vykazuj´ırozd´ıln´evlastnosti v porovn´an´ıs Portlandsk´ymcementem. Za ´uˇcelemzlepˇsen´ıpˇredpovˇediv´ysledn´ych vlastnost´ıkompozit˚una b´azismˇesn´ych ce- ment˚uje v t´etopr´acipouˇzitkomplement´arn´ı,experiment´alnˇe-modelovac´ıpˇr´ıstup.
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