Comportement au jeune âge et différé d'un BFUP écrouissant sous les effets thermomécaniques

This thesis is dedicated to study the early age behavior and time dependant as well as the thermo-mechanical response under restraint of a hardening Ultra High Performance Fiber Reinforced Concrete (UHPFRC). The knowledge of the UHPFRC behavior is indispensable to estimate the cracking risk in composites structures. The phenomena which develop during the hydration progress of the material as the capillary network development and the physico-mechanical properties were considered. The effect of temperature curing conditions on these phenomena was characterized. The test and predicted (issue from modeling and numerical simulations) results are presented and discussed in this report. The tested UHPFRC is characterized by high mechanical performances with a faster evolution of the Young modulus with regard to the other properties. The measured mechanical properties can be predicted very well with the CEB-FIB model. The tested UHPFRC is characterized by a low degree of hydration due to the low water-binder (w/b) ratio. This experimental result was confirmed by a numerical estimation by means of the adapted Powers and Waller models as well as a numerical estimation through the heat realized during the hydration process. A linear relationship between the mechanical performances and the degree of hydration was shown and the action of the microstructure evolution on the mechanical performances development was elucidated. It was attributed to the beneficial effect of the unhydrated particles of silica fume and cement because of the pore size refinement in the microstructure. Besides, the current UHPFRC is characterized by a fast autogenous shrinkage kinetics related to the dominant self-desiccation during the first days of the hydration. Thanks to a numerical estimation with Laplace and Kelvin laws, self desiccation measurement under various temperatures were used to distinguish and to put in evidence the effect of the temperature on the porous structure, the capillary pressures and consequently on the contraction of the solid matrix. The contribution and the beneficial effect of fibres towards the autogenous shrinkage were also showed. In fact, fibres act as internal restraint and can prevent the free matrix deformation. The high temperatures improve widely the rate of hydration at early age (7 days) and so lead to increase initially the autogenous shrinkage. In the long term, an inverse effect of the temperature was observed on the evolution of the degree of hydration and the measured physico-mechanical properties, which was attributed to the influence of the temperature on the ions haste and distribution during the hydration process. The influence of the temperature on the degree of hydration and the compressive strength was characterized and modeled and the corresponding parameters were used to estimate the energy of activation of the studied UHPFRC. The dominant role of the autogenous shrinkage at early age was clarified and the associated stresses, which develop at the early age under total restraint, were quantified by means of the TSTM. These stresses remain moderate. The UHPFRC creep potential is important. UHPFRC exhibits high creep. This was attributed to the high volume of paste (88 %), which is subjected to creep. Existing models in the literature were used; certain models predict the UHPFRC behavior in a satisfactory way and with a certain precision. One notes that the early age stress predictions are dependent on the software used and especially on the creep model. In our case, the generalized Maxwell model was used.

Autogenous Shrinkage and Hydration Kinetics of SH-UHPFRC under Moderate to Low Temperature Curing Conditions

Mohammadhadi Kazemi Kamyab

Strain Hardening Ultra High Performance Fiber Reinforced Concrete (SH-UHPFRC) were used successfully over the last 8 years in numerous cast in place rehabilitation applications as long lasting waterproofing layers (20 to 30 mm thickness) and, combined with rebar, to increase the structural load bearing capacity of existing bridge decks or building slabs (50 to 70 mm thickness). In composite applications on reinforced concrete substrates, SH-UHPFRC provide a deformation capability (strain hardening) larger than their free shrinkage which makes localized macro cracking at service state very unlikely. On the other hand some specific conditions of microclimatic state of the substrate (moisture and thermal conditions) and climatological (temperature and humidity) of the site such as casting at low temperatures (winter conditions) might increase the autogenous shrinkage and thus eigenstresses of the freshly cast SH-UHPFRC and hinder the development of its tensile strength or/and deformability. Combination of these specific circumstances could compromise the SH-UHPFRC protective functions due to the occurrence of localized macro cracks, making the objective of using SH-UHPFRC as a onetime intervention strategy in rehabilitation application obsolete. Advancement in hydration at early age leads to formation of partially emptied capillary spaces contributing to self-desiccation, decrease of the relative humidity and increase of the capillary depression. Since water is under depression, the solid porous material is under compression forcing the material to shrink. From the aforementioned, it can be deduced that the autogenous shrinkage is a force driven phenomenon: a force is applied on the ageing viscoelastic porous skeleton and the apparent structural response of the bulk cementitious material is the autogenous shrinkage strain. Based on the aforementioned two levels of investigation were considered in this thesis: I. Material level: ageing viscoelastic porous skeleton of hydrating cementitious material II. Structural level: autogenous shrinkage development under the action of its driving forces The objective of this thesis was to study the development of the autogenous shrinkage and its relation with the development of microstructure and mechanical properties in SH-UHPFRC cured at moderate and low temperature conditions (1 to 20°C). Focus was put on: (1) kinetics and magnitude of hydration of silica fume and cement, (2) activation energy of the processes, (3) stiffness (E modulus and Poisson ratio) development, and (4) states of water and pore development. Finally a cross link analysis of information obtained from material and structural level was carried out to better highlight the mechanisms and driving forces of autogenous shrinkage. CM22-TKK, a SH-UHPFRC developed at MCS for rehabilitation applications, on the basis of CEMTECmultiscale® fibrous mixes, was used. Silica fume is one of the major constituents of CM22-TKK (26% by mass of cement). Extent of the silica fume pozzolanic reaction significantly affects the pore size distribution of the UHPFRC matrix which then influences the development of the relative humidity, self-desiccation and finally autogenous deformation. Detailed experimental investigation performed showed that only maximum 8% by mass of cement out of 26% silica fume used in the recipe reacts in moderate and low temperature curing conditions. Finally, a model of silica-fume degree of reaction as a function of curing temperature (5 to 250 °C) was proposed on the basis of a detailed literature survey of existing works with low W/B mixes. The activation energy of the thermo-mechanical properties was evaluated for thermo (cumulative heat of hydration) and mechanical properties development (such as dynamic Elastic modulus, dynamic Poisson’s ratio and compressive strength). A single activation energy Ea of 27.4 KJ/mol could successfully model the activation of all properties. Since maturity was not a proper reference to compare the autogenous deformations at various temperatures, a more fundamental reference such as degree of hydration was used. Experimental investigation was carried out using different techniques such as isothermal calorimetry and 29Si solid NMR to evaluate the development of the degree of hydration of cement and silica fume in UHPFRC at moderate and low temperature curing conditions. The ultimate degree of hydration of cement in CM22-TKK for a closed system was 0.34. There was a close correspondence between the experimental results and the predictions of the volumetric phase distribution models of Waller (0.28) and Jensen (0.32). Finally, the De Schutter et al. 1996 model was used to describe the mechanical properties (Emodulus and Poisson ratio) as function of degree of hydration. Nondestructive and non-invasive 1H-NMR was used to evaluate volumetric phase distribution development at 20°C, especially the classification of the water types (capillary, gel and C-S-H interlayer water) which brought fully new and valuable information about the hydration kinetics and pore size development. The results were also compared with Jensen volumetric phase distribution model to check the advantages and limitation of both approaches. Finally experimental investigation was carried out to follow the development of autogenous shrinkage and eigenstresses (in case of restrained shrinkage) of CM22-TKK cured in isotherm conditions (1 to 20°C). Eigenstresses were obtained and used to highlight the effect of the viscous response of the material at the different temperatures investigated. The previously mentioned results on the kinetics of the silica fume reaction, cement hydration and evolution of states of water and development of stiffness were then put into perspective with the trends observed on the autogenous shrinkage and eigenstresses development.

EPFL2013

Processing of fibre and porosity gradients in cellular thermoplastic composites

Manuel Bühler

The aim of this study has been to develop processing techniques for novel bioresorbable thermoplastic cellular composites, reinforced with continuous inorganic fibres, for use as biodegradable scaffolds for bone tissue engineering. As the implanted composite scaffold starts to degrade, it should be progressively replaced by natural bone tissue, which should consequently support increasing proportions of the applied mechanical loads. In order to simulate natural high performance porous structures such as bone or light wood, composites with simultaneous gradients in fibre content and porosity were studied. In order to carry out investigations over wide ranges of fibre content and porosity and to ensure biocompatibility and bioresorbability, it was decided to focus on foamable poly(L-lactic acid) (PLA) and continuous glass fibres. As well as improved mechanical reinforcement due to the high aspect ratio, the use of continuous glass fibres offers the possibility of achieving higher loadings than with short fibres or particles, increasing the potential range of mechanical properties. For processing the composites, a fibre winding technique developed in house was used to prepare unidirectional preforms with gradient structures tailored at the fibre bundle level. PLA fibre bundles, containing 36 monofilaments were prepared on a spinning line, and mingled with glass fibre bundles comprising 250 or 1000 monofilaments. During the winding process, the PLA fibres were intimately mixed with the reinforcing fibres, to ensure a good impregnation during subsequent processing steps. Moreover it was possible to maintain the relative positions of the fibres during pre-consolidation of graded composites. The resulting preforms had a porosity of 25% and could be further consolidated to decrease the porosity, or foamed in an autoclave to obtain cellular composites (foams) with porosities of up to 90%. It was observed that, independently of the applied foaming conditions, the presence of continuous fibres reduced the porosity by an amount equivalent to twice the fibre volume fraction. This processing method provided composites with a simultaneous gradient in fibre content and porosity. In order to predict the Young's modulus and the collapse strength of the cellular composites a model was proposed, which combines the buckling of composite columns within a porous structure with the property predictions for neat polymer foams. In neat foams with a porosity of 60%, the Young's modulus was calculated to be 0.25 GPa. By adding a fibre volume fraction of 14% the modulus reached 1.2 GPa. The respective collapse strengths were 5 MPa and 16 MPa. Experimental results were consistent with the predictions and validated the model. The model determines the fibre content required for composites with a given porosity and stiffness. Gradient cellular composites were obtained with a range of porosity between 50% to 90% and a range of stiffness between 100 and 1500 MPa. Furthermore the processing parameters can be adjusted to maintain a desired porosity when fibres are added. Thus, composites that fulfill the mechanical requirements for bone scaffolds can be achieved in a rational manner. The long term behaviour of the foams was tested under physiological conditions. Viscoelasticity tests provided evidence for the important role of the unidirectionally oriented fibres. Whereas the cells in neat foams collapsed after at most two days when loaded at 0.69 MPa, the fibre reinforced foams resisted longer and their creep strain was well described by a power law. The fatigue properties were compared to reported values of natural trabecular bone. None of the neat foams with a porosity of 74% resisted to the first load cycle of 7.3 MPa. With a fibre volume fraction of 11% and a comparable porosity of 72%, the composite scaffolds resisted for at least 11'000 loading cycles. To compare, trabecular human bone failed after 1909 cycles, when loaded with 8.5 MPa. It was concluded that the reinforced composites have the potential to replace natural bone. Preliminary in vitro results with human foetal osteoblasts and in vivo tests on femurs of rats were promising because the cells proliferated well on the composite substrates. Further investigations for applications in bone tissue engineering can be planned. Furthermore, the studied process and the obtained results are envisaged for other material systems to prepare cellular composites for novel lightweight applications in transportation and building industry.

EPFL2008

Processing of fibre and porosity gradients in cellular thermoplastic composites

Manuel Bühler

EPFL2008

Autogenous Shrinkage and Hydration Kinetics of SH-UHPFRC under Moderate to Low Temperature Curing Conditions

Mohammadhadi Kazemi Kamyab

EPFL2013