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Two fly ash-based geopolymer concretes with quartz aggregates or with expanded clay (lightweight) aggregates were exposed to the ISO 834-1 standard fire curve in a small-scale fire test set-up. Acoustic emission measurements during fire exposure and subsequent cooling were employed to study spalling events and cracking during the tests. Optical microscopy and additional acoustic measurements were conducted after the testing to better understand the crack propagation in the samples. The testing revealed that neither of the concretes were susceptible to spalling, which is particularly notable for the concrete with quartz aggregates, as it is a high-strength concrete. This behavior is attributed to the relatively high permeability of the concretes and their low amount of chemically bound water. Significant crack formation was detected only around the temperature of the alpha–beta quartz transition (573 °C) and on cooling. Because of aggregate deformations at the quartz transition temperature, deterioration after heating was more significant in the geopolymer concrete with quartz aggregates. Crack formation also occurred in the concrete with expanded clay aggregates, caused by shrinkage of the geopolymer paste on cooling. Acoustic emission measurements proved to be a valuable tool to investigate processes during high temperature exposure.
Application of electrochemical methods for studying steel corrosion in alkali-activated materials
(2023)
Alkali-activated materials (AAMs) are binders that can complement and partially substitute the current use of conventional cement. However, the present knowledge about how AAMs protect steel reinforcement in concrete elements is incomplete, and uncertainties exist regarding the application of electrochemical methods to investigate this issue. The present review by EFC WP11-Task Force ‘Corrosion of steel in alkali-activated materials’ demonstrates that important differences exist between AAMs and Portland cement, and between different classes of AAMs, which are mainly caused by differing pore solution compositions, and which affect the outcomes of electrochemical measurements. The high sulfide concentrations in blast furnace slag-based AAMs lead to distinct anodic polarisation curves, unusually low open circuit potentials, and low polarisation resistances, which might be incorrectly interpreted as indicating active corrosion of steel reinforcement. No systematic study of the influence of the steel–concrete interface on the susceptibility of steel to corrosion in AAMs is available. Less common electrochemical methods present an opportunity for future progress in the field.
The RILEM TC 281–CCC "Carbonation of concrete with supplementary cementitious materials" is studying the effect of supplementary cementitious materials (SCMs) on natural and accelerated carbonation of blended cements. In this context a large database with carbonation depths over time has been set-up with currently 910 concrete and mortar mixes, which have been tested at different curing conditions. The collected data includes information on chemical composition and physical properties of the raw materials, on mix-design, compressive strength, curing and carbonation testing conditions. Data for a large variety of binders (with up to 94 % SCMs) and mix designs (with w/b ratios ranging from 0.26 to 0.75) were collected from the literature and unpublished material testing projects. Natural carbonation was recorded for several years in many cases, and indoor as well as outdoor results are included. However, in this contribution only lab conditions are considered. Carbonation kinetics are investigated considering the binder composition and mix design. Furthermore, the accuracy of accelerated carbonation testing is evaluated. As described in literature, the w/CaOreactive-ratio is a decisive factor for carbonation resistance but curing and exposure conditions influence the results as well. Even with identical test conditions, the scatter is very large.
The aim of this chapter is to give an overview of basic and advanced state-of-the-art microstructural and spectroscopic analytics to investigate inorganic material corrosion in the context of biochemically aggressive sewers. The chapter covers optical methods, electron beam, X-ray and neutron techniques (SEM, MLA, XRF, XRD, CT, Neutron radiography and tomography), and spectroscopic methods (MAS-NMR, FT-IR, and Raman). For each technique, a short section on the fundamental scientific background of the method precedes and examples of data output from the latter in respect to the corrosion of cementitious materials including reinforced concrete is presented.
Alkali-activated materials such as geopolymers are currently receiving a lot of attention because of their potential to be used as binders for concrete with advantageous engineering properties and reduced manufacturing CO2 emissions. Knowledge of the durability of steel in these concretes and related properties of alkali-activated materials is a prerequisite for their application as building materials, if they are to be used for steel reinforced elements. However, to date only limited data exists on this topic. The present contribution focuses on durability-related transport properties of geopolymer-based mortars (as model systems for concrete). We report results of accelerated carbonation, rapid chloride migration (RCM) and air permeability measurements as well as porosity data 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. Thus, there exists no simple correlation between air permeability (of harshly dried mortars) and durability-related transport coefficients for the studied alkali-activated materials.
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; possible reasons for this behavior are discussed.
Alkali-activated materials such as geopolymers are currently receiving a lot of attention because of their potential to be used as binders for concrete with advantageous engineering properties and reduced manufacturing CO2 emissions. Knowledge of the durability of steel in these concretes and related properties of alkali-activated materials is a prerequisite for their application as building materials, if they are to be used for steel reinforced elements. However, to date only limited data exists on this topic. The present contribution focuses on durability-related transport properties of geopolymer-based mortars (as model systems for concrete). We report results of accelerated carbonation, rapid chloride migration (RCM) and air permeability measurements as well as porosity data 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. Thus, there exists no simple correlation between air permeability (of harshly dried mortars) and durability-related transport coefficients for the studied alkali-activated materials.
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; possible reasons for this behavior are discussed.
Concretes produced from salt aggregate and hybrid alkaline cements, an alkali-activated slag/fly ash blend, or a Portland cement were exposed to a magnesium chloride-rich saline solution ([Mg2+] = 3.6 m, [Cl−] = 8.3 m), representing a solution formed after contact of surface water with evaporite rock (rock salt) in a nuclear waste repository. The hydration and deterioration of the concretes were studied with X-ray diffraction, thermogravimetric analysis, pH mapping and permeability measurements. The results show that calcium silicate hydrate (C-S-H) or sodium-substituted calcium aluminium silicate hydrate (C-N-A-S-H) and Friedel's salt were the major reaction products in the concretes prior to exposure to the saline solution. During exposure to the saline solution, increasing amounts of C-S-H/C-N-A-S-H dissolved, and gypsum and a secondary AFm phase formed. The durability of the concretes improved with increasing amounts of Portland clinker in the cements, due to the associated differences in permeability and chemical resistance. Nevertheless, a massive increase of permeability occurred for all concretes, likely caused by crack formation due to the formation of gypsum from anhydrite in the salt aggregate. Thus, the behavior of the concretes differed from, and was more complex than, the behavior of plain cement pastes.
Blast furnace cements (CEM III) and alkali-activated slags are binders for concretes with several advantageous engineering properties, and their increased adoption in construction industry could contribute to reducing the CO2 emissions associated with cement production and use. However, the current knowledge about how these cements protect steel reinforcement in concretes against corrosion is very incomplete, which impedes their large-scale application. This knowledge gap is mainly due to the fact that these cements release sulfide and other reduced sulfur species into the concrete pore solution, the consequences of which for the state of the reinforcement and electrochemical measurements are not fully understood.
The present contribution first describes peculiarities of electrochemical measurements of steel in sulfide-containing cementitious materials and related solutions as reported in the literature and a recent report by EFC Working Party 11. It is demonstrated that the high sulfide concentrations in these systems lead to low open circuit potentials and low polarisation resistances, which may be incorrectly interpreted as indicating active corrosion of the steel.
Second, preliminary results of an ongoing project [funded by the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) – 458297195] related to the passivation and corrosion initiation of steel in sulfide-containing solutions and mortars are presented. Eight mortars based on one alkali-activated blast furnace slag (BFS), three alkali-activated BFS/fly ash blends, one sodium sulfate-activated CEM III/C (‘hybrid cement’), one CEM III/C, one CEM III/B, and one CEM I (ordinary Portland cement, OPC) were produced, and their pore solutions expressed and analysed after 7, 14, 28, and 56 days of curing. The pH values of the solutions differed systematically, with the highest pH values recorded for the CEM I and the alkali-activated BFS/fly ash blends with a high proportion of fly ash, and the lowest pH recorded for the CEM III/B. The redox potentials of the solutions were between −500 mV and −340 mV vs. Ag/AgCl for the alkali-activated binders, approx. +10 mV vs. Ag/AgCl for the CEM I, and in between for the CEM III/B and the CEM III/C. As expected, the electrical conductivity was highest for the alkali-activated binders. These results are explained by the chemical compositions of the pore solutions of the mortars.
Finally, a test set-up to investigate the behaviour of steel in sulfide-containing solutions and the changes on subsequent oxygen and/or chloride addition is introduced. Preliminary electrochemical measurements of steel in sulfide-containing solutions are presented and discussed in the context of the above-mentioned data from the literature and the compositions of the pore solutions of the studied mortars.