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 - Sommer, Konstantin A1 - Agudo Jácome, Leonardo A1 - Hesse, René A1 - Bettge, Dirk T1 - Revealing the nature of melt pool boundaries in additively manufactured stainless steel by nano-sized modulation JF - Advanced engineering materials N2 - In the current study, the 3D nature of the melt pool boundaries (MPBs) in a 316 L austenitic steel additively manufactured by laser-based powder bed fusion (L-PBF) is investigated. The change of the cell growth direction and its relationship to the MPBs is investigated by transmission electron microscopy. A hitherto unreported modulated substructure with a periodicity of 21 nm is further discovered within the cell cores of the cellular substructure, which results from a partial transformation of the austenite, which is induced by a Ga+ focused ion beam. While the cell cores show the modulated substructure, cell boundaries do not. The diffraction pattern of the modulated substructure is exploited to show a thickness ≥200 nm for the MPB. At MPBs, the cell walls are suppressed, leading to continuously connecting cell cores across the MPB. This continuous MPB is described either as overlapping regions of cells of different growing directions when a new melt pool solidifies or as a narrow planar growth preceding the new melt pool. KW - Additive manufacturing KW - Austenitic steel 316L KW - Melt pool boundary KW - Microstructural characterization KW - Transmission electron microscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547295 DO - https://doi.org/10.1002/adem.202101699 SN - 1527-2648 VL - 24 IS - 6 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manzoni, Anna Maria A1 - Mohring, Wencke A1 - Hesse, René A1 - Agudo Jácome, Leonardo A1 - Stephan-Scherb, C. T1 - Early material damage in equimolar CrMnFeCoNi in mixed oxidizing/sulfiding hot gas atmosphere JF - Advanced engineering materials N2 - The challenges to use more varied fuels at medium and high temperatures above 500 °C need to be addressed by tuning the materials toward a better resistance against increased corrosion. As a first step the corrosion processes need to be better understood, especially in the case of the unavoidable and highly corrosive sulfur-based gases. Herein, oxidation/sulfidation of an equimolar CrMnFeCoNi high-entropy alloy is studied at an early stage after hot gas exposure at 600 °C for 6 h in 0.5% SO2 and 99.5% Ar. The oxidation process is studied by means of X-ray diffraction, scanning and transmission electron microscopy, and supported by thermodynamic calculations. It is found that the sulfur does not enter the bulk material but interacts mainly with the fast-diffusing manganese at grain boundary triple junctions at the alloy surface. Submicrometer scaled Cr–S–O-rich phases close to the grain boundaries complete the sulfur-based phase formation. The grains are covered in different Fe-, Mn-, and Cr-based spinels and other oxides. KW - High entropy alloy KW - Sulfiding KW - Corrosion KW - Transmission electron microscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543495 DO - https://doi.org/10.1002/adem.202101573 SN - 1527-2648 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ávila Calderón, Luis Alexander A1 - Rehmer, Birgit A1 - Schriever, Sina A1 - Ulbricht, Alexander A1 - Agudo Jácome, Leonardo A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Skrotzki, Birgit A1 - Evans, Alexander T1 - Creep and creep damage behavior of stainless steel 316L manufactured by laser powder bed fusion JF - Materials Science and Engineering: A N2 - This study presents a thorough characterization of the creep properties of austenitic stainless steel 316L produced by laser powder bed fusion (LPBF 316L) contributing to the sparse available data to date. Experimental results (mechanical tests, microscopy, X-ray computed tomography) concerning the creep deformation and damage mechanisms are presented and discussed. The tested LPBF material exhibits a low defect population, which allows for the isolation and improved understanding of the effect of other typical aspects of an LPBF microstructure on the creep behavior. As a benchmark to assess the material properties of the LPBF 316L, a conventionally manufactured variant of 316L was also tested. To characterize the creep properties, hot tensile tests and constant force creep tests at 600 °C and 650 °C are performed. The creep stress exponents of the LPBF material are smaller than that of the conventional variant. The primary and secondary creep stages and the times to rupture of the LPBF material are shorter than the hot rolled 316L. Overall the creep damage is more extensive in the LPBF material. The creep damage of the LPBF material is overall mainly intergranular. It is presumably caused and accelerated by both the appearance of precipitates at the grain boundaries and the unfavorable orientation of the grain boundaries. Neither the melt pool boundaries nor entrapped gas pores show a significant influence on the creep damage mechanism. KW - 316L KW - Laser Powder Bed Fusion (LPBF) KW - Creep behavior KW - Additive Manufacturing KW - AGIL PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539373 DO - https://doi.org/10.1016/j.msea.2021.142223 SN - 0921-5093 VL - 830 SP - 142223 PB - Elsevier B.V. AN - OPUS4-53937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Suárez Ocaño, Patricia T1 - The Al4-xZr5(Ox-y) Trojan horse in the AlMo0.5NbTiTa0.5Zr refractory high entropy superalloy N2 - Unlike conventional alloys, which typically consist of one main element, high-entropy alloys (HEAs) contain five or more principal elements, which broaden chemical complexity and with it a realm of synergistic mechanisms. The AlMo0.5NbTa0.5TiZr HEA initiated a subclass of Al-containing refractory (r)HEAs that has recently drawn attention [2]. The alloy has a superalloy-resembling B2/bcc nanostructure, which inspired its name refractory high entropy superalloy (RSA). With high-temperature (HT) compressive strengths beyond conventional Ni-based superalloys, this nanostructure could be used for improved HT structural applications. However, in the application-relevant HT regime the Al-Zr-rich B2 phase decomposes to form a hexagonal Al-Zr-based intermetallic (Al4-xZr5; x: 0..1) [3,4]. This work explores the fascinating yet fatal micromechanisms associated to this phase transformation, in the context of creep, annealing and oxidation experiments performed between 800 and 1200 °C. The material was produced by arc-melting and heat treatment in argon, which lead to grain boundaries decorated with up to 7%. Interrupted constant-load creep tests were performed under vacuum (at 10-4 Pa), at 900–1100 °C with external tensile stresses of 30–120 MPa. Oxidation experiments were separately conducted for 24 hours at 800 and 1000 °C in both dry (21% O2 + 79% N2) and humid (8% O2 + 74% N2 + 18% H2O) air. After the experiments, the samples were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy to reveal degradation mechanisms. Crystallographic texture, orientation relationships and stabilization of an oxygen-containing iso structure (Al4-xZr5(Ox-y); y: 0..x) of the Al-Zr-rich intermetallic are found and discussed. T2 - BCC Superalloy Network Opening Workshop CY - Reutte, Austria DA - 08.02.2024 KW - High entropy alloy KW - Superalloy KW - Degradation KW - Electron microscopy KW - Microstructure PY - 2024 AN - OPUS4-59833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocano, Patricia A1 - Agudo Jácome, Leonardo A1 - Lopez-Galilea, I. A1 - Darvishi Kamachali, Reza A1 - Fries, S. G. T1 - Data regarding the experimental findings compared with CALPHAD calculations of the AlMo0.5NbTa0.5TiZr refractory high entropy superalloy JF - Data in brief N2 - This contribution contains the raw data used to compare experimental results with thermodynamic calculations using the CALPHAD method, which is related to the research article “The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: experimental findings and comparison with calculations using the CALPHAD method” [1] , and therefore this article can be used as a basis for interpreting the data contained therein. The AlMo0.5NbTa0.5TiZr refractory superalloy was characterized in the cast and annealed condition (1400 °C for 24 h) in order to measure grain size and to identify and measure the size and area fraction of the phases present. The raw data of this article include X-ray diffraction (XRD) measurements, microstructural characterization by scanning and transmission electron microscopy (SEM and TEM), and elemental analysis by energy dispersive X-ray spectroscopy (EDX). XRD includes the determination of phases and the lattice parameters (A2, B2, and hexagonal structure). Microstructural analysis by scanning and transmission electron microscopy includes (1) identification of composition, size, and volume fraction of the present phases and (2) determination of grain size. Based on these experimental data, it is possible to identify similarities and discrepancies with the data calculated using the CALPHAD method for the alloy under study in Ref. [1] , which provides the basis for better and more efficient development of reliable databases. KW - Transmission electron microscopy KW - Scanning electron microscopy KW - Microstructural characterization KW - Refractory high entropy alloys PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568009 DO - https://doi.org/10.1016/j.dib.2022.108858 SN - 2352-3409 VL - 46 SP - 1 EP - 19 PB - Elsevier CY - Amsterdam AN - OPUS4-56800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Piesker, Benjamin A1 - Ávila Calderón, Luis Alexander A1 - Mohr, Gunther A1 - Rehmer, Birgit A1 - Agudo Jácome, Leonardo A1 - Hilgenberg, Kai A1 - Evans, Alexander A1 - Skrotzki, Birgit T1 - Tensile and Low‐Cycle Fatigue Behavior of Laser Powder Bed Fused Inconel 718 at Room and High Temperature JF - Advanced Engineering Materials N2 - This study investigates the room‐ and high‐temperature (650 °C) tensile and low‐cycle‐fatigue behavior of Inconel 718 produced by laser powder bed fusion (PBF‐LB/M) with a four‐step heat treatment and compares the results to the conventional wrought material. The microstructure after heat treatment is characterized on different length scales. Compared to the wrought variant, the elastic and yield properties are comparable at both test temperatures while tensile strength, ductility, and strain hardening capacity are lower. The fatigue life of the PBF‐LB/M variant at room temperature is slightly lower than that of the wrought material, while at 650 °C, it is vice versa. The cyclic stress response for both material variants is characterized by cyclic softening, which is more pronounced at the higher test temperature. High strain amplitudes (≥0.7%) at room temperature and especially a high testing temperature result in the formation of multiple secondary cracks at the transitions of regions comprising predominantly elongated grain morphology and columns of stacked grains with ripple patterns in the PBF‐LB/M material. This observation and pronounced crack branching and deflection indicate that the cracks are controlled by sharp micromechanical gradients and local crystallite clusters. KW - Additive manufacturing KW - Fatigue damage KW - Heat treatment KW - Inconel 718 KW - Laser powder bed fusion KW - Low-cycle fatigue KW - Tensile strength PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599316 DO - https://doi.org/10.1002/adem.202302122 SN - 1527-2648 SP - 1 EP - 17 PB - Wiley AN - OPUS4-59931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, W. A1 - Gemming, T. A1 - Giebeler, L. A1 - Qu, J. A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, B. A1 - Gonzalez-Martinez, I. T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy JF - Ultramicroscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as ‘‘electron beam-induced fragmentation’’ or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field 𝐵 = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. 𝐵 = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy KW - Electron beam-induced charging PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600170 DO - https://doi.org/10.1016/j.ultramic.2024.113978 VL - 262 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-60017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feng, Wen A1 - Gemming, Thomas A1 - Giebeler, Lars A1 - Qu, Jiang A1 - Weinel, Kristina A1 - Agudo Jácome, Leonardo A1 - Büchner, Bernd A1 - González-Martínez, Ignacio T1 - Influence of magnetic field on electron beam-induced Coulomb explosion of gold microparticles in transmission electron microscopy JF - Ultramicroscopy N2 - In this work we instigated the fragmentation of Au microparticles supported on a thin amorphous carbon film by irradiating them with a gradually convergent electron beam inside the Transmission Electron Microscope. This phenomenon has been generically labeled as “electron beam-induced fragmentation” or EBIF and its physical origin remains contested. On the one hand, EBIF has been primarily characterized as a consequence of beam-induced heating. On the other, EBIF has been attributed to beam-induced charging eventually leading to Coulomb explosion. To test the feasibility of the charging framework for EBIF, we instigated the fragmentation of Au particles under two different experimental conditions. First, with the magnetic objective lens of the microscope operating at full capacity, i.e. background magnetic field B = 2 T, and with the magnetic objective lens switched off (Lorenz mode), i.e. B = 0 T. We observe that the presence or absence of the magnetic field noticeably affects the critical current density at which EBIF occurs. This strongly suggests that magnetic field effects play a crucial role in instigating EBIF on the microparticles. The dependence of the value of the critical current density on the absence or presence of an ambient magnetic field cannot be accounted for by the beam-induced heating model. Consequently, this work presents robust experimental evidence suggesting that Coulomb explosion driven by electrostatic charging is the root cause of EBIF. KW - Electron beam-induced fragmentation KW - Coulomb explosion KW - X-ray diffraction KW - Lorenz transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600247 DO - https://doi.org/10.1016/j.ultramic.2024.113978 SN - 0304-3991 VL - 262 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-60024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - Lopez-Galilea, I. A1 - Darvishi Kamachali, Reza A1 - Roik, J. A1 - Agudo Jácome, Leonardo T1 - The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: Experimental findings and comparison with calculations using the CALPHAD method JF - Materials and design N2 - Detailed microstructural characterization of the AlMo0.5NbTa0.5TiZr refractory high entropy superalloy in the as-cast state is reported for first time and compared with the state annealed at 1400 oC for 24 h. The former shows a dendritic structure, with a mixture of A2/B2 phases < 20 nm in both the dendritic and interdendritic regions. A mostly amorphous phase, rich in Al and Zr, is found within the interdendritic region. The annealed state reproduced the combination of A2/B2/Al-Zr-rich phases reported previously. Calculations from two relevant ThermoCalc databases were compared with the experimental results. Equilibrium calculations were compared with results for the annealed alloy, whereas solidification paths calculated using Scheil-Gulliver model were used for comparison with the as-cast alloy. A previously hypothesized spinodal decomposition during cooling as the mechanism responsible for the patterned A2/B2 microstructure is confirmed via the CALPHAD calculations, pointing to its use as an efficient design tool for such alloys. Finally, the comparison between the experimental and computational findings allowed better understanding the solidification path and equilibrium stability of this alloy, giving a base to make better decisions on the field of new refractory superalloy design. KW - CALPHAD database analysis KW - Refractory superalloys KW - Chemically complex alloy KW - Characterization KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545906 DO - https://doi.org/10.1016/j.matdes.2022.110593 SN - 1873-4197 VL - 217 SP - 1 EP - 13 PB - Elsevier CY - Amsterdam AN - OPUS4-54590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert A1 - Roohbakhshan, Farshad A1 - Fedelich, Bernard A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Cyclic operation performance of 9-12% Cr ferritic-martensitic steels part 2: Microstructural evolution during cyclic loading and its representation in a physically-based micromechanical model T2 - Fit for Future - Advanced Manufacturing Technologies, Materials and Lifetime - Proceedings of the 45th MPA-Seminar N2 - 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. T2 - 45. MPA-Seminar CY - Leinfelden-Echterdingen, Germany DA - 01.10.2019 KW - Tempered Martensite Ferritic Steels KW - P92 KW - TEM KW - EBSD KW - Micromechanical model PY - 2019 SP - 80 EP - 85 PB - MPA (Materialprüfungsanstalt Universität Stuttgart) CY - Stuttgart AN - OPUS4-50052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Famy, A. A1 - Agudo Jácome, Leonardo A1 - Schönhals, Andreas T1 - Effect of Silver Nanoparticles on the Dielectric Properties and the Homogeneity of Plasma Poly(acrylic acid) Thin Films JF - The Journal of Physical Chemistry C N2 - For the first time, structure−electrochemical relationships of thin films of a plasma-polymerized acrylic acid/carbon dioxide AA/CO2 (75/25%) copolymer modified by implanted silver nanoparticles are discussed. The pulsed plasma polymerization of AA/CO2 was utilized and adjusted to obtain a maximal amount of COOH Groups forming an almost uncross-linked polymer structure. The prepared polymer layer is rinsed by a silver nitrate solution to impregnate Ag+ ions. This step is followed by its reduction of Ag+ with NaBH4 as a chemical route in comparison to the reduction by sunlight as an ecofriendly photoreduction method. The chemical composition and morphology of the topmost surface layer of the AA/CO2 polymer thin film were investigated by X-ray photoelectron spectroscopy and atomic force microscopy. Moreover, the molecular mobility, conductivity, and thermal stability of the polymer layer were analyzed using broadband dielectric spectroscopy. The dielectric properties of the AA/ CO2 polymer thin film were studied in the presence of Ag+ ions or Ag0. It was found that a cross-linked polymer layer with a smooth surface and high conductivity was obtained in the presence of Ag+/ Ag0. KW - Nanoparticles PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c06712 SN - 1932-7447 VL - 124 IS - 41 SP - 22817 EP - 22826 PB - ACS AN - OPUS4-51468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Suárez Ocaño, Patricia A1 - Manzoni, Anna Maria A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Laplanche, G. A1 - Agudo Jácome, Leonardo T1 - Influence of cooling rate on the microstructure and room temperature mechanical properties in the refractory AlMo0.5NbTa0.5TiZr superalloy JF - Journal of Alloys and Compounds N2 - Refractory chemically complex alloys with bcc-based microstructures show great potential for high-temperature applications but most of them exhibit limited room-temperature ductility, which remains a challenge. One such example is the AlMo0.5NbTa0.5TiZr alloy, mainly consisting of a nano-scaled structure with an ordered B2 matrix and a high-volume fraction of aligned cuboidal and coherently embedded A2 precipitates. This work aims to investigate how the cooling rate after hot isostatic pressing of the AlMo0.5NbTa0.5TiZr alloy affects its microstructure and its resulting hardness and fracture toughness at room temperature. A slow cooling rate of 5 °C/min leads to a coarse microstructure consisting of aligned slabs (mean A2 precipitate ≈ 25 nm) with a nanohardness of about 8 GPa. In contrast, after the fastest cooling rate (30 °C/min), the A2 precipitates become more cubic with an edge length of ≈ 16 nm, resulting in an increase in nanohardness by 10 %. The fracture toughness is roughly independent of the cooling rate and its mean value (≈ 4.2 MPa∙m1/2) resembles that of some B2 intermetallics and other A2/B2 alloys. As the lattice misfit between the A2 and B2 phases is known to play a key role in microstructure formation and evolution, its temperature dependence between 20 and 900 °C was investigated. These findings offer insights into the evolution of the microstructure and room-temperature mechanical properties of the AlMo0.5NbTa0.5TiZr alloy, which could help the development of advanced chemically complex alloys. KW - High entropy alloy KW - Lattice misfit KW - Scanning electron microscopy KW - Transmission electron microscopy KW - X-ray diffraction KW - Refractory alloy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572809 DO - https://doi.org/10.1016/j.jallcom.2023.169871 SN - 0925-8388 VL - 949 SP - 169871 PB - Elsevier B.V. AN - OPUS4-57280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbricht, Jürgen A1 - Agudo Jácome, Leonardo A1 - Jürgens, Maria A1 - Roohbakhshan, Farshad A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - Cyclic loading performance and related microstructure evolution of ferritic-martensitic 9-12% Cr steels T2 - Fit for Future - Advances in Materials, Manufacturing and Assessment. Proceedings of the 44th MPA-Seminar N2 - The current competitive situation on electricity markets forces 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. T2 - 44th MPA-Seminar CY - Leinfelden/Stuttgart, Germany DA - 17.10.2018 KW - Ferritic-martensitic steels KW - Cyclic loading KW - Microstructure evolution PY - 2018 SP - 259 EP - 265 AN - OPUS4-47118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eggeler, G. A1 - Wieczorek, N. A1 - Fox, F. A1 - Berglund, S. A1 - Bürger, D. A1 - Dlouhý, A. A1 - Wollgramm, P. A1 - Neuking, K. A1 - Schreuer, J. A1 - Agudo Jácome, Leonardo A1 - Gao, S. A1 - Hartmaier, A. A1 - Laplanche, G. T1 - On shear testing of single crystal Ni-base superalloys JF - Metallurgical and Materials Transactions A N2 - Shear testing can contribute to a better understanding of the plastic deformation of Ni-base superalloy single crystals. In the present study, shear testing is discussed with special emphasis placed on its strengths and weaknesses. Key mechanical and microstructural results which were obtained for the high-temperature (T ≈ 1000 °C) and low-stress (τ ≈ 200 MPa) creep regime are briefly reviewed. New 3D stereo STEM images of dislocation substructures which form during shear creep deformation in this regime are presented. It is then shown which new aspects need to be considered when performing double shear creep testing at lower temperatures (T < 800 °C) and higher stresses (τ > 600 MPa). In this creep regime, the macroscopic crystallographic [11−2](111) shear system deforms significantly faster than the [01−1](111) system. This represents direct mechanical evidence for a new planar fault nucleation scenario, which was recently suggested (Wu et al. in Acta Mater 144:642–655, 2018). The double shear creep specimen geometry inspired a micro-mechanical in-situ shear test specimen. Moreover, the in-situ SEM shear specimen can be FIB micro-machined from prior dendritic and interdendritic regions. Dendritic regions, which have a lower γ′ volume fraction, show a lower critical resolved shear stress. T2 - EuroSuperalloys 2018 CY - Oxford, UK DA - 09.09.2018 KW - Superalloy single crystals KW - Shear testing KW - Creep mechanisms KW - In-situ SEM micro shear deformation KW - Transmission electron microscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-456591 DO - https://doi.org/10.1007/s11661-018-4726-9 SN - 1073-5623 SN - 1543-1940 VL - 49A IS - 9 SP - 3951 EP - 3962 PB - Springer US CY - New York AN - OPUS4-45659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mujica Roncery, L. A1 - Agudo Jácome, Leonardo A1 - Aghajani, A. A1 - Theisen, W. A1 - Weber, S. T1 - Subsurface characterization of high-strength high-interstitial austenitic steels after impact wear JF - Wear N2 - The microstructure of the subsurface after impact wear of three high-strength high interstitial austenitic steels has been analysed using transmission electron microscopy (TEM) in alloys with C and N as interstitial elements. In all cases, a nanocrystalline region followed by a transition zone and a cold-worked area are present. Additionally, microhardness and nano-scratching tests were conducted to study the wear-related properties of the impact subsurface and the base material. The results of the microstructural analysis reveal that the following mechanisms are involved during impact wear: abrasion (ploughing), microcrack formation associated with contact fatigue, entrapment and adhesion of SiO2 particles. The analysis of the wear-related properties indicates that the subsurface acts as a self-protective layer that prevents the deterioration of the substrate. KW - Impact wear KW - TEM KW - Nano-scratch test KW - High interstitial austenitic steel PY - 2018 DO - https://doi.org/10.1016/j.wear.2018.02.016 SN - 0043-1648 VL - 402-403 SP - 137 EP - 147 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-44290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cao, L. A1 - Thome, P. A1 - Agudo Jácome, Leonardo A1 - Somsen, C. A1 - Cailletaud, G. A1 - Eggeler, G. T1 - On the influence of crystallography on creep of circular notched single crystal superalloy specimens JF - Materials Science & Engineering A N2 - The present work contributes to a better understanding of the effect of stress multiaxiality on the creep behavior of single crystal Ni-base superalloys. For this purpose we studied the creep deformation and rupture behavior of double notched miniature creep tensile specimens loaded in three crystallographic directions [100], [110] and [111] (creep conditions: 950 °C and 400 MPa net section stress). Crystal plasticity finite element method (CPFEM) was used to analyze the creep stress and strain distributions during creep. Double notched specimens have the advantage that when one notch fails, the other is still intact and allows to study a material state which is close to rupture. No notch root cracking was observed, while microstructural damage (pores and micro cracks) were frequently observed in the center of the notch root region. This is in agreement with the FEM results (high axial stress and high hydrostatic stress in the center of the notched specimen). Twinning was observed in the notch regions of [110] and [111] specimens, and <112> {111} twins were detected and analyzed using orientation imaging scanning electron microscopy. The present work shows that high lattice rotations can be detected in SXs after creep fracture, but they are associated with the high strains accumulated in the final rupture event. KW - Single crystal Ni-Base superalloys KW - Double notched creep specimen KW - Stress distribution KW - Lattice rotation KW - Cracks PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506060 DO - https://doi.org/10.1016/j.msea.2020.139255 SN - 0921-5093 VL - 782 SP - 139255 PB - Elsevier B. V. AN - OPUS4-50606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Weber, Kathrin A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Elucidation of orientation relations between Fe-Cr alloys and corrosionproducts after high temperature SO2 corrosion JF - Corrosion Science N2 - The early stages of corrosion of Fe-Cr-model alloys (2 and 9 % Cr) were investigated after exposure at 650 °C in0.5 % SO2containing gas by electron backscattered diffraction (EBSD) and transmission electron microscopy(TEM). The impact of the grain orientation of the base alloy on the orientation relations of the corrosion productsis presented. After 2 min–5 min exposure the formation of a multi-layered corrosion zone was discovered. Aclear orientation relationship between ferrite and the (Fe,Cr)3O4 spinel could be demonstrated. The obtainedresults show the importance of the grain orientation on oxidation resistance. KW - Iron KW - TEM KW - SEM KW - High temperature corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508911 DO - https://doi.org/10.1016/j.corsci.2020.108809 VL - 174 SP - 1 EP - 11 PB - Elsevier AN - OPUS4-50891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agudo Jácome, Leonardo A1 - Pöthkow, K. A1 - Paetsch, O. A1 - Hege, H.-C. T1 - Three-dimensional reconstruction and quantification of dislocation substructures from transmission electron microscopy stereo pairs JF - Ultramicroscopy N2 - A great amount of material properties is strongly influenced by dislocations, the carriers of plastic deformation. It is therefore paramount to have appropriate tools to quantify dislocation substructures with regard to their features, e.g., dislocation density, Burgers vectors or line direction. While the transmission electron microscope (TEM) has been the most widely-used equipment implemented to investigate dislocations, it usually is limited to the two-dimensional (2D) observation of three-dimensional (3D) structures. We reconstruct, visualize and quantify 3D dislocation substructure models from only two TEM images (stereo pairs) and assess the results. The reconstruction is based on the manual interactive tracing of filiform objects on both images of the stereo pair. The reconstruction and quantification method are demonstrated on dark field (DF) scanning (S)TEM micrographs of dislocation substructures imaged under diffraction contrast conditions. For this purpose, thick regions (> 300 nm) of TEM foils are analyzed, which are extracted from a Ni-base superalloy single crystal after high temperature creep deformation. It is shown how the method allows 3D quantification from stereo pairs in a wide range of tilt conditions, achieving line length and orientation uncertainties of 3% and 7°, respectively. Parameters that affect the quality of such reconstructions are discussed. KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) KW - Stereoscopy KW - Visualization PY - 2018 DO - https://doi.org/10.1016/j.ultramic.2018.08.015 SN - 0304-3991 VL - 195 SP - 157 EP - 170 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-46355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - Navigating the Nanoworld: Understanding Materials Properties with the Transmission Electron Microscope N2 - The field of materials science is defined as “the study of the properties of solid materials and how those properties are determined by a material’s composition and structure.”. Many –if not most– of the materials that are produced nowadays owe their properties to structures engineered down to the nanoscopic level. This need has been partly realized thanks to the understanding of materials’ building blocks via characterization techniques that reach this level of resolution. Transmission electron microscopy, since its first implementation in the early 1930s (in Berlin), has been implemented to achieve imaging –and spectral– analysis at lateral resolutions down to the atomic level. In this contribution, a series of practical examples will be presented, where applied materials are characterized by a range of transmission electron microscopy techniques to understand structural and functional properties of a wide range of materials. Among these materials examples will be presented on structural conventionally and additively manufactured metallic alloys, high entropy alloys, dissimilar aluminum-to-steel welds, magnetic nanoparticles, ceramic coatings, high temperature oxidation products. Addressed will be either the effect of processing route or that of the exposure to experimental conditions similar to those found in the respective intended applications. T2 - UA/UAB/UAH MSE Graduate Seminar CY - Online meeting DA - 19.01.2022 KW - Transmission electron microscopy (TEM) KW - Characterization KW - Microstructure KW - 3D PY - 2022 AN - OPUS4-54238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - Agudo Jácome, Leonardo T1 - Thermodynamic study of a refractory complex concentrated alloy (rCCA) using the CALPHAD method N2 - Multi-principal-element alloys (MPEAs), have recently come to the attention of the scientific community due to their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime. The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed. T2 - EUROMAT 2019 CY - Stockholm, Sweden DA - 01.09.2019 KW - Chemically Complex Alloy KW - CALPHAD KW - Electromicroscopy PY - 2019 AN - OPUS4-50730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Sommer, Konstantin A1 - Hesse, René A1 - Bettge, Dirk T1 - Revealing the Nature of Melt Pool Boundaries in Additively Manufactured Stainless Steel by Nano-sized Modulation N2 - Additive manufacturing (AM) of metallic alloys has gained momentum in the past decade for industrial applications. The microstructures of AM metallic alloys are complex and hierarchical from the macroscopic to the nanometer scale. When using laser-based powder bed fusion (L-PBF) process, two main microstructural features emerge at the nanoscale: the melt pool boundaries (MPB) and the solidification cellular substructure. Here, details of the MPB are revealed to clearly show the three-dimensional nature of MPBs with changes of cell growth of direction and their relation to their surrounding cellular substructure, as investigated by transmission electron microscopy (TEM) for L-PBF 316L austenitic stainless steel (cf. Figure 1). A hitherto unknown modulated substructure with a period of 21 nm is further discovered within cells as the result of a partial Ga+-focused ion beam-induced ferritic transformation of the austenite. Cell cores and cell boundaries differ notably regarding the modulated substructure. T2 - 3. Fachtagung Werkstoffe und Additive Fertigung 2022 CY - Dresden, Germany DA - 11.05.2022 KW - Additive manufacturing KW - Austenitic steel 316L KW - Melt pool boundary KW - Microstructural characterization KW - Transmission electron microscopy PY - 2022 AN - OPUS4-54836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Pöthkow, K. A1 - Paetsch, O. A1 - Hege, H.-C. T1 - 3D reconstruction and quantification of dislocation substructures from TEM stereo pairs N2 - Dislocations are the carriers of plastic deformation. As such, their characterization offers important information on the properties they affect. In this contribution, a new tool is presented, which is incorporated in Amira ZIB Edition and allows for three-dimensional (3D) imaging and quantification of dislocations substructures from thick regions an electron-transparent specimen. In the tool, the dislocation segments are traced on diffraction contrast images that are obtained in the transmission electron microscope (TEM). The uncertainties related to the experimental setup and to the proposed method are discussed on the base of a tilt series. T2 - AVIZO / AMIRA User Meeting CY - Berlin, Germany DA - 14.11.2018 KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) PY - 2018 AN - OPUS4-47394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Elert, Anna Maria A1 - Hodoroaba, Vasile-Dan A1 - Agudo Jácome, Leonardo A1 - Altmann, Korinna A1 - Silbernagl, Dorothee A1 - Sturm, Heinz T1 - Short- and long-range mechanical and chemical interphases caused by interaction of Boehmite (γ-AlOOH) with anhydride-cured epoxy resins JF - Nanomaterials N2 - Understanding the interaction between boehmite and epoxy and the formation of their interphases with different mechanical and chemical structures is crucial to predict and optimize the properties of epoxy-boehmite nanocomposites. Probing the interfacial properties with atomic force microscopy (AFM)-based methods, especially particle-matrix long-range interactions, is challenging. This is due to size limitations of various analytical methods in resolving nanoparticles and their interphases, the overlap of interphases, and the effect of buried particles that prevent the accurate interphase property measurement. Here, we develop a layered model system in which the epoxy is cured in contact with a thin layer of hydrothermally synthesized boehmite. Different microscopy methods are employed to evaluate the interfacial properties. With intermodulation atomic force microscopy (ImAFM) and amplitude dependence force spectroscopy (ADFS), which contain information about stiffness, electrostatic, and van der Waals forces, a soft interphase was detected between the epoxy and boehmite. Surface potential maps obtained by scanning Kelvin probe microscopy (SKPM) revealed another interphase about one order of magnitude larger than the mechanical interphase. The AFM-infrared spectroscopy (AFM-IR) technique reveals that the soft interphase consists of unreacted curing agent. The long-range electrical interphase is attributed to the chemical alteration of the bulk epoxy and the formation of new absorption bands. KW - Nanocomposites KW - Interphase KW - Intermodulation AFM KW - Electron microscopy KW - Infrared nano AFM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483672 UR - https://www.mdpi.com/2079-4991/9/6/853/htm DO - https://doi.org/10.3390/nano9060853 SN - 2079-4991 VL - 9 IS - 6 SP - 853, 1 EP - 20 PB - MDPI AN - OPUS4-48367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Roohbakhshan, Farshad A1 - Nolze, Gert A1 - Fedelich, Bernard A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Cyclic Operation Performance of 9-12% Cr Ferritic-Martensitic Steels. Part 2: Microstructural Evolution during Cyclic Loading and its Representation in a Physically-based Micromechanical Model N2 - The current trend towards cyclic, “flexible” operation of fossil-fueled power plants constitutes a major issue regarding lifetime and operational safety of the respective installations and their components, as was outlined in our complementary contribution (Part 1). The present contribution reports on the investigation of the microstructure evolution in cyclically loaded ferritic-martensitic steels and its representation in a physically-based micromechanical model. For this purpose, specimens of P92 steel grade from the mechanical test programme outlined in our companion contribution (Part 1) were analyzed by scanning electron microscopy (SEM), including backscattered diffraction (EBSD) mapping, and transmission electron microscopy (TEM). A novel method was implemented to improve angular resolution of EBSD scans. Additionally, a correlative microscopy approach was developed and used to correlate EBSD and TEM measurements on the same locations of thick regions of electron transparent specimens. By applying these techniques, a detailed quantitative microstructure description of the as-received material condition, namely in terms of subgrain morphology and dislocation density/distributions, was established. Comparisons of as-received and cyclically loaded conditions from tests interrupted at different stages of lifetime indicate a rapid redistribution of in-grain dislocations with a strong interaction between mobile dislocations and low angle grain boundaries (LABs). The proposed micromechanical model is formulated in a viscoplastic self-consistent (VPSC) scheme, which is a mean-field approach that allows us to include the crystal details at the level of slip systems while avoiding the considerable computational costs of full-field approaches (such as the classical crystal plasticity finite element analysis). Being physically-based, the model uses dislocation densities and includes the interaction between dislocations, e.g. annihilation of mobile dislocations, and evolution of microstructure, e.g. the grain coarsening. Particularly, the constitutive laws for dislocation evolution and interaction between dislocations and low angle boundaries are calibrated based on two-dimensional discrete dislocation dynamic (2D DDD) simulations, which are performed at a micro-/meso-scale. The results of the beforementioned EBSD experiments are considered as a direct input, involving e.g. the amount of geometrically necessary dislocations, average misorientations and grain characteristics. T2 - 45th MPA-Seminar 2019 CY - Leinfelden-Echterdingen, Germany DA - 01.10.2019 KW - Tempered martensite ferritic steel KW - Dislocation KW - Electron backscattered diffraction (EBSD) KW - Transmission electron microscopy (TEM) KW - Microstructure KW - Physically based material model PY - 2019 AN - OPUS4-49346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo A1 - Jürgens, Maria A1 - Sonntag, Nadja A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Cyclic operation performance of 9 -12% cr ferritic martensitic steels part 1: cyclic mechanical behavior under fatigue and creep fatigue loading N2 - 9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in fossil fueled power plants due to their excellent creep and oxidation resistance, but changes in electricity markets during the last two decades have considerably changed the typical working conditions of these facilities. The growing share of renewable energy sources in power generation forces most of these plants into flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue, raising the question which fundamental processes govern the reaction of ferritic-martensitic steels to cyclic load and temperature variations. The present contribution reports on current findings obtained in a multidisciplinary project funded by German Ministry of Education and Research (BMBF) which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses and related micromechanical modeling. In the present first part of our contribution, an overview will be given on the results obtained in the mechanical testing programme of the project. Mechanical analyses were carried out on P91 and (mainly) P92 steel grades, particularly looking at softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods. For this purpose, cylindrical specimens were extracted from thick-walled steam pipes, orthogonal to the pipe axis, and subjected to strain controlled cyclic loading (± 0.2 to ±0.5 % mechanical strain) to different degrees of softening at temperatures up to 620 °C. The test results will be presented and discussed with a focus on the impact of hold periods (i.e. combined creep-fatigue conditions) on mechanical softening, lifetime and crack formation. Details on the microstructural evolution and their representation in a micromechanical model will be given in a second, complementary contribution to this conference. T2 - 45. MPA-Seminar CY - Stuttgart, Germany DA - 01.10.2019 KW - Tempered Martensite Ferritic Steels KW - Low Cycle Fatigue KW - Creep-Fatigue KW - Thermo-Mechanical Fatigue KW - P92 PY - 2019 AN - OPUS4-50050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kianinejad, Kaveh A1 - Darvishi Kamachali, Reza A1 - Khedkar, Abhinav A1 - Manzoni, Anna A1 - Agudo Jácome, Leonardo A1 - Schriever, Sina A1 - Saliwan Neumann, romeo A1 - Megahed, Sandra A1 - Heinze, Christoph A1 - Kamrani, Sepideh A1 - Fedelich, Bernard T1 - Creep anisotropy of additively manufactured Inconel-738LC: Combined experiments and microstructure-based modeling JF - Materials Science and Engineering: A N2 - The current lack of quantitative knowledge on processing-microstructure–property relationships is one of the major bottlenecks in today’s rapidly expanding field of additive manufacturing. This is centrally rooted in the nature of the processing, leading to complex microstructural features. Experimentally-guided modeling can offer reliable solutions for the safe application of additively manufactured materials. In this work, we combine a set of systematic experiments and modeling to address creep anisotropy and its correlation with microstructural characteristics in laser-based powder bed fusion (PBF-LB/M) additively manufactured Inconel-738LC (IN738LC). Three sample orientations (with the tensile axis parallel, perpendicular, and 45° tilted, relative to the building direction) are crept at 850 °C, accompanied by electron backscatter secondary diffraction (EBSD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations. A crystal plasticity (CP) model for Ni-base superalloys, capable of modeling different types of slip systems, is developed and combined with various polycrystalline representative volume elements (RVEs) built on the experimental measurements. Besides our experiments, we verify our modeling framework on electron beam powder bed fusion (PBF-EB/M) additively manufactured Inconel-738LC. The results of our simulations show that while the crystallographic texture alone cannot explain the observed creep anisotropy, the superlattice extrinsic stacking faults (SESF) and related microtwinning slip systems play major roles as active deformation mechanisms. We confirm this using TEM investigations, revealing evidence of SESFs in crept specimens. We also show that the elongated grain morphology can result in higher creep rates, especially in the specimens with a tilted tensile axis. KW - Additive manufactured Ni-base superalloys KW - Creep KW - Crystal plasticity KW - Superlattice extrinsic stacking faults PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601576 DO - https://doi.org/10.1016/j.msea.2024.146690 SN - 0921-5093 VL - 907 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-60157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -