TY - JOUR A1 - Abel, Andreas A1 - Rosalie, Julian M. A1 - Reinsch, Stefan A1 - Zapala, Pawel A1 - Michels, Heiner A1 - Skrotzki, Birgit T1 - Influence of Mo and B additions in intermetallic near-Fe3Al alloys on microstructure and mechanical properties JF - Intermetallics N2 - Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms. KW - Materials Chemistry KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials KW - General Chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-585284 DO - https://doi.org/10.1016/j.intermet.2023.108074 VL - 163 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-58528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, M. A1 - Bettge, Dirk A1 - Hilgenberg, Kai A1 - Binder, M. A1 - Dollmeier, K. A1 - Dreyer, M. A1 - Klöden, B. A1 - Schlingmann, T. A1 - Schmidt, J. T1 - Reproducibility and Scattering in Additive Manufacturing: Results from a Round Robin on PBF-LB/M AlSi10Mg Alloy T1 - Reproduzierbarkeit und Streuung bei der additiven Fertigung: Ergebnisse eines Ringversuchs mit einer PBF-LB/M AlSi10Mg-Legierung JF - Practical Metallography N2 - The round robin test investigated the reliability users can expect for AlSi10Mg additive manufactured specimens by laser powder bed fusion through examining powder quality, process parameter, microstructure defects, strength and fatigue. Besides for one outlier, expected static material properties could be found. Optical microstructure inspection was beneficial to determine true porosity and porosity types to explain the occurring scatter in properties. Fractographic analyses reveal that the fatigue crack propagation starts at the rough as-built surface for all specimens. Statistical analysis of the scatter in fatigue using statistical derived safety factors concludes that at a stress of 36.87 MPa the fatigue limit of 107 cycles could be reached for all specimen with a survival probability of 99.999 %. N2 - Im Rahmen eines Ringversuchs wurde durch die Untersuchung der Pulverqualität, der Prozessparameter, der Gefügefehler, der Festigkeit und der Ermüdung die Zuverlässigkeit bestimmt, die Nutzer von AlSi10Mg-Proben erwarten können, die mit pulverbettbasiertes Schmelzen mittels Laser (engl. Laser Powder Bed Fusion) gefertigt worden sind. Abgesehen von einem Ausreißer wurden die erwarteten statischen Materialeigenschaften erreicht. Eine optische Gefügeprüfung diente dazu, die tatsächliche Porosität und Arten von Porosität zu ermitteln, um die bei den Eigenschaften auftretende Streuung zu erklären. Fraktographische Unterschungen zeigen eine bei allen Proben von der rauen Oberfläche im As-built-Zustand ausgehende Ermüdungsrissausbreitung. Aus der statistischen Analyse der Streuung bezüglich der Ermüdung unter Anwendung von statistischen abgeleiteten Sicherheitsfaktoren geht hervor, dass alle Proben die Dauerfestigkeit von 107 Zyklen bei einer Spannung von 36,87 MPa mit einer Überlebenswahrscheinlichkeit von 99,999 % erreichten. KW - Additive manufacturing KW - Reproducibility KW - Reliability PY - 2022 DO - https://doi.org/10.1515/pm-2022-1018 SN - 2195-8599 VL - 59 IS - 10 SP - 580 EP - 614 PB - De Gruyter AN - OPUS4-55935 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, J. A1 - Farris, L. A1 - Nolze, Gert A1 - Reinsch, Stefan A1 - Cios, G. A1 - Tokarski, T. A1 - Thompson, S. T1 - Microstructure evolution in Inconel 718 produced by powder bed fusion additive manufacturing JF - Journal of manufacturing and materials processing N2 - Inconel 718 is a precipitation strengthened, nickel-based super alloy of interest for the Additive Manufacturing (AM) of low volume, complex parts to reduce production time and cost compared to conventional subtractive processes. The AM process involves repeated rapid melting, solidification and reheating, which exposes the material to non-equilibrium conditions that affect elemental segregation and the subsequent formation of solidification phases, either beneficial or detrimental. These variations are difficult to characterize due to the small length scale within the micron sized melt pool. To understand how the non-equilibrium conditions affect the initial solidification phases and their critical temperatures, a multi-length scale, multi modal approach has been taken to evaluate various methods for identifying the initial phases formed in the as-built Inconel 718 produced by laser-powder bed fusion (L-PBF) additive manufacturing (AM). Using a range of characterization tools from the bulk differential thermal analysis (DTA) and x-ray diffraction (XRD) to spatially resolved images using a variety of electron microscopy tools, a better understanding is obtained of how these minor phases can be properly identified regarding the amount and size, morphology and distribution. Using the most promising characterization techniques for investigation of the as-built specimens, those techniques were used to evaluate the specimens after various heat treatments. During the sequence of heat treatments, the initial as-built dendritic structures recrystallized into well-defined grains whose size was dependent on the temperature. Although the resulting strength was similar in all heat treated specimens, the elongation increased as the grain size was refined due to differences in the precipitated phase distribution and morphology. KW - Metal additive manufacturing KW - Inconel 718 KW - Heat treatment KW - Grain boundary precipitates KW - Laves phase PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542758 DO - https://doi.org/10.3390/jmmp6010020 SN - 2504-4494 VL - 6 IS - 1 SP - 1 EP - 20 PB - MDPI CY - Basel AN - OPUS4-54275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Bettge, Dirk A1 - Kratzig, Andreas A1 - Knauer, S. T1 - Factors Influencing Droplet Corrosion in Dense Phase CO2 T2 - Proceedings NACE International Corrosion Conference 2019 N2 - Recent studies have shown that even at a very low concentration of impurities (less than 100 ppmv of SO2, NO2, O2 and H2O) the droplet formation and condensation of sulfuric and nitric acids in dense phase CO2 are possible and observable. To reveal the mechanism of droplet corrosion in dense phase CO2 at high pressure and low temperature, further studies on factors that affect wettability and resulting corrosion behaviors of transport pipeline steels are needed. In this study, effects of surface morphology were investigated by varying surface roughness of carbon steel coupons exposed to CO2 stream containing impurities to measure the wettability by contact angle and to observe the condensation as well as possible droplet corrosion that followed. Other considered factors were: pH of the droplet, temperature, droplet volume, and exposure time. T2 - NACE International Corrosion Conference 2019 CY - Nashville, TN, USA DA - 24.03.2019 KW - CCUS KW - Dense phase KW - CO2 KW - Droplet KW - Corrosion KW - Condensation KW - Carbon steel PY - 2019 SP - 13017-1 EP - 13017-13 PB - NACE International CY - Houston AN - OPUS4-47915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weinel, Kristina A1 - Schultz, J. A1 - Wolf, D. A1 - Kalady, M. F. A1 - Agudo, Leonardo A1 - Lubk, A. A1 - Büchner, B. A1 - Grundy, N. A1 - Gonzalez-Martinez, I. T1 - Electron-beam-induced synthesis and characterization of disordered plasmonic gold nanoparticle assemblies N2 - Several studies have been shown that the electron beam can be used to create nanomaterials from microparticle targets in situ in a transmission electron microscope (TEM). Here, we show how this method has to be modified in order to synthesize plasmonic gold nanoparticles (NPs) on insulating silicon oxide substrate by employing a scanning electron microscope with a comparatively low acceleration voltage of 30 kV. The synthesized NPs exhibit a random distribution around the initial microparticle target: Their average size reduces from 150 nm to 3 nm with growing distance to the initial Au microparticle target. Similarly, their average distance increases. The synthesized NP assemblies therefore show distinctly different plasmonic behaviour with growing distance to the target, which allows to study consequences of random hybridization of surface plasmon in disordered system, such as Anderson localization. To reveal the surface plasmons and their localization behaviour we apply electron energy loss spectroscopy in the TEM. T2 - DPG spring conference, condensed matter section CY - Berlin, Germany DA - 17.03.2024 KW - Scanning electron microscopy KW - Gold nanoparticle synthesis KW - Disordered assemblies KW - Localized plasmons PY - 2024 AN - OPUS4-59763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, F. A1 - Ngai, S. A1 - Zhou, X. Y. A1 - Zaiser, E. A1 - Manzoni, Anna Maria A1 - Wu, Y. A1 - Zheng, W. W. A1 - Zhang, P. A1 - Thompson, G. B. T1 - Tracking maze-like hierarchical phase separation behavior in a Fe-Si-V alloy JF - Journal of Alloys and Compounds N2 - Optimizing the properties of next-generation high-temperature and corrosion-resistant alloys is rooted in balancing structure-property relationships and phase chemistry. Here, we implement a complementary approach based on transmission electron microscopy (TEM) and atom probe tomography (APT) to ascertain aspects of hierarchical phase separation behavior, by understanding the microstructural evolution and the three-dimensional (3D) nanochemistry of a single crystal Fe79.5Si15.5V5.0 (at%) alloy. A maze-like hierarchical microstructure forms, in which a complex network of metastable disordered α plates (A2 phase) emerges within ordered α1 precipitates (D03 phase). The supersaturation in α1 (D03) precipitates with Fe and V drives the formation of α (A2) plates. The morphology of α (A2) plates is discussed concerning crystal structure, lattice misfit, and elastic strain. Phase compositions and a ternary phase diagram aid the thermodynamic assessment of the hierarchical phase separation mechanism via the Gibbs energy of mixing. A perspective on the stabilization of hierarchical microstructures beyond Fe79.5Si15.5V5.0 is elaborated by comparing hierarchical alloys. We find that the ratio of elastic anisotropy (Zener ratio) serves as a predictor of the hierarchical particles’ morphology. We suggest that the strengthening effect of hierarchical microstructures can be harnessed by improving the temporal and thermal stability of hierarchical particles. This can be achieved through phase-targeted alloying aiming at the hierarchical particles phase by considering the constituents partitioning behavior. Beyond Fe79.5Si15.5V5.0, our results demonstrate a potential pathway for improving the properties of high-temperature structural materials. KW - Atom probe tomography KW - Transmission electron microscopy KW - Hierarchical microstructure KW - Phase separation PY - 2023 DO - https://doi.org/10.1016/j.jallcom.2023.172157 SN - 0925-8388 VL - 968 SP - 1 EP - 17 PB - Elsevier B.V. AN - OPUS4-58343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodrigues, A. C. P. A1 - Feller, A. A1 - Agudo Jácome, Leonardo A1 - Azevedo, C. R. F. T1 - Use of synthetic Fe3O4-rich tribofilms to investigate the effect of microconstituents, temperature and atmosphere on the friction coefficient during pin-on-disc tribotest JF - Surface Topography: Metrology and Properties N2 - This work investigates the effect of the tribotesting parameters (temperature, atmosphere, and third body chemical composition) on the coefficient of friction (CoF) during pin-on-disc dry (PoD) sliding tribotests using artificial third bodies. The third body comprised nanometric Fe3O4-based binary to quaternary chemical compositions containing copper, graphite, and zirconia. These mixtures were manually or ball-milled prepared, and pin-on-disc tribotests were conducted at 23 °C and 400 °C under air or nitrogen atmospheres. Combining PoD and artificial third body to create synthetic tribofilms might be useful for testing new formulations of Cu-free friction materials. Microstructural characterisation of the tribofilms was used to study the stability of the Fe3O4, copper, and graphite nanoparticles under different testing conditions to understand their effects on the CoF. For the Fe3O4-C-ZrO2-X systems, the ball milling mixing promoted the formation of turbostratic graphite in the tribofilm, impairing the lubricating effect of the graphite under air atmosphere at 23 °C. The formation of monoclinic CuO in the tribofilms during tribotests at 400 °C under air and N2 atmospheres promoted a lubricating effect. KW - Tribology KW - Microstructure KW - Oxide KW - Transmission electron microscopy PY - 2022 DO - https://doi.org/10.1088/2051-672X/ac9d51 SN - 2051-672X VL - 10 IS - 4 SP - 044009-1 EP - 044009-18 PB - IOP Pobilishing AN - OPUS4-56467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Lawrence, M. J. A1 - Celorrio, V. A1 - Wang, Q. A1 - Gu, M. A1 - Sun, Z. A1 - Agudo Jácome, Leonardo A1 - Russell, A. E. A1 - Huang, L. A1 - Rodriguez, P. T1 - Nickel confined in 2D earth-abundant oxide layers for highly efficient and durable oxygen evolution catalysts JF - Journal of Materials Chemistry A N2 - Low cost, high-efficiency catalysts towards water splitting are urgently required to fulfil the increasing demand for energy. In this work, low-loading (<20 wt%) Ni-confined in layered metal oxide anode catalysts (birnessite and lepidocrocite titanate) have been synthesized by facile ion exchange methodology and subjected to systematic electrochemical studies. It was found that Ni-intercalated on K-rich birnessite (Ni-KMO) presents an onset overpotential (ηonset) as low as 100 mV and overpotential at 10 mA cm−2 (η10) of 206 mV in pH = 14 electrolyte. By combining electrochemical methods and X-ray absorption and emission spectroscopies (XAS and XES), we demonstrate Ni sites are the active sites for OER catalysis and that the Mn3+ sites facilitate Ni intercalation during the ion-exchange process, but display no observable contribution towards OER activity. The effect of the pH and the nature of the supporting electrolyte on the electrochemical performance was also evaluated. KW - Confined catalyst KW - Low-loading KW - Layered manganese oxide KW - Oxygen evolution reaction KW - Transmission electron microscopy (TEM) PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515027 DO - https://doi.org/10.1039/D0TA04031B SN - 2050-7496 SN - 2050-7488 VL - 8 IS - 26 SP - 13340 EP - 13350 PB - Royal Society of Chemistry CY - London AN - OPUS4-51502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Svetlov, I. L. A1 - Epishin, A. I. A1 - Petrushin, N. V. A1 - Gerstein, G. A1 - Nolze, Gert A1 - Maier, H. J. T1 - Creep of Directionally Solidified Eutectics Ni/Ni3 Al–NbC under Thermal Cycling JF - Inorganic Materials: Applied research N2 - A nickel-based eutectic alloy with a γ/γ'-NbC structure was directionally solidified with a planar front. The specimens were tested for creep under sawtooth thermal cycling in the temperature range from 600 to 1100°C. It has been established that the lifetime under the conditions of thermal cycling is about five times shorter than it is predicted by the linear damage accumulation rule on the basis of results of isothermal creep tests. Faster creep under thermal cycling is caused by the rapid coarsening of the γ/γ' microstructure due to the periodic partial dissolution and reprecipitation of the γ' phase in heating and cooling half-cycles. KW - High temperature nickel-based eutectic alloys KW - γ/γ' matrix KW - Carbide phase NbC KW - In-situ composites KW - Creep under thermal cycling PY - 2022 DO - https://doi.org/10.1134/S2075113322040347 SN - 2075-1133 VL - 13 IS - 4 SP - 1099 EP - 1108 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-55163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mosquera Feijoo, Maria A1 - Oder, Gabriele A1 - Saliwan Neumann, Romeo A1 - Buchheim, Michaela A1 - Kranzmann, Axel A1 - Olbricht, Jürgen T1 - Impact of Sample Geometry and Surface Finish on VM12‑SHC Ferritic–Martensitic Steel Under Cyclic Steam Atmosphere Operating Conditions JF - Oxidation of Metals N2 - The steam side oxidation of ferritic–martensitic VM12-SHC steel was investigated under thermo-cyclic conditions in water steam at 620/320 °C and 30 bar with a focus on assessing the influence of pre-oxidation time, specimen geometry and surface finish. The specimens were pre-oxidized under isothermal conditions in water steam at 620 °C and 30 bar for 500 h or 1500 h. After pre-oxidation treatment, all specimens were subjected up to 258 thermal cycles. Three different geometries—rectangular coupons, U-shaped ring segments and ring samples—were investigated to evaluate the influence of open/closed shape, and flat/curved surface on corrosion rate. At the same time, two types of surface finish were considered: “as received” and “ground.” The formation of a protective scale by pre-oxidation was investigated. EBSD and ESMA analyses revealed that the Cr-content of the alloy appeared to be insufficient for obtaining a protective oxide scale under studied conditions, at the same time the anayses confirmed that initial oxidation depends on presence of minor alloying elements as Si and Mn, strong oxide formers which can alter the kinetics and morphology of the corrosion reaction. Moreover, rectangular coupons with small wall thickness and flat surface exhibited the highest corrosion rate, while “ground” curved samples showed only local oxidation. This indicates that for same pre-oxidation time, oxidation kinetics is controlled by curvature. KW - Cyclic steam oxidation KW - 12%Cr steel KW - Specimen geometry KW - Surface treatments PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551808 DO - https://doi.org/10.1007/s11085-022-10114-6 SN - 0030-770X SP - 1 EP - 18 PB - Springer AN - OPUS4-55180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -