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Thermally-induced moisture transport in high-performance concrete studied by X-ray-CT and 1H-NMR
(2019)
The thermohydraulic damage mechanism is one of the primary causes for explosive spalling of highperformance concrete. This paper presents the spatially- and temporally-resolved analysis of the thermally-induced moisture transport and reconfiguration processes by means of X-ray-CT and 1HNMR.
Thermal testing results for a high-performance concrete, which is sensitive to explosive spalling and which was prepared with and without added polypropylene fibres, are presented in this paper. These results indicate that the addition of fibres leads to a faster and deeper migration of the drying front and, thus, to a lower likelihood of vapour-pressure induced explosive spalling.
Intensified Alkali-Silica Reaction (ASR) damage has occurred on German roadways in recent years, leading to requirements for compulsory pre-construction investigation of aggregate alkali sensitivity using concrete tests with external alkali supply. However, since these tests are time-consuming and cost-intensive, there is interest in replacing them with a solubility test on pure aggregate in 0.1 M KOH solution at 80°C with a defined NaCl content (1wt.-%). In this context, the influence of aggregate pore structure on SiO2 and Al2O3 solubility was investigated in this project. This paper compares the results of porosity studies with X-ray Computed Tomography (3D-CT) and the Brunauer-Emmett-Teller (BET) method on individual quarried and river gravel granules of both rhyolite and greywacke. For visualization and quantification of both externally accessible and fully enclosed surfaces of granules using X-ray 3D-CT, special software tools were developed. The results demonstrated that the river gravel granules had significantly larger externally accessible surfaces than the quarried granules. BET measurements on individual stones showed, as expected, that measured surfaces were about three orders of magnitude larger than those from the X-ray 3D-CT analyses due to the higher spatial resolution of BET. There was no apparent correlation between the X-ray 3D-CT and BET surface areas. Mercury porosimetry measurements indicate that this may be due to the presence of significant porosity below the spatial resolution of the X-ray 3D-CT. A comparison of SiO2 and Al2O3 solubility measurements with the X-ray 3D-CT and BET surface area data resulted only in weak, inconclusive correlations, indicating the need for further experimental investigation.
Durch den großflächigen Einsatz der Computertomographie (CT) in unterschiedlichen Industriebereichen steigen auch die Anforderungen an die quantitative Bildanalyse. Subjektive Bildwahrnehmung muss durch objektive Algorithmen ersetzt werden. In diesem Artikel stellt die Bundesanstalt für Materialforschung und -prüfung (BAM), die seit den 1980er Jahren an der Entwicklung der industriellen CT beteiligt ist, anhand ausgewählter Beispiele den aktuellen Stand ihrer Analysemethoden an verschiedenen Anwendungsbeispielen der CT vor.
Unilateral thermal exposure of concrete building components induces moisture transport processes that have a significant influence on the spalling behaviour of dense high-strength concrete (HSC). These transport processes are based on evaporation and condensation mechanisms of liquid and gaseous water in the pores as well as the chemically bound water within the concrete. The low permeability of HSC and the formation of a saturated zone within building components (also known as a moisture clog) leads to high water-vapour pressures, which contributes to explosive spalling. The formation of these pressures has already been verified by means of pore-pressure measurement techniques. In addition, the redistribution of the moisture within concrete specimens subject to unilateral thermal exposure has been demonstrated on fractured surfaces. Investigations by means of the nuclear magnetic resonance (NMR) relaxometry technique and neutron radiography have shown one-dimensional changes in moisture distribution during thermal exposure.
However, none of these methods has been able to depict the moisture distribution in three dimensions (3D), so the link between pore size, concrete micro-structure and moisture content is missing. The research project presented in this paper aims to fill this gap by developing a new multi-level test methodology to characterise non-destructively the temporal course of spatial moisture distribution during unilateral thermal exposure. The procedure used during this programme included the collection of X-ray 3D-computed tomography (CT) measurements using a miniaturised specimen subjected to in-situ thermal exposure and the comparison of those CT results with the results of one-dimensional NMR-relaxometry before and after the heating process.
In the first step, a mobile heating device was developed, built and tested. To simulate a unilaterally-heated construction component, a cylindrical specimen made of HSC (Ø = 40 mm, L = 100 mm) was cast into an impermeable glass ceramic shell. The ceramic shell ensured a one-dimensional moisture flux and limited the thermal expansion of the concrete. An additional high-temperature wool (HTW) insulating shell ensured a one-dimensional heat flux. The heating device, which operated using infrared radiation (IR), allowed the unilateral heating of the specimens up to 300 °C using variable heating regimes.
In the second step, the mobile heating device was integrated into the CT-scanner, which enabled the collection of measurements before, during and after heating. By subtraction of successive 3D-CT images, X-ray attenuation differences could be resolved three-dimensionally in the specimen and interpreted as changes in the moisture content.
Initial results show that this test methodology can monitor the 3D changes of moisture content inside the specimen during thermal exposure. It enables the researcher to visualise areas with moisture accumulation as well as dehydrated areas inside the specimen. Comparative one-dimensional NMR-relaxometry measurements confirm the results of the CT image analysis.
It is known that the spalling risk of dense, high-strength concretes (HSC) can be reduced by the addition of polypropylene (PP) fibres and, in particular, PP-fibres that have been pre-treated using electron irradiation. It is presumed that the enhanced reduction in spalling resulting from electron irradiation pre-treatment of the fibres can be attributed to enhanced penetration of the molten fibre material into the micro-cracks around the fibres, due to their significantly decreased viscosity. So far there has been no experimental evidence for this. Against this background, this paper gives a com-parative analysis of the mode of action of PP-fibres with and without pre-treatment using multi-scale test methodology.
Initially, fire tests on small-scale building components with accompanying damage monitoring veri-fied that the amount of PP-fibres can be halved by using pre-treated PP-fibres without reducing the fire performance of HSC. Detailed investigations of PP-fibres carried out in a completed research project funded by DFG (the German Research Foundation) using digital scanning calorimetry and thermogravimetry measurements (DSC/TG) as well as viscometer measurements showed that the pre-treatment has no significant influence on the melting temperature of the PP-fibres. However, a drastic reduction of the melt viscosity due to the electron irradiation was detectable. Additional dila-tation tests showed that the expansion behaviour of both fibre types and their melts do not differ significantly [1]. Rather, both fibre types generate high pressures when their thermal expansion is hindered. Further detailed investigations by means of continuous heating tests with a low heating rate were carried out on separately produced concrete cylinders. These tests showed that the pre-treatment of the PP-fibres causes earlier dehydration in conjunction with stagnation of thermal expansion of the concrete cylinders (temperature reduction from 180 °C to 170 °C). This is accompanied by in-creased acoustic emission activity during the thermal expansion tests. This leads to the assumption that the pre-treatment of PP-fibres results in earlier micro-crack development. However, it was not possible to confirm this assumption by microscopic examination of drilling cores with a diameter of 30 mm exposed to defined temperatures in the range between 150°C and 300°C. Microscopic obser-vations and additional X-ray 3D computed tomography (3D-CT) scans on miniaturised drilling cores exposed to temperature cycles showed a similar networking of fibre beds by means of micro-cracks in HSC for both fibre types. However, energy dispersive X-ray spectroscopy and wavelength disper-sive X-ray spectroscopy revealed fundamental differences in the penetration capacity of the fibre melts of the two fibre types. The increased penetration of the pre-treated PP-fibre melt revealed in these tests, confirms the initial working hypothesis.
Although concrete itself is not a combustible material, concrete mixtures with high density, such has high-performance concretes (HPCs), are susceptible to significant damage during fires due to explosive spalling. Past research has shown that the inclusion of polymer fibers in high density concrete can significantly mitigate fire damage due to the contribution of the fibers to increased permeability levels at high temperature. This allows vapor pressures caused by the evaporation of internal water during fire to escape from the material without causing significant spalling. Recent microscopic investigations have also shown that the addition of polypropylene (PP) fibers to high-density HPC with a high amount of fine-aggregate has a considerable influence on the nature and character of crack formation due to autogenous shrinkage. Initial cracks, which originate from the fiber beds, undergo further expansion and propagation when concrete is subjected to thermal exposure in excess of 170 °C. It is thus of interest to determine whether the resulting cracks join the adjacent fiber beds and therefore contribute to a significant increase in the permeability of the concrete, which is directly correlated to lower pore pressures and reduced spalling during fire.
In this study, X-ray Computed Tomography (CT) was applied to provide a clear demonstration of the interaction between polymer fibers and cracking during thermal exposure. For this purpose, two concrete samples containing different polymer fiber types were subjected to incremental application of a defined thermal exposure. CT images were acquired before and after each thermal exposure and powerful image processing tools were used to segment the various material components, such as polymer fibers, cracks, aggregates and cement matrix, in each image. This enabled a detailed analysis of crack formation and propagation as well as the visualization and quantification of polymer fiber characteristics within the concrete. This paper will provide a description of the distribution and orientation characteristics of the polymer fibers within each sample obtained through the CT-based analysis. Using these results, the impact of fiber distribution and orientation characteristics on actual cracking geometries have been measured and visualized. This paper will also provide recommendations for further optimization of the selected materials and propose improved methods for future CT-based analysis techniques.
Water migration in one-side heated concrete: 4D in-situ CT monitoring of the moisture-clog-effect
(2019)
Explosive spalling due to fire exposure in concrete structures can lead severe damage and, in the worst case, to premature component failure. For this reason, an in situ investigation of water Migration in concrete due to surface heating was undertaken.
During these experiments, a miniaturized concrete specimen within a confining and insulating double-hull was subjected to surface heating during simultaneous X-ray computed tomography (CT) scanning. Through the use of subtraction-based Image analysis techniques, it was possible to observe and quantify not only drying within areas of the concrete matrix close to the heated surface, but also the migration of moisture to both pore and matrix regions deeper within the specimen. It was also discovered that the correction of CT images for specimen deformation using DVC and variable detector performance using calibrated image filters significantly improved the quality of the results. This clearly demonstrates the potential of X-ray CT for evaluation of other rapid-density-change phenomena in concrete and other building materials.
Although concrete itself is not a combustible material, concrete mixtures with high density, such has high-performance concretes (HPCs), are susceptible to significant damage during fires due to explosive spalling. Past research has shown that the inclusion of polymer fibres in high density concrete can significantly mitigate this fire damage. The exact mechanisms causing this increased spalling resistance are not yet fully under-stood, but it is thought that the fibres facilitate moisture transport during fire exposure, which in turn contributes to relief of internal stresses in the spalling-susceptible region. In this study, X-ray Computed Tomography (CT) was applied to observe the interaction between polymer fibres and cracking during thermal exposure. For this purpose, two concrete samples containing different polymer fibre types were subjected to incremental application of a defined thermal exposure. CT images were acquired before and after each thermal exposure and powerful image processing tools were used to segment the various material components. This enabled a detailed analysis of crack formation and propagation as well as the visualization and quantification of polymer fibre characteristics within the concrete. The results demonstrated that the orientation of both fibres and cracks in polymer-fibre reinforced concrete tend to be anisotropic. The results also indicated that crack geometry characteristics may be correlated with fibre orientation, with cracks tending to run parallel to fibre beds. Clear quantitative relationships were also observed between heating and increasing cracking levels, expressed in terms of both crack surface area and crack volume.
This paper focuses on the experimental evaluation of one of the key microstructural Parameters of a short-fiber reinforced composite – the orientation distribution of fibers. It is shown that computed tomography (CT) produces results suitable for reconstruction of the orientation distribution function. This function is used for calculation of the effective elastic properties of polymer-fiber reinforced concrete. Explicit formulas are derived for overall elastic moduli accounting for orientation distribution in the frameworks of the noninteraction approximation, the Mori–Tanaka–Benveniste scheme, and the Maxwell scheme.
The approach illustrated can be applied to any kind of composite material.
Beton ist das meistbenutzte Baumaterial der Welt. Sein Herstellungsprozess ist auch für schätzungsweise 5% der globalen Kohlenstoffemissionen verantwortlich. Daher können selbst kleine Verbesserungen in der Festigkeit oder Haltbarkeit zu einer erheblichen Verringerung der Bau- und Wartungskosten, der Umweltschäden und der Gefahr für die Menschen führen. Um das grundlegende Verhalten dieses Materials zu verstehen, ist es notwendig, seine Leistung während thermischer, chemischer und mechanischer Prozesse (d. h. in-situ) zu beobachten. Es wird eine zerstörungsfreie Messmethode benötigt, die in der Lage ist, nicht nur Änderungen des Materials wie Feuchtigkeitsumverteilung, Korrosion und Dehnung zu messen, sondern auch die innere Struktur des Materials im Dreidimensionalen aufzulösen, so dass Versagensmechanismen und Transportphänomene direkt auf bestimmte Eigenschaften der heterogenen Materialstruktur bezogen werden können (wie z.B. die Übergangszone zwischen Gesteinskörnungen und Zementstein oder die Orientierung von eingebetteten Fasern).
Die Röntgencomputertomographie (CT) hat sich als ideal für solche Zwecke erwiesen. Neuere Forschungen an der BAM werden vorgetragen, die die Fähigkeiten der CT zur Identifizierung quantitativer Materialeigenschaften wie Faserorientierung, Rissoberfläche, Korrosionsverteilung und Änderungen des volumetrischen Feuchtigkeitsanteils demonstrieren. Der Nutzen dieser leistungsstarken Analysewerkzeuge wird dann anhand der Ergebnisse einer Reihe von Ex-situ und In-situ Testprogrammen für Bedingungen wie mechanische Belastung, Wassertransport und thermische Exposition gezeigt. Speziell entwickelte In-situ Testmaschinen für diese verschiedenen Testprogramme werden ebenfalls beschrieben. Die von der CT gelieferten quantitativen Charakterisierungsinformationen haben sich als ideale Grundlage für die Kalibrierung bzw. Validierung von numerischen Simulationen erwiesen. CT ist auch wesentlich für die Beantwortung von vielen anwendungsspezifischen Fragen, u.a. wie sich verschiedene Gießverfahren auf die Materialleistung auswirken, welche Mineralien sich als Zuschlagstoffe anfällig für langfristige chemische und hydraulische Prozesse erweisen und wie Polymerfasern den Druckaufbau in Beton während der thermischen Belastung beeinflussen.
Um das grundlegende Verhalten des Betons zu verstehen, wird eine zerstörungsfreie Messmethode benötigt, die in der Lage ist, nicht nur Änderungen des Materials wie Feuchtigkeitsumverteilung, Korrosion und Dehnung zu messen, sondern auch die innere Struktur des Materials im Dreidimensionalen aufzulösen, so dass Versagensmechanismen und Transportphänomene direkt auf bestimmte Eigenschaften der heterogenen Materialstruktur bezogen werden können. Die Röntgencomputertomographie (CT) hat sich als ideal für solche Zwecke erwiesen. Diese Präsentation demonstriert die Fähigkeiten der CT zur Identifizierung quantitativer Materialeigenschaften wie Faserorientierung, Rissoberfläche, Korrosionsverteilung und Änderungen des volumetrischen Feuchtigkeitsanteils. Durch die Beschreibung der Ergebnisse einer Reihe von Ex-situ und In-situ Testprogrammen für Bedingungen wie mechanische Belastung, Wassertransport und thermische Exposition, sind auch die Nutzungsmöglichkeiten von diesem Verfahren dargestellt.
The water-transport characteristics of concrete have a major impact on its resistance to damaging chemical processes such as Alkali-Silica-Reaction (ASR). Water transport in samples of damaged and undamaged concrete was measured using in-situ CT. The resulting measurements of water-front movement relative to time and the change in 3D-moisture distribution within the samples, are needed for calibration and validation of water-transport numerical models.
This presentation includes the results of a number of case studies of concrete properties using computed tomography (CT) in combination with various in-situ testing techniques, including those of mechanical loading, water transport, and fire. The results of these case studies demonstrate the potential of CT as an approach for obtaining unique, quantitative data about the structure of materials. This data can serve as the basis for calibrating and validating a new generation of numerical models that have a stronger foundation in micromechanical theory. This will contribute to the development of more accurate and versatile simulation approaches for concrete and other building materials.
This paper describes a novel methodology for quantitative in-situ moisture measurement without tracking agents using X-ray computed tomography (XCT). The high levels of grey-scale precision required for the measurement of moisture without tracking agents resulted in the need for an additional image calibration procedure to correct for water-related X-ray scattering and for equipment-variability related artefacts arising during in-situ testing. This calibration procedure was developed on the basis of existing principles of XCT image cor-rection. Resulting images of moisture distribution exhibit a high level of agreement with expected material behaviour. This research demonstrated that XCT can be successfully used to measure both moisture-front movement over time and changes in 3D moisture distribution within samples. This approach to moisture measurement lays the groundwork for the planned future investigation of the interaction between cracking induced by varying chemical and mechanical processes and water transport in concrete.
Die Präsentation demonstriert die Fähigkeiten der Röntgencomputertomographie (CT) zur Identifizierung quantitativer Materialeigenschaften wie Faserorientierung und Korrosionsverteilung sowie die Implementierung von CT-Daten innerhalb numerischer Simulationen. Die besondere Stärke der CT, als zerstörungsfreies Prüfverfahren, ermöglicht es, das Materialverhalten und den Versagensprozess während mechanischer, hydraulischer und thermischer Prozesse zu beobachten. Die Ergebnisse einer Reihe von Ex-situ und In-situ Testprogrammen unter Bedingungen wie mechanische Belastung, Wassertransport und thermische Exposition, stellen die Nutzungsmöglichkeiten dieser Verfahren in Kombination mit der CT in eindrucksvoller Weise dar.
Simulating fiber-reinforced concrete mechanical performance using CT-based fiber orientation data
(2019)
The main hindrance to realistic models of fiber-reinforced concrete (FRC) is the local materials property variation, which does not yet reliably allow simulations at the structural level. The idea presented in this paper makes use of an existing constitutive model, but resolves the problem of localized material variation through X-ray computed tomography (CT)-based pre-processing. First, a three-point bending test of a notched beam is considered, where pre-test fiber orientations are measured using CT. A numerical model is then built with the zone subjected to progressive damage, modeled using an orthotropic damage model. To each of the finite elements within this zone, a local coordinate system is assigned, with its longitudinal direction defined by local fiber orientations. Second, the parameters of the constitutive damage model are determined through inverse analysis using load-displacement data obtained from the test. These parameters are considered to clearly explain the material behavior for any arbitrary external action and fiber orientation, for the same geometrical properties and volumetric ratio of fibers. Third, the effectiveness of the resulting model is demonstrated using a second, “control” experiment. The results of the “control” experiment analyzed in this research compare well with the model results. The ultimate strength was predicted with an error of about 6%, while the work-of-load was predicted within 4%. It demonstrates the potential of this method for accurately predicting the mechanical performance of FRC components.
The proposed BAM project SealWasteSafe will advance the state of the art for the construction and monitoring of safe sealing systems for underground repositories of radioactive or toxic waste. During this project, a novel salt concrete exhibiting neither significant cracking nor shrinkage will be optimized for use in the sealing systems. The composition of this material will be based on alkali-activated materials, which are characterized by particularly small thermal deformations during the hardening reaction. Quality assurance and continuous monitoring systems developed during this project will be demonstrated not only for high reliability, but also for resistance to highly alkaline environments and to water intrusion along cables or at sensor locations. A variety of sensors will be used in combination with wireless Radio Frequency Identification (RFID) technology to record moisture, temperature, and, if necessary, corrosion activity within the sealing system. Distributed Fibre Optic Sensor (FOS) technology will also be used for strain, temperature, and moisture content measurement. Ultrasound-based measuring methods will be utilized for the detection of cracks and delaminations. Additionally, digital image correlation and acoustic emission analysis will be used for deformation measurements and crack detection. A novel borehole probe and advanced ultrasound imaging techniques will be further developed to track cracks and delaminations within the host rock in 3D. The surface-based Large Aperture Ultrasound System (LAUS) will also be utilized to detect cracks and delaminations deep below the exterior surface of the sealing system. Although the focus of this project will be on the host rock salt, the resulting technologies will be intentionally developed in a way that facilitates their adaptation to other host rocks.
The closure of underground nuclear waste disposal facilities requires reliable gas- and water-tight engineered barriers. In Germany, barriers made from salt concrete have been evaluated in full scale. While the barriers seem to fulfill the requirements regarding permeability, some unexpected cracks have been detected at the surface and at depth. In cooperation between the Federal Company for Radioactive Waste Disposal (BGE) and the Federal Institute for Materials Research and Testing (BAM), several experiments have been carried out to evaluate the applicability for ultrasonic measurements in crack detection and general quality assurance. Both commercial instruments and specially developed devices have been tested on site.
Using commercial ultrasonic echo devices designed for concrete inspection it was possible to detect cracks and objects in salt concrete up to a depth of 2 m. The check for delamination in shotcrete is another field of application. A unique device available at BAM, the wide aperture, deep penetration instrument LAUS, was able to locate cracks and objects up to a depth of 8 m so far, which is thought to be a record for ultrasonic echo measurements in concrete. Adapted imaging procedures, partly adopted from geophysics, helped to reveal 3D structure at depth.
In addition, we have developed ultrasonic probes to be deployed in boreholes, currently at up to 20 m depth. They can collect information on cracks and other features in a radius of about 1.5 m around the borehole in the current version and might be used in echo or transmission mode. Evaluation experiments have been performed at an experimental barrier at the ERAM site in Morsleben, Germany. The results showed several empty and injected cracks as well as built-in instrumentation. The results have been verified using borehole endoscopy as well as core examination and will be used to set up a reliable quality assurance system for engineered barriers. All instruments are based on ultrasonic shear wave transducers with a frequency range between 25 kHz and 100 kHz. Current research focuses on the improvement of the hardware (e. g. optimization of array characteristics) and imaging techniques such as Reverse Time Migration, both aiming at the improvement of depth of penetration, resolution and probability of detection.
With a goal to improve our understanding of the relationships between microstructural features and ultrasonic signal behavior, concrete specimens of varying water-to-cement ratio were imaged using X-ray computed tomography (CT), and subsequently subjected to ultrasonic testing. From the CT scans, measurements were made of cement paste density and number of interfaces. Ultrasonic signals produced using a through-transmission configuration were analyzed and fit to a diffusion model to separate absorption from scattering attenuation. The results showed that at the frequencies tested, ultrasonic dissipation rate correlated weakly with paste density, while diffusivity correlated well with number of interfaces, but only if entrained air is considered separately. Cement paste density was found to be very well predicted by diffusivity, leading to a clear power-law relationship between diffusivity and compressive strength.
This poster provides an overview of ultrasonic investigations of an engineered test barrier at ERAM Morsleben, which were completed as part of contractual work with the Bundesgesellschaft für Endlagerung mbH (BGE). This includes both experiments with the Large Aperture Ultrasound System (LAUS) and the ultrasonic borehole array. Also included in the poster is a description of the planned BAM thematic project “SealWasteSafe”. In particular, the proposed geopolymer materials are described and future research requirements are detailed.