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C. Romero Rodriguez

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Self-healing concrete technology has been widely investigated in the past decade as a solution against degradation and/or loss of functionality in cracked concrete elements. Many self-healing mechanisms have been proposed and proven to work experimentally in the literature. Among these systems, the use of encapsulated mineral-producing healing agents seems to be the best working combination of components to successfully heal the cracks. The involved triggering-healing mechanisms usually consist of complex physical phenomena. Hence proper optimization of the proposed self-healing material is not possible through often resource- and time-consuming experimental campaigns. Instead, numerical modelling could be a useful tool for timely and exhaustive investigation of the self-healing mechanisms, as well as the design of appropriate experimental setups. Yet, while research on self-healing concrete seems to keep growing, comparatively the amount of modelling work devoted to the optimized design of the material has not advanced.
This thesis aims to provide a modelling framework for the study of the main aspects of a capsule-based self-healing cement-based system, namely the mechanical triggering of the self-healing system, the healing process itself and the assessment of the recovered property.
For the self-healing mechanism to work, the triggering of enough capsules along the crack is desired. Notwithstanding, this crack steering optimization comes at the expense of proper mechanical behaviour of the composite. Whereas the earlier aspect has been studied in the past, in this thesis a numerical optimization of the triggering of capsules is carried out taking into account also the achievement of acceptable mechanical performance of the material. To illustrate this, the case of self-healing cement paste with bacteria-embedded polylactic acid (PLA) capsules was selected. A 3D mesoscale lattice model was implemented herein to simulate a uniaxial tensile test on the system composed of cement paste, PLA capsule and their interface. Previous studies on the mechanical behaviour of cement paste with inclusions (i.e. capsules) have shown that the interface transition zone around the inclusion presents microstructural and mechanical properties that are totally different from those of the matrix. Therefore, a meticulous study was first conducted to obtain the mechanical properties of the interface of various types of PLA capsules with respect to bulk cement paste. Nanoindentation was performed to obtain maps of hardness and elastic modulus in the interfaces. 2D microscale lattice modelling of uniaxial tensile test on the mapped locations was performed then to obtain the overall tensile strength and stiffness of the interface. Moreover, hydrates assemblage and chemical composition around the PLA particles were studied through Backscattering Electron images and Energy Dispersive X-ray Spectroscopy. The ratios between resulting tensile strength and elastic modulus of the interface with respect to bulk paste were obtained for each PLA type which were then used as input for the mesoscale model. Cement paste samples with PLA capsules were imaged through X-ray micro Computed Tomography before and after fracture to obtain the capsules distribution to input in the mesoscale model and the fracture surface for validation, respectively. The experimental and simulated stress-strain curves showed excellent correspondence, especially on the elastic phase, hence validating the proposed model. An exhaustive numerical investigation of the material was performed then to analyse the influence of dosage, size and shape of the PLA capsules, as well as of the interface properties on the mechanical behaviour of the composite and the triggering of the PLA capsules. The results show that interface properties close to but lower than the cement matrix do not entail substantial losses of tensile strength and elastic modulus, whereas the amount of triggered capsules is maximized. Optimum dosage, shape and size of the PLA capsules were also obtained.
To illustrate the healing process and the recovery of the functional property within the proposed modelling framework, the case of crack self-sealing in cement mortar with superabsorbent polymers (SAP) was investigated. These healing admixtures steer the crack propagation and become exposed along the fracture surface. Upon contact with ingress water they immediately absorb water and swell, thus providing a water-blocking effect and preventing harming species to further penetrate into the mortar matrix from the crack surfaces. In order to design such self-sealing systems in an efficient way, a three-dimensional mesoscale lattice model is proposed to simulate capillary absorption of water in sound and cracked cement-based materials containing SAP. The numerical results yield the moisture content distribution in cracked and sound domain, as well as the absorption and swelling of SAP embedded in the matrix and in the crack. In a first instance, the model was validated for mortar without SAP, by means of time-resolved X-ray micro Computed Tomography. Additionally, the water absorption and swelling of SAP embedded within the mortar were imaged and quantified over time to better model their role during capillary water absorption in such composite materials. The performance of the model with the presence of SAP was validated by using experimental data from the literature, as well as experimentally-informed input parameters. The validated model was then used to investigate the role of SAP properties and dosage in cementitious mixtures, on the water penetration into the material from cracks. Furthermore different crack widths were considered in the simulations. The model shows good agreement with experimental results. The obtained results show that increasing the SAP water absorption capacity, while reducing their cement solution absorption capacity improves the crack self-sealing effect more efficiently than increasing their dosage. Other guidelines for the selection of appropriate SAP are given for different crack widths. Moreover, it is suggested that capillary water absorption test in cracked concrete is sensitive enough to detect small localized changes in crack width due to the healing of the cracks. ...
Concrete structures perform poorly when withstanding thermal shock events, usually requiring repair or replacement after one single instance. In certain industries (such as petrol, metallurgic and ceramics), these events are not only likely but frequent, which represents a considerable financial burden. One option to solve this issue would be to decrease the heating rate imposed onto the concrete material through the use of a protective surface layer. In this work, the suitability of dunite and microgabbro as protective materials is explored through X-ray diffraction, thermal dilation, optical microscopy, X-ray microtomography, thermo-gravimetric analysis and a compressive test. Further, the thermal dilation was used as an input to simulate a composite concrete-rock wall and the respective stresses caused by a thermal shock event. The dehydration of chrysotile in dunite and the decomposition of analcime, chamosite and pumpellyite in microgabbro were both favourable for the performance of the stones in the desired application. The thermal stability and deformation were found in the range of what can be applied directly on concrete; however, it was clear that pre-heating treatment results in a far more durable system in a cyclic thermal load situation. ...
Lattice models have been used to simulate mass transport to predict durability of cementitious materials. In particular, the use of dual lattice meshes allows for the coupling of fracture and transport processes, which commonly occur at the same time in these materials. Literature has shown good agreement between simulations and experimental results. Nevertheless, work regarding relevant computational aspects of the numerical model are scarce. In this study, a Voronoi-discretized lattice model is used to simulate unsaturated moisture transport in cement-base materials through the Richards equation. First, investigations regarding the choice of elemental volume approximation, time-stepping procedure and quadrature are evaluated. After validation of the approximations, simulated moisture transport in sound concrete was compared to experiments and mesh and time step sensitivity were discussed. A new approach to model capillary absorption of water in cracked concrete was also proposed and its advantages with respect to existing approaches are discussed by comparing to experimental measurements. The results confirm that the model can accurately predict the transport processes for the earlier stage of capillary absorption. Furthermore, moisture ingress in cracked concrete is simulated for different crack configurations and the use of different approaches is suggested accordingly. Finally, guidelines regarding the approximations used for optimization of the computations are presented. ...
Industries such as metal, ceramics and petrochemicals suffer from high temperature spills. Such events exert a unique form of loading in concrete structures that cannot be accurately simulated by heating of samples in an oven. Calcium aluminate cement (CAC) based concrete is the industry standard for such environment, and while much is known regarding its heating, literature considering hot spills on concrete surfaces is scarce. In this paper, slag is heated up to the same temperature as in a steel factory and then poured on top of cement paste samples with W/C ratios of 0.20 and 0.40. A combination of FEM, TGA, XRD and SEM/EDS was used to investigate the effects of hot spill on the samples. The rapid expansion caused by the thermal shock generated cracks in only some of the samples, while the high temperature environment and unidirectional escape of water caused chemical changes in all samples. ...
For many 3D printed cementitious materials, air voids may play a dominant role in the interlayer bond strength. However, to date, far too little attention has been paid to reveal the air void characteristics in 3D printed cementitious materials. Therefore, to fill this gap, this study attempts to provide an example of systematically characterizing the typical air void system of 3D printed cementitious materials via different image acquisition and analysis techniques. Two printable limestone and calcined clay-based mixtures were employed to prepare the printed samples. The micrographs were acquired by using optical image scanning and X-ray computed tomography. Afterwards, air void metrics in printed cementitious materials were determined, i.e., content, distribution, size, and shape. The results revealed that most of the air voids with the diameter in the range of 10–1000 μm were distributed evenly in the layer region of printed samples. Large air voids (1000–6000 μm) were enclosed mainly between the printed filaments (interface region), which resulted in the relatively higher local porosity than that of layer region. Additionally, the majority of air voids displayed irregular and elongated shapes, which could be attributed to the extrusion and layer-wise manufacturing processes in 3D printing. Finally, a comparison between optical image scanning and X-ray computed tomography was given. ...
This study presents an experimental investigation of the rate-dependent mechanical properties of cement paste at the microscale. With the use of a nanoindenter, micro-cantilever beams with the size of 300 μm × 300 μm × 1650 μm were loaded at five different strain rates from around 10−6/s to 10−2/s until failure. It is found that with increasing strain rate, the stress-strain curves show less and delayed pre-peak nonlinearity. Both the flexural strength and the elastic modulus of beams increase with increasing strain rate, while the strain at peak stress exhibits an opposite trend. Examination of the fracture surface indicates that with increasing strain rate the possibility of a crack to pass through stronger components of the hydration products is increased. The experimental observations and possible mechanisms leading to changes in mechanical responses are discussed. It is suggested that at least two micromechanical processes, namely creep and Stéfan effect, are mainly responsible for the rate-dependent behaviour of cement paste within the investigated strain rate range and their dominances seem to vary with the strain rate. At lower strain rate, the strain rate sensitivity of cement paste is thought to be dominated by the creep effect, while at higher strain rate the Stéfan effect appears to be the governing factor. ...
Conference paper (2021) - C. Romero Rodriguez, R. Ye, Aikaterini Varveri, E. Rossi, Giovanni Anglani, Paola Antonaci, E. Schlangen, B. Šavija
Coupling of carbonation and chlorides ingress mechanisms is very common in concrete under certain exposure conditions such as coastal environments. The aggravation/ mitigation of corrosion by the existence of carbonation lies on the fact that microstructural changes due to carbonation result in changes on the transport properties of the material. In this study we investigate and quantify evolving transport properties of ordinary Portland cement paste, such as porosity, tortuosity and intrinsic permeability. Dual X-ray micro computed tomography (micro CT) is used for the quantification of porosity. Furthermore Dynamic Vapour Sorption (DVS) measurements are carried out to resolve water retention and relative permeability curves. The authors expect to provide insights into the mechanisms of accelerated carbonation in both types of cement paste, as well as data for input and validation of numerical and analytical models on this degradation phenomenon. ...
This paper presents a method to numerically investigate the microstructural effect on the creep behavior of cement paste at the microscale. The lattice fracture model is extended to consider local time-dependent deformations of calcium-silicate-hydrate phases in the cement paste by imposing local forces. The term “experimentally informed model” is used herein as the heterogeneous microstructures of hardened cement pastes were obtained by using the X-ray computed microtomography and directly implemented into the model. The mechanical and creep properties of different constituents at the resolution of 5 µm were inversely identified from the fracture and creep bending tests on cementitious microcantilever beams at the microscale. The model is then validated through the comparison with the testing results of cement pastes with different w/c ratios and microstructures. It is found that the developed model can successfully reproduce experimentally observed behaviors and be applied to explain the experimental results in detail. With the method presented in this paper, the relationship between the volume fractions of different components and the global creep behavior of cement paste can be established. The validation of the model performed at the microscale forms a basis for the multiscale analysis of concrete creep. ...
Since self-healing of cementitious materials can theoretically improve the service-life of concrete structures, it has gathered significant attention from both researchers and industry during the last two decades. Many researchers have proposed different methods to assess and quantify the self-healing capacity (i.e. the ability of cementitious materials to heal cracks) that is generated in concrete autogenously as well as autonomously. Even though many methodologies can be found in the literature, a way to accurately quantify the healing products produced by any self-healing mechanism has not been yet achieved. In this study, a methodology is proposed to observe and to quantify in-time formation of healing products based on active thin sections. Thin sections of Portland cement paste have been prepared with no epoxy impregnation to facilitate reactions between the cement matrix and the surrounding environment. Artificial cracks (260 μm wide) were induced at 28 days of age and the crystal growth was continuously monitored up to 28 days of self-healing. Through image analysis of the micrographs, it was calculated that the autogenous self-healing capacity of paste (triggered by portlandite carbonation in uncontrolled indoor conditions) was around 55% after 28 days of self-healing. Healing products were further characterised through Environmental Scanning Electron Microscope analysis. Based on the results obtained in this study, the proposed methodology seems to be promising to compare the self-healing mechanisms triggered by different healing agents. ...
Journal article (2020) - Stefan Chaves Figueiredo, Claudia Romero Rodríguez, Zeeshan Y. Ahmed, Derk H. Bos, Yading Xu, Theo M. Salet, Oguzhan Çopuroglu, Erik Schlangen, Freek P. Bos
Extrusion based additive manufacturing of cementitious materials has demonstrated strong potential to become widely used in the construction industry. However, the use of this technique in practice is conditioned by a feasible solution to implement reinforcement in such automated process. One of the most successful ductile materials in civil engineering, strain hardening cementitious composites (SHCC) have a high potential to be employed for three-dimensional printing. The match between the tailored brittle matrix and ductility of the fibres enables these composites to develop multiple cracks when loaded under tension. Using previously developed mixtures, this study investigates the physical and mechanical performance of printed SHCC. The anisotropic behavior of the materials is explored by means of mechanical tests in several directions and micro computed tomography tests. The results demonstrated a composite showing strain hardening behavior in two directions explained by the fibre orientation found in the printed elements. Moreover, the printing technique used also has guaranteed an enhanced bond in between the printed layers. ...
This study aims to investigate the influences of different grades of calcined clay on 3D printability, compressive strength (7 days), and hydration of limestone and calcined clay-based cementitious materials. Calcined clays that contained various amounts of metakaolin were achieved by blending low-grade calcined clay (LGCC) and high-grade calcined clay (HGCC) in three different proportions. The results revealed that increasing the HGCC% ranging from 0 wt% to 50 wt% in calcined clay could: (1) increase the flow consistency; (2) impressively improve the buildability, and reduce the printability window of the fresh mixtures; (3) enhance and accelerate the cement hydration. The reduction of mean interparticle distance induced by increasing HGCC% may be the primary reason for the enhancement of buildability and very early-age hydration. However, increasing HGCC% led to an increase of air void content in the interface region of the printed sample, which weakened the compressive strength of the printed sample at 7 days. Besides, it confirmed that the cold-joint/weak interface was easily formed by using the fresh mixture with a high structuration rate. ...
Book chapter (2020) - Claudia Romero Rodriguez, Maxim Deprez, Fernando F. de Mendonca Filho, Stefanie van Offenwert, Veerle Cnudde, Erik Schlangen, Branko Šavija
Superabsorbent Polymers (SAP) have been recently subject of investigation as smart admixtures for cement-based materials. The properties of these polymers enable their use for internal curing, increasing freeze/thaw resistance, boosting autogenous self-healing and providing a crack self-sealing effect in cementitious composites. Except for the earliest application, the functioning of these beneficial effects invloves the absorption by the polymers of ingress water in the hardened cementitious matrix and later release, as well as their capacity to complete multiple absorption/desorption cycles. In this work, the absorption of water in mortar with superabsorbent polymers is monitored during the first 60 min of absorption through micro-CT. The experimental series included the presence of cracks. The registration and differentiation of sub-minute (18 s) scans enabled the individuation of bulk water content distribution in the mortar with a resolution of 55 μm. The swollen volume of SAP could also be quantified and studied in time. The results point out that although embedded SAP absorb water from the matrix, this absorption is slow and reduced with respect to water absorption during mixing for the used SAP. Same effect is observed for SAP in the cracks. ...
Journal article (2020) - Ding Siang Ng, Suvash Chandra Paul, Vivi Anggraini, Sih Ying Kong, Tanvir Shams Qureshi, Claudia Romero Rodriguez, Qing feng Liu, Branko Šavija
This study explores the effects of different types of nanoparticles, namely nano-SiO2 (NS), nano-TiO2 (NT), and nano-Fe2O3 (NF) on the fresh properties, mechanical properties, and microstructure of cement mortar containing fly ash as a supplementary cementitious material. These nanoparticles existed in powder form and were incorporated into the mortar at the dosages of 1%, 3%, and 5% wt.% of cement. Also, fly ash has been added into in mortars with a constant dosage of 30% wt.% of cement. Compressive and flexural strength tests were performed to evaluate the mechanical properties of the mortar specimens with different nanoparticles at three curing ages, 7, 14, and 28 days. Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) tests were conducted to study the microstructure and the hydration products of the mortars. To elucidate the effects of nanoparticles on the binder phase, additional experiments were performed on accompanying cement pastes: nanoindentation and open porosity measurements. The study shows that, if added in appropriate amounts, all nanoparticles investigated can result in significantly improved mechanical properties compared to the reference materials. However, exceeding of the optimal concentration results in clustering of the nanoparticles and reduces the mechanical properties of the composites, which is accompanied with increasing the porosity. This study provides guidelines for further improvement of concretes with blended cements through use of nanoparticles. ...
Carbonation of hydrated cement paste (HCP) causes numerous chemo-mechanical changes in the microstructure, e.g., porosity, strength, elastic modulus, and permeability, which have a significant influence on the durability of concrete structures. Due to its complexity, much is still not understood about the process of carbonation of HCP. The current study aims to reveal the changes in porosity and micromechanical properties caused by carbonation using micro-beam specimens with a cross-section of 500 μm x 500 μm. X-ray computed tomography and micro-beam bending tests were performed on both noncarbonated and carbonated HCP micro-beams for porosity characterization and micromechanical property measurements, respectively. The experimental results show that the carbonation decreases the total porosity and increases micromechanical properties of the HCP micro-beams under the accelerated carbonation. The correlation study revealed that both the flexural strength and elastic modulus increase linearly with decreasing porosity. ...
Recent studies have shown that concrete containing Phase Change Materials (PCM) with low transition temperatures may reduce the number of freeze/thaw cycles suffered by the cementitious composite in temperate climates. Nevertheless, the positive influence of such admixtures on the frost resistance of cement-based materials has not been directly shown, nor the negative. In this study, mortars with different contents of microencapsulated PCM by volume of cement paste were studied with regard to the progression of their internal and salt scaling damages during freeze/thaw cycles. X-ray micro tomography was used to monitor damage development and spatial distribution in the mortars. Furthermore, the pore system and microstructure of the PCM-modified mortars were characterized to unveil the causes of the observed macroscopic behavior during frost weathering. The results show that limited amounts of PCM in mortar, namely 10% by volume of cement paste, results beneficial for the frost and scaling resistance of the composite. Whereas, for larger PCM additions, like 30% by volume of paste, the changes in microstructure, porosity and mechanical strength brought in by these admixtures resulted in worsened performance against freeze/thawing cycles. ...
For a single batch material, time intervals and nozzle standoff distances between two subsequent layers are two critical printing parameters that influence the mechanical performance of the printed concrete. This paper presents an experimental and numerical study to investigate the impacts of these printing parameters on the interlayer bond strength of the 3D printed limestone and calcined clay-based cementitious materials. All samples were manufactured by a lab-scale 3D printer equipped with a hybrid back- and down-flow nozzle (rectangular opening). The uniaxial tensile test was employed to quantify the interface adhesion of printed specimens. Moreover, the greyscale value image of microstructure, as well as the air void content and distribution of the printed specimens were acquired by X-ray computed tomography and characterized by image analysis. The experimental results showed that extending the time interval between construction of two layers could decrease the bond strength, whereas only increasing the nozzle standoff distance exhibited limited effects on that. The weak bond strength could be attributed to the high local porosity at the interface of the specimen. Additionally, numerical simulations of the uniaxial tensile test were conducted using a 2D lattice fracture model, which can predict the bond strength of printed specimens for different void content in the interface layer. ...
Journal article (2020) - C. Romero Rodriguez, F. França de Mendonça Filho, L. Mercuri, Y. Gan, E. Rossi, G. Anglani, P. Antonaci, E. Schlangen, B. Šavija
In this study, the interface between different types of bacteria-embedded self-healing polylactic acid capsules (PLA) and cement paste is investigated. Particularly, the changes in microstructure and mechanical properties of the interface with respect to bulk cement paste were studied. First, nanoindentation was performed to obtain maps of hardness and elastic modulus in the interfaces. Lattice modeling of uniaxial tensile test on the mapped locations was performed then to obtain the overall tensile strength and stiffness of the interface. Moreover, hydrates assemblage and chemical composition around the PLA particles were studied through Backscattering Electron images and Energy Dispersive X-ray Spectroscopy. The ratios between resulting tensile strength and elastic modulus of the interface with respect to bulk paste were obtained for each PLA type. The results suggest that PLA can be tailored to optimize the physico-mechanical properties of the interface and hence, the mechanical behavior and triggering efficiency of the self-healing system. ...
Journal article (2019) - Freek Bos, Zeeshan Y. Ahmed, Claudia Romero Rodriguez, Stefan Chaves Figueiredo
Recent years have seen a rapid growth of additive manufacturing methods for concrete construction. Potential advantages include reduced material use and cost, reduced labor, mass customization and CO2 footprint reduction. None of these methods, however, has yet been able to produce additively manufactured concrete with material properties suitable for structural applications, i.e. ductility and (flexural) tensile strength. In order to make additive manufacturing viable as a production method for structural concrete, a quality leap had to be made. In the project ‘3D Concrete Printing for Structural Applications’, 3 concepts have been explored to achieve the required structural performance: applying steel fiber reinforcement to an existing printable concrete mortar, developing a strain-hardening cementitious composite based on PVA fibers, and embedding high strength steel cable as reinforcement in the concrete filament. Whereas the former produced only an increase in flexural tensile strength, but limited post-peak resistance, the latter two provided promising strain hardening behavior, thus opening the road to a wide range of structural applications of 3D printed concrete. ...
Journal article (2019) - C. Romero Rodríguez, S. Chaves Figueiredo, M. Deprez, D. Snoeck, E. Schlangen, B. Šavija
Recently the concept of crack self-sealing has been investigated as a method to prevent degradation and/or loss of functionality of cracked concrete elements. To obtain self-sealing effect in the crack, water swelling admixtures such as superabsorbent polymers (SAP) are added into the cementitious mix. In order to design such self-sealing systems in an efficient way, a three-dimensional mesoscale numerical model is proposed to simulate capillary absorption of water in sound and cracked cement-based materials containing SAP. The numerical results yield the moisture content distribution in cracked and sound domain, as well as the absorption and swelling of SAP embedded in the matrix and in the crack. The performance of the model was validated by using experimental data from the literature, as well as experimentally-informed input parameters. The validated model was then used to investigate the role of SAP properties and dosage in cementitious mixtures, on the water penetration into the material from cracks. Furthermore different crack widths were considered in the simulations. The model shows good agreement with experimental results. From the numerical investigation guidelines are suggested for the design of the studied composites. ...
Conference paper (2019) - L. Mercuri, Claudia Romero Rodriguez, Yading Xu, Stefan Chaves Figueiredo, Renee Mors, Emanuele Rossi, G. Anglani, P. Antonaci, Branko Šavija, E. Schlangen
Soft inclusions, such as capsules and other particulate admixtures are increasingly being used in cementitious materials for functional purposes (i.e. self-healing and self-sensing of concrete). Yet, their influence on the fracture behaviour of the material is sometimes overlooked and requires in-depth study for the optimization of mechanical and/or smart properties. An experimental investigation is presented herein on the role of bacteria-based lactate-derived particles on the fracture behaviour of cement paste in tensile configuration. These admixtures are currently used for the purpose of self-healing. Digital Image Correlation was used to obtain strain contours on the surface of the samples during the test. The influence of soft particles addition and age of the samples on the fracture mechanics of the composite were investigated. ...