Early-age cracking risk induced by autogenous deformation is high for cementitious materials of low water-binder ratios. The autogenous deformation, viscoelastic properties, and stress evolution are three important factors for understanding and quantifying the early-age cracking risk. This paper systematically reviewed the experimental and modelling techniques of the three factors. It is found that the Temperature Stress Testing Machine is a unified experimental method for all these three factors, with a strain-controlled mode for stress evolution, hourly-repeated loading scheme for viscoelastic properties, and free condition for autogenous deformation. Such unified method provides basis for developing various models. By coupling a hydration model for volume fractions of hydrates, a homogenization model for upscaling of viscoelastic properties, and capillary pressure theory for self-desiccation shrinkage, a unified model directly mapping the mix design to the early-age stress can be constructed, which can help optimize the mix design to reduce the early-age cracking risk.

Engineered cementitious composite (ECC) is widely employed in engineering due to its high toughness and ductility. The Interfacial Transition Zone (ITZ) between the fibers and the matrix plays a vital role in influencing the strength and durability of ECC. This study introduces a numerical method to simulate fiber pull-out behaviors, specifically the fiber debonding and slipping. A birth-death method is proposed to account for the mechanical transition from fiber debonding stage to slipping stage. The contributions of various phases in the ITZ are explicitly considered. Furthermore, nanoindentation tests and Backscattered Electron (BSE) imaging were conducted to determine the microstructures of ITZ and local mechanical properties of each phase within the ITZ. A series of fiber pullout experiments with polyvinyl alcohol (PVA) fibers were conducted to calibrate and validate the model. Subsequently, the validated model was employed to explore the influence of w/c ratios, fiber orientations and bonding properties on the interfacial behavior. The microstructure-informed model proposed herein effectively predicts fiber pull-out behavior, facilitating a thorough exploration of fracture mechanisms throughout the pull-out process, and serves as the basis for multiscale modeling of ECC.

The article ‘Effect of matrix self-healing on the bond-slip behavior of micro steel fibers in ultra-high-performance concrete’, written by Salam Al-Obaidi, Shan He, Erik Schlangen and Liberato Ferrara, was originally published in volume 56, issue 9, article 161 without Open Access.

This study investigates the structural behaviour and self-healing performance of hybrid reinforced concrete (RC) beams, enhanced with a 1.5-cm-thick self-healing cover composed of bacteria-embedded strain hardening cementitious composite (SHCC), for its potential in crack width control and crack healing. The research focuses on the performance under both flexural and shear loading, examining aspects such as load-bearing capacity, surface crack pattern, crack propagation between layers, and healing effectiveness. Results demonstrate the successful activation of the healing function, alongside improvements in structural performance. Under flexural loading, hybrid beams exhibited greater load-bearing capacity and significantly improved crack control ability. The maximum crack width of the hybrid beams exceeded 0.3 mm at 124.7 kN load, whereas in the control beam the largest crack exceeded 0.3 mm at only 59.8 kN load. Under shear loading, while the influence of the cover on structural capacity was minimal, it notably improved post-peak ductility and energy dissipation. Interface delamination was not observed in both cases. The results of the current study demonstrate the potential of delivering the self-healing mechanism precisely where it is most needed, which presents a scalable and economically viable strategy for integrating self-healing technology into standard construction practices.

Temperature Stress Testing Machine (TSTM) is a universal testing tool for many properties relevant to early-age cracking of cementitious materials. However, the complexity of TSTMs require heavy lab work and thus hinders a more thorough parametric study on a range of cementitious materials. This study presents the development and validation of a Mini-TSTM for efficiently testing the autogenous deformation (AD), viscoelastic properties, and their combined results, the early-age stress (EAS). The setup was validated through systematic tests of EAS, AD, elastic modulus, and creep. Besides, the heating/cooling capability of the setup was examined by tests of coefficient of thermal expansion by temperature cycles. The results of EAS correspond well to that of AD, which qualitatively validates the developed setup. To quantitatively validate the setup, a classical viscoelastic model was built, based on the scenario of a 1-D uniaxial restraint test, to predict the EAS results with the tested AD, elastic modulus, and creep of the same cementitious material as the input. The predicted EAS matched the testing results of Mini-TSTM with good accuracy in 6 different cases. The viscoelastic model also provided quantitative explanations for why variations in early AD do not influence the EAS results. The testing and modelling results together validate the developed Mini-TSTM setup as an efficient tool for studying early-age cracking of cementitious materials. At the end, the potential limitations of the Mini-TSTM are discussed and its applicability for concrete with aggregate size up to 22 mm is demonstrated.

This paper presents a state-of-the-art review on the application of additive manufacturing (AM) in self-healing cementitious materials. AM has been utilized in self-healing cementitious materials in three ways: (1) concrete with 3D-printed capsules/vasculatures; (2) 3D concrete printing (3DCP) with fibers or supplementary cementitious materials (SCMs); and (3) a combination of (1) and (2). 3D-printed capsules/vascular systems are the most extensively investigated, which are capable of housing larger volumes of healing agents. However, due to the dimension restraints of printers, most of the printed vasculatures/capsules are in small scale, making them difficult for upscaling. Meanwhile, 3DCP shows great potential to lower the environmental footprint of concrete construction. Incorporation of fibers and SCMs helps improve the autogenous healing performance of 3DCP. Besides, 3D-printed concrete with hollow channels as the vasculature could further improve the autonomous healing and scalability of self-healing cementitious materials. Finally, possible directions for future research are discussed.

This paper describes the development of a discrete lattice model for simulating structures formed from self-healing cementitious materials. In particular, a new approach is presented for simulating time dependent mechanical healing in lattice elements. The proposed formulation is designed to simulate the transient damage and healing behaviour of structures under a range of loading conditions. In addition, multiple and overlapping damage and healing events are considered. An illustrative example demonstrates the effects of varying the healing agent curing parameters on the computed mechanical response. The model is successfully validated using published experimental data from two series of tests on structural elements with an embedded autonomic self-healing system. The meso-scale model gives detailed information on the size and disposition of cracking and healing zones throughout an analysis time history. The model also provides an accurate means of determining the volume of healing agent required to achieve healing for all locations within a structural element. The importance of the information provided by the model for the design of self-healing cementitious material elements is highlighted.

The current study investigates short-term and long-term crack-healing behaviour of mortars embedded with bacteria-based poly-lactic acid (PLA) capsules under both ideal and realistic environmental conditions. Two sets of specimens were prepared and subjected to different healing regimes, with the first set kept in a mist room for varying short durations (i.e., 1 week, 2 weeks, 3 weeks and 8 weeks) and the second set placed in an unsheltered outdoor environment for a long-term healing process (i.e., 1 year). Alteration of microstructure because of self-healing was characterized by backscattered electron (BSE) imaging and energy dispersive X-ray spectroscopy (EDS) via crack cross-sections. Results show that visible crack healing enabled by bacteria began after 2 weeks in a humid environment. The healing products initially precipitated at crack mouths and gradually moved deeper into cracks, with the precipitated calcium carbonate crystals growing larger over time. After 8 weeks, healing products can be found even a few millimetres deep inside cracks. Observations of crack healing in a realistic environment revealed significant differences compared to healing under controlled conditions. While no healing products can be found at crack mouths, a substantial healing process was observed throughout the entire crack depth. It is likely that the environmental actions such as rainfall and/or freeze and thaw cycles may have worn away the healing products at crack mouths and thus led to a deeper ingress of oxygen into cracks, which promoted the activation of healing agents and associated calcium carbonate precipitation deep inside a crack.

This study investigates the bond-slip behavior of micro steel fibers embedded into an Ultra-High-Performance Concrete (UHPC) matrix as affected by the self-healing of the same matrix in different exposure conditions. The UHPC matrix contains a crystalline admixture as a promoter of the autogenous self-healing specially added to enhance the durability in the cracked state. For the aforesaid purpose, some samples were partially pre-damaged with controlled preload (fiber pre-slip at different levels) and subjected to one-month exposure in 3.5% NaCl aqueous solution and in tap water to study the fiber corrosion, if any, and the effects of self-healing; after that, they were subjected to a pull-out test, to be compared with the behavior of analogous non-pre-slipped samples undergoing the same curing history. Moreover, some samples were cured in the chloride solution, intended to simulate a marine environment, to study the effect of marine curing on the pull-out behavior of steel fiber. The steel fiber corrosion and self-healing products attached to the surface of the steel fiber were analyzed via Scanning Electron Microscopy (SEM), and Energy -Dispersive Spectroscopy (EDS). The results indicate that the newly healed particles formed on the highly damaged fiber-matrix interface significantly enhance the friction phase of the bond-slip behavior and result in a significant residual capacity compared to non-pre-slipped specimens. On the other hand, the self-healing effect in specimens subjected to low damage pre-slip contributed more to the chemical adhesion region of the bond-slip behavior. Owning to the dense microstructure of the matrix, curing in 3.5% NaCl aqueous solution was not found to significantly affect the pull-out resistance as compared to the samples cured in tap water.

The properties of the interfacial transition zone (ITZ) between microfiber and cement-based matrix are of primary significance for the overall behavior of strain hardening cementitious composites (SHCCs). However, due to the relatively small diameter of polymeric microfibers (e.g., PVA fiber), it is technically difficult to obtain quantitative and representative information of the properties of the ITZ. In the current study, a new method that is able to quantitatively characterize the microstructural features of the ITZ surrounding a well-aligned microfiber was reported. With the method, the porosity gradients within the ITZs between PVA fiber and cement paste matrices with different water to cement (w/c) ratios were determined. The results show that the matrix surrounding a microfiber were more porous than the bulk matrix. The thickness of this porous region can extend up to 100 microns away from the fiber surface even at a relatively low water to cement ratio (w/c = 0.3). It is thus believed that the method could facilitate the investigation and modification of fiber/matrix bond properties and also contribute to the development of SHCC with superior properties.

In the current study, experiments and numerical simulations were carried out to investigate the cracking behavior of reinforced concrete beams consisting of a very thin layer (i.e., 1 cm in thickness) of SHCC in the concrete cover, tension zone. A novel type of SHCC/concrete interface that features a weakened chemical adhesion but an enhanced mechanical interlock bonding was developed to facilitate the activation of SHCC. The study involved testing hybrid SHCC/concrete beams that have various types of interfaces. The results were compared to the control reinforced concrete beams that do not have SHCC in the cover. Four-point bending tests were performed with the beams and Digital Image Correlation (DIC) was utilized to track the development of crack pattern and crack width. Results show that hybrid beams possessed similar load bearing capacity but exhibited a significantly improved cracking behavior as compared to the control beam. With a 1-cm-thick layer of SHCC, the maximum crack width of the best performing hybrid beam exceeded 0.3 mm at 53.3 kN load, whereas in the control beam the largest crack exceeded 0.3 mm at 32.5 kN load. The hybrid beam with the proposed new interface formed 10 times more cracks in SHCC than the hybrid beam with a simple smooth interface and had an average crack width less than 0.1 mm throughout the loading. The lattice model has successfully showcased its ability to predict and offer valuable insights into the fracture behavior of hybrid systems. The simulation results indicate that the presence of a weak interface bond, coupled with mechanical interlocking, can effectively facilitate the activation of SHCC, resulting in the formation of more cracks and a delayed progression towards the maximum crack width. As the volume ratio of SHCC used in the hybrid beams is only 6%, the current study highlights the strategic use of minimum amount of SHCC in the critical region to efficiently enhance the performance of hybrid structures.

In 3D concrete printing, fast structuration is a prerequisite for ideal buildability. This paper aims to study the impact of inorganic additives, i.e., CaCl₂ and gypsum, on structural build-up and very early-age hydration of limestone-calcined clay-cement (LC3) pastes within the first 70–80 min. Results show that, increasing the dosage of CaCl₂ or gypsum can accelerate storage modulus G' and static yield stress evolution with time, as well as increase chemically bound water (H) content and total specific surface area (SSA_total). Furthermore, good correlations were found between G' and H content, as well as static yield stress and the ratio of free water content to SSA_total. The acceleration by CaCl₂ can be attributed to stimulating C₃S and C₃A hydration and promoting crystal formation, i.e., ettringite, portlandite, and Friedel's salt. Additionally, the increase in gypsum percentage led to a large amount of unreacted gypsum in the system, resulting in an increase in SSA_total.

The trend to 3D and heterogeneous integration enable driving multi-functional blocks in one package. Flip-chip integration is currently playing an important role and is based on solder joints. To overcome the limitations of solder joints, all-copper interconnects have been investigated to meet electrical, thermal, and reliability demands in 3D integration. The underfill process is widely applied in flip-chip encapsulation technology. We propose a novel wafer-scale all-Cu interconnect method combining epoxy-based photo-patternable polymer as self-aligned underfill layer with the patterned copper nanoparticles interconnects. The resulting test wafers were able to pattern 20 µm pitch copper nanoparticle-paste interconnects on both substrates with and without photoimageable polymer. The Cu paste was applied to form the interconnects and was sintered after bonding process. Free-standing nanocopper is sintered to obtain mechanical properties with a Young's modulus of 112 GPa. All-Cu interconnects with diameter of 50 µm and 100 µm were measured to achieve the specific contact resistance, ranging from 1.4 × 10-5O· cm2 to 1.0 × 10-5O· cm2 at different sintering temperature when epoxy-based underfill existing. And its resistivity was 4.54× 10-4 O· cm, compared to 5.86× 10-4O· cn for the all-Cu interconnects without underfill.

We propose a new numerical method to analyze the early-age creep of 3D printed segments with the consideration of stress history. The integral creep strain evaluation formula is first expressed in a summation form using superposition principle. The experimentally derived creep compliance surface is then employed to calculate the creep strain in the lattice model with a combination of stored stress history. These strains are then converted into element forces and applied to the analyzed object. The entire numerical analysis consists of a sequence of linear analyses, and the viscosity is modelled using imposed local forces. The model is based on the incremental algorithm and one of the main advantages is the straightforward implementation of stress history consideration. The creep test with incremental compressive loading is utilized to validate this model. The modelling results are in good agreement with experimental data, demonstrating the feasibility of the lattice model in early-age creep analysis under incremental compressive loading. To understand the impact of early-age creep on structural viscoelastic deformation during the printing process, additional analyses of a printed segment are carried out. These simulation results highlight the need to consider creep for accurate prediction of viscoelastic deformation during the printing process.

This paper employs computer vision techniques to predict the micromechanical properties (i.e., elastic modulus and hardness) of cement paste based on an input of Backscattered Electron (BSE) images. A dataset comprising 40,000 nanoindentation tests and 40,000 BSE micrographs was built by express nanoindentation test and Scanning Electron Microscopy (SEM). A Residual Convolutional Neural Network (Res-Net) model, which differs from a typical Convolutional Neural Network (CNN) architecture by a shortcut connection, was employed and compared with a simple table model. The models were trained, tuned, and tested over a training, validation and testing set comprising 70%, 15% and 15% of the 40,000 data pairs, respectively. The following conclusions were drawn: 1) Express nanoindentation tests can provide reliable information for cement paste. Deconvolution based on Gaussian Mixture Model (GMM) can obtain almost invariant statistics for each phase; 2) Based on averaged greyscale values of each BSE image, a table model can predict the elastic modulus and hardness with R² of 0.80 and 0.83, respectively; 3) Based on the intensity of each pixel as well as their patterns in each BSE image, the Res-Net model can predict the elastic modulus and hardness with a R² of 0.85 and 0.88, respectively. Deconvolution of the Res-Net prediction obtains similar invariant statistics as derived by the nanoindentation tests, which gives strong evidence of the applicability of the Res-Net model.

Limestone-calcined clay-cement (LC3), as one of the most promising sustainable cements, has been under development over the past decade. However, many uncertainties remain regarding its rheological behaviors, such as the metakaolin content of calcined clay. This study aims to investigate the effect of increasing the content of fine-grained metakaolin in calcined clay on the rheology of LC3 pastes. Rheological behaviors and early-age hydration of studied mixtures were characterized using flow curve, constant shear rate, small amplitude oscillatory shear and isothermal calorimetry tests. Results show that increasing the content of fine-grained metakaolin decreased flowability but promoted structural build-up and early-age hydration. These phenomena can be attributed to the decrease of mean interparticle distance caused by the increased amount of fine-grained metakaolin, which may enhance colloidal interactions, C-S-H nucleation and direct contact between particles. Overall, modifying the fine-grained metakaolin content is a feasible approach to control the rheology of LC3 pastes.

In the current study, experiments were carried out to investigate the cracking behaviour of reinforced concrete beams consisting of 1-cm-thick layer of Strain Hardening Cementitious Composite (SHCC) in the concrete cover zone. The hybrid SHCC/concrete beams with different types of interfaces were tested and compared with control reinforced concrete beams without a SHCC layer. A new SHCC/concrete interface that features a weakened chemical adhesion but an enhanced mechanical bonding was also developed to facilitate the activation of SHCC. The beams were tested in four-point bending configuration, while Digital Image Correlation (DIC) was used to evaluate crack pattern development and crack widths. Results show that hybrid beams possessed similar load bearing capacity but exhibited an improved cracking behaviour as compared to the control beam. The maximum crack width of the best performing hybrid beams exceeded 0.3 mm at approximately 53.3 kN load, whereas in the control beam it exceeded 0.3 mm at only 32.5 kN load. It is thus expected that the hybrid beams developed in the current study will possess an improved durability and enhanced self-healing potential as a result of having smaller cracks, leading to an extended service life at the expense of minimal additional cost.

This study investigates the microstructural changes of cement paste due to the inclusion of polymeric microfiber at different water-to-cement (w/c) ratios. A procedure to quantify the porosity of epoxy impregnated interfacial transition zone (ITZ) is also presented. Results show that the microstructures of the ITZ beneath and above a microfiber, with respect to the gravity direction, are largely different. Though the ITZ at both sides of the fiber are more porous than the bulk matrix, the porosity of the lower ITZ (i.e., the ITZ beneath a fiber) is significantly higher than the upper side (i.e., the ITZ above a fiber). This difference can be attributed to the combined effects of fiber on the initial packing of surrounding cement grains and on the settlement of the fresh mixture. The porosity gradients of the upper ITZs are found to be nearly identical for all the tested w/c ratios, while the porosity gradients of the lower ITZs become steeper when the w/c is higher. The lower side is also found to be the preferred location for the precipitation of calcium hydroxide crystals. Results of energy-dispersive X-ray spectroscopy (EDS) and nano-indentation analyses confirm that the chemical and mechanical properties of the ITZ are also asymmetric.

Copper nanoparticles (CuNPs) sintering for flip-chip interconnects is a promising solution for 3D and heterogeneous integration to overcome the limitation of solder materials. To this end, we perform the photolithographic stencil printing method to pattern CuNPs, and the form of flip-chip interconnects is completed after CuNPs sintering process. This paper aims to study the effect of sintering processing parameters (time, pressure, temperature) on the mechanical properties of CuNPs bumps when applying the novel method to approach the Cu interconnects. We fabricated seven groups of specimens of sintered CuNPs bumps, built with a diameter of 100 μm and sintered. The nanoindentation tests assessed the mechanical property to get Young's modulus and hardness. Results clarify that Young's modulus is strongly affected by pressure. An suggested combination of parameters (the 25 MPa and 260 °C for 15 min) give the highest modulus of 126 GPa and the hardness of 1.76 GPa. Moreover, the observations by scanning electron microscopy (SEM) reveal the microstructure and porosity evolution versus different processing parameters.