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The current understanding of the carbonation of alkali-activated concretes is ham-pered inter alia by the wide range of binder chemistries used. To overcome some of the limitations of individual studies and to identify general correlations between their mix design parameters and carbonation resistance, the RILEM TC 281-CCC working group 6 compiled carbonation data for alkali-activated concretes and mortars from the literature. For comparison purposes, data for blended Portland cement-based concretes with a high percentage of SCMs (≥ 66 % of the binder) were also included in the database. A preliminary analysis of the database indicates that w/CaO ratio and w/b ratio exert an influence on the carbonation resistance of alkali-activated concretes but, contrary to what has been reported for concretes based on (blended) Portland cements, these are not good indicators of their carbonation resistance when considered individually. A better indicator of the carbonation resistance of alkali-activated concretes under conditions approxi-mating natural carbonation appears to be their w/(CaO + Na2O + K2O) ratio. Furthermore, the analysis points to significant shortcomings of tests at elevated CO2 concentrations for low-Ca alkali-activated concretes, indicating that even at a concentration of 1 % CO2, the outcomes may lead to inaccurate predictions of the carbonation coefficient under natural exposure conditions.
Slags from the nonferrous metals industry have great potential to be used as feedstocks for the production of alkali-activated materials. Until now, however, only very limited information has been available about the structural characteristics of these materials. In the work presented herein, synthetic slags in the CaO–FeOx–SiO2 system, representing typical compositions of Fe-rich slags, and inorganic polymers (IPs) produced from the synthetic slags by activation with alkali Silicate solutions have been studied by means of X-ray absorption near-edge structure (XANES) spectroscopy at the Fe K-edge. The iron in the slags was largely Fe2+, with an average coordination number of approximately 5 for the iron in the amorphous fraction. The increase in average oxidation number after alkali-activation was conceptualized as the consequence of slag dissolution and IP precipitation, and employed to calculate the degrees of reaction of the slags. The degree of reaction of the slags increased with increasing amorphous fraction. The iron in the IPs had an average coordination number of approximately 5; thus, IPs produced from the Fe-rich slags studied here are not Fe-analogs of aluminosilicate geopolymers, but differ significantly in terms of structure from the latter.
Alkali-activated slag materials are known for their high Chloride penetration resistance. This makes them potentially applicable as repair systems for damaged steel-reinforced concrete structures, which are exposed to chloride attack. For this purpose, the influence of the activator composition, i.e. the SiO2 and Na2O concentration of the alkaline solution on a) the compressive strength, b) shrinkage and mass change and c) the resistance against chloride penetration of four alkali-activated slag mortars (AASM) were studied. An ordinary Portland cement-based mortar was used as the reference sample. Increasing SiO2 and Na2O concentrations increased the strength, shrinkage and mass loss of the AASMs. The resistance of the mortars against chloride penetration was evaluated using the non-steady-state migration coefficient Dnssm obtained from NT BUILD 492. The results indicate that the Dnssm is related to differences in the pore solution of the AASMs rather than to differences in their microstructure. An upcoming study of the authors is going to evaluate this hypothesis by the accelerated chloride penetration (diffusion) test.
Mixing and curing of geopolymers and related alkali-activated materials without storage and handling of highly alkaline solutions possesses advantages regarding safety and economic viability; one possible approach is to produce these materials from solid silica feedstocks and solid sodium aluminate, and subsequent mixing with water. We present a comparison between geopolymers and geopolymer-zeolite composites synthesized by this route from different silica feedstocks (by-product silica from chlorosilane production, microsilica, rice husk ash) and with different SiO2/Al2O3 ratios, using results from XRD, NMR, SEM, thermal analysis, mechanical and acid resistance testing. The use of rice husk ash favors formation of a fully amorphous geopolymer with high strength. Utilization of the other silica feedstocks leads to formation of geopolymer-zeolite composites, the amount and kind of zeolites depending on the feedstock and the SiO2/Al2O3 ratio. These composites show beneficial dehydration behavior, viz. no distinct dehydration step of thermal strain, with the phase assemblage after heating to 1000 °C controlled by the starting composition. Mortars produced from both, the geopolymers as well as the compo¬sites, exhibit high resistance to sulfuric acid attack, making them promising materials for the construction and the repair of industrial and sewer structures.
One-part alkali-activated (geopolymer) mortars based on three different silica-rich starting materials and sodium aluminate, with and without ground granulated blast furnace slag (GGBFS) addition, were tested regarding sulfuric acid resistance according to DIN 19573:2016-03 (70 days at pH = 1). Corresponding pastes were characterized by XRD, SEM, chemical analysis, 29Si MAS NMR and 1H-29Si CPMAS NMR after water storage and after acid exposure. The mortars exhibited a high resistance against sulfuric acid attack, with the best ones conforming to the requirements of DIN 19573:2016-03. The analytical results showed that this was due to precipitation of silica gel at the acid-mortar interface, which formed a mechanically stable layer that protected the subjacent mortar and thus inhibited further degradation. The addition of GGBFS decreased the acid resistance via formation of expansive calcium sulfate phases.
One-part geopolymers (OPGs) are a sort of alkali-activated materials (AAMs) which production avoids the use of highly-alkaline activator-solutions and contributes to a better acceptance of alternative mineral binders in terms of safety-related and economic aspects. In the present contribution OPGs were synthesized by blending silica sources (two industrial silicas and two biogenic silicas) with sodium aluminate and only water must be added to initiate the hardening, i.e. mixing is performed in the same way as for conventional Portland cements. The OPGs were characterized by XRD, and SEM and the degrees of reaction of the silicas were determined by a chemical dissolution method.
The industrial silicas led to the formation of geopolymer-zeolite composites, that contained, besides geopolymeric gel, crystalline tectosilicates (e.g. zeolite A and hydrosodalite) and depending on the starting composition also unreacted silica. The biogenic silicas provided a higher reactivity and avoided the formation of crystallite by-products. The differences in the microstructures caused differences in the mechanical strength of the specimens.
The treatment of the OPG composites at moderate elevated temperatures revealed promising behavior on thermal dehydration in terms of shrinkage and residual strength up to 700 °C. Above 700 °C sintering and partial melting occurred, and new phase formation commenced. After exposure to 1000 °C the specimens appeared virtually amorphous or formed stuffed silica structures of nepheline- or carnegieite-type type.
The investigations of the OPG based mortars on their resistance against sulfuric acid in accordance with DIN 19573 (Appendix A) revealed very high residual strengths up to 78 % after treatment with H2SO4 (pH 1) for 70d. A mechanism of dissolution of the primary aluminosilicate reaction products of the pastes and the precipitation of a silica gel that protects the remaining aluminosilicates and decelerates further corrosion was found to be the main reason for the good performance under acidic conditions. The addition of CaO-containing feedstocks enhanced hardening, but at a certain content the resistance against sulfuric acid decreased, due to the formation of gypsum on exposure to sulfate.
In addition, the mortars exhibited excellent shrinkage behavior as well as good bond to concrete substrates with pull-off strength up to > 3 MPa. The workability of the fresh mortars provided very good manual applicability; automatic applications such as sprayed and spun mortars will require further optimization regarding rheological properties. In summary, the studied OPG are promising materials for the construction and the repair of concrete structures, such as sewers, that are affected by biogenic sulfuric acid corrosion.
Intumescent coatings for fire protection offer advantages over (non-intumescent) cementitious coatings and boards regarding speed of construction, architectural aesthetics, sometimes costs, and other features. However, conventional organic intumescent coatings as well as soluble silicate (waterglass) coatings form foams with low mechanical stability, and the latter coatings generally suffer from low resistance against humidity. Therefore, the search for novel intumescent coatings for more demanding conditions (e.g., abrasive environments) is a necessity in the context of steadily increasing requirements of society and industry.
In this contribution, we present results on intumescent aluminosilicate coatings for fire protection that form foams with significantly increased mechanical strength. Two base formulations, a metakaolin/silica-based mix, adapted from Krivenko et al., and a silica/corundum-based mix, developed at Curtin University, as well as formulations modified with additives (Al(OH)3, Mg(OH)2, B2O3, Na2B4O7), were applied to steel plates (75 mm × 75 mm) and exposed to simulated fire conditions (fire curve according to ISO 834-1:1999). Temperature-time curves were recorded to assess the degree at which the coatings insulated the substrate. In addition, XRD, TG, oscillatory rheometry, and SEM were employed to characterise the coatings.
The coatings were observed to partly expand during hardening due to H2 formation. When the hardened coatings were exposed to elevated temperatures they intumesced as expected, with the degree and nature of expansion dependent on the formulation. Oscillatory rheometry provided insights into the intumescent processes in an apparently brittle material. It revealed that the hardened aluminosilicate coatings became viscous (loss factor > 1) at 75–225 °C, in the temperature range of major water release, as opposed to a “standard” metakaolin-based geopolymer, which continued to behave as a solid. This explains the intumes¬cent behavior of the coatings, i.e. further expansion and foam formation. Microstructural analysis confirmed pore expansion and coalescence; XRD showed that the phases formed after heating (max. temperature ~840 °C) were of ceramic-type.
The fire protection (defined here as the time for the steel substrate to reach the critical temperature of 500 °C) depended mainly on the thick¬ness of the fully expanded coating, i.e. after intumescence. An alumino¬silicate coating free of additives with an original thickness of 12 mm was able to protect the steel for >30 min. The addition of 10 % anhydrous borax (Na2B4O7) caused a significant improvement, such that an original coating thickness of only 6 mm was sufficient to protect the steel for ~30 min. This was caused by the formation of sodium metaborate dihydrate (NaB(OH)4) in the coating that led to a significantly extended dehydration plateau in the temperature-time curve at ~100 °C during the fire exposure.
While calcined clays in general have been credited with a great potential to mitigate CO2 emissions related to cement production and consumption, calcined brick clays are currently understudied in this regard. In the present work, two brick clays, a low-grade kaolinitic clay, and a mixed clay composed of 50% brick clay and 50% low-grade kaolinitic clay were studied regarding transformations on calcination, and strength and durability performance as well as pore structure of mortars made with the blended cements. All calcined clays exhibited pozzolanic reactivity, with the performance of the brick clays inferior to the low-grade kaolinitic clay. However, the mixed clay performed very similar to the low-grade kaolinitic clay, which points to a viable option for optimal use of brick clays in cementitious systems. The carbonation resistance of the blended cement mortars was generally worse than that of the plain Portland cement mortar, as expected, but the former exhibited a significantly improved chloride penetration resistance. The latter improvement was due to pore structure refinement in the blended cement mortars, compared to the Portland cement mortar.
Materials with a high acid resistance are required in different important infrastructures. Examples include repair systems for sewer structures, where biogenic sulfuric acid corrosion is the major degradation mechanism. Low-calcium alkali-activated materials (AAMs) have been repeatedly observed to exhibit high acid resistance. However, the reasons for the high acid resistance of these materials were not fully under¬stood until recently, and the use of highly alkaline activator solutions to produce AAMs appears to hamper their commercial uptake. These issues have been tackled by characterising one-part AAMs and studying their alteration when exposed to sulfuric acid.
One-part AAMs were synthesized by mixing blends of solid silica and sodium aluminate with water, and subsequent curing at 60–80 °C. Acid resistance testing was performed according to DIN 19573, i.e. exposure to sulfuric acid at pH = 1 for 70 days. Characterisation of the cured and the acid-exposed materials was done by XRD, ATR-FTIR, SEM as well as 29Si, 27Al and 1H MAS NMR spectroscopy, including cross-polarisation and double-resonance methods.
Materials synthesized from industrial silicas were gel-zeolite composites, containing a substantial amount of unreacted ‘excess’ silica, while materials synthesized from rice husk ash were fully amorphous, containing ‘excess’ hydrous alumina. The sulfuric acid resistance of mortars based on these binders conformed to the requirements of DIN 19573 for sewer repair applications. The high acid resistance was caused by precipitation of silica gel at the mortar–solution interface, inhibiting further degradation. The presence of alumina gel may inhibit bacterial activity, potentially further improving performance in sewer environments.
The phase assemblage of silica/sodium aluminate-based one-part AAMs can be adjusted via choice of the silica starting material. Properly designed materials exhibit excellent acid resistance, caused by precipi¬tation of silica gel which protects subjacent regions, and they may also inhibit bacterial activity.
Alkali-activated materials are ideal for the repair of concrete structures in harsh environmental conditions due to their high durability in chemically aggressive environments. However, slag-based mortars, in particular, are prone to shrinkage and associated cracks. In this respect, the application of steel fibres is one solution to reduce the formation of shrinkage induced cracks and to improve post cracking behaviour of these mortars. This study investigated the influence of two different types of steel fibres on the tensile properties of two alkali-activated mortars. Direct tensile tests and single fibre pull-outs were performed to analyse the determining failure modes both on macro and micro scale. Mechanical testing was accompanied by non-destructive testing methods such as digital image correlation and acoustic emission for a detailed analysis of the fracture process.