The use of alkaline activator in alkali-activated materials (AAMs) may pose risk of alkali-silica reaction (ASR), and the variations in the mixture design could have great influence on the performance of AAMs system. In this case, this paper investigated the effects of slag fineness (3000–8000 cm²/g) and water-to-binder (w/b) ratio (0.5–0.8) on ASR behavior of alkali-activated slag (AAS) mortars under accelerated mortar testing conditions as specified in ASTM C1260. The length change, mass gain, microstructure and formation of ASR products were examined to evaluate the degradation caused by ASR. It was found for the first time that slag fineness induces a “pessimum effect” in the ASR expansion of AAS mortars. On the other hand, there is a “pessimum effect” in the influence of w/b ratio on ASR expansion in the early-stage (≤14d), and the induced expansion increased with an increase in w/b ratio in the late-stage (>14d). The mechanism governing the effect of slag fineness and w/b ratio is complicated and cannot be explained solely by the properties of ASR products. This work contributes to the understanding of ASR in AAMs system and could provide a basis for the mixture optimization of AAMs.

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With the development of waste recovery techniques, previous research has revealed that coarse fractions of municipal solid waste incineration (MSWI) bottom ash (BA) after proper treatment could be applied in the construction sector, while the fines are seldom recovered in practice and normally landfilled. This study explores the potential application of fine MSWI BA (0–2 mm) as a supplementary cementitious material (SCM) in Portland cement (PC) mixtures. Mechanical and chemical pre-treatment approaches have been designed with various conditions to optimize the treating process. The chemical and mineralogical compositions, as well as the metallic Al content in BA were characterized before and after the pre-treatment. It was found that both methods are effective in removing the metallic Al content in BA, Moreover, BA derived from mechanical treatment exhibited more contribution to the hydration reaction in PC mixtures, as revealed by the amount of reaction products and mineral phases formed in hardened trial mixtures. BA obtained was further partially blended in PC mortars to evaluate the performance as compared to SCMs and inert fillers. It was found that treated BA resulted in a slight retarding effect on the reaction kinetics. Treated BA behaved better than the coal fly ash to contribute to the strength development, while the inclusion of BA did not lead to significant influences on the workability.

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Hoewel geopolymeerbeton op laboratoriumschaal uitgebreid is onderzocht, zijn praktische toepassingen en ervaringen nog maar beperkt beschikbaar. Bovendien bestaan er voor een brede en grootschalige constructieve toepassing een aantal uitdagingen. Er is een onderzoeksproject gestart waarin een zelfverdichtend geopolymeerbeton (ZGB) is ontwikkeld voor toepassing in een brug. In de tweede fase van het onderzoek zijn de mogelijkheden voor productie op industriële schaal onderzocht.@en

Alkali-activated concrete (AAC) is regarded as a promising alternative construction material to reduce the CO₂ emission induced by Portland cement (PC) concrete. Due to the diversity in raw materials and complexity of reaction mechanisms, a commonly applied design code is still absent to date. This study attempts to directly correlate the AAC mix design parameters to their performances through an artificial intelligence approach. To be specific, 145 fresh property data and 193 mechanical strength data were collected from laboratory tests on 52 AAC mixtures, which were used as inputs for the machine learning algorithm. Five independent random forest (RF) models were established, which are able to predict fresh and hardened properties (in terms of compressive strength, slump values, static/dynamic yield stress, and plastic viscosity) of AAC with equivalent accuracy reported in the literature. Moreover, an inverse optimization was performed on the RF model obtained to reduce the sodium silicate dosages, which may further mitigate the environmental impact of producing AAC. The present RF model gives practical information on AAC mix design cases.

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This paper presents an experimental study on the interface bonding properties of polyvinyl alcohol (PVA) fiber in alkali-activated slag/fly ash (AASF) pastes. Three interface bonding properties (i.e., the chemical bonding energy Gd, the initial frictional bond strength τ0, and slip-hardening behavior) were determined using single-fiber pullout tests. The microstructure and chemical composition of the reaction products in the fiber/matrix interfacial transition zone (ITZ) and the nearby matrix were also characterized to reveal the influence of PVA fiber to its surrounding matrix. It is found that Gd increases primarily with increasing Ca/(Si+Al) ratio of C-(N-)A-S-H gel. Unlike that in cementitious materials, the inclusion of PVA fiber in AASF pastes promotes the formation of a high-Ca C-(N-)A-S-H phase rather than crystalline portlandite near the fiber surface. This study provides useful guidance for tailoring the interface bonding properties of AASF and also the development of high-performance composites such as strain-hardening geopolymer composites.@en

This work evaluated the reactivity and leaching potential of municipal solid waste incineration (MSWI) bottom ash as supplementary cementitious material (SCM) and precursor for alkali-activated materials (AAM). The chemical composition of the amorphous phase in MSWI bottom ash was found to be in the same range as that of Class F coal fly ash. The reactivity of MSWI bottom ash as SCM and AAM precursor was tested to be much lower than that of blast furnace slag, but similar to that of Class F coal fly ash. The method of thermodynamic modeling was found useful in providing references for the mix design of MSWI bottom ash-based AAM. Grinding MSWI bottom ash into powder for the application of SCM and AAM precursor increased its leaching potential. Based on the findings of this study, recommendations were provided on how to use MSWI bottom ash to prepare blended cement pastes and AAM.

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In this paper, the authors characterized two types of zonation within slag rims in aged alkali-activated slag (AAS) systems through SEM and TEM technology. These two elemental zonation were closely related to the pore structure of AAS pastes, thus providing strong implication for the transport- and durability-related performance of AAS systems. The first type of zonation occurred in the rims of AAS specimens under sealed curing. It was found that lath-like hydrotalcite-like phase accumulated near the boundary while a generally homogeneous and foil-like C-(N-)A-S-H gel phases precipitated in the following sub-zone. When slag rims were thick enough, a new Mg-rich region occurred. The second type of zonation was noticed in the carbonated AAS pastes. For this kind of distribution pattern, C-(N-)A-S-H gel phases were observed near the boundary. Following, the accumulation of Mg and Ca occurred alternatively. Additionally, transformation mechanism between these two types of zonation was also proposed.

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The results of phase 1 of an interlaboratory test, coordinated by the RILEM TC 267-TRM “Tests for Reactivity of Supplementary Cementitious Materials” showed that the R³ (rapid, relevant, reliable) test method, by measurement of heat release or bound water, provided the most reliable and relevant determination of the chemical reactivity of supplementary cementitious materials (SCMs), compared to other test methods. The phase 2 work, described in this paper aimed to improve the robustness of the test procedure and to develop precision statements for the consolidated test procedure. The effect of the pre-mixing and mixing conditions, and the impact of the mix design on the test method robustness were assessed and fixed for optimal conditions to carry out the R³ heat release test. The effect of the drying step was evaluated to define the R³ bound water test procedure in more detail. Finally, the robustness of the consolidated final test methods was determined by an interlaboratory study to define the precision statements.

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This study aims to interpret the early-stage rheology of alkali-activated slag (AAS) paste from microstructure perspectives. The microstructures visualized by cryogenic scanning electron microscopy (cryo-SEM) revealed the essential distinction between hydroxide and silicate-activated slag pastes. The hydroxide-based mixture showed typical suspension features, where slag particles were dispersed in the hydroxide activators. In the hydroxide media, even at very early ages (5 min), the solid grains were attached to each other through rigid connections of reaction products, which resulted in high yield stress. As for the silicate-based mixtures, an emulsion phase has been observed between slag particles, which consists of discontinuous water droplets and continuous silicate gels. Fine emulsions with smaller water droplets were observed as the silicate modulus of activators increased, which dispersed the slag particles but on the other hand improved the viscosity of the paste. With increasing water to binder ratio, both yield stress and viscosity of AAS pastes significantly reduced.

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In this paper, both synthetic slag and commercial slag covering the common composition range were employed to estimate the correlation between slag chemistry and reactivity through hydraulicity and dissolution tests. It was found that slag reactivity was favorably affected by increasing Al₂O₃ and MgO contents, while the adverse effect of decreasing CaO/SiO₂ ratio could be compensated by higher amounts of Al₂O₃ and/or MgO. When calorimetric measurement was used to assess the reactivity of slag, the effect of sulfur species incorporated in commercial slag should be taken into consideration as a small quantity of it could lead to a major difference of cumulative heat release due to the formation of ettringite. Moreover, a novel graphical method was proposed to estimate the reactivity of slag considering its chemical composition from a new perspective, i.e. a cartesian coordinate system based on (CaO/SiO₂)−(MgO + Al₂O₃).

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In Nederland wordt veel aandacht besteed aan geopolymeerbeton als een van de mogelijkheden om de CO₂-voetafdruk van beton te verlagen. Hoewel dit materiaal op laboratoriumschaal uitgebreid is onderzocht, zijn praktische toepassingen en ervaringen nog maar beperkt beschikbaar. Bovendien bestaan er voor een brede en grootschalige constructieve toepassing een aantal uitdagingen op technologisch en technisch gebied. Er is een onderzoeksproject gestart waarin een zelfverdichtend geopolymeerbeton (ZGB) is ontwikkeld voor toepassing in een prefab voorgespannen verkeersbrug. Dit onderzoek is uitgevoerd door het Microlab en de sectie Betonconstructies van de TU Delft, Haitsma Beton en de Universiteit Gent en en wordt door de provincie Fyslân ondersteund als launching customer.@en

RILEM TC 267 TRM– “Tests for Reactivity of Supplementary Cementitious Materials” recommends the Rapid Reliable Relevant (R3) test as a method for determining the chemical reactivity of supplementary cementitious materials (SCMs) in Portland cement blends. In this paper, the R3 test was applied to 52 materials from a wide range of conventional and alternative SCMs with the aim to validate such test. An excellent correlation was found between the cumulative heat release and the bound water determined following the R3 test method. Comparison of the R3 test results to mortar compressive strength development showed that all conventional SCMs (e.g. blast furnace slag and fly ashes) followed the same trend, with the notable exception of very reactive calcined kaolinitic clays. It is discussed, through an in-depth statistical regression analysis of the R3 reactivity test results and the 28 days relative compressive strengths, how reactivity threshold values for classification of the chemical reactivity of SCMs could be proposed based on the R3 test results.@en

Strain hardening cementitious composite (SHCC) is a special class of ultra-ductile material which has autogenous self-healing capability due to its intrinsic tight crack widths. To further improve its healing ability, healing agent (HA) can be incorporated in SHCC, enabling it also the autonomous self-healing mechanism. In this study, the effects of adding bacteria-embedded polylactic acid (PLA) capsules on the mechanical properties of SHCC with different amounts of HA (i.e., 1.25%, 2.5%, 5% by weight to binder) were investigated. Experiments were conducted to examine the composite performance, matrix properties and single fiber pullout behavior of the SHCCs, followed by microscopy characterization of the fiber/matrix interface microstructure. Results show that the inclusion of the PLA-HA up to 5% by weight to binder influenced the tensile performance (i.e., tensile strength and ductility) of SHCC only to a very small extent but significantly reduced the average residual crack widths. The inclusion of HA at a high dosage (5%) increased the crack tip toughness (J_tip) of the matrix by lowering elastic modulus and increasing fracture toughness. Single fiber pullout results show that the fiber/matrix bond properties were enhanced by the addition of the HA, which can be attributed to the formation of a denser interfacial transition zone (ITZ) with less calcium hydroxide crystals as revealed by the scanning electron microscope (SEM) micrographs. The improved bond properties led to higher fiber bridging complementary energy and thus partially sustained the tensile strain capacity as verified by the micromechanical model.

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Alkali-activated Materials (AAMs), including those classified as geopolymer, are obtained through the reaction between a solid precursor and an alkaline solution. Compared with ordinary Portland cement (OPC) binders, these materials maintain comparable mechanical properties but have the advantage of reducing greenhouse gas emissions and utilization of industrial by-products and residuals which helps to meet sustainability goals. AAMs are thus considered an environment-friendly construction material with great potential for next-generation concrete. AAMs are inherently brittle. The low ductility of AAMs makes them prone to cracking and corresponding performance degradation, which is detrimental to their durability. Based on the concept of strain-hardening cementitious composite (SHCC), one solution relates to a family of fiber-reinforced composites that have high tensile ductility and multiple-cracking characteristics, i.e., strain-hardening geopolymer composite (SHGC). While much effort has been taken to develop conventional SHCC, scientific and technical knowledge of SHGC is still in the very early stage of development. This PhD project deals with the development of a cement-free strain-hardening geopolymer composite (SHGC) as a high-performance construction material using industrial wastes and by-products through alkaline activation technology: The fracture properties and other mechanical properties of the alkali-activated slag/fly ash (AASF) paste as the matrix for SHGC were experimentally tested. The microstructure and chemistry of the reaction products were investigated to understand the fracture mechanism. It was found that the fracture properties of pastes are strongly related to the chemical composition (Ca/Si ratio) of the main reaction product, i.e., C-(N-)A-S-H gel. The fracture properties were also found to be dominated by a cohesion/adhesion-based mechanism. Furthermore, the compressive strength of AASF paste is primarily determined by its capillary porosity. The fiber/matrix properties, including chemical bonding energy, initial frictional bond, and slip-hardening behavior of fiber during the pullout process were also experimentally studied. The chemistry and microstructure of the reaction product in the fiber/matrix interfacial transition zone (ITZ) were characterized. Their influence on the interface bonding properties was also investigated. It is found that the chemical bonding between PVA fiber and AASF matrix increases with increasing Ca/Si and Ca/(Si+Al) ratio of C-(N-)A-S-H gel. Hence, changing the slag content and the alkali activator Ms appears to be an effective way to modify chemical bonding. Unlike the formation of portlandite near the PVA fiber surface in conventional SHCC, a high-Ca C-(N-)A-S-H phase was formed in the fiber-matrix ITZ of SHGC. This explains the higher chemical bonding energy found in SHGC compared to that in conventional SHCCs. Furthermore, the adhesion mechanism of the PVA molecule in reaction products was studied using MD simulation. The study suggests that the adhesion between PVA fiber and C-(N-)A-S-H gel is primarily due to electrostatic interactions rather than van der Waals interactions. Based on the result of fracture properties of the matrix and fiber/matrix interface properties, the SHGC is then systematically developed following a micromechanics-based design approach. The experimentally-attained matrix and interface properties served as input for the numerical micromechanics model to simulate the crack bridging behavior. Through the micromechanical modeling, the optimal fiber length and volume were selected and the behavior of mixtures with different fiber/matrix combinations was predicted. With this approach, researchers and materials engineers can design and tailor future SHGC more efficiently than by using the commonly used trial-and-error method. Finally, the environmental impact of the SHGC with the most promising performance was also evaluated. This evaluation was conducted using a cradle-to-gate life-cycle assessment (LCA) of SHGC compared to that of conventional SHCC materials. The developed SHGC demonstrates a very promising environmental profile. It has a significant reduction of the global warming potential (GWP) and a lower or similar total environmental impact compared to conventional SHCC materials. In addition, the results also provide recommendations for further improvements in mixture design for the future development of SHGC. This study successfully developed a sustainable slag/fly ash-based SHGC with a lower carbon footprint than conventional SHCC. It is considered a good example to utilize industrial by-products as secondary resources and at the same time contribute to a circular economy. Furthermore, this study helps to understand the fracture properties of AAMs. It also clarifies the adhesion mechanism of PVA fiber in AAMs. All of these give promising guidance for researchers and engineers to design fiber-reinforced AAMs with required fracture properties and interface bonding properties. In particular, it contributes to the design and tailoring strategies for high-performance composite, for instance, SHGC, through proper mixture design. @en

Alkali activated materials (AAMs) have received worldwide attention due to its lower embodied energy and environmental impact than that of traditional cementitious materials. However, the activators with high alkalinity may raise the risk of alkali silica reaction (ASR) induced deterioration when reactive aggregates are used, which thereby limits the commercial use of AAMs. Not speaking the ASR induced long-term expansion, the early-age reaction of AAMs prepared with reactive aggregates is largely unknown. In this paper, isothermal calorimetry, thermogravimetry (TG) and mercury intrusion porosimetry (MIP) were adopted to study the heat evolution, mineralogical changes and pore structures of early-age ordinary Portland cement (OPC) mortar and water-glass activated slag/fly ash mortars. In each system, emphasis were made to understand the differences between mixtures prepared with standard inert quartz sands and reactive fine aggregates. The results show that the mortars prepared with reactive aggregates generated more heat in the wetting and dissolution stage. Particularly, the water-glass activated slag mortar presented the highest heat flow peak. Meanwhile, the results of TG illustrate that higher amount of reaction products were formed in water-glass activated mortars prepared with reactive aggregates than that with inert quartz sands. These findings suggest that the reactive aggregates are evidently involved in the early-age alkaline reaction of AAMs system.@en

In recent years, the rapid industrialization and urbanization led to the explosive growth of municipal solid waste incineration (MSWI) bottom ashes (BA) production. However, most of them are directly landfilled, which not only brings environmental burden but also results in loss of potential resources. Present researches have proved that MSWI BA could be utilized as a replacement in Portland cement concrete. However, several drawbacks such as volume expansion, leaching behaviour, and relatively lower strength have been reported. In this study, as-received BA was pretreated to remove the metallic aluminium which is responsible for the hydrogen-induced expansion when blended in OPC concretes. Subsequently, the treated BA samples were used as a substitution for cement at the replacement level of 10%. Micronized sand (M300) was selected as reference materials to investigate the role of treated BA in blended cement system, either as filler or binder material. In the experimental program, the hydration process of different mixtures was monitored by isothermal calorimeter and hydration products were determined by X-ray diffraction (XRD) and Thermalgravimetric analysis (TGA). Results showed that the pretreatment effectively removed the metallic aluminum in BA and no severe expansion or strength decrement were detected. The treated BA showed limited reactivity comparing with Portland cement, however, it still worked better than micronized sand as a filler substitution.@en

This paper aims to study the adhesion mechanism of polyvinyl alcohol (PVA) fiber within alkali-activated slag/fly ash (AASF) matrix using molecular dynamics (MD) simulation in combination with systematic experimental characterization. The adhesion of PVA to C-(N-)A-S-H gel with different Ca/(Si+Al) and Al/Si ratios was modeled using MD simulation, with the related adsorption enthalpy calculated and the adhesion mechanism explored. The experimentally attained chemical bonding energy of PVA fiber in AASF coincides well with the simulation results. In both cases, the adhesion enhances primarily with increasing Ca/(Si+Al) ratio of C-(N-)A-S-H gel. Additionally, MD simulation indicates preferential element distributions of Ca around PVA molecule, which was confirmed experimentally by the detection of the Ca-rich C-(N-)A-S-H gel in the interfacial transition zone (ITZ). This study provides further insights into the adhesion mechanism of PVA fiber to C-(N-)A-S-H gel formed in AASF, which is particularly valuable for the future development of PVA-based high-performance alkali-activated composites.

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Alkali activated slag (AAS) has shown promising potential to replace ordinary Portland cement as a binder material. Synthesized from industrial by-products, AAS can show high strength, thermal resistance and good durability. However, AAS has been reported to exhibit high autogenous shrinkage. Autogenous shrinkage is a critical issue for building materials since it can induce micro- or macro-cracking when the materials are under restrained conditions. Hence, this work aims at mitigating the autogenous shrinkage of AAS by means of internal curing. The influences of internal curing on microstructure formation and autogenous shrinkage are investigated. The results show that internal curing provided by superabsorbent polymers is a promising way to reduce the autogenous shrinkage of AAS.@en

This study presents a comprehensive experimental investigation on the fracture properties of hardened alkali-activated slag/fly ash (AASF) pastes in relation to the microstructure formation and reaction product composition. The main reaction product in AASF is C-(N-)A-S-H gel along with minor hydrotalcite phase, with the polymerization of C-(N-)A-S-H gel substantially governed by its Ca/Si ratio. Strong positive correlations are identified between the Ca/Si ratios of C-(N-)A-S-H gel and the fracture properties K_Ic (J_tip), whereas, the compressive strength of AASF pastes is primarily determined by its capillary porosity (>0.01 μm). The disagreements between the Ca/Si ratios and corresponding intrinsic mechanical properties of C-(N-)A-S-H gel as proof by contradiction indicate that the fracture properties K_Ic (J_tip) of AASF pastes could be dominated by a cohesion/adhesion-based mechanism. These findings provide promising guidance for fine-tuning the fracture properties of AASF and also advise on the tailoring strategies for high-performance composite such as strain-hardening geopolymer composite.

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Alkali activated concrete (AAC) has not received broader industry acceptance, one reason of which lies in the uncertainties in the durability against shrinkage and potential cracking. Many studies reported that AAC exhibit larger autogenous shrinkage than OPC concrete. However, it is unable to deduce that AAC should show higher cracking potential than OPC concrete only based on the higher autogenous shrinkage of AAC. The cracking potential of concrete is determined by multiple factors including autogenous shrinkage, creep/relaxation, elastic modulus, and tensile properties of the concrete. However, very few studies have considered these parameters. Furthermore, the influence of precursors (e.g. slag or fly ash) on the cracking potential of AAC induced by autogenous shrinkage is also rarely studied. The aim of this study, therefore, is to investigate the autogenous shrinkage-induced cracking potential of slag and fly ash-based AAC. The free autogenous shrinkage of the specimens is measured by Autogenous Deformation Testing Machine (ADTM). The autogenous shrinkage-induced stress and cracking of the concrete under restraint condition is tracked by Thermal Stress Testing Machine (TSTM). Additionally, the influence of precursors on the autogenous shrinkage induced cracking potential is discussed.

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