TY - CONF A1 - Stawski, Tomasz A1 - Van Driessche, A. T1 - Particle-mediated origins of mesocrystalline disorder in calcium sulfate single crystals N2 - Calcium sulfate minerals are abundant in natural and engineered environments and they exist in the form of three hydrates: gypsum (CaSO4·2H2O), bassanite (CaSO4·0.5H2O), and anhydrite (CaSO4). Due to their relevance in natural and industrial processes, the formation pathways of these calcium sulfate phases from aqueous solution have been the subject of intensive research1. The state-of-the-art of the calcium sulfate formation mechanisms builds upon and goes beyond what we have come to appreciate in the astounding intricacy of other mineral formation processes from ions in aqueous solutions. The original, and rather naive, 'textbook' image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species2. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. In this context, a number of studies have already revealed that nucleation in the CaSO4-H2O system is non-classical, where the formation of the different crystalline phases involves several steps including a common amorphous precursor1, 3, 4. In this contribution we show that the formation of the amorphous phase involves the aggregation of small primary particles into larger disordered aggregates exhibiting a "brick-in-the-wall" structure5, 6. The actual crystallization occurs by the restructuring and coalescence of the particles ("bricks") into a given calcium sulfate phase depending on the physicochemical conditions of the solution. Importantly, the rearrangement process does not continue until a (nearly-)perfect homogeneous single crystal is obtained. Instead it comes to a stop, or at least significantly slows down. Such a process thus yields a final imperfect mesocrystal, composed of smaller domains rather than a continuous crystal structure, within which the domains are separated by an amorphous (i.e. less ordered) calcium sulfate phase. Hence, the non-classical crystallization process of CaSO4 yields a final imperfect mesocrystal with an overall morphology resembling that of a single crystal, yet composed of smaller nano-domains. Importantly, these observations reveal that organic-free calcium sulfate mesocrystals grown by a particle mediated-pathway preserve in the final crystal structure a “memory” or “imprint” of their non-classical nucleation process, something that has been overlooked until now. Furthermore, the nano-scale misalignment of the structural sub-units within these crystals can propagate through the length-scales, and be expressed macroscopically as misaligned zones/domains in large single crystals. Indeed, by considering large anhydrite crystals from the famous Naica Mine (“Cueva de los cristales”) we observed a suite of correlated self-similar void defects spanning multiple length-scales7. These flaws, in the macroscopic crystal, stem from “seeds of imperfection” originating from a particle-mediated nucleation pathway. Hence, building a crystal could be viewed as Nature stacking blocks in a game of Tetris, whilst slowly forgetting the games core concept and failing to fill rows completely. T2 - ECCG: European Conference on Crystal Growth 7 CY - Paris, France DA - 25.07.2022 KW - Anhydrite KW - SAXS KW - Single crystal KW - Mesocrystal PY - 2022 AN - OPUS4-56276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Nolze, Gert T1 - Investigation of the competitive grain growth during solidification of single crystals of nickel-based superalloys N2 - The competitive growth of columnar grains in a single-grain selector, which is used for directional solidification of single-crystal blades from nickel-based superalloys, has been investigated by electron backscattered diffraction and local X-ray diffraction analysis. It has been found that the competitive grain growth in a starter block is determined by the crystallographic factor: rapidly growing grains with the axial orientation close to the [001] direction dominate in this part of the casting. For the competitive grain growth in a helicoidal separator, the geometric factor (the position of a grain at the input of the separator) is also important. The results obtained suggest that an appropriate geometry of the single-grain selector was chosen. In addition, the distribution of the orientations of columnar grains obtained by electron backscattered diffraction, can be used for approximate estimation of the yield of suitable (i.e., with the deviation of the axial orientation from the [001] direction within a specified tolerance) single-crystal blades. KW - Electron backscatter diffraction KW - Single crystal KW - Growth competition KW - Nickel alloy PY - 2006 U6 - https://doi.org/10.1134/S1063774506040298 SN - 1063-7745 SN - 1562-689X VL - 51 IS - 4 SP - 710 EP - 714 AN - OPUS4-38028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Bhattacharya, Biswajit A1 - Akhmetova, Irinia A1 - Emmerling, Franziska T1 - Mechanochemical and solution syntheses of two novel cocrystals of orcinol with two N,N0-Dipyridines: Structural diversity with varying ligand flexibility N2 - We studied the influence of coformers flexibility on the supramolecular assembly of 5-substituted resorcinol. Two cocrystals of orcinol (ORL) with two dipyridine molecules, i.e. 1,2-di(4-pyridyl)ethane (ORLeBPE) and 1,2-di(4-pyridyl)ethylene (ORLeBPY), were prepared by mechanochemical synthesis and slow evaporation of solvent. The new crystalline solids were thoroughly characterized by single crystal Xray diffraction (SCXRD), powder X-ray diffraction analysis (PXRD), Fourier-transform infrared spectroscopy (FT-IR), differential thermal analysis (DTA), and thermogravimetric analysis (TGA). Structural determination reveals that in both cocrystals, the phenolepyridine, i.e. OeH/N(py) heterosynthon takes the main role in the formation of cocrystals. In ORLeBPE, the components form infinite 1D zig-zag chains, which are extended to 2D layer structure by inter-chain CeH/O interactions between BPE hydrogen atoms and hydroxyl oxygen atoms of ORL. In ORLeBPY, the components form a 0D fourcomponent complex. Formation of the discrete assemblies is attributed to the comparative rigid nature of BPY, which restricts the formation of an extended network. KW - Cocrystal KW - Single crystal KW - X-ray diffraction KW - Mechanochemistry PY - 2020 U6 - https://doi.org/10.1016/j.molstruc.2020.128303 SN - 0022-2860 VL - 1217 SP - 128303 PB - Elsevier B.V. AN - OPUS4-51023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fedelich, Bernard A1 - Kindrachuk, Vitaliy A1 - Becker, M. T1 - Simulation of non-isothermal mechanical tests on a single crystal nickel-basis superalloy N2 - Gas turbines are widely used for a variety of purposes including power generation, compression or as jet engines in aircrafts. The critical components of a gas turbine are the high-pressure turbine blades which operate under severe conditions. These include thermo-mechanical loadings over temperatures ranging from room temperature up to 1100°C. While a large number of constitutive models for single crystals have been proposed, most applications are restricted to special loading scenarios, temperature range and deformation mechanisms. In particular, a number of models are focused on pure creep. Only a few papers consider application of both creep and fatigue. Applications of the constitutive models to long-term stress relaxation are even scarcer. The new model assumes deformation-induced softening and can properly reproduce the viscous behavior at different time scales. The model has been calibrated with the uniaxial tests at 800°C and 950°C in [001], [011] and [111] specimens of a nickel-basis superalloy. The predicted creep, short- and long-term relaxation and cyclic tests are in reasonable agreement with the experimental observations. T2 - Eigth International Conference on Low Cycle Fatigue CY - Dresden, Germany DA - 27.06.2017 KW - Constitutive law KW - Superalloy KW - Single crystal KW - Creep KW - Low cycle fatigue PY - 2017 AN - OPUS4-40923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kindrachuk, Vitaliy A1 - Fedelich, Bernard A1 - Becker, M. ED - Beck, T. ED - Charkaluk, E. T1 - Constitutive modelling of viscoplastic deformation in single crystal nickel-basis superalloys subjected to cyclic and creep loadings at high-temperatures N2 - Gas turbines are widely used for a variety of purposes including power generation, compression or as jet engines in aircrafts. The critical components of a gas turbine are the high-pressure turbine blades which operate under severe conditions. These include thermo-mechanical loadings over temperatures ranging from room temperature up to 1100°C. While a large number of constitutive models for single crystals have been proposed, most applications are restricted to special loading scenarios, temperature range and deformation mechanisms. In particular, a number of models are focused on pure creep. Only a few papers consider application of both creep and fatigue. Applications of the constitutive models to long-term stress relaxation are even scarcer. The new model assumes deformation-induced softening and can properly reproduce the viscous behavior at different time scales. The model has been calibrated with the uniaxial tests at 800°C and 950°C in [001], [011] and [111] specimens of a nickel-basis superalloy. The predicted creep, short- and long-term relaxation and cyclic tests are in reasonable agreement with the experimental observations. T2 - Eighth International Conference on Low Cycle Fatigue (LCF8) CY - Dresden, Germany DA - 27.06.2017 KW - Constitutive law KW - Single crystal KW - Superalloy KW - Creep KW - Low cycle fatigue PY - 2017 SP - 371 EP - 376 PB - DVM e.V. CY - Berlin AN - OPUS4-40928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Epishin, A. A1 - Fedelich, Bernard A1 - Link, T. A1 - Nolze, Gert A1 - Feldmann, Titus A1 - Viguier, B. A1 - Poquillon, D. A1 - Le Bouar, Y. A1 - Ruffini, A. A1 - Finel, A. T1 - Creep of the single-crystal nickel-base superalloy CMSX-4 at a super-solvus temperature N2 - Data about the creep of metals and their alloys at temperatures close to the melting point are very limited. The reason is that most engineering alloys are used at temperatures below 0.6-0.8 of their melting point, so, investigation of creep at higher temperatures has usually no practical relevance. For some special applications however it is important, in our case hot isostatic pressing (HIP) of single-crystal turbine blades cast from nickel-base superalloys. In order to remove porosity the blades are HIPed at temperatures above GammaP-solvus where superalloy has no strengthening GammaP-phase and therefore is very soft. E.g., the company Howmet Castings hips the superalloy CMSX-4 at 1288°C, which corresponds to a homologous temperature of about 0.97=1561 K/1612 K (solidus temperature). Knowledge about the creep of CMSX-4 at this temperature and understanding of the creep mechanisms are necessary to model the kinetics of pore closure during HIP. CMSX-4 single-crystals of [001] orientation and few single-crystals of different orientations, [011], [123] and [111], were tested under creep conditions at 1288°C in the stress range between 4 and 16 MPa. At this temperature which is above the GammaP-solvus (for CMSX-4 1280°C) the superalloy has single phase structure representing the Gamma-solid solution of nickel strengthened by solute atoms. On creep curves of CMSX-4 single-crystals of different orientations measured at 1288°C/10 MPa it is seen that despite such a high homological temperature, 0.97, CMSX-4 shows very high anisotropy of creep rate. The average creep rate of [001] single-crystal in the range 0-30% strain is about 11.5 time faster than that for [111], a ratio, which is even higher than at the practically relevant temperatures 750-1100°, see e.g.. Approximation the strain rate – stress dependence by the Norton power law gave a stress exponent n of about 6 which is an indication of dislocation creep. The specimen shape after testing, analysis of traces of plastic deformation by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) investigations indicate on dislocation slip on the octahedral system <011>{11-1}.This result however does not support the current doctrine that at high temperatures creep of metals and alloys are climb controlled. It is concluded from the obtained results that even at such a high homologous temperature, 0.97, dislocation movement by slip is more preferable than by climb if only relatively week obstacles are present like solute atoms and low angle boundaries (LABs). It is remarkable that under used testing conditions the necking and recrystallization behavior of differently oriented single-crystals is very different. E.g., the [001] single-crystal showed very large local strain during necking, Phi=99.8%, and no recrystallization (see Fig. 3a), while the [111] single-crystal small necking, Phi=62%, accompanied by recrystallization. Such a specific deformation and recrystallization has to be undestood. The obtained creep data of CMSX-4 was introduced in a finite element model in order to simulate pore closure during commercial HIP at a temperature of 1288°C. T2 - International Conference on Creep and Fracture of Engineering Materials and Structures CY - Saint Petersburg, Russia DA - 19.06.2017 KW - Creep KW - Superalloy KW - CMSX4 KW - Hot isostatic pressing (HIP) KW - Single crystal PY - 2017 AN - OPUS4-40903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Treninkov, I. A. A1 - Petrushin, N. V. A1 - Epishin, A. I. A1 - Svetlov, I. L. A1 - Nolze, Gert A1 - Elyutin, E. S. T1 - Experimental Determination of Temperature Dependence of Structural–Phase Parameters of Nickel-Based Superalloy N2 - The temperature dependences of the periods of the crystal lattices of the γ and γ' phases, their dimensional mismatch (misfit), and volume fraction of the γ' phase of an experimental single-crystal hightemperature nickel-based alloy have been determined by X-ray diffraction analysis in the temperature range of 18–1150°C. The temperature ranges in which intense changes in the structural and phase characteristics of the alloy under study take place have been determined. KW - X-ray diffraction analysis KW - High temperatures KW - Nickel-based superalloys KW - Single crystal KW - Crystal lattice period PY - 2022 U6 - https://doi.org/10.1134/s2075113322010373 SN - 2075-1133 VL - 13 IS - 1 SP - 171 EP - 178 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-54466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gadelmeier, C. A1 - Haas, S. A1 - Lienig, T. A1 - Manzoni, Anna Maria A1 - Feuerbacher, M. A1 - Glatzel, U. T1 - Temperature Dependent Solid Solution Strengthening in the High Entropy Alloy CrMnFeCoNi in Single Crystalline State N2 - The main difference between high entropy alloys and conventional alloys is the solid solution strengthening effect, which shifts from a single element to a multi-element matrix. Little is known about the effectiveness of this effect at high temperatures. Face-centered cubic, equiatomic, and single crystalline high entropy alloy CrMnFeCoNi was pre-alloyed by arc-melting and cast as a single Crystal using the Bridgman process. Mechanical characterization by creep testing were performed at temperatures of 700, 980, 1100, and 1200°C at different loads under vacuum and compared to single-crystalline pure nickel. The results allow a direct assessment of the influence of the chemical composition without any disturbance by grain boundary sliding or diffusion. The results indicate different behaviors of single crystalline pure nickel and CrMnFeCoNi. At 700°C CrMnFeCoNi is more creep-resistant than Ni, but at 980°C both alloys show a nearly similar creep strength. Above 980°C the creep behavior is identical and the solid solution strengthening effect of the CrMnFeCoNi alloy disappears. KW - High entropy alloys KW - Single crystal PY - 2020 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-514572 VL - 10 IS - 11 SP - 1412 PB - MDPI AN - OPUS4-51457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Petrushin, N. V. A1 - Epishin, A. I. A1 - Svetlov, I. L. A1 - Nolze, Gert A1 - Elyutin, E. S. A1 - Solov'ev, A. E. T1 - Influence of the Sign of the γ/γ' Misfit on the Structure and Creep Strength of Single Crystals of Nickel-Based Superalloys N2 - Using the method of directional solidification, single crystals of experimental nickel-based superalloys with negative, zero, and positive γ/γ' misfits are obtained. The γ' solvus, solidus, and liquidus temperatures of the alloys are determined, and the microstructures of the alloys after directional solidification, heat treatment, and creep tests are investigated. Creep tests are performed at temperatures of 800 and 1000°C. It is found that single crystals of the alloy with a negative γ/γ' misfit have the highest creep resistance and lifetime (the crystal lattice period of the γ' phase is smaller than that of the γ matrix). KW - Nickel-based superalloys KW - Single crystal KW - Creep KW - Creep strength KW - Microstructure, γ/γ' misfit PY - 2023 U6 - https://doi.org/10.1134/s207511332301029x SN - 2075-1133 VL - 14 IS - 1 SP - 13 EP - 22 AN - OPUS4-59505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -