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The RILEM technical committee TC 247-DTA ‘Durability Testing of Alkali-Activated Materials’ conducted a round robin testing programme to determine the validity of various durability testing methods, originally developed for Portland cement based-concretes, for the assessment of the durability of alkali-activated concretes. The outcomes of the round robin tests evaluating sulfate resistance, alkali-silica reaction (ASR) and freeze–thaw resistance are presented in this contribution. Five different alkali-activated concretes, based on ground granulated blast furnace slag, fly ash, or metakaolin were investigated. The extent of sulfate damage to concretes based on slag or fly ash seems to be limited when exposed to an Na2SO4 solution. The mixture based on metakaolin showed an excessive, very early expansion, followed by a dimensionally stable period, which cannot be explained at present. In the slag-based concretes, MgSO4 caused more expansion and visual damage than Na2SO4; however, the expansion limits defined in the respective standards were not exceeded. Both the ASTM C1293 and RILEM AAR-3.1 test methods for the determination of ASR expansion appear to give essentially reliable identification of expansion caused by highly reactive aggregates. Alkali-activated materials in combination with an unreactive or potentially expansive aggregate were in no case seen to cause larger expansions; only the aggregates of known very high reactivity were seen to be problematic. The results of freeze–thaw testing (with/without deicing salts) of alkali-activated concretes suggest an important influence of the curing conditions and experimental conditions on the test outcomes, which need to be understood before the tests can be reliably applied and interpreted.
Additive manufacturing (AM) of alkali-activated materials is a promising method for producing ceramic precursors, construction elements and other parts. A recently introduced AM process is laser-induced slip casting of lithium aluminate/microsilica slurries, which yields parts with excellent mechanical strengths. To clarify the underlying mechanisms, μ-Raman spectroscopy was applied to parts produced by the process, and the dissolution and hydration of lithium aluminate was studied inter alia using conventional and in-situ X-ray diffraction. The results show that significant dissolution of lithium aluminate occurs, particularly at increased temperatures during laser interaction, which leads to an increase of pH and precipitation of an akopovaite-like Li-Al-CO3 layered double hydroxide. The increase of the pH is likely to induce dissolution of the microsilica and possibly formation of a hydrous lithium aluminosilicate gel. These observations explain the strength evolution of the studied parts and can also aid the development and improvement of related AM methods.
In this study, a multi-proxy approach combining 29Si, 27Al and 1H MAS-NMR, FEG-EPMA, XANES at the Cu K-edge and XRD analytics with hydrochemical tools such as ICP-OES analyses, oxygen-isotope signatures, and thermodynamic modelling was applied to K-silicate-activated metakaolin specimens - with and without CuSO4·5H2O addition - exposed to sulfuric acid at pH = 2 for 35 days. The results revealed a multistage deterioration mechanism governed by (i) acid diffusion, (ii) leaching of K-A-S-H, (iii) microstructural damage related to precipitation of expansive (K,Ca,Al)-sulfate-hydrate phases (iv) complete dissolution of the K-A-S-H framework, (v) and formation of silica gel in the outermost corroded regions. Copper ions were mainly located in layered spertiniite-chrysocolla-like phases in the as-cured materials. The results demonstrate an overall negative effect of Cu addition on chemical material durability, implying that the reported higher durability of Cu-doped AAM in biocorrosion environments can be best explained by bacteriostatic effects.
Der kritische, Korrosion auslösende Chloridgehalt für die Beurteilung der Korrosions-beständigkeit von Betonstahl in Geopolymerbetonen ist von großer Bedeutung für die Dauerhaftigkeitsprognose für bewehrte Elemente aus solchen Materialien. Es sind kaum experimentelle Daten in der Fachliteratur vorhanden und die vorliegenden Werte unterscheiden sich zwischen den Studien erheblich. In diesem Projekt wurde der kritische, Korrosion auslösende Chloridgehalt für Betonstahl (BSt 500) in flugaschebasierten (Ca-armen) Geopolymermörtel für verschiedene Beaufschlagungskombinationen bestimmt: Chloridbeaufschlagung mit 1 M NaCl-Lösung; Auslaugen in entionisiertem Wasser und anschließende Chloridbeaufschlagung im 1 M NaCl-Lösung; Auslaugen in entionisiertem Wasser, Carbonatisierung in Luft bei 20 °C und natürlicher CO2 Konzentration und anschließende Chloridbeaufschlagung mit 1 M NaCl-Lösung. Für Referenz-Zwecke wurde zusätzlich der Korrosion auslösende Chloridgehalt für eine Portland-Zement Mischung bei Auslagerung in 1 M NaCl-Lösung bestimmt.
Properties of alkali-activated mortars with salt aggregate for sealing structures in evaporite rock
(2021)
Concrete structures for sealing of tunnels in the host rock are an essential part of systems for nuclear waste storage. However, concretes based on blended cements or magnesium oxychloride cements, which are commonly considered for this application, can deteriorate severely due to a significant heat of hydration and associated deformation and cracking. Alkali-activated materials (AAMs) offer a potential solution to this problem because of their low heat release during hardening. To explore their suitability for the construction of sealing structures in evaporite rock, various AAMs with salt aggregate were studied regarding fresh properties, heat release, mechanical properties and microstructure. The heat of reaction of the AAMs was up to 55% lower than that of a blended cement designed for sealing structures, indicating significant benefits for the intended application. Other relevant properties such as mechanical strength and permeability depended strongly on the mix-design of the AAMs and curing conditions.
The contribution reports on durability-related transport properties of geopolymer-based mortars. We show results of accelerated carbonation, rapid chloride migration (RCM), accelerated chloride diffusion, and air permeability measurements for fly ash-based geopolymer mortars, including mixes containing ground granulated blast furnace slag (GGBFS). In addition, we report polarization resistance data and corrosion potential vs. time curves for carbon steel bars embedded in two of the fly ash-based geopolymer mortars and a CEM I-based mortar (as reference).
Despite comparable total porosities, the carbonation depths, the chloride migration coefficients and the air permeabilities of the mortars differed significantly. In general, the addition of GGBFS to the binders improved the performance (decreased transport coefficients); however, this was not found to be true for the air permeability in all cases. This latter effect can be explained by drying damage of the C-(A-)S-H gel in GGBFS-containing binders. On the other hand, low transport coefficients can also be achieved by optimization of the binder formulation without the addition of GGBFS, which is also reflected in the material’s air permeability.
The corrosion potential vs. time curves in combination with polarization resistance values reveal that the steel reinforcement in geopolymer mortars assumed a passive state. However, this happened considerably later than for steel in CEM I-based mortars. The free corrosion potential of carbon steel reinforcement in the geopolymer mortars had different values than the free corrosion potential values for the CEM I-based mortar for both the active and the passive state.
The development of alkali‐activated materials (AAMs) as an alternative to Portland cement (PC) has seen significant progress in the past decades. However, there still remains significant uncertainty regarding their long term performance when used in steel‐reinforced structures. The durability of AAMs in such applications depends strongly on the corrosion behaviour of the embedded steel reinforcement, and the experimental data in the literature are limited and in some cases inconsistent. This letter elucidates the role of the chemistry of AAMs on the mechanisms governing passivation and chloride‐induced corrosion of the steel reinforcement, to bring a better understanding of the durability of AAM structures exposed to chloride. The corrosion of the steel reinforcement in AAMs differs significantly from observations in PC; the onset of pitting (or the chloride ‘threshold’ value) depends strongly on the alkalinity, and the redox environment, of these binders. Classifications or standards used to assess the severity of steel corrosion in PC appear not to be directly applicable to AAMs due to important differences in pore solution chemistry and phase assemblage.
Additive manufacturing (3D printing) of ceramics and other materials offers significant advantages compared to conventional production processes for several applications. While ceramics have been extensively investigated in this regard, additive manufacturing of geopolymers have received much less attention to date. In the present contribution we study a ‘standard’ metakaolin-based geopolymer, a fly ash-based geopolymer and a silica-based one-part geopolymer regarding their suitability for additive manufacturing via selective laser curing. Model geometries such as bars and cuboids could be produced by this route. After selective laser curing the specimens were additionally cured at 80 °C for 24 h. The specimens were studied by means of scanning electron microscopy (SEM) and powder X-ray diffraction (XRD). SEM showed that the precursors in all geopolymers had reacted partially and geopolymeric gel had formed. XRD confirmed these results and additionally revealed that the crystalline byproducts (zeolites) in the one-part geopolymer differed from the byproducts observed in conventionally produced samples. This indicates that also the geopolymerization reactions differ between the two synthesis routes. The mechanical strength after selective laser curing and 80 °C-curing appeared to be highest for the metakaolin-based geopolymer. However, SEM also showed that a significant volume of macropores remained in most regions of all specimens, while some regions in the metakaolin-based geopolymer appeared to be significantly denser. These preliminary results demonstrate that selective laser curing offers potential for the production of geopolymers, but more research has to be undertaken to optimize the process.
Die Bestimmung der Rauheit von Bauteiloberflächen stellt eine wichtige Messaufgabe im Bauwesen dar. Vor allem bei der Betoninstandsetzung, im Straßenbau und bei der Herstellung von Stahlbeton-Halbfertigteilen ist die Rauheit – gemessen als Rautiefe – eine wichtige Kenngröße. Zurzeit werden Messungen der Rautiefe mittels volumetrischer Verfahren (Sandflächenverfahren) durchgeführt. Diese bereits seit mehreren Jahrzehnten angewandten Verfahren sind jedoch auf horizontale bzw. wenig geneigte und trockene Oberflächen beschränkt. Darüber hinaus hängen die erzielten Ergebnisse sehr stark von der angewandten Prüfvorschrift, den darin vorgeschriebenen Prüfmitteln und Geräten und dem jeweiligen Anwender ab.
Als Alternative zu den volumetrischen Verfahren wurde an der Bundesanstalt für Materialforschung und -prüfung (BAM) ein automatisiertes, laserbasiertes Messverfahren entwickelt, mit dem Rautiefen von Bauteiloberflächen in Anlehnung an bereits standardisierte Verfahren bestimmt werden können. Der vorliegende Beitrag befasst sich zunächst mit den konventionellen Prüfverfahren, beschreibt die wichtigsten Zusammenhänge und zeigt die Grenzen dieser Methoden auf. Im zweiten Teil wird das an der BAM entwickeltes Messsystem, als zielführendes Alternativverfahren für die konventionellen Methoden, vorgestellt und dessen Leistungsfähigkeit näher beschrieben.
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 aluminosilicate gel-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 aluminosilicate gel-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 composites, exhibit high resistance to sulfuric acid attack, making them promising materials for the construction and the repair of industrial and sewer structures.