This paper aims to improve the activity of high-calcium fly ash (FA) by using a wet carbonation treatment process. The results indicated that carbonation products, i.e. calcite, were attached to the surface of FA, which accelerated cement hydration primarily at the early stage. Significant improvement of early age strength and a decrease in setting time were therefore found in blended cement. Additionally, carbonation significantly reduced the amount of free calcium oxide (f-CaO) in FA, increasing its volume stability. Krstulovic-Dabic model was used to simulate the hydration process of blended paste, and the distribution of pore sizes and hydration products were also measured. Together with the filler effect of nano-sized calcite, the formation of carboaluminate phases refined the pore structure of blended paste. Furthermore, the amounts and mechanical properties of outer hydration products in blended paste increased.

The classically lattice model assumes the local elements behave elastic brittle, neglecting the ductility of the mortar matrix. This leads to the simulated load⁃displacement response more brittle than the realistic. To solve the aforementioned issue, a piece⁃wise approach was introduced to describe the elastic⁃plastic constitutive relation of lattice element. The fracture process and the load⁃displacement response were obtained through the sequentially⁃linear solution approach. The model was calibrated using the uniaxial tension and compression tests. It is found that the model can precisely simulate the fracture process and load⁃displacement response. Moreover, the model was used to model the size effect in uniaxial tension and the influence of the specimen’s slenderness and boundary confinement on the fracture behavior under compression. It offers a new theoretical method and approach for studying the fracture of concrete.

Considering the application scenarios of rubber granules from waste tires in the bitumen modification process (wet or dry process), both aerobic and anaerobic aging of rubber may occur. The current study aims to investigate the thermal aging behavior of waste tire rubber samples using nanoindentation and environment scanning electron microscopy (ESEM) tests. Both aerobic and anaerobic aging tests with different durations were conducted on rubber samples. The complex moduli of aged rubber samples were measured by nanoindentation tests. The surface morphology and elemental composition of aged samples were obtained by ESEM tests together with the energy dispersive X-ray analysis. Results have shown that for both aerobic and anaerobic aging, the equilibrium modulus derived from the complex modulus curve first increases and then decreases with aging time. However, the time needed for the aerobically aged sample to reach the maximum equilibrium modulus is shorter than the anaerobic case. Aging results in crack propagation and an increase of sulfur content on the rubber surface until it reaches the peak. The degree of crosslinking reflected by sulfur content for anaerobic aging is higher than aerobic aging. The morphological change and elemental change of rubber correlate well with the change of mechanical properties. The aging of rubber from the waste truck tire at 180°C can generally be separated into two stages: crosslinking dominant stage and chain scission dominant stage.

Properties of concrete are, to a large extent, dependent on the properties of its binding constituent, hydrated cement paste. Therefore, knowledge of properties of hydrated cement paste is crucial for predicting concrete behaviour. This paper presents an experimentally informed approach for modelling elastic and transport properties of cement paste. The models used realistic microstructural information-obtained by X-ray computed tomography-as input for property determination. The properties were then determined using discrete numerical models, namely, models based on a lattice approach. Modelling results were compared with literature data, showing excellent correlations. Furthermore, dependence of properties of cement paste on the total porosity, based on the modelling results, was explored. Finally, a correlation between elastic and transport properties for the explored range of Portland cement pastes was established. It is seen that the models can be used for property prediction, but also for exploring correlations between different parameters.

Cementitious materials are widely used in construction. For their low ductility, they typically need to be reinforced by steel rebars, which cause potential corrosion problems. Polymeric reinforcement, which does not have corrosion problems, has been used to replace steel rebars. However, a relatively high reinforcing ratio is usually required for the cementitious composites reinforced by conventional polymeric reinforcement. Owing to the customizability of 3D printing technology, polymeric reinforcement with a functionally graded structure is able to be manufactured, which significantly reduces the reinforcing ratio of the reinforced cementitious composites meanwhile improves their mechanical properties. In this present study, 3D printed polymeric octet lattice structures were used as reinforcement to develop cementitious composites with enhanced ductility. Four-point bending experiments were performed on the plain mortar, and the reinforced specimens and a finite element model was used to simulate the experiments numerically. A good agreement between experiments and simulations was found: the reinforced specimens have a significantly increased flexural ductility comparing to plain mortar. Composites reinforced by vertically functionally graded lattice structures have a significantly lower reinforcing ratio while exhibiting obviously higher normalized ductility. In addition, the fracture behavior of the reinforced cementitious composites was evaluated using a fracture energy based analytical model. The analysis shows that, from the perspective of fracture energy release, the steady state cracking criteria were not satisfied by the cementitious composites developed in this study so that multiple cracking and strain hardening behavior was not obtained. However, according to numerical predictions, increasing strength of the printed reinforcement material by 40% would allow these behaviors to be potentially achieved. This work shows that additive manufacturing has great potential for developing reinforcement for cementitious materials to reduce the reinforcing ratio and enhance ductility.

The investigation of new compositions is crucial for the expansion of possible applications of glass, from the typical applications for building engineering, in the form of cast blocks or float glass, to more advanced technologies, such as 3D-printed glass or glass-to-metal connections. Since high melting temperatures and brittleness are two important drawbacks of glass, this work aims to improve both properties. Characterisation techniques, such as thermal analysis, nano-indentation, and UV/VIS spectroscopy, are used to evaluate the properties of the samples. The modification of the properties is achieved via changes in the composition of the glass, using compounds such as phosphorus pentoxide, aluminium oxide and boron oxide. Then, the choice of different glass formers and modifiers contributes to the development of compositions with lower melting and glass transition temperatures. The reduction of the melting temperature allows a saving of energy during the manufacturing. The structures of the glasses differ from the standard soda–lime–silica and borosilicate glasses, leading to a different mechanical behaviour. Furthermore, these new compositions incorporate up to 35% of fly ash in their formulas. The valorisation of these by-products reduces costs and gas emission.

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.

This paper presents a validation process of the developed multi-scale modelling scheme on mortar composites. Special attention was paid to make the material structure of real and virtual mortar specimens comparable at the meso-scale. The input mechanical parameters of cement paste (both bulk cement paste and interfacial transition zone) at the meso-scale were derived from results of micromechanical modelling through a volume averaging approach. Two constitutive relations for local elements were assumed and tested. By comparing with the experiments, the model using linear-elastic constitutive relation showed to be capable to reproduce the experimental load-displacement response satisfactorily in terms of the elastic stage and peak load. However, in the non-elastic stage a more realistic load-displacement curve can be simulated by considering the softening of cement paste using a step-wise approach. More importantly, the proposed multi-scale modelling scheme is validated by the experimental measurements. The proposed development offers the opportunity for the meso-scale model to become fully predictive.

Application of micromechanical modelling of hydrated cement paste (HCP) gains more and more interests in the field of cementitious materials. One of the most promising approaches is the use of so-called microstructure informed micromechanical models, which provides a direct link between microstructure and mechanical properties. In order to properly model the micromechanical properties of HCP, advanced mechanical models, well-characterised microstructures and proper input parameters are required. However, due to the complex material structure of HCP, this is not an easy to achieve for any of the three aforementioned aspects. Therefore, this paper aims at reviewing of the techniques that have been developed to contribute to the micromechanical modelling. Basic principles, corresponding research results, recent advances and limitations are given. It is expected that this review can help researchers make reasonable choices on techniques for the micromechanical modelling of cementitious materials.

This work aims to understand deformation and fracture processes in blast furnace slag cement pastes made using CEM III/B which is commonly used in the Dutch infrastructure sector. First, based on our previous work on Portland cement pastes, a micromechanical model utilizing nanoindentation and X-ray computed tomography (CT) for input is created. Statistical analysis are carried out and shows that grayscale values from X-ray CT scans of slag pastes can be linearly correlated with nanoindentation measurements of elastic modulus. Simulations of uniaxial tension are then performed for varying w/c ratios using the Delft lattice model and microstructure obtained from X-ray CT. In addition, advanced micromechanical experiments for estimating the micro-scale tensile strength and elastic modulus are performed. Experimental and simulation results are then critically discussed and compared. It shows that simulation results match the measured tensile strength quite well although some discrepancy does exist at lower w/c ratios. In addition, the observations are compared to our previous findings on ordinary Portland cement pastes. It is found that tensile strength and elastic moduli of slag pastes at 28 days are higher than those of Portland cement pastes with the same w/c ratio. This study will form a basis for micromechanical testing and modelling of blended cement paste systems in the future.

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.

Auxetic behavior refers to material with negative Poisson's ratio. In this research, a new type of cementitious auxetic material is developed. A novel crack bridging auxetic mechanism is discovered which is in contrast with a local buckling mechanism commonly employed to trigger auxetic behavior. Taking advantage of 3D printing techniques, cementitious cellular composite (CCC) specimens with auxetic cellular structures were produced. Meanwhile, cementitious materials with different fiber content were used as constituent material. Uniaxial compression and cyclic loading tests were performed on the CCCs. Experiments show that with proper constituent material, CCCs can exhibit auxetic behavior which is induced by crack bridging process of the cementitious constituent material. In addition, strain hardening behavior can be identified in the stress-strain curve under uniaxial compression and consequently high specific energy absorption is obtained. Furthermore, 2.5% of reversible deformation which is significantly higher than conventional cementitious materials under cyclic loading is obtained within 25,000 cycles. Obvious fatigue damage is observed in the first 3000 cycles, afterwards signs of mechanical properties recovering can be found. The discovered auxetic mechanism indicates a new designing direction for brittle materials to achieve auxetic behaviors.

This work proposes a method for numerically investigating the fracture mechanism of cement paste at the microscale based on X-ray computed tomography and nanoindentation. For this purpose, greyscale level based digital microstructure was generated by X-ray microcomputed tomography with a resolution of 2 μm/voxel length. In addition, statistics based micromechanical properties (i.e. Young's modulus and hardness) were derived from the grid nanoindentation test which was set to have an interaction volume the same as the resolution of the digital microstructure. A linear relationship between the two probability density functions of greyscale level and local Young's modulus was assumed and verified by the two-sample Kolmogorov-Smirnov (K–S) statistic. Based on this assumption, the fracture and deformation of a digital cubic volume with a dimension of 100 μm under uniaxial tension was simulated using a lattice fracture model. In addition, the influence of heterogeneity on fracture response was studied. Furthermore, the proposed method was compared with the results obtained from a traditional approach used previously by the authors in which discrete phases (capillary pore, anhydrous cement clinker, outer and inner hydration products) were considered. The two methods show similar crack patterns and stress-strain responses. The proposed method is regarded more promising as it captures also the gradient of material properties (within the discrete phases) in the cement paste.

A method is presented to model deformation and fracture behavior of 3D printed disordered lattice materials under uniaxial tensile load. A lattice model was used to predict crack pattern and load-displacement response of the printed lattice materials. To include the influence of typical layered structures of 3D printed materials in the simulation, two types of printed elements were considered: horizontally and vertically printed elements. Strengths of these elements were measured: 3 mm cubic units consist of lattice elements with two printing directions were printed and their strengths were tested in uniaxial tension. Afterwards, the measured element strengths and bulk material strength, respectively, were used as model input. Uniaxial tensile tests were also performed on the printed lattice materials to obtain their crack pattern and load-displacement curves. Simulations and experimental results were comparatively analyzed. For both levels of disorder considered, only when measured strengths were assigned to the elements with identical printing direction, are the predicted crack patterns and load-displacement curves in agreement with experimental results. The results emphasize the importance of considering printing direction when simulating mechanical performance of 3D printed structures. The influence of disorder on lattice material mechanical properties was discussed based on the experiments and simulations.

One of the major problems with the bone implant surfaces after surgery is the competition of host and bacterial cells to adhere to the implant surfaces. To keep the implants safe against implant-associated infections, the implant surface may be decorated with bactericidal nanostructures. Therefore, fabrication of nanostructures on biomaterials is of growing interest. Here, we systematically studied the effects of different processing parameters of inductively coupled plasma reactive ion etching (ICP RIE) on the Ti nanostructures. The resultant Ti surfaces were characterized by using scanning electron microscopy and contact angle measurements. The specimens etched using different chamber pressures were chosen for measurement of the mechanical properties using nanoindentation. The etched surfaces revealed various morphologies, from flat porous structures to relatively rough surfaces consisting of nanopillars with diameters between 26.4 ± 7.0 nm and 76.0 ± 24.4 nm and lengths between 0.5 ± 0.1 μm and 5.2 ± 0.3 μm. The wettability of the surfaces widely varied in the entire range of hydrophilicity. The structures obtained at higher chamber pressure showed enhanced mechanical properties. The bactericidal behavior of selected surfaces was assessed against Staphylococcus aureus and Escherichia coli bacteria while their cytocompatibility was evaluated with murine preosteoblasts. The findings indicated the potential of such ICP RIE Ti structures to incorporate both bactericidal and osteogenic activity, and pointed out that optimization of the process conditions is essential to maximize these biofunctionalities.

The aim of this work is to investigate the mechanical performance of hardened cement paste (HCP) under compression at the micrometre length scale. In order to achieve this, both experimental and numerical approaches were applied. In the experimental part, micrometre sized HCP specimens were fabricated and subjected to uniaxial compression by a flat end tip using nanoindenter. During the test, the load-displacement curves can be obtained. In the modelling part, virtual micrometre sized specimens were created from digital material structures obtained by X-ray computed tomography. A computational compression test was then performed on these virtual specimens by a discrete lattice fracture model using the local mechanical properties calibrated in the authors' previous work. A good agreement is found between the experimental and numerical results. The approach proposed in this work forms a general framework for testing and modelling the compression behaviour of cementitious material at the micrometre length scale.

The aim of this work is to predict the micromechanical properties of interfacial transition zone (ITZ) by combining experimental and numerical approaches. In the experimental part, hardened cement paste (HCP) cantilevers (200 μm × 100 μm × 100 μm) attached to a quartzite aggregate were fabricated and tested using micro-dicing saw and nanoindenter, respectively. In the modelling, comparable digital specimens were produced by the X-ray computed tomography (XCT) and tested by a discrete lattice model. The fracture model was calibrated by the experimental load-displacement curves and can reproduce the experimental observations well. In the end, the calibrated model was used to predict the mechanical behaviour of ITZ under uniaxial tension, which can be further used as input for the multi-scale analysis of concrete.

This work aims to investigate the mechanical properties of the cement paste-aggregate interface by combining experimental and numerical approaches. The multi-phase interface microstructure was obtained by X-ray computed tomography (XCT) and submitted to a discrete fracture lattice model for fracture analysis. Apart from the modelling, a benchmark test at the micro-scale has been conducted for the purpose of calibration. With the approach proposed in this work, a framework to model and test the micromechanical properties of the cement paste-aggregate interface at the microscale has been formed.

The aim of this work is to investigate the fracture process of concrete under various boundary conditions. Although numerous concrete fracture tests have been reported, showing the failure behavior of concrete, their evaluation is ambiguous due to the limitations of specimen size and experimental conditions. Therefore, it is necessary to use simulation models to better understand the fracture process. This is done herein by using a three-dimensional lattice model to simulate the failure behavior of concrete under different loading conditions ranging from uniaxial compression, tension, splitting, three point bending to shear by using a single set of input parameter. In addition, several influence factors including boundary condition and slenderness are also taken into consideration to give more detailed information about the fracture process of concrete.

Nanoindentation is usually used to investigate local elastic properties and hardness of materials. In this paper, the nanoindenter served as a loading tool to perform micro scale bending tests and measure the global response of micro-scale specimens. For testing, cement paste cantilever beams with a square cross-section of 300 μm × 300 μm were fabricated using a micro dicing saw. Monotonic, cyclic and sustained loading bending tests were conducted on the beams using the nanoindenter. The load-deflection behaviours of micro-cantilever beams subjected to various loading conditions are presented in this paper. The interpretation of experimental results regarding the measured deflection of beam is discussed. With this micro-scale test method, the fracture strength as well as time-dependent responses of cement paste at the micrometre level can be assessed in a straightforward manner.