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The 87Sr/86Sr isotope ratio can, in principle, be used for provenancing of cement. However, while commercial cements consist of multiple components, no detailed investigation into their individual 87Sr/86Sr isotope ratios or their influence on the integral 87Sr/86Sr isotope ratio of the resulting cement was conducted previously. Therefore, the present study aimed at determining and comparing the conventional 87Sr/86Sr isotope ratios of a diverse set of Portland cements and their corresponding Portland clinkers, the major component of these cements. Two approaches to remove the additives from the cements, i.e. to measure the conventional 87Sr/86Sr isotopic fingerprint of the clinker only, were tested, namely, treatment with a potassium hydroxide/sucrose solution and sieving on a 11-µm sieve. Dissolution in concentrated hydrochloric acid/nitric acid and in diluted nitric acid was employed to determine the 87Sr/86Sr isotope ratios of the cements and the individual clinkers. The aim was to find the most appropriate sample preparation procedure for cement provenancing, and the selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated cements with those of the corresponding clinkers. None of the methods to separate the clinkers from the cements proved to be satisfactory. However, it was found that the 87Sr/86Sr isotope ratios of clinker and cement generally corresponded, meaning that the latter can be used as a proxy for the clinker 87Sr/86Sr isotope ratio. Finally, the concentrated hydrochloric acid/nitric acid dissolution method was found to be the most suitable sample preparation method for the cements; it is thus recommended for 87Sr/86Sr isotope analyses for cement provenancing.
Monitoring of repositories for radioactive waste requires techniques which can be applied long-term under harsh conditions. In this work, the reliability and suitability of materials and a capacitive sensor for measuring relative humidity are investigated, which are to be embedded in the special concrete components for the closure structures of underground repository. Preliminary tests with accelerated aging of the materials used, validation of the sensors under difficult conditions, investigations of the surfaces after aging by pH 14 solution, defined exposure of the sensors in a climatic chamber and the microscope images are discussed. The results will be used for further development and optimization of the RFID based sensor systems which can be applied to monitor the condition of different building structures without cabling.
Within the project SealWasteSafe, we advance construction materials and monitoring concepts of sealing structures applied for underground disposal of nuclear or toxic waste. As these engineered barriers have high demands concerning integrity, an innovative alkali-activated material (AAM) is improved and tested on various laboratory scales. This AAM has low reaction kinetics related to a preferential slow release of the heat of reaction in comparison to alternative salt concretes based on Portland cement or magnesium oxychloride cements. Hence, crack formation due to thermally induced strain is reduced. After successful laboratory scale analysis (Sturm et al., 2021), the AAM is characterised on a larger scale by manufacturing test specimens (100–300 L).
Conventional salt concrete (DBE, 2004) and the newly developed AAM are compared using two specimen geometries, i.e. cylindrical and cuboid. A comprehensive multisensor monitoring scheme is developed to compare the setting process of AAM and salt concrete for these manufactured specimens. The analysed parameters include temperature and humidity of the material, acoustic emissions, and strain variations. Passive sensor systems based on radiofrequency identification technology (RFID) embedded in the concrete, enable wireless access to temperature and humidity measurements and are compared to conventional cabled systems. Additionally, fibre-optic sensors (FOS) are embedded to record strain, but also have potential to record temperature and moisture conditions. Part of this project aims at demonstrating the high reliability of sensors and also their resistance to highly alkaline environments and to water intrusion along cables or at sensor locations. Further technical improvements were implemented so that first results clearly show the scalability of the setting process from previous small-scale AAM experiments and particularly the high potential of the newly developed approaches.
Furthermore, ultrasonic methods are used for quality assurance to detect obstacles, potential cracks and delamination. On the one hand, both active and passive ultrasonic measurements complement the results obtained from the multisensor monitoring scheme for the produced specimens. On the other hand, the unique large aperture ultrasonic system (LAUS) provides great depth penetration (up to nearly 10 m) and can thus be applied at in situ sealing structures built as a test site in Morsleben by the Federal Company for Radioactive Waste Disposal (Bundesgesellschaft für Endlagerung, BGE) as shown by Effner et al. (2021). An optimised field lay-out identified from forward modelling studies and advanced imaging techniques applied to the measured data will further improve the obtained results. To characterise the inside of the test engineered barrier and achieve a proof-of-concept, an ultrasonic borehole probe is developed to enable phased arrays that can further improve the detection of potential cracks. Modelling results and first analysis of semispherical specimens confirmed the reliability of the directional response caused by the phased arrays of the newly constructed ultrasonic borehole probe.
Overall, the project SealWasteSafe improves the construction material, multisensor monitoring concepts and ultrasonics for quality assurance. This will help to develop safe sealing structures for nuclear waste disposal. The outcomes are particularly valuable for salt as a host rock but partly also transferrable to alternative conditions.
Due to environmental concerns regarding the use of Portland cement as the principal binder material in concrete and mortar it is imperative to identify alternative materials that could reduce the carbon footprint of the construction industry. One alternative to address these issues is the use of alkali activated materials, in particular, when based on waste streams that currently have no or only limited industrial application. This paper reports a preliminary study into the synthesis of geopolymer mortar utilizing Brown Coal Fly Ash. The ash had a CaO content of ~39%, indicating that synthesis at ambient or low temperature may be feasible. The paper reports initial trials on the effect of curing temperature, ambient to 120 °C, on the mechanical properties of the mortars produced. The results showed that ambient cured mortar achieved a compressive strength of 6.5 MPa at 3 days. A curing temperature of 60 °C gave the optimum results with a compressive strength of almost 20 MPa and a flexural strength of 3.5 MPa obtained.
Die Hauptfunktion von Verschlussbauwerken für End- und Zwischenlager von radioaktiven Abfällen besteht in der Erhaltung der geologischen Barriere. Vor allem soll ein potenzieller Stofftransport durch eine möglichst geringe Permeabilität des Bauwerks verhindert bzw. auf vernachlässigbare Werte herabgesetzt werden. Die in-situ-Permeabilität des Verschlussbauwerks steht dabei in direktem Zusammenhang mit dessen Poren- und Makrostruktur, welche bei Bauwerken auf Basis von Beton insbesondere durch Schwind-verformungen und durch thermisch induzierte Rissbildung infolge der Reaktionswärmeentwicklung des Bindemittels gestört werden kann. Die Betone müssen daher neben einer hohen chemischen Langzeitstabilität auch eine geringe bzw. langsame Wärmeentwicklung während der Erhärtungsreaktionen aufweisen. Als hybride Zemente werden Mischungen aus Portlandzement, Betonzusatzstoffen und einem alkalischen Aktivator bezeichnet. Dabei können u. a. Alkalisulfate, Alkalicarbonate, Alkalisilicate und Alkalihydroxide als Aktivatoren zum Einsatz kommen. Aufgrund ihrer hohen chemischen Stabilität im salinaren Milieu sind Betone aus solchen Zementen potenziell besonders gut als Verfüllmaterial für End- und Zwischenlager im Steinsalz geeignet. In der vorliegenden Studie wurden daher hybride Zemente hinsichtlich ihrer Wärmeentwicklung in einem isothermen Kalorimeter sowie hinsichtlich Phasenbestand und Festigkeiten untersucht. Hybride Zementleime wurden auf Basis von Portlandklinker, Hüttensandmehl, Flugasche und Natriumsulfat hergestellt und die Zusammensetzungen systematisch variiert, um den Einfluss der Komponenten auf Wärmeentwicklung, Phasenbestand und mechanische Eigenschaften der Leime zu untersuchen; zusätzlich wurden zu Vergleichszwecken ein Zementleim auf Basis der Betonrezeptur M2 sowie eine alkalisch aktivierte Flugasche untersucht.
Hybrid cements are composites made of Portland cement or Portland clinker and one or more supplementary cementitious materials like slag, fly ash or metakaolin, activated with an alkali salt. To date, their hydration mechanism and the phase formation at various temperatures is insufficiently understood, partly due to the large variability of the raw materials used. In the present study, three hybrid cements based on ground granulated blast furnace slag, fly ash, Portland clinker and sodium sulfate, and an alkali-activated slag/fly ash blend were cured at 10 and 21.5°C, and subsequently analyzed by XRD, 27Al MAS NMR, and TGA. The compressive strength of the hybrid cements was higher by up to 27% after 91-day curing at 10°C, compared to curing at 21.5°C. The experimental results as well as thermodynamic modeling indicate that the differences in compressive strength were related to a different phase assemblage, mainly differing amounts of strätlingite and C-N-A-S-H, and the associated differences of the volume of hydration products. While the strätlingite was amorphous to X-rays, it could be identified by 27Al MAS NMR spectroscopy, TGA and thermodynamic modeling. The microstructural properties of the hybrid cements and the alkali-activated slag/fly ash blend as well as the compatibility between thermodynamic modeling results and experimental data as a function of curing temperature and time are discussed.
The project "SealWasteSafe" of the Bundesanstalt für Materialforschung und -prüfung (BAM, Berlin) deals with sealing structures applied for underground disposal of nuclear waste from two perspectives: (1) material improvement for application in sealing constructions and (2) feasibility study regarding multi-sensor approaches to ensure quality assurance and long-term monitoring.
One specimen of 150 l made of alkali-activated material, which was found innovative and suitable for sealing constructions based on preliminary laboratory studies, and, for comparison purpose, another one made of salt concrete, are manufactured with an integrated multi-sensory setup for quality assurance and long-term-monitoring. The specimens were left in their cast form and additionally thermally insulated to simulate the situation in the repository. The multi-sensory concept comprises RFID technology embedded in the specimens suppling material temperature and moisture measurements, integrated fibre optic sensing allowing strain measurement and acoustic emission testing for monitoring possible crack formation. Overall, the suitability and the functionality of the sensors embedded into and attached to strongly alkaline (pH > 13 for the AAM) and salt corrosive (NaCl) environment was proven for the first 672 h.
First temperature measurement based on RFID succeeded after 626 h for the alkali-activated material and after 192 h for the conventional salt concrete. Strain measurement based on distributed fibre optic sensing turned out the alkali-activated material with > 1 mm m-1 undergoing approximately twice the compression strain as the salt concrete with strains < 0.5 mm m-1. In contrast, the acoustic emission first and single hits representing crack formation in numbers, was found for alkali-activated material half of that detected at the salt concrete.
One-part geopolymers offer advantages over conventional geopolymers with regard to handling and storage of feedstocks. However, they often suffer from a low degree of reaction, a high amount of crystalline byproducts, and consequently low strength. In this study, one-part geopolymers were produced from rice husk ash (RHA) and sodium aluminate, and investigated by XRD, ATR-FTIR, SEM and compressive strength testing. The compressive strength of the material was 30 MPa, i.e. significantly higher than for comparable one-part geopolymers. This is attributed to an almost complete reaction of the RHA and the absence of crystalline byproducts (zeolites) in the hardened geopolymer.
Chemical admixtures like superplasticisers or stabilising agents are of ever increasing importance for modern concrete technology. They liberate the workability of concrete from its dependency on water content, and thus, open the gate towards innovative and future oriented concrete technologies such as selfcompacting concrete. Meanwhile admixtures have become common practice in concrete technology, but the understanding of these highly complex polymers in the entire concrete system lags far behind their application. Due to its complex time-dependent, multi-phase and multi-scale behaviour, flowable concrete systems are highly complicated and cannot be described comprehensively by simple models. It is therefore extremely challenging to identify the relevant parameters that predominantly control flow phenomena on different size scales, since these may occur on any scale between the nano scale (e.g. superplasticizer adsorption) and macro scale (e.g. grading of the aggregates). The present study discusses fundamental mechanisms at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation, and links these effects to macroscopic flow phenomena. Methods are discussed that appear promising interdisciplinary tools for enhancement of the understanding of the relevant interactions that are responsible for the macroscopic flow of flowable concrete.
The production and processing of ordinary Portland cement are responsible for nearly 5% of the world C02 emissions. Due to the world’s increasing requirement for building materials, this air pollution is growing up in the next decades. Alternative cement such as geopolymers can reduce these emissions effectively, Conventional geopolymer binders, produced ffom fly ash or metakaolin as aluminosilicate source and water-glass or alkali hydroxide Solutions as activator, are often used and studied. It is known that under appropriate conditions the starting materials form a three-dimensional aluminosilicate structure and create a gel-like matrix, In our case, a silica source from wastewater treatment of chlorosilane production and solid sodium aluminate as starting materials are initiated to harden by water. This procedure is known as “just add water” or “one-part” geopolymer formulation. These composites have significant advantages for use on construction site, but their Chemical structure is not extensively analyzed. In this work, a well known one-part geopolymer is investigated by 'H and 27A1 magic-angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. Furthermore, it is shown that overlapping NMR lines can resolved with echo experiments and