TY - CONF A1 - Suárez Ocano, Patricia T1 - I n situ monitoring of growing oxidation of the chemically complex alloy AlMo 0.5 NbTa 0.5 TiZr in the high temperature regime using synchrotron radiation Preliminary results N2 - The chemically complex alloys (CCAs) that contain mostly refractory elements (rCCAs), may be highly resistant to heat and load, which makes them attractive candidates for use at extremely high temperatures associated with many technological applications, e.g. aeroengine turbines. However, the field of CCAs, especially their resistance in harsh (oxidative) and hot environment is still young and not much experimental evidence for the understanding mechanisms in this regime is available, which the proposed study addresses. For safe use in structural applications, in addition to their mechanical performance, the environmental resistance of this alloy is also critical. Surface degradation can significantly decrease the mechanical resistance during high temperature exposure, leading to premature failure. The AlMo0.5NbTa0.5TiZr rCCA only contains Al as a protection candidate and it is composed of a coherent B2/bcc nanoscopic cube-on-cube interweave and an hexagonal phase. The evaluation of the oxidation process in the AlMo0.5NbTa0.5TiZr rCCA in the heat-treated state has not been assessed yet. The proposed study focusses on a deeper understanding of the formation mechanism and growth kinetics of oxides at high temperature in the AlMo0.5NbTa0.5TiZr rCCA using synchrotron radiation. Due to the envisaged high temperature structural applications, the alloy is evaluated in an oxidation environment specifically between 800°C and 1000°C. T2 - Large scale facility-based techniques SPP meeting CY - Online meeting DA - 02.11.2021 KW - Refractory chemically complex alloys KW - Oxidation behavior KW - Microstructural analysis KW - Synchrotron radiation PY - 2021 AN - OPUS4-54383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocaño, Patricia A1 - Agudo Jácome, Leonardo T1 - Oxidation Behavior of the AlMo0.5NbTa0.5TiZr Chemically Complex Alloy N2 - The chemically complex alloys that contain mostly refractory elements (rCCAs), may be highly resistant to heat and load, which makes them attractive candidates for use at extremely high temperatures associated with technological applications such as aeroengine turbines. However, the oxidation behavior remains an emerging field within the CCA community. The fully heat treated AlMo0.5NbTa0.5TiZr rCCA contains a dual-phase microstructure that resembles the γ/ γ’ pattern of the well-known Ni-base superalloys, however with a continuous Al-Zr-Ti-rich B2 ordered matrix embedding Mo-Nb-Ta-rach bcc precipitates. The question thus arises what is the oxidation behavior of this rCCA alloy? In this study, this question is addressed via in situ and ex situ X-ray diffraction (XRD) in dry and humid air in the 800–1000 °C regime. Electron microscopic investigations complement the findings. In situ synchrotron experiments were carried out at the KMC2 beamline of the Helmholtz Zentrum Berlin (HZB), with a wavelength of 1.5418 Å at 800 and 950 °C under dry and humid (≈ 40% rH, laboratory air) air for 12 h. Scanning and transmission electron microscopy was performed before and after exposure to spatially resolve the scale development ex situ. In general, 12 h exposure led to an oxide scale which internal oxidation reaches several tens of microns, and which is dominated by Zr-, Ti- and Mo-containing oxides although aluminum oxide was also always present. Main differences are observed between temperatures, while the humidity played a lesser role. T2 - International Conference on High Entropy Materials (ICHEM) 2023 CY - Knoxville, TN, USA DA - 18.06.2023 KW - High entropy superalloy KW - High temperature oxidation KW - In situ synchrotron diffraction KW - Electron microscopy PY - 2023 AN - OPUS4-63857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia T1 - Incipient Oxidation and Deformation Mechanisms of the Chemically Complex Alloy AlMo 0.5 NbTa 0.5 TiZr in the high temperature regime N2 - The development of refractory chemically complex alloys (rCCAs) has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy. It was named as “high entropy superalloy” as it resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. However, the continuous phase in Ni Base alloys is an fcc solution and the cuboidal γ’ precipitates present the L12 intermetallic structure. On the opposite, this CCA has a reversed microstructure where the continuous matrix is formed by an ordered B2 phase which contains cuboidal precipitates of a disordered BCC phase. Some of the most importat results of microstructural analysis, creep test and oxidation are presented in the following work. The as-cast sample shows a bcc/B2 structure with hexagonal phase precipitates in amorphous state whereas the annealed sample also shows a combination of these phases but with larger bcc precipitates and a fully crystallized hexagonal intermetallic. It was found that porosity was higher in the annealed samples (Kinkerdall effect) and the hardness was higher in samples with faster cooling rate due smaller nanostructure. Norton plots show both diffusion and dislocation controlled deformation, and it was found different kinetics between dry and humid air oxidation with the presence of spallation. T2 - CONVEMI 2021 (Venezuelan congress of microscopy and microanalysis) CY - Online meeting DA - 29.10.2021 KW - High entropy superalloys KW - Mechanical properties KW - Oxidation behavior KW - Microstructural analysis PY - 2021 AN - OPUS4-54382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocaño, Patricia A1 - Agudo Jácome, Leonardo T1 - Creep degradation of the high entropy superalloy AlMo0.5NbTa0.5TiZr N2 - The refractory high entropy superalloy (RSA) AlMo0.5NbTa0.5TiZr was the first of a class, with a dual-phase microstructure that resembles that of γ/γ’ in Ni-base superalloys), and the open question whether it performs better as structural alloy under high temperature (HT) applications. Here, we address the HT creep behavior and its associated microstructural degradation of this RSA. The material was produced by arc-melting, heat treatment in argon (24 h @ 1400 °C + 4 h hot isostatic pressure @ 1370 °C & 170 MPa). Interrupted vacuum creep tests were performed at 900-1100 °C and 30-120 MPa. Scanning (S) and transmission (T) electron microscopy (EM) were used to reveal degradation mechanisms. At 1100 °C (Fig.1, middle), the dual A2/B2 microstructure coarsens and partially transforms into a Zr-Al-rich phase (red arrow). An additional external load pronounces directional coarsening. Results are further discussed on the base dislocation and additional damage mechanisms. T2 - International Conferende on Strength of Materials (ICSMA) 2022 CY - Metz, France DA - 26.06.2022 KW - High entropy superalloy KW - Rrafting KW - Dislocation creep KW - Phase transformation PY - 2022 AN - OPUS4-63856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia T1 - Microstructural characterization of the AlMo 0.5 NbTa 0.5 ZrTi refractory complex concentrated alloy N2 - A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community and the AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. The AlMo0.5NbTa0.5TiZr rCCA was studied by SEM, EDX, EBSD and TEM, showing the presence of a nanoscopic basket-wave structure inside the grains, with two BCC phases. Additionally, thermodynamic calculations on the AlMo0.5NbTa0.5TiZr alloy were done with two different proprietary databases that anticipate two BCC-disordered phases with distinct constitutions as well as an HCP phase. T2 - Symposium on Advanced Mechanical and Microstructural Characterization of High-Entropy Alloys CY - Bochum, Germany DA - 03.02.2020 KW - High Entropy Alloy KW - EBSD KW - Microstructure Characterization PY - 2020 AN - OPUS4-50729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia T1 - Creep Properties of the Refractory Chemically Complex AlMo 0.5 NbTa 0.5 TiZr Alloy N2 - The development of refractory CCAs has been explored for potential use in high temperature applications. An example of this is the AlMo0.5NbTa0.5TiZr alloy, which resembles the well-known γ/γ’ microstructure in Ni-Base superalloys with cuboidal particles embedded in a continuous matrix. The aim of this work is to evaluate the alloy’s mechanical behavior under tension in the temperature range 800-1000°C, by applying creep tests under vacuum (excluding oxidation effects). Some little temperature influence on minimum creep rate @ 1000 and 1100 °C was found and at a first glance, and Norton plots shows that deformation is probably both diffusion and dislocation controlled. However, further work is needed to stablish deformation and degradation micro mechanisms in the studied creep regime. T2 - SPP Kick-Off Meeting 2nd Phase CY - Online meeting DA - 14.04.2021 KW - Creep behavior KW - Chemically complex alloy KW - Microstructure PY - 2021 AN - OPUS4-53389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia T1 - High temperature and low stress creep behavior of the refractory chemically complex alloy AlMo 0.5 NbTa 0.5 TiZr N2 - The refractory chemically complex alloy (rCCA) AlMo0.5NbTa0.5TiZr, with a density of 7.4 g/cm3, shows a compressive ultimate strength of 772 MPa at 1000 °C, comparatively surpassing Ni-base and other rCCAs. Its dual-phase microstructure, with a high volume fraction (≈ 62%) of cuboidal and plate-like particles coherently embedded in a continuous matrix, resembles the well-known pattern of the γ/γ" in Ni-base superalloys. Its developers have thus implied that it could stand as structural alloy for high temperature (HT) applications. Here, we report the HT creep properties and the underlying microstructural changes of the rCCA AlMo0.5NbTa0.5TiZr to propose deformation and degradation micromecanisms for this regime. The material was produced by arc-melting and subsequently heat treated in argon: at 1400 °C for 24 h plus a hot isostatic pressure treatment at 1370 °C and 170 MPa for 4 h, with a cooling rate of 10 K/min. Miniaturized tensile specimens (≈ 28 x 7 x 2 mm) were cut and polished to a quality of 1 μm. Creep tests were conducted in vacuum in the respective temperature and stress range 800-1200 °C and 30-120 MPa. For observation, thin slices were extracted from the gauge length, away from the fracture surface, grinded to a thickness of 100 μm, and electropolished to electron transparency. The microstructure was observed on the electropolished specimens using scanning (S) as well as transmission (T) electron microscopy (EM). The Norton plot gives Norton exponents of about 3.1 and 3.2 for temperatures of 1000 and 1100 °C, respectively. Curiously, creep rate minima are very close for a stress level of 30. The starting microstructure reflects a macroscopically lean coarse grain structure and a microscopically fine-meshed basketweave structure with coherency dislocations only around coarsened particles usually close to subgrain boundaries. Results are discussed on the base of variations of this starting microstructure after interrupted and ruptured creep tests. T2 - 15th International Conference on Creep and Fracture of Engineering Materials and Structures CY - Online meeting DA - 14.06.2021 KW - Creep behavior KW - Chemically complex alloy KW - Cow stress PY - 2021 AN - OPUS4-53388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia T1 - Effect of the heat treatment in the microstructure of a refractory chemically complex alloy N2 - A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community. The AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. After a two-stage heat treatment, this rCCA morphologically resembles the typical a two-phase microstructure of the latter. The objective of this work consists in determining the effect of the two stages of the heat treatment on the microstructure of the AlMo0.5NbTa0.5TiZr alloy to eventually improve it in terms of homogeneity and porosity. T2 - Third International Conference on High Entropy Materials (2020) CY - Berlin, Germany DA - 27.09.2020 KW - Annealing KW - Hot isostatic pressing KW - Refractory chemically complex alloy KW - Microstructure PY - 2020 AN - OPUS4-53386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suarez Ocano, Patricia T1 - Exploring the impact of heat treatment on room and high temperature strength of 316L stainless steel fabricated by PBF-LB N2 - Laser Powder Bed Fusion (PBF-LB/M) enables the fabrication of 316L stainless steel components with superior strength and intricate geometries. The alloy PBF-LB/M/316L features a fully austenitic microstructure with hierarchical characteristics— such as fine dislocation structures, segregated elements, low-angle grain boundaries, and nano-dispersed silicates—that enhance strength and ductility. Additionally, it includes metallurgical defects and residual stresses. Apart from process control, heat treatments (HTs) are used to tailor the microstructure for specific loading conditions. This study investigate the effects of post-processing HTs on the hierarchical microstructure and tensile properties of PBF-LB/M/316L at room and high temperature. The heat treatments, ranging from 400 °C to 900 °C for 1 to 4 hours, focus on sub-recrystallization temperatures to preserve the microstructural hierarchy. The HTs applied had minimal impact on the grain shape, size, or texture of PBF-LB/M/316L. However, significant modifications occurred in the solidification cellular substructure after HTs at 800 °C and 900 °C, when compared to a heat-treated condition at 450 °C. HTs at 800 °C notably decreased dislocation density and enlarged cellular structures, though they remained partially intact. After 1 hour at 900 °C, the cellular substructure dissipated, correlating with a further reduction in dislocation density. These microstructural changes resulted in a decreased yield strength and increased work hardening capacity at both room and high temperature, highlighting the critical link between HT parameters, microstructural evolution, and mechanical performance. T2 - The 20th International Conference on Strength of Materials (ICSMA 20) CY - Kyoto, Japan DA - 02.06.2025 KW - Additive manufacturing KW - 316L stainless steel KW - Heat treatments KW - Tensile properties KW - Microstructure PY - 2025 AN - OPUS4-63914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia T1 - Effect of heat treatment on the hierarchical microstructure and properties of 316L stainless steel produced by Laser Powder Bed Fusion (PBF-LB/M). N2 - Laser Powder Bed Fusion (PBF-LB/M) of AISI 316L stainless steel has gained popularity due to its exceptional capacity to produce complex geometries and hierarchical microstructures, which can increase the yield strength while maintaining good ductility. Nevertheless, owing to high thermal gradients encountered during the process, the as printed 316L stainless steel often exhibit microstructural heterogeneities and residual stresses, which can limit its performance in demanding environments. Hence, employing heat treatments which balance the reduction of residual stresses while retaining improved static strength may be beneficial in various scenarios and applications. This study investigates the impact of post-processing heat treatments on the microstructure of 316L stainless steel manufactured via PBF-LB/M, along with its correlation with micro-hardness properties. To this end, 6 different heat treatments, i.e., 450 °C for 4h, 700 °C for 1h, 700 °C for 3h, 800 °C for 1h, 800 °C for 3h, and 900 °C for 1h, were applied to different specimens and Vickers hardness measurements (HV1) were performed in all states. At 800 °C, although the cellular structure appears to be retained, there is an observable increase in cellular size. However, while treatments exceeding 900 °C indicate no significant grain growth compared to other conditions, the cellular structure is entirely dissolved, which leads to a reduced Vickers hardness. The effect of the heat treatments on other microstructural features such as grain size and morphology, melt pool boundaries (MPB), crystallographic texture, chemical segregation, dispersoids and phase stability are also discussed in the present work T2 - 4th Symposium on Materials and Additive Manufacturing CY - Berlin, Germany DA - 12.06.2024 KW - Additive manufacturing KW - Heat treatment KW - Microstructure PY - 2024 AN - OPUS4-60304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suarez Ocano, Patricia T1 - Influence of heat-treatment-induced microstructural evolution on the Low Cycle Fatigue behavior of 316L stainless steel fabricated by Laser Powder Bed Fusion N2 - Additive manufacturing, particularly the laser powder bed fusion (PBF-LB/M) process, has gained significant attention in recent years due to its ability to produce complex geometries with enhanced mechanical properties. Among the various materials used, 316L stainless steel is highly favored for cyclically loaded components due to its exceptional mechanical strength, high-temperature performance, and corrosion resistance, making it widely applicable across various industries. 316L SS fabricated by PBF-LB/M (PBF-LB/M/316L) exhibits a unique hierarchical microstructure, with high density of low-angle grain boundaries (LAGBs), nano-dispersed silicates, chemical micro-segregations, and solidification-induced cellular structures. Particularly, the submicron-sized cellular features enriched with chromium (Cr) and molybdenum (Mo), along with high dislocation densities, contribute to a superior strength-ductility balance compared to conventionally manufactured 316L SS. The dispersed silicate particles act also as a strengthening phase, impeding dislocation movement and enhancing plastic deformation resistance. This study explores the effect of heat treatments on the low-cycle fatigue (LCF) behavior of PBF-LB/M/316L at room temperature (RT) and 600 °C. First, three heat treatment conditions were applied to the as-built material: 450 °C for 4 hours (HT450/4), 800 °C for 3 hours (HT800/3), and 900 °C for 1 hour (HT900/1) to investigate their influence on microstructural evolution. Microstructural analysis revealed that the HT450/4 condition preserved the cellular structure with high dislocation density, while the HT800/3 condition showed partial dissolution of cells together with reduction in segregated elements along the cell walls and a reduced dislocation density. The HT900/1 condition resulted in complete segregation and cellular structure dissolution with comparable dislocation density to HT800/3 while maintaining the crystallographic texture and grain morphology. Intermetallic χ phase was mostly observed at the grain boundaries in HT800/3, but not in HT900/1. Fully reversed LCF tests were conducted under strain-controlled conditions with a strain amplitude of 0.8 %. Tests were interrupted at specific intervals to analyze the interaction between hierarchical microstructural features and deformation mechanisms in the three heat-treated conditions. Due to the pronounced dislocation cell structures and elemental segregation, the microstructure of the HT450/4 condition significantly impact deformation and damage mechanisms during cyclic loading, which in turn, differ from the conventional produced counterparts. The results provide insights into the relationship between microstructural features and fatigue performance, highlighting key deformation and failure mechanisms under cyclic loading. T2 - FEMS 2025 EUROMAT 18th European Congress and Exhibition on Advanced Materials and Processes CY - Granada, Spain DA - 14.09.2025 KW - Additive manufacturing KW - 316L stainless steel KW - Heat treatments KW - Low Cycle Fatigue KW - Microstructure PY - 2025 AN - OPUS4-64238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suarez Ocano, Patricia T1 - Effect of the powder composition on the microstructure and mechanical properties of 316L stainless steel fabricated by laser powder bed fusion N2 - Additive manufacturing (AM) has seen rapid growth in recent decades, with Laser Powder Bed Fusion (PBF-LB/M) emerging as the leading technique for producing high-density, geometrically complex metal parts. Austenitic stainless steel 316L is one of the most studied alloys for PBF-LB/M due to its excellent strength, ductility, and corrosion resistance [1]. The microstructure formed during PBF-LB/M processing can improve certain mechanical properties compared to conventionally manufactured 316L [2]. However, the current 316L standards allow broad ranges for key alloying elements, particularly Cr and Ni. While such variations have little effect on conventionally produced alloys, emerging evidence shows that they can markedly alter the microstructure and mechanical properties in PBF-LB/316L—even within specification limits [3]. This study investigates through microstructural and thermodynamical assessment, how two powders of nominally standard 316L composition (Alloys A and B) respond to identical PBF-LB/M processing parameters. Despite identical printing conditions, Alloy A exhibited twice the grain size and five times higher low-angle grain boundary (LAGB) density compared to Alloy B . Conversely, Alloy B showed a significantly higher density of Σ3 twin boundaries, nearly absent in Alloy A. These microstructural differences are attributed primarily to variations in Cr and Ni content in the liquid, which may influence icosahedral short-range ordering (ISRO) mechanism [4]. ISRO potentially facilitates twin boundary formation, ultimately refining grain structure [5]. This work highlights the critical impact of compositional control on final part microstructures and consequent mechanical properties and emphasizes the need to reassess compositional tolerances for AM-specific applications. T2 - 5th Symposium on Materials and Additive Manufacturing (Additive 2026) CY - Kassel, Germany DA - 24.03.2026 KW - Additive manufacturing KW - 316L stainless steel KW - Chemical composition KW - Lcosahedral short-range ordering mechanism KW - Grain size PY - 2026 AN - OPUS4-65738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -