5.1 Mikrostruktur Design und Degradation
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- Beitrag zu einem Tagungsband (31) (entfernen)
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- Corrosion (13)
- CCS (6)
- CO2 (5)
- Steel (4)
- CCUS (3)
- CO2 quality (3)
- Carbon steel (3)
- Geothermal (3)
- Impurities (3)
- Martensitic steel (3)
Organisationseinheit der BAM
- 5 Werkstofftechnik (31)
- 5.1 Mikrostruktur Design und Degradation (31)
- 7 Bauwerkssicherheit (14)
- 7.6 Korrosion und Korrosionsschutz (14)
- 5.2 Metallische Hochtemperaturwerkstoffe (2)
- 5.5 Materialmodellierung (2)
- 6 Materialchemie (2)
- 9 Komponentensicherheit (2)
- 9.0 Abteilungsleitung und andere (2)
- 5.6 Glas (1)
Komponenten von Fahrrädern werden im Betrieb vorwiegend schwingend beansprucht. Typische Werkstoffe sind Stahl, Aluminiumlegierungen, Messing, CFK und thermoplastische Kunststoffe. Da es sich, unabhängig von der Preiskategorie, um konstruktiven Leichtbau handelt, werden einige Bauteile betriebsfest mehr oder weniger weit oberhalb der Dauerfestigkeit ausgelegt. Die im normalen Betrieb auftretenden Schäden sind daher weit überwiegend Schwingbrüche. Andere Schadensmechanismen wie z.B. Korrosion spielen quantitativ eine untergeordnete Rolle. Schwingbrüche treten nach einer Periode unbemerkten Risswachstums oft ohne Vorwarnung und ohne makroskopische Verformung auf. Im Falle von sicherheitsrelevanten Komponenten wie Rahmen, Gabeln, Lenkern, Sattelstützen, Kurbelarmen oder Pedalen kann dies zu erheblichen Personenschäden führen, die den Wert des ursächlichen Bauteilschadens weit überschreiten.
Über einen langjährigen Zeitraum wurden gebrochene Komponenten aus dem Alltag und aus Gerichtsverfahren analysiert. Das Hauptaugenmerk lag hierbei auf der fraktographischen Analyse, teilweise wurden die zu Grunde liegenden Schadensursachen ermittelt. Einflussfaktoren sind beispielsweise konstruktive Kerben an ungünstigen Stellen, aber auch Werkstoffwahl und Fertigungsqualität spielen eine Rolle. In den meisten Fällen wurde jedoch die konstruktive Lebensdauer überschritten. Diese wird praktisch nie mitgeteilt, und eine wiederkehrende Prüfung sicherheitsrelevanter Bauteile findet nicht statt.
Im Sinne der Vermeidung von Schäden und Unfällen könnte darauf hingewirkt werden, für sicherheitsrelevante Komponenten Lebensdauern besser abzuschätzen und von der Laufleistung abhängige Sichtprüfungen zu empfehlen.
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.
Flipping the classroom is a method to let students study on their own and then take time to discuss their questions and do extended hands-on lectures or exercises in class – or in the case of the covid-19 pandemic during plenary online sessions. First year mechanical engineering students use different teaching materials (mainly lecture videos, lightboard videos and micromodule lectures) to study from a distance and comprehend the principle underlying science in theory. Then the online plenary lectures offer the opportunity to apply their knowledge and transfer different scientific aspects of the course to get the bigger picture. Exercises, worked solutions, selfassessed tests and peer-instruction during present time help students to check on their learning progress. However, the self-study periods and (online) plenary sessions need to be guided carefully. To meet the course learning outcome and overcome the diversity of a first year class various practical leads have to be fulfilled to turn flipped classroom teaching into success.
Mit Beginn der Covid-19 Pandemie und dem damit verbundenen ausschließlichen Lehren im online-Format war die Hoffnung verbunden ein Blended Learning Lehrformat für die Studieeingangsphase ohne viel konzeptionelle Änderungen übertragen zu können. Der Kurs Werkstofftechnik als Grundlagenfach für den Maschinenbau baut sich auf inverted classroom Lehrszenarien auf, deren Lerngrundlage hierfür eigens produzierte und auf das Lernziel abgestimmte Lehrfilme und Lightboard-Vorlesungen darstellen. Im Kontext der Studieneingangsphase bieten audiovisuell stimulierende Lehrfilme umfassende Lernmedien, wenn sie analog der Lerninhalte einem technischen und didaktischen Qualitätsanspruch genügen. In der Praxis des SS2020 und WS2020/21 hat sich gezeigt, dass die Moderation und Durchführung eines online-Kurses sich deutlich von dem eins blended learning-Kurses unterscheidet. Um denselben Lernerfolg bei Studierenden zu erzielen, müs-sen Anforderungen viel genauer und detaillierter verfasst werden, Studierende enger und persönlicher begleitet werden und Lehrfilme und Lernmedien in einen Gesamtzusammenhang gestellt werden. Im Folgenden werden aus persönlicher Erfahrung heraus niederschwellige, zum Teil ungewöhnliche praktische Erfahrungen zur erfolgreichen Umsetzung von Lehrfilm-basierten inverted classroom Lehrszenarien zusammengefasst und im Hinblick auf die online-Lehre bewertet.
Carbon Capture Utilization and Storage (CCUS) is a promising technology to reach the target for reduction of CO2 emissions, e.g. from fossil-fuel operated power plants or cement mills. Crucial points for a sustainable and future-proof CCUS procedure are reliability and cost efficiency of the whole process chain, including separation of CO2 from the source, compression of CO2, its subsequent transportation to the injection site and injection into geological formations, e.g. aquifers.
Most components that are in contact with CO2-stream consist of steel. Depending on the operating conditions (e.g. temperature, pressure, and CO2-stream composition) specific suitable steels should be used. The compressed CO2-stream is likely to contain process specific impurities; small amounts of SO2 and NO2 in combination with oxygen and water are most harmful.
One approach, as currently preferred by pipeline operators, is to clean the CO2-stream to such levels, acceptable for carbon steel, commonly used as pipeline material. Another consideration would be, to use more corrosion resistant alloys for CO2-streams with higher amounts of impurities.
Due to the absence of certified benchmarks for upper limits, systematic experiments with impurities in the CO2-stream were carried out reflecting mainly transport and injection conditions.
Within the COORAL project (German acronym for “CO2 purity for capture and storage”) levels of impurities in the CO2-stream, being acceptable when using specific steels, were evaluated. Material exposure to dense or multiphase carbon dioxide (CO2) containing specific amounts of water vapor, oxygen (O2) sulfur dioxide (SO2), nitrogen dioxide (NO2), carbon monoxide (CO) can be a challenge to steels. In some situations, condensation of impurities and reaction products from the CO2 stream can occur.
CO2 saturated brine is supposed to rise in the well when the injection process is interrupted. The material selection shall ensure that neither CO2 nor brine or a combination of both will leak out of the inner tubing.
This COORAL-work was extended by a follow-up project, called CLUSTER. Here the additional influence of impurities was investigated when merging CO2 streams from different sources, combined within a “so-called” cluster.
Results are summarized within the following table regarding suitability for different parts of the process chain.
In CCS environment (carbon capture and storage) pipes are loaded statically and/or cyclically and at the same time exposed constantly to the highly corrosive hot thermal water. Experimental procedures such as ambient pressure immersions tests, in-situ corrosion fatigue experiments using a flexibly designed corrosion chamber at ambient pressure and a specially designed corrosion chamber at high pressure. Experimental set-ups for push/pull and rotation bending load are introduced. The corrosion behavior and lifetime reduction of high alloyed steels (X46Cr13, 1.4043), (X5CrNiCuNb16-4, 1.4542) and (X2CrNiMoN22-5-3, 1.4462) is demonstrated (T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 l/h, CO₂).
Immersion tests of potential injection pipe steels 42CrMo4, X20Cr13, X46Cr13, X35CrMo4 and X5CrNiCuNb16-4 at T=60 °C and ambient pressure and p=100 bar were performed for 700 h - 8000 h in a CO₂-saturated synthetic aquifer environment similar to CCS-sites in the Northern-German-Basin. Main corrosion products are FeCO₃ and FeOOH. Highest surface corrosion rates at ambient pressure are 0.8 mm/year for 42CrMo4 and lowest 0.01 mm/year for X5CrNiCuNb16-4. Corrosion rates at 100 bar (max. 0.01 mm/year for 42CrMo4, X20Cr13, X46Cr13) are generally lower than at ambient pressure (<0.01 mm/year for X35CrMo4, X5CrNiCuNb16-4). Heat treatment to martensitic microstructure offers good corrosion resistance.
The collaborative project “Impacts of impurities in CO2 streams captured from different emitters in a regional cluster on transport, injection and storage (CLUSTER)” aimed to set up recommendations on how to define “reasonable minimum composition thresholds” that CO2 streams should meet when accessing CO2 transport pipeline networks. Within CLUSTER, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the whole CCS chain. Investigations included, amongst others, impacts on:
• corrosion of pipeline steel,
• pipeline network design and related transport costs,
• alteration of well bore cements,
• pressure development and rock integrity,
• geochemical reactions, and
• petrophysical and geomechanical rock properties.
All investigations are based on a generic CCS chain scenario. In this scenario, CO2 streams are captured from a spatial cluster of eleven emitters and collected in a regional pipeline network. Emitters comprise seven fossil fuel-fired power plants equipped with different capture technologies, two cement plants, one refinery and one integrated iron and steel plant. In total, 19.78 Mio t CO2 (including impurities) are captured in the emitter cluster annually. The combined CO2 stream is transported in a trunk line with a length of 400 km (100 km of these offshore) and is injected into five generic storage structures. The storage reservoirs are saline aquifers of the Buntsandstein.
The investigations revealed beneficial and deteriorating impacts of different impurities and combinations thereof. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the modelled variable compositions and mass flow rates were observed. Based on the results, the CLUSTER project team recommends not to define “minimum composition thresholds” for CO2 streams as strict threshold values for each individual impurity in the stream. Instead, CO2 stream compositions and variabilities for specific CCS projects should be constrained with regard to a set of parameters including i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of CO2 stream composition, and iv) impurity combinations to be avoided.
Study of Polyaniline/Silicon Dioxide based Coating on Carbon Steel in Artificial Geothermal Brine
(2021)
Geothermal brines are corrosive in nature because of their salt contents and high temperatures. Therefore, they pose a major challenge to geothermal power-plants, which are mostly built of low alloyed steels, e.g., carbon steel. Carbon steel is susceptible to uniform and localized corrosion when exposed to geothermal brines having acidic-saline properties. To overcome this limitation, geothermal power plants should be built by either high alloyed materials or by integrating protection systems on carbon steel, such as coatings and inhibitors. We studied a coating system containing polyaniline/silicon dioxide basing on locally available resources that provides protection against corrosion of carbon steel and enhance the thermal resistance in geothermal environments. Here, exposure and electrochemical tests of coated carbon steels were performed in an artificial geothermal brine. The solution had a pH of 4, with the composition of 1,500 mg/L of chlorides, which is based on the chemical analysis of geothermal brine found in Sibayak, Indonesia. All exposure tests were conducted using autoclaves at 150 °C with a total pressure of 1 MPa, which was performed for up to six months to evaluate the durability of the coating system. Post-experimental analyses were performed by assessing the surface of specimens using optical and electron microscopes. On the other hand, electrochemical tests were performed for seven days at 25 °C and 150 °C to investigate the kinetics of electrochemical reactions by measuring open circuit potential and electrochemical impedance spectra. Experimental results showed the corrosion resistance of PANI/SiO2 composite coatings, where polyaniline and SiO2 play their roles as stabilizers.
Al2O3 coatings are often used as protective layers on steels against electrochemical and high-temperature corrosion because they are chemically inert and stable at elevated temperatures. This study presents preliminary work on the possibilities of using Al2O3 sol-gel coatings for corrosion protection of martensitic stainless steels in geothermal environments. Al2O3 sol-gel coatings were applied on UNS S42000, which is known to be susceptible to uniform and localized corrosion. The coated steel specimens were then tested in two types of artificial geothermal water, which simulate the geothermal fluids found in Sibayak (SBY), Indonesia, and North German Basin (NGB), Germany, respectively. SBY has pH 4 and 1.5 g/L of chloride ions, whereas NGB has a pH of 6 and 166 g/L of chloride ions. All experiments were carried out in autoclaves at 150 °C and 1 MPa under the deaerated condition. Evaluations were performed by investigating the surface profiles of both uncoated and coated steels before and after the corrosion test using a Laser Scanning Microscope (LSM) and Scanning Electron Microscope (SEM). Finally, Electrochemical Impedance Spectroscopy (EIS) was performed to compare the corrosion resistance of Al2O3 coated steels in SBY and NGB solutions. It was observed from the corrosion test that Al2O3 coatings are more suitable for use in the geothermal water with a higher pH.
The collaborative project “Impacts of impurities in CO2 streams captured from different emitters in a regional cluster on transport, injection and storage (CLUSTER)” aimed to set up recommendations on how to define “reasonable minimum composition thresholds” that CO2 streams should meet when accessing CO2 transport pipeline networks. Within CLUSTER, we investigated potential impacts of CO2 streams with different and temporally variable compositions and mass flow rates along the whole CCS chain. Investigations included, amongst others, impacts on: Corrosion of pipeline steel, pipeline network design and related transport costs, alteration of well bore cements, pressure development and rock integrity, geochemical reactions, and petrophysical and geomechanical rock properties.
All investigations are based on a generic CCS chain scenario. In this scenario, CO2 streams are captured from a spatial cluster of eleven emitters and collected in a regional pipeline network. Emitters comprise seven fossil fuel-fired power plants equipped with different capture technologies, two cement plants, one refinery and one integrated iron and steel plant. In total, 19.78 Mio t CO2 (including impurities) are captured in the emitter cluster annually. The combined CO2 stream is transported in a trunk line with a length of 400 km (100 km of these offshore) and is injected into five generic storage structures. The storage reservoirs are saline aquifers of the Buntsandstein.
The investigations revealed beneficial and deteriorating impacts of different impurities and combinations thereof. Overall, no fundamental technical obstacles for transporting, injecting and storing CO2 streams of the modelled variable compositions and mass flow rates were observed. Based on the results, the CLUSTER project team recommends not to define “minimum composition thresholds” for CO2 streams as strict threshold values for each individual impurity in the stream. Instead, CO2 stream compositions and variabilities for specific CCS projects should be constrained with regard to a set of parameters including i) the overall CO2 content, ii) maximum contents of relevant impurities or elements, iii) acceptable variability of CO2 stream composition, and iv) impurity combinations to be avoided.
Development and characterization of starch film and the incorporation of silver nanoparticles
(2020)
Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties.
During carbon sequestration the CO2-induced corrosion of injection pipe steels is a relevant safety issue when emission gasses are compressed into deep geological layers. The reliability of the high alloyed steel X35CrMo17 suitable as injection pipe for the geological onshore CCS-site (Carbon Capture and Storage) in the Northern German Basin, is demonstrated in laboratory experiments in equivalent corrosive environment (T = 60 °CC, p = 1–100 bar, aquifer water, CO2-flow rate of 9 L/h, 700–8000 h exposure time). Corrosion kinetics and microstructure were characterized and compared to other potential injection pipe steels (42CrMo4, X46Cr13, X20Cr13 and X5CrNiCuNb16-4).
Coupons of X5CrNiCuNb16-4 that may be used as injection pipe with 16% Chromium and 0.05% Carbon (1.4542, AISI 630) were exposed for 3000 h to CO2-saturated saline aquifer water similar to the conditions in the Northern German Basin at ambient pressure and 60 °C. Surface corrosion layers and pits reveal carbonate corrosion products on the surface such as FeCO3 and FeOOH as the main precipitation phases with no dependence on the original surface roughness. Corrosion rates for polished and technical surfaces were below 0.005 mm/year compared to corrosion rates of 0.035 mm/year after shot peening.
In CCS environment (carbon capture and storage) pipes are loaded statically and/or cyclically and at the same time exposed constantly to the highly corrosive hot thermal water. Experimental procedures such as ambient pressure immersions tests, in-situ corrosion fatigue experiments using a flexibly designed corrosion chamber at ambient pressure and a specially designed corrosion chamber at high pressure. Experimental set-ups for push/pull and rotation bending load are introduced. The corrosion behavior and lifetime reduction of high alloyed steels (X46Cr13, 1.4043), (X5CrNiCuNb16-4, 1.4542) and (X2CrNiMoN22-5-3, 1.4462) is demonstrated (T=60 °C, geothermal brine: Stuttgart Aquifer flow rate: 9 l/h, CO2 ).
The commercial usage of latent thermal energy storages primarily depends on the development of a suitable phase change material (PCM). For industrial high temperature applications above 400 °C multicomponent chloride eutectics are promising and therefore discussed seriously. The profound thermodynamic investigation of such eutectics requires a much greater amount of specimen material than conventional calorimeter can handle. Therefore, a special adiabatic calorimeter was developed and designed. With a specimen mass of > 100 g the typical thermodynamic measurements with a commercial calorimeter can be extended by cycle stability measurements, which are often decisive for practical application of PCM. Furthermore, by implementing corrosion specimens inside the calorimeter high temperature corrosion experiments according to ISO 21608 can be performed inside the calorimeter. Adiabatic measuring conditions can be provided by using two separate heating systems. Therefore, the outer “protective system” follows the temperature curve of the inner “measuring system” minimizing the temperature difference between the heating systems and simultaneously preventing heat losses from the measuring systems.
The current competitive situation on electricity markets forces conventional power plants into cyclic operation regimes with frequent load shifts and starts/shutdowns. In the present work, the cyclic mechanical behavior of ferritic-martensitic 9-12 % Cr steels under isothermal and thermomechanical loading was investigated for the example of grade P92 material. A continuous softening was observed under all loading conditions. The introduction of hold periods to the applied cycles reduced material lifetime, with most prominent effects at technologically relevant small strain levels. The microstructural characterization reveals a coarsening of the original “martensitic” lath-type microstructure to a structure with polygonal subgrains and reduced dislocation density. The microstructural data forms the input for a physically-based modelling approach.
Specific amounts of oxidizing and reductive impurities as well as some moisture were added to dense phase CO2 to replicate CO2 streams from sources in a CCS pipeline network. Due to the moisture content being only 50 ppmV no visible acid condensation took place. To simulate stress conditions at the inside pipeline surface due to fluid pressure (10 MPa) specimens were preloaded using a load frame. Experiments conducted at 278 K and at 313 K revealed the highest corrosion rate at lower temperature. Corrosive effect of impurities was strongest applying mixed atmosphere, containing oxidizing and reductive components, closely followed by CO2 streams with pure oxidizing character. By far, the lowest corrosion rate (10x lower) resulted from reductive atmosphere. In general, at constant temperature and pressure the CO2 stream composition strongly influences the morphology, thickness and composition of the corrosion products. Applying oxidizing or mixed impurities, iron hydroxides or oxides (e.g. goethite, hematite) occur as dominating corrosion products, capable to incorporate different amounts of sulfur. In contrast, using reductive atmosphere very thin corrosion layers with low crystallinity were developed, and phase identification by XRD was unfeasible. SEM/EDX analysis revealed the formation of Fe-O compounds, most likely attributed to the oxygen partial pressure in the system induced by CO2 (≥0.985 volume fraction) and volatile H2O. In addition to the surface covering corrosion layer, secondary phases had grown locally distributed on top of the layer. These compounds are characteristic for the applied atmosphere and vary in number, shape and chemical composition.
The work presents the microstructure, chemical composition and mechanical properties of Inconel 686 coatings after high - temperature corrosion in environment of aggressive gases and ashes. To produce the Ni - based coatings the QS Nd:YAG laser cladding process was carried out. As the substrate used 13CrMo4-5 boilers plate steel. Ni - base alloys characterize the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. Formed clad were characterized by high quality of metallurgical bonding with the substrate material and sufficiently low amount of the iron close to the clad layer surface. After corrosion experiment the oxide scale on the substrate and clad created. The scale on 13CrMo4-5 steel had 70 μm thickness while the scale of the clad had less than 10 μm. The microstructure, chemical composition of the obtained clad and scales were investigated by scanning electron microscope (SEM) and electron probe microanalyzer (EPMA) equipped with the EDS detectors.
Die Abbildung von Bruchflächen im Rasterelektronenmikroskop (REM) liefert hochaufgelöste Bilddaten, die für die mikrofraktografische Bewertung von Bruchmechanismen unerlässlich sind. Die Ermittlung von Bruchmechanismen ist oft ein wichtiger Teil von Schadensanalysen zur Ermittlung der Bruchursache. Durch den Abbildungsprozess im REM gehen räumliche Informationen im Normalfall größtenteils verloren und können daher nicht zur Präzisierung des Bruchmechanismus herangezogen werden.
Um räumliche Informationen von Probenoberflächen im REM zu erfassen, gibt es verschiedene Methoden. Die für die Ermittlung der 3D-Topografie bereits länger eingeführten Verfahren mittels Proben- oder Strahlkippung können die Berechnung des Oberflächenmodells erst nach der seriellen Aufnahme mehrerer Bilder vornehmen. Mit der Verwendung eines segmentierten Rückstreudetektors ist dagegen die Erzeugung eines 3D-Oberflächenmodells während der Bildaufnahme praktisch in Echtzeit möglich. Die Probentopografie wird gleichzeitig mit dem Bildeinzug dargestellt und gespeichert.