Report of RILEM TC 281-CCC: outcomes of a round robin on the resistance to accelerated carbonation of Portland, Portland-fly ash and blast-furnace blended cements.

Many (inter)national standards exist to evaluate the resistance of mortar and concrete to carbonation. When a carbonation coefficient is used for performance comparison of mixtures or service life prediction, the applied boundary conditions during curing, preconditioning and carbonation play a crucial role, specifically when using latent hydraulic or pozzolanic supplementary cementitious materials (SCMs). An extensive interlaboratory test (ILT) with twenty two participating laboratories was set up in the framework of RILEM TC 281-CCC 'Carbonation of Concrete with SCMs'. The carbonation depths and coefficients determined by following several (inter)national standards for three cement types (CEM I, CEM II/B-V, CEM III/B) both on mortar and concrete scale were statistically compared. The outcomes of this study showed that the carbonation rate based on the carbonation depths after 91 days exposure, compared to 56 days or less exposure duration, best approximates the slope of the linear regression and those 91 days carbonation depths can therefore be considered as a good estimate of the potential resistance to carbonation. All standards evaluated in this study ranked the three cement types in the same order of carbonation resistance. Unfortunately, large variations within and between laboratories complicate to draw clear conclusions regarding the effect of sample pre-conditioning and carbonation exposure conditions on the carbonation performance of the specimens tested. Nevertheless, it was identified that fresh and hardened state properties alone cannot be used to infer carbonation resistance of the mortars or concretes tested. It was also found that sealed curing results in larger carbonation depths compared to water curing. However, when water curing was reduced from 28 to 3 or 7 days, higher carbonation depths compared to sealed curing were observed. This increase is more pronounced for CEM I compared to CEM III mixes. The variation between laboratories is larger than the potential effect of raising the CO2 concentration from 1 to 4%. Finally, concrete, for which the aggregate-to-cement factor was increased by 1.79 in comparison with mortar, had a carbonation coefficient 1.18 times the one of mortar. Supplementary Information: The online version contains supplementary material available at 10.1617/s11527-022-01927-7.

Elastic Wave Monitoring of Cementitious Mixtures Including Internal Curing Mechanisms.

The mitigation of autogenous shrinkage in cementitious materials by internal curing has been widely studied. By the inclusion of water reservoirs, in form of saturated lightweight aggregates or superabsorbent polymers, additional water is provided to the hydrating matrix. The onset of water release is of high importance and determines the efficiency of the internal curing mechanism. However, the monitoring of it poses problems as it is a process that takes place in the microstructure. Using acoustic emission (AE) sensors, the internal curing process is monitored, revealing its initiation and intensity, as well as the duration. In addition, AE is able to capture the water evaporation from saturated specimens. By ultrasonic testing, differences in the hydration kinetics are observed imposed by the different methods of internal curing. The results presented in this paper show the sensitivity of combined AE and ultrasound experiments to various fundamental mechanisms taking place inside cementitious materials and demonstrate the ability of acoustic emission to evaluate internal curing in a non-destructive and easily implementable way.

Addressing the need for standardization of test methods for self-healing concrete: an inter-laboratory study on concrete with macrocapsules.

Development and commercialization of self-healing concrete is hampered due to a lack of standardized test methods. Six inter-laboratory testing programs are being executed by the EU COST action SARCOS, each focusing on test methods for a specific self-healing technique. This paper reports on the comparison of tests for mortar and concrete specimens with polyurethane encapsulated in glass macrocapsules. First, the pre-cracking method was analysed: mortar specimens were cracked in a three-point bending test followed by an active crack width control technique to restrain the crack width up to a predefined value, while the concrete specimens were cracked in a three-point bending setup with a displacement-controlled loading system. Microscopic measurements showed that with the application of the active control technique almost all crack widths were within a narrow predefined range. Conversely, for the concrete specimens the variation on the crack width was higher. After pre-cracking, the self-healing effect was characterized via durability tests: the mortar specimens were tested in a water permeability test and the spread of the healing agent on the crack surfaces was determined, while the concrete specimens were subjected to two capillary water absorption tests, executed with a different type of waterproofing applied on the zone around the crack. The quality of the waterproofing was found to be important, as different results were obtained in each absorption test. For the permeability test, 4 out of 6 labs obtained a comparable flow rate for the reference specimens, yet all 6 labs obtained comparable sealing efficiencies, highlighting the potential for further standardization.

The Contribution of Elastic Wave NDT to the Characterization of Modern Cementitious Media.

To mitigate autogenous shrinkage in cementitious materials and simultaneously preserve the material's mechanical performance, superabsorbent polymers and nanosilica are included in the mixture design. The use of the specific additives influences both the hydration process and the hardened microstructure, while autogenous healing of cracks can be stimulated. These three stages are monitored by means of non-destructive testing, showing the sensitivity of elastic waves to the occurring phenomena. Whereas the action of the superabsorbent polymers was evidenced by acoustic emission, the use of ultrasound revealed the differences in the developed microstructure and the self-healing of cracks by a comparison with more commonly performed mechanical tests. The ability of NDT to determine these various features renders it a promising measuring method for future characterization of innovative cementitious materials.

Complementing urea hydrolysis and nitrate reduction for improved microbially induced calcium carbonate precipitation.

Microbial-induced CaCO3 precipitation has been widely applied in bacterial-based self-healing concrete. However, the limited biogenetic CaCO3 production by bacteria after they were introduced into the incompatible concrete matrix is a major challenge of this technology. In the present study, the potential of combining two metabolic pathways, urea hydrolysis and nitrate reduction, simultaneously in one bacteria strain for improving the bacterial CaCO3 yield has been investigated. One bacterial strain, Ralstonia eutropha H16, which has the highest Ca2+ tolerance and is capable of performing both urea hydrolysis and nitrate reduction in combined media was selected among three bacterial candidates based on the enzymatic examinations. Results showed that H16 does not need oxygen for urea hydrolysis and urease activity was determined primarily by cell concentration. However, the additional urea in the combined medium slowed down the nitrate reduction rate to 7 days until full NO3- decomposition. Moreover, the nitrate reduction of H16 was significantly restricted by an increased Ca2+ ion concentration in the media. Nevertheless, the overall CaCO3 precipitation yield can be improved by 20 to 30% after optimization through the combination of two metabolic pathways. The highest total CaCO3 precipitation yield achieved in an orthogonal experiment was 14 g/L. It can be concluded that Ralstonia eutropha H16 is a suitable bacterium for simultaneous activation of urea hydrolysis and nitrate reduction for improving the CaCO3 precipitation and it can be studied later, on activation of multiple metabolic pathways in bacteria-based self-healing concrete.

Bacillus sphaericus LMG 22257 is physiologically suitable for self-healing concrete.

The suitability of using a spore-forming ureolytic strain, Bacillus sphaericus, was evaluated for self-healing of concrete cracks. The main focus was on alkaline tolerance, calcium tolerance, oxygen dependence, and low-temperature adaptability. Experimental results show that B. sphaericus had a good tolerance. It can grow and germinate in a broad range of alkaline pH. The optimal pH range is 7 âˆ¼ 9. High alkaline conditions (pH 10 âˆ¼ 11) slow down but not stop the growth and germination. Oxygen was strictly needed during bacterial growth and germination, but not an essential factor during bacterial urea decomposition. B. sphaericus also had a good Ca tolerance, especially at a high bacterial concentration of 108 cells/mL; no significant influence was observed on bacterial ureolytic activity of the presence of 0.9M Ca2+. Furthermore, at a low temperature (10 °C), bacterial spores germinated and revived ureolytic activity with some retardation. However, this retardation can be counteracted by using a higher bacterial concentration and by supplementing yeast extract. It can be concluded that B. sphaericus is a suitable bacterium for application in bacteria-based self-healing concrete.

Application of microorganisms in concrete: a promising sustainable strategy to improve concrete durability.

The beneficial effect of microbially induced carbonate precipitation on building materials has been gradually disclosed in the last decade. After the first applications of on historical stones, promising results were obtained with the respect of improved durability. An extensive study then followed on the application of this environmentally friendly and compatible material on a currently widely used construction material, concrete. This review is focused on the discussion of the impact of the two main applications, bacterial surface treatment and bacteria based crack repair, on concrete durability. Special attention was paid to the choice of suitable bacteria and the metabolic pathway aiming at their functionality in concrete environment. Interactions between bacterial cells and cementitious matrix were also elaborated. Furthermore, recommendations to improve the effectiveness of bacterial treatment are provided. Limitations of current studies, updated applications and future application perspectives are shortly outlined.

Circular design, material properties, service life and cradle-to-cradle carbon footprint of lime-based building materials.

The massive extraction of virgin raw materials has substantially intensified the focus on circular economy of building materials. As a Cradle-to-Cradle service life and circular approach for lime-based construction materials (LBCM) is lacking, the present study evaluates the environmental impact and feasibility of creating a fully recycled second-life render (SL) by designing a closed-loop upcycling process for first-life renders (FL). To achieve this, a second-life binder was thermally activated (900, 1000, 1100, 1200 °C), while its microstructure, compressive strength, and thermal conductivity were investigated. SL had up to 33 % open porosity (FL 29 %), its compressive strength ranged from 2.5 to 3.4 MPa (FL 4.4 MPa) and the thermal conductivity from 1.002 to 1.107 W/mK (FL 1.231 W/mK). Resistance of SL and FL against sulfate attack was found to be equivalent, measured based on the recent RILEM TC 271-ASC recommendation. The environmental impact indicators integrating material properties and durability confirm that the second life-render can reduce CO2 emissions up to 55 %. The present research provides insights into unlocking essential sustainability gains through circular practices in the life-cycle of LBCM.

Influence of temperature on the effectiveness of a biogenic carbonate surface treatment for limestone conservation.

So far, most studies on microbiologically induced carbonate precipitation for limestone conservation have been performed at temperatures optimal for the activity of the calcinogenic bacteria (i.e., 20-28 °C). Successful application in practice, however, requires adequate performance in a wide range of environmental conditions. Therefore, the aim of this study was to select microorganisms that are most suited for biodeposition at temperatures relevant for practice. In a first step, ureolytic microorganisms were screened for their growth and ureolytic activity at different temperatures (10, 20, 28, and 37 °C). Large differences in calcinogenic activity could be observed between experiments performed on agar plates and those performed in solution and in limestone. In a second step, the influence of temperature on the performance of the biodeposition treatment with different ureolytic microorganisms was evaluated, both on the consolidative and protective effect of the treatment. In contrast with the experiments on agar plates, the Sporosarcina psychrophila strains failed to produce significant amounts of calcium carbonate on limestone in conditions relevant for practice, even at 10 °C. This resulted in a poor performance of the treatment. From experiments performed on limestone prisms, it appeared that the mesophilic Bacillus sphaericus produced the highest amount of carbonate in the shortest amount of time at all temperatures tested. As a result, compared to the untreated specimens, the highest consolidative (64 % lower weight loss upon sonication) and protective effect (46 % decreased sorptivity) were observed for the treatments with this species. From this study, it appears that among all ureolytic strains tested, B. sphaericus is most suited for biodeposition applications in practice.

Phase Evolution of Hybrid Alkali Sulfate-Activated Ground-Granulated Blast Furnace Slag Cements.

In this study, a hybrid alkali-activated ground-granulated cement consisting of 70% blast furnace slag (GGBFS) and 30% Portland cement (PC) activated with sodium sulfate was studied. Results were compared with those of a blended system without an activator. The addition of the activator significantly increased the kinetics and degree of reaction of these cements, particularly at early curing ages (2 days), without leading to significant changes in the phase assemblage. The main reaction product formed was an aluminum-substituted calcium silicate hydrate (C-A-S-H) type gel, with a Ca/Si ratio comparable to that of the activator-free blended cement; however, in the presence of the activator, sorption of sulfur was observed in the C-A-S-H phase. The formation of secondary phases including ettringite and Ca- or Mg-rich layered double hydroxides was also identified in these cements depending on the curing age and activation addition. This study demonstrates the effectiveness of sodium sulfate in accelerating the phase assemblage evolution in high-GGBFS-content PC-blended cements without leading to significant changes in the reaction products formed, particularly at advanced curing ages. This represents a step forward in the development of cements with a reduced clinker factor.

Capillary Imbibition in Cementitious Materials: Effect of Salts and Exposure Condition.

Concrete structures are often exposed to harsh environmental conditions during their service life. Therefore, the investigation of transport properties and deterioration of concrete in different environments is an important topic. This paper reports the influence of salts (NaCl and Na2SO4) and exposure conditions (ideal laboratory (20 °C, 95% RH), a city and sea environment; including sheltered and exposed conditions) on capillary imbibition in cementitious materials with different water to cement ratios (0.4 and 0.6). First, the pore structure was assessed by water absorption under vacuum, torrent permeability, resistivity, and moisture content. The second part revolves around the capillary imbibition phenomenon with different imbibition liquids (water, NaCl, and Na2SO4). The results showed that, among the studied exposure conditions, sheltered conditions resulted in the largest porosity values and capillary imbibition rates (CIR). The influence of the imbibing liquid on the CIR depends on the w/c of the concrete. The CIR value for samples with a w/c of 0.4 is lower for Na2SO4 as imbibing liquid in comparison to water and NaCl. The sulfates might cause a pore blocking effect leading to a decreased CIR. For concrete with a w/c of 0.6, there was no significant difference between the different imbibition liquids. The influence of the pore blocking effect is probably smaller due to the larger porosity in this case. The findings of this research are important to understand the influence of real-life exposure conditions and therefore the influence of relative humidity, temperature, carbonation, and chloride ingress on the capillary imbibition phenomenon.

Influence of pore structure on the effectiveness of a biogenic carbonate surface treatment for limestone conservation.

A ureolytic biodeposition treatment was applied to five types of limestone in order to investigate the effect of pore structure on the protective performance of a biogenic carbonate surface treatment. Protective performance was assessed by means of transport and degradation processes, and the penetration depth of the treatment was visualized by microtomography. Pore size governs bacterial adsorption and hence the location and amount of carbonate precipitated. This study indicated that in macroporous stone, biogenic carbonate formation occurred to a larger extent and at greater depths than in microporous stone. As a consequence, the biodeposition treatment exhibited the greatest protective performance on macroporous stone. While precipitation was limited to the outer surface of microporous stone, biogenic carbonate formation occurred at depths of greater than 2 mm for Savonnières and Euville. For Savonnières, the presence of biogenic carbonate resulted in a 20-fold decreased rate of water absorption, which resulted in increased resistance to sodium sulfate attack and to freezing and thawing. While untreated samples were completely degraded after 15 cycles of salt attack, no damage was observed in biodeposition-treated Savonnières. From this study, it is clear that biodeposition is very effective and more feasible for macroporous stones than for microporous stones.

The Durability of Mortar Containing Alkali Activated Fly Ash-Based Lightweight Aggregate.

Beneficiating fly ash as valuable construction material such as artificial lightweight aggregate (LWA) could be an alternative solution to increase the utilization of the industrial by-product. However, generally, LWA is characterized by high porosity and a related high water absorption, which on the one hand allows production of lightweight mortar, but on the other hand can affect its performance. Thus, in this research, the durability performance of mortar composed with alkali-activated fly ash-based LWA, and commercial expanded clay (EC) LWA was investigated. The fly ash LWA was prepared in a pan granulator, with a 6-molar solution of NaOH mixed with Na2SiO3 in a Na2SiO3/NaOH weight ratio of 1.5 being used as activator (FA 6M LWA). The results revealed that mortar containing FA 6M LWA had equivalent mechanical strength with mortar containing EC LWA. The mortar containing FA 6M LWA had comparable capillary water uptake and chloride migration resistance with the reference and EC LWA mortar. Furthermore, the addition of FA 6M LWA was proven to enhance the carbonation resistance in the resulting mortar, due to the denser interfacial transition zone (ITZ) of mortar with LWA.

Effect of the Mechanical Load on the Carbonation of Concrete: A Review of the Underlying Mechanisms, Test Methods, and Results.

As one of the major causes of concrete deterioration, the carbonation of concrete has been widely investigated over recent decades. In recent years, the effect of mechanical load on carbonation has started to attract more attention. The load-induced variations in crack pattern and pore structure have a significant influence on CO2 transport which determines the carbonation rate. With different types of load, the number, orientation, and position of the induced cracks can be different, which will lead to different carbonation patterns. In this review paper, the carbonation in cracked and stress-damaged concrete is discussed first. Then, literature about the effect of sustained load during carbonation is compared in terms of load type and load level. Finally, the advantages and disadvantages of possible test methods for investigating the effect of sustained load on carbonation are discussed with respect to loading devices, load compensation, and specimen size.

Chemical Shrinkage of Low Water to Cement (w/c) Ratio CEM I and CEM III Cement Pastes Incorporating Silica Fume and Filler.

Chemical shrinkage (CS) is the reason behind early age cracking, a common problem for concrete with low water to cement ratios (w/c < 0.35) known as Ultra-High- and High-Performance Concrete (U-HPC). However, to avoid the crack development initiated by autogenous shrinkage, a precise measurement of CS is required, as the values obtained can determine the correct amount of internal curing agent to be added in the mixture to avoid crack formation. ASTM C1608 is the standardized method for performing CS tests. In this study, recommendations are provided to improve the reliability of results obtained with this standard method, such as good compaction of samples and the use of superplasticizer (SP) for low w/c ratios (≤0.2). Cement pastes with CEM I and CEM III have been tested at different w/c ratios equal to 0.2, 0.3 and 0.4 with and without the addition of superplasticizer. CS results following ASTM-C1608 dilatometry showed that the presence of mineral additions such as silica fume and filler reduced the chemical shrinkage, while CS increased with increasing w/c. Low w/c ratio pastes of CEM III had slightly higher CS rates than CEM I, while the opposite was noticed at higher w/c. SEM images illustrated the importance of a careful compaction and SP use.

First Large Scale Application with Self-Healing Concrete in Belgium: Analysis of the Laboratory Control Tests.

Due to the negative impact of construction processes on the environment and a decrease in investments, there is a need for concrete structures to operate longer while maintaining their high performance. Self-healing concrete has the ability to heal itself when it is cracked, thereby protecting the interior matrix as well as the reinforcement steel, resulting in an increased service life. Most research has focused on mortar specimens at lab-scale. Yet, to demonstrate the feasibility of applying self-healing concrete in practice, demonstrators of large-scale applications are necessary. A roof slab of an inspection pit was cast with bacterial self-healing concrete and is now in normal operation. As a bacterial additive to the concrete, a mixture called MUC+, made out of a Mixed Ureolytic Culture together with anaerobic granular bacteria, was added to the concrete during mixing. This article reports on the tests carried out on laboratory control specimens made from the same concrete batch, as well as the findings of an inspection of the roof slab under operating conditions. Lab tests showed that cracks at the bottom of specimens and subjected to wet/dry cycles had the best visual crack closure. Additionally, the sealing efficiency of cracked specimens submersed for 27 weeks in water, measured by means of a water permeability setup, was at least equal to 90%, with an efficiency of at least 98.5% for the largest part of the specimens. An inspection of the roof slab showed no signs of cracking, yet favorable conditions for healing were observed. So, despite the high healing potential that was recorded during lab experiments, an assessment under real-life conditions was not yet possible.

Properties of Alkali Activated Lightweight Aggregate Generated from Sidoarjo Volcanic Mud (Lusi), Fly Ash, and Municipal Solid Waste Incineration Bottom Ash.

Production of artificial lightweight aggregate (LWA) from industrial by-products or abundant volcanic mud is a promising solution to prevent damaging the environment due to the mining of natural aggregate. However, improvements are still needed in order to control the high water absorption of LWA and strength reduction in resulting concrete or mortar. Hence in this research, fly ash, municipal solid waste incineration bottom ash (MSWI BA), and Sidoarjo volcanic mud (Lusi) were employed as a precursor and activated using NaOH 6 M and Na2SiO3 in producing LWA. The influence of the type of the precursors on the physical properties of resulting LWA was investigated. The effect of replacing natural fine aggregate with the resulting LWA on the compressive strength and volume density of mortar was also determined. Finer particles, a high amount of amorphous phase, and low loss on ignition (LOI) of the raw material improved the properties of resulting LWA. Mortar compressive strength was decreased by 6% when replacing 16% by volume of natural fine aggregate with fly ash based LWA. Compared to the expanded clay LWA, the properties of alternative LWAs in this study were slightly, but not significantly, inferior. Alternative LWA becomes attractive when considering that expanded clay LWA requires more energy during the sintering process.

The Influence of Superabsorbent Polymers and Nanosilica on the Hydration Process and Microstructure of Cementitious Mixtures.

Superabsorbent polymers (SAPs) are known to mitigate the development of autogenous shrinkage in cementitious mixtures with a low water-to-cement ratio. Moreover, the addition of SAPs promotes the self-healing ability of cracks. A drawback of using SAPs lies in the formation of macropores when the polymers release their absorbed water, leading to a reduction of the mechanical properties. Therefore, a supplementary material was introduced together with SAPs, being nanosilica, in order to obtain an identical compressive strength with respect to the reference material without additives. The exact cause of the similar compressive behaviour lies in the modification of the hydration process and subsequent microstructural development by both SAPs and nanosilica. Within the present study, the effect of SAPs and nanosilica on the hydration progress and the hardened properties is assessed. By means of isothermal calorimetry, the hydration kinetics were monitored. Subsequently, the quantity of hydration products formed was determined by thermogravimetric analysis and scanning electron microscopy, revealing an increased amount of hydrates for both SAP and nanosilica blends. An assessment of the pore size distribution was made using mercury intrusion porosimetry and demonstrated the increased porosity for SAP mixtures. A correlation between microstructure and the compressive strength displayed its influence on the mechanical behaviour.

Severe Sulfuric Acid Attack on Self-Compacting Concrete with Granulometrically Optimized Blast-Furnace Slag-Comparison of Different Test Methods.

The corrosion by severe sulfuric acid attack at pH 2 of two self-compacting concrete (SCC) types that are based on ordinary Portland cement (OPC) and granulometrically optimized blast-furnace slag cement was evaluated by three complementary tests that were performed in different research institutes. The use of SCC is a smart and promising solution to improve the performance of concrete in an aggressive environment, especially regarding ready-mixed concrete applications, since good compaction is less dependent on workmanship. The relevance and practical advantages of the different test protocols and the influence of the experimental parameters are discussed. It appears that the frequency of renewing the acid solution during the exposure period is the main parameter that influences the mass loss and the rate of degradation, while the sample geometry and the ratio between the volume of solution and concrete surface area had no clear influence. Nevertheless, there was reasonable agreement between the methods regarding the magnitude of the concrete degradation (resulting in a mass loss of about 2.5 kg/m² in six months time). The use of granulometrically optimized slag cement provided a moderate increase of the concrete resistance against acid attack, and this practice might be recommended in order to increase the durability of structures exposed to sulfuric acid media. The fact that the difference in comparison with SCC-OPC was rather limited shows that the influence of the cement type becomes less relevant in the case of concrete with low w/c ratio and optimized concrete technology.

Evaluation of the Self-Healing Ability of Mortar Mixtures Containing Superabsorbent Polymers and Nanosilica.

Addition of superabsorbent polymers (SAPs) to cementitious mixtures promotes the self-healing ability of the material. When cracking occurs; SAPs present inside the crack will swell upon contact with water and subsequently release this water to stimulate the further hydration of unhydrated cement particles and the calcium carbonate crystallization. However; the inclusion of SAPs affects the mechanical performance of the cementitious material by the creation of macro-pores as water is retracted from the swollen SAP. To counteract the reduction in strength, part of the cement is replaced by nanosilica. In this research, different mixtures containing either SAPs or nanosilica and a combination of both were made. The samples were subjected to wet-dry cycles simulating external conditions, and the self-healing efficiency was evaluated by means of the evolution in crack width, by optical measurements, and a water permeability test. In samples containing SAPs, an immediate sealing effect was observed and visual crack closure was noticed. The smaller influence on the mechanical properties and the good healing characteristics in mixtures containing both nanosilica and SAPs are promising as a future material for use in building applications.