5 Werkstofftechnik
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- 5 Werkstofftechnik (41) (entfernen)
Eingeladener Vortrag
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Nachdem im Verbundprojekt COORAL das Hauptaugenmerk auf überkritisches CO2 gelegt wurde, d. h. Transport über kurze Strecken bei erhöhter Temperatur, wurde in CLUSTER ein größeres lokales Transport-Netzwerk betrachtet, bei dem CO2 bei geringeren Temperaturen, also vorwiegend im flüssigen Zustand transportiert wird. Wurden in COORAL die CO2-Ströme von Kohlekraftwerken untersucht, ging es in CLUSTER zusätzlich um die Emissionen von relevanten Industrien, deren CO2-Emissionen nicht ohne Weiteres vermieden werden können.
Aufgrund der Erfahrungen in COORAL konnte eine Auswahl von kommerziellen Werkstoffen getroffen werden, die für einen konkreten Einsatz für CCS zur Verfügung stünden. Die gemischten und fluktuierenden CO2-Zusammensetzungen sind bei geeigneten Begrenzungen der Begleit¬stoffe im CO2 bezüglich Korrosionsvorgänge beherrschbar. Die Machbarkeit eines lokalen CCS-Clusters erscheint daher gegeben, soweit dies die Anlagen für Kompression, Transport und Injektion betrifft.
In failure analysis, micro-fractographic analysis of fracture surfaces is usually performed based on practical knowledge which is gained from available studies, own comparative tests, from the literature, as well as online databases. Based on comparisons with already existing images, fracture mechanisms are determined qualitatively. These images are mostly two-dimensional and obtained by light optical and scanning electron imaging techniques. So far, quantitative assessments have been limited to macrocopically determined percentages of fracture types or to the manual measurement of fatigue striations, for example. Recently, more and more approaches relying on computer algorithms have been taken, with algorithms capable of finding and classifying differently structured fracture characteristics. For the Industrial Collective Research (Industrielle Gemeinschaftsforschung, IGF) project “iFrakto” presented in this paper, electron-optical images are obtained, from which topographic information is calculated. This topographic information is analyzed together with the conventional 2D images. Analytical algorithms and deep learning are used to analyze and evaluate fracture characteristics and are linked to information from a fractography database. The most important aim is to provide software aiding in the application of fractography for failure analysis. This paper will present some first results of the project.
This contribution provides current findings regarding materials susceptibility for carbon capture, utilization and storage (CCUS) applications. Basing on results gathered in 2 German long-term projects (COORAL and CLUSTER) suitable materials are introduced as well as dominating impurities of the CO2-stream and corrosion mechanisms. Investigations cover the whole CCUS process chain and provide material recommendations for certain parts.
A global transition towards more sustainable, affordable and reliable energy systems is being stimulated by the Paris Agreement and the United Nation's 2030 Agenda for Sustainable Development. This poses a challenge for the corrosion industry, as building climate‐resilient energy systems and infrastructures brings with it a long‐term direction, so as a result the long‐term behaviour of structural materials (mainly metals and alloys) becomes a major prospect. With this in mind “Corrosion Challenges Towards a Sustainable Society” presents a series of cases showing the importance of corrosion protection of metals and alloys in the development of energy production to further understand the science of corrosion, and bring the need for research and the consequences of corrosion into public and political focus. This includes emphasis on the limitation of greenhouse gas emissions, on the lifetime of infrastructures, implants, cultural heritage artefacts, and a variety of other topics.
For reliability and safety issues of injection wells, corrosion resistance of materials used needs to be determined. Herein, representative low-cost materials, including carbon steel X70/1.8977 and low alloyed steel 1.7225, were embedded in mortar to mimic the realistic casing-mortar interface. Two types of cement were investigated: (1) Dyckerhoff Variodur commercial Portland cement, representing a highly acidic resistant cement and (2) Wollastonite, which can react with CO2 and become stable under a CO2 stream due to the carbonation process. Exposure tests were performed under 10 MPa and at 333 K in artificial aquifer fluid for up to 20 weeks, revealing crevice corrosion and uniform corrosion instead of expected pitting corrosion. To clarify the role of cement, simulated pore water was made by dispersing cement powder in aquifer fluid and used as a solution to expose steels. Surface analysis, accompanied by element mapping on exposed specimens and their crosssections, was carried out to trace the chloride intrusion and corrosion process that followed.
According to the definition of the ASM handbook [1,3], a defect is "an imperfection. that can be shown to cause failure by a quantitative analysis and that would not have occurred in the absence of the imperfection". The topic of the present three-part review is a discussion of defects which can cause failure in cyclically loaded structures. The features discussed comprise material defects such as non-metallic inclusions, pores or micro-shrinkages, etc. and geometric defects such as surface roughness and secondary notches which have their origin in manufacturing, and defects such as surface damage due to scratches, impact events or contact fatigue as well as corrosion pits which arise in service. In this first part, the discussion is prefaced by an introduction to basic aspects which are essential for a deeper understanding of the characteristics and mechanisms how the defects influence fatigue crack initiation and propagation. These include the life cycle of a fatigue crack from initiation up to fracture, crack arrest, multiple crack initiation and coalescence, and the material and geometrical properties affecting these.
Defects as a root cause of fatigue failure of metallic components. II: Non-metallic inclusions
(2019)
This second part of the review on defects as root cause of fatigue failure comprises the origin, the nature and the effects of non-metallic inclusions. Topics addressed are the different kinds of inclusions formed during the manufacturing process, various types of mis-match causing local stresses and, as a consequence, fatigue crack initiation, and effects of characteristics such as size, morphology, localization, spatial distribution and orientation of the defects on the fatigue behavior. Methods for inclusion counting and sizing are discussed along with statistical aspects necessary to be considered when evaluating structural components.
This third part of the review on defects as root cause of fatigue failure addresses cavities (pores, micro-shrinkages, unmelted regions), defective microstructures and microcracks as material defects and defects due to local damage during manufacturing, service and maintenance such as dents, scratches and localized corrosion. In addition, damage due to contact fatigue and the effect of surface roughness are discussed in the context of fatigue failure. Also addressed is the competition between different kinds of defects in controlling the initiation and early growth of fatigue cracks.
Many microstructural features exhibit non-trivial geometries, which can only be derived to a limited extent from two-dimensional images. E.g., graphite arrangements in lamellar gray cast iron have complex geometries, and the same is true for additively manufactured materials and three-dimensional conductive path structures. Some can be visualized using tomographic methods, but some cannot be due to weak contrast and/or lack of resolution when analyzing macroscopic objects. Classic metallography can help but must be expanded to the third dimension. The method of reconstructing three-dimensional structures from serial metallographic sections surely is not new. However, the effort required to manually assemble many individual sections into image stacks is very high and stands in the way of frequent application. For this reason, an automated, robot-supported 3D metallography system is being developed at BAM, which carries out the steps of repeated preparation and image acquisition on polished specimen.
Preparation includes grinding, polishing and optionally etching of the polished surface. Image acquisition comprises autofocused light microscopic imaging at several magnification levels. The image stacks obtained are then pre-processed, segmented, and converted into 3D models, which in the result appear like microtomographic models, but with high resolution at large volume. Contrasting by classical chemical etching reveals structures that cannot be resolved using tomographic methods. The integration of further imaging and measuring methods into this system is underway. Some examples will be discussed in the presentation.
Die AG Fraktographie im DVM/DGM-Gemeinschaftsgremium „Elektronenmikroskopie in der Materialforschung“ betreibt seit 2013 eine fraktographische online-Datenbank („FractoDB“), die für das interessierte Fachpublikum kostenfrei zur Verfügung steht. Die Analyse und Bewertung von Bruchflächen und der darauf befindlichen Bruchmerkmale ist ein wichtiger Teilaspekt der Schadensanalyse bei der Suche nach Schadensmechanismen und Schadensursachen. Risse und Brüche an realen Bauteilen können nur dann bewertet werden, wenn gut dokumentierte Vergleichsbrüche aus Laborversuchen zur Verfügung stehen, sei es an Proben oder an Vergleichs-Bauteilen. Daher trägt die AG Fraktographie Bildmaterial zusammen, führt systematisch Laborversuche und Ringversuche durch und analysiert Brüche aus Schadensfällen. Die gewonnenen Daten werden zu Datensätzen zusammengestellt und über die Datenbank zugänglich gemacht. Derzeit ist ein Bestand von über 400 Datensätzen mit insgesamt über 4.500 Bildern verfügbar, welcher durchsucht werden kann und in Anlehnung an die VDI 3822 organisiert ist. Weitere Aktivitäten der AG Fraktographie, die in der FractoDB abgebildet werden, sind u.a. die Entwicklung einer fraktographischen Symbolik und die Analyse von Bruchmerkmalen mittels Machine Learning. Über die aktuellen Ergebnisse und Planungen wird berichtet.
Die Fraktographische Online-Datenbank der AG Fraktographie – Entwicklungsstand und weitere Planung
(2023)
Vortrag zum aktuellen Stand der fraktographischen online-Datenbank. Darstellung des AGM/DVM Gemeinschaftsausschusses REM in der Materialforschung und seiner Arbeitsgruppen Fraktographie, EBSD und 2D/3D-Prüfung. Ziele und Inhalte der fraktographischen Datenbank, Aufruf zum Mitmachen. Durchführung von Vergleichsversuchen, Entwicklung einer fraktographischen Symbolik, Ringversuch, Vorhaben iFrakto mit Entwicklung einer KI-gestützten Bruchflächenanalyse.
This work examined the droplet corrosion of CO2 pipeline steels caused by impurities in CO2 supercritical/dense phase at 278 K, simulating the underground transport condition. The wetting properties of carbon steels (X52 and X70) as well as martensitic steel UNS S41500, and superaustenite UNS N08031 were studied by contact angle measurement, revealing reactive wetting behavior of carbon steels. Exposure tests with CO2 saturated water droplet on steel surface showed that the impurities (220 ppmv SO2 and 6700 ppmv O2) diffused into the droplet and then reacted with metal coupons in supercritical/dense phase condition, forming the corrosion product instantly during pumping process. Due to the active wetting behavior, the carbon steels suffered from heavily attack, while negligible corrosion product was observed in cases of martensitic steel UNS S41500 and superaustenite UNS 08031 coupons. Condensation experiments that were carried out on fresh polished coupons in CO2 with 1200 ppmv H2O showed that the formation and aggregation of droplet is dependent on the presence of impurities. Without SO2 and O2, the same concentration of H2O did not cause observable corrosion process after a week of exposure. With 220 ppmv SO2 and 6700 ppmv O2 even low water concentration (5-30 ppmv) still resulted in heterogeneous nucleation and subsequent growth of droplets, leading to corrosive process on carbon steel surface albeit to a lesser extent.
In this work, the focus was set on the corrosion process of condensate as drops on the surface of carbon steels (X52, X70), martensitic steel UNS S41500, and superaustenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the transportation condition in a buried pipeline). Exposure tests were performed at both normal pressure and high pressure where CO2 is supercritical or in dense phase. The drop, 1 ‑ 10 μL in volume, was prepared by dropping CO2 saturated ultra-pure water onto the surface of steel coupons in a one-liter-autoclave. The CO2 gas stream, simulating the oxyfuel flue gas with varying concentration of impurities (SO2 and O2 ), was then pumped into the autoclave to observe the condensation and corrosion impacts of impurities. Comparable exposure tests were carried out with the same gas mixture and the same volume of water as vapor to observe the drop formation and the corrosion process that follows. The wettability and stability of drops on the surface of steel coupons in CO2 supercritical/dense phase environment was evaluated additionally by contact angle measurement.
The research focus of this study was set on the corrosion process of condensate as droplets on the surface of carbon steels (X52, X70) martensitic steel UNS S41500, and super austenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the offshore transportation condition in a buried pipeline). The possibility of dew/droplet formation on the steel surface and wetting behavior of corresponding materials were evaluated by contact angle measurement in dense CO2 at 278 K. To observe the effect of impurities (SO2 and O2) on droplet corrosion process, exposure tests were carried out in the mixed atmosphere with a drop, 1 ‑ 10 µL in volume, of CO2 saturated ultra-pure water on steel surface. Comparable exposure tests were carried out with the same gas mixture and the same volume of water, as vapor, to observe the droplet formation and the corrosion process that follows. Effects of surface roughness on the droplet formation and its corrosion process were further studied and showed no significant role upon long time exposure. The results from droplet experiments were compared to those from the bulk electrolyte for the further recommendation on the quality control of gas stream along with the use of carbon steels as transport pipelines in CCS - Carbon Capture and Storage system.
Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature
(2020)
The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products.
To reveal the corrosion resistance of casing steel/mortar interface in CO2 injection condition, sandwich samples were prepared and exposed up to 20 weeks in aquifer fluid under 10 MPa and 60 °C. Cross section analysis revealed the crevice corrosion as main mechanism instead of pitting corrosion, which would be expected to happen in the extremely high Chloride concentration. Detailed analysis using EDS line scan shown the slow diffusion of Chloride, suggesting why pitting did not happen after 20 weeks. To mimic the passivated steel surface, the steel coupon was passivated in simulated pore solution having pH 13.5 for 42 days. The passivated coupon was further exposed to NGB solution for 28 days. Electrochemical characterization was performed along the exposure processes to reveal the change in impedance, indicating the corrosion resistance of steel casing/mortar interface.
Carbon Capture and Storage (CCS) is identified as an excellent technology to reach the target of CO2 reduction. However, the safety issue and cost effectiveness hinder the future of CCS. For the reliability and safety issues of injection wells the corrosion resistance of the materials used needs to be determined.
In this study, representative low cost materials including carbon steel 1.8977 and low alloyed steel 1.7225 were embedded in cement to mimic the realistic casing-cement interface. Electrochemical studies were carried out using these metal-cement specimens in comparison with those made of metal only in CO2 saturated synthetic aquifer fluid, at 333 K, to reveal the effect of cement on the steel performance. The results showed the protective effect of cement on the performance of pipeline metals during polarisation process. However, the corrosion current density was high in all cases, with and without cement, indicating that the corrosion resistance of these materials is low. This conclusion was supported by the surface analysis of the polarized specimens, which revealed both homogenous and pitting corrosions.
Bei der Untersuchung von Bruchflächen werden zunächst Beobachtungen gemacht, d.h. makroskopische und mikroskopische Merkmale analysiert und in Bildern dokumentiert. Im zweiten Schritt werden anhand der gefundenen Merkmale Rissverlauf und Bruchmechanismen ermittelt. Abschließend sollen diese Ergebnisse in einem Bericht oder Gutachten zusammengefasst werden. Hierbei ist eine skizzenhafte Darstellung der fraktographischen Befunde hilfreich für das Verständnis des Lesers. Ein vorgefertigter fraktographischer Symbolsatz würde dies erheblich vereinfachen.
Skizzen von fraktographischen Befunden sind in der Literatur recht häufig zu finden, z.B. in der VDI 3822 oder dem ASM Handbook Fractography, allerdings gibt es hierzu keine umfassende Systematik, wie sie z.B. aus der Meteorologie (Wetterkarten), Geographie (Landkarten, Seekarten) oder Geologie (Bodenkarten) seit langer Zeit bekannt sind. Deshalb wird hier der Versuch unternommen, einen Symbolsatz zu entwickeln und zur Verfügung zu stellen, mit dessen Hilfe fraktographische Befunde in eindeutiger und übersichtlicher Weise veranschaulicht werden können. Der fraktographische Symbolsatz ("Fracto Graphics") befindet sich in Entwicklung, ist offen zur Diskussion sowie für Verbesserungen.
Die klassische Metallographie basiert auf Abbildungen einzelner Schliffebenen und kann auf räumliche Formen und Anordnungen des Gefüges nur bedingt schließen. Die Idee, aus metallographischen Serienschliffen dreidimensionale Gefügestrukturen zu rekonstruieren, ist daher naheliegend und nicht neu. Allerdings ist der Aufwand, in Handarbeit viele Einzel-Schliffe zu präparieren und zu Bildstapeln zusammenzusetzen, sehr hoch und steht einer häufigen Anwendung entgegen.
Deshalb wird an der BAM ein Roboter-gestütztes 3D-Metallographie-System entwickelt, das an einer Schliffprobe die Schritte Präparation und Bildeinzug vollautomatisch mit vielen Wiederholungen ausführt. Die Präparation umfasst Schleifen, Polieren und optional Ätzen der Schlifffläche, der Bildeinzug autofokussierte lichtmikroskopische Aufnahmen bei mehreren Vergrößerungsstufen. Der erhaltene Bildstapel wird anschließend vorverarbeitet, segmentiert und in ein 3D-Modell umgesetzt, das einer mikrotomographischen Aufnahme ähnelt, allerdings mit besserer lateraler Auflösung bei großem Volumen. Im Gegensatz zu tomographischen Verfahren besteht die Möglichkeit der Kontrastierung durch klassische chemische Ätzung. Die Integration eines REMs ist geplant. Bislang durchgeführte Arbeiten verdeutlichen die Möglichkeiten der Darstellung von Heißgas-Korrosionsschichten, Grauguss-Werkstoffen und Keramik-basierten mikroelektronischen Strukturen (Vias).