Scientific Events

Location: Max-Planck-Institut für Eisenforschung GmbH
Due to its high diffusivity hydrogen atoms alloy with metals even at room temperature. At this temperature, the materials microstructure remains rather stable. When the system size is reduced to the nano-scale, microstructural defects as well as mechanical stress significantly affect the thermodynamics and kinetics properties of the system.[1-6] Effects will be demonstrated on Niobium-H and Palladium-H thin films.Hydrogen absorption in metal systems commonly leads to lattice expansion. The lateral expansion is hindered when the metal adheres to a rigid substrate, as for thin films. Consequently, high mechanical stresses arise upon hydrogen uptake. In theory, these stresses can reach about -10 GPa for 1 H/M. Usually, metals cannot yield such high stresses and deform plastically. Thereby, maximum compressive mechanical stress of -2 to -3 GPa is commonly measured for 100 nm Nb thin films adhered to Sapphire substrates. It will be shown that phase transformations change in the coherency state upon film thickness reduction. The coherency state affects the nucleation and growth behaviour of the hydride phase as well as the kinetics of the phase transformation.[1] It will be further demonstrated that plastic deformation can be hindered and even suppressed upon film thickness reduction. In this case the system behaves purely elastic and ultra-high stress of about -10 GPa can be experimentally reached.[2] These high mechanical stresses result in changes of the materials thermodynamics. In the case of Nb-H thin films of less than 8 nm thickness, the common phase transformation from the α-phase solid solution to the hydride phase is completely suppressed, at 300 K.[3,4,5] The experimental results go in line with the σDOS model that includes microstructural and mechanical stress effects on the chemical potential [6]. [1] V. Burlaka, K. Nörthemann, A. Pundt, „Nb-H Thin Films: On Phase Transformation Kinetics“, Def. Diff. Forum 371 (2017) 160. [2] M. Hamm, V. Burlaka, S. Wagner, A. Pundt, “Achieving reversibility of ultra-high mechanical stress by hydrogen loading of thin films”, Appl. Phys. Letters 106 (2015) 243108. [3] S. Wagner, A. Pundt, “Quasi-thermodynamic model on hydride formation in palladium-hydrogen thin films: Impact of elastic and microstructural constraints “, Int. J. Hydrog. Energy 41 (2016) 2727. [4] V. Burlaka, S. Wagner, M. Hamm, A. Pundt, “Suppression of phase transformation in Nb-H thin films below switchover-thickness”, Nano Letters 16 (2016) 6207. [5] S. Wagner, P. Klose, V. Burlaka, K: Nörthemann, M. Hamm, A. Pundt, Structural Phase Transitions in Niobium Hydrogen Thin Films: Mechanical Stress, Phase Equilibria and Critical Temperatures, Chem. Phys. Chem. 20 (2019) 1890–1904. [6] S. Wagner, A. Pundt, Hydrogen as a probe for defects in materials: Isotherms and related microstructures of palladium-hydrogen thin films, AIMS Materials Science 7 (2020), 399–419. [more]

New in-situ and operando techniques for correlative microscopy and chemical imaging : Case studies in mapping hydrogen and other low-Z elements in energy materials

Development of innovative characterization tools is of paramount importance to advance the frontiers of science and technology in nearly all areas of research. In order to overcome the limitations of individual techniques, correlative microscopy has been recognized as a powerful approach to obtain complementary information about the investigated materials. High-resolution imaging techniques such as Transmission Electron Microscopy (TEM) or Helium Ion Microscopy (HIM) offer excellent spatial resolution. However, the analytical techniques associated with TEM such as Energy Dispersive X-ray spectroscopy (EDX) or Electron Energy-Loss Spectroscopy (EELS) are inadequate for the analysis of (i) isotopes, (ii) trace concentrations (< 0.1 at. % or < 1000 ppm) and (iii) light elements (H, Li, B). Secondary Ion Mass Spectrometry (SIMS), on the other hand, has several advantages such as the possibility to analyse elements and isotopes of all elements of the periodic table while also providing high-sensitivity to detect even trace concentrations. However, the main drawbacks of SIMS are (i) difficulty in quantification and (ii) lateral resolution of SIMS imaging is fundamentally limited by ion-solid interaction volume to ~10 nm. Owing to the complementary strengths of SIMS imaging, we developed new in-situ and operando instrumentations for correlative microscopy combining electron microscopy and SIMS imaging. In this presentation, we will discuss the instrumentation development aspects of correlative microscopy techniques based on SIMS imaging. With a range of examples from energy materials, we will show the powerful correlative microscopy possibilities that emerge due to these new in-situ and operando methods and compare with ex-situ correlation. Our recent work in the application of these methods in hydrogen containing materials and Li ion batteries will be reviewed. [more]

Mesoscale simulation of grain boundaries

The mechanical behavior of most metals in engineering applications is dominated by the grain size. Physics-based models of the interaction between dislocations and the grain boundary are important to correctly predict the plastic deformation behavior of polycrystalline materials. Dislocation-grain boundary interaction is complex and a challenge to model. In this talk, I will present a short history, opportunities, and challenges for modeling grain boundaries at the mesoscale using discrete dislocation dynamics. This includes an effective model and a novel model for physical transmission of dislocations through grain boundaries with a residual grain boundary dislocation. In addition, I will provide an outlook how these models can and should be calibrated using micromechanical experiments on bicrystals. [more]
Our aim is to understand processes that lead to the emergence of catalytic function though direct observation using a combination of operando scanning and transmission electron microscopy. Starting with simple model catalysts, such as polycrystalline metal foils, we observe the propagation of chemical waves and reveal how catalytic activity depends on grain orientation, coupling mechanisms and reaction conditions. In the case of redox-reactions on non-noble metals, we find that the active catalyst is operating near a phase-boundary where metallic and oxidized phases co-exist. Real-time imaging reveals fascinating oscillatory redox dynamics that increase in complexity with increasing chemical potential of the gas-phase. When moving from simple model catalysts to industrially relevant metal nanoparticles supported on reducible oxide carriers, we apply in-situ transmission electron microscopy to study effects related to a strong metal-support interaction (SMSI) under reactive conditions. Using the archetypical titania supported platinum nanoparticles as a reference system, and hydrogen oxidation as model redox reaction, it will be shown that the well-described encapsulated state of platinum particles is lost as soon as the system is exposed to a redox-active environment. Structural incoherence at the platinum-titania interface lowers the barrier for redox processes, which give rise to dynamic reconstructions and particle migration. The particle orientation on the support determines the structure of the interface and the resulting particle dynamics, migration, and sintering behaviour. The aim of the presentation is to demonstrate that active catalysts are dynamically adapting to the reaction environment and that catalytic function is related to the catalysts ability to participate in the reaction through reversible changes in its structure and/or (local) composition. [more]
Many of the functional materials we hope to leverage for next-generation technological applications — such as computing, energy harvesting and storage, or communication devices — draw their unique and sometimes exotic properties from a suite of interactions between the atoms, spins, and charges in a crystalline lattice. With direct, real-space access to these order parameters down to the atomic scale, the scanning transmission electron microscope (STEM) is a powerful tool to probe the fundamental framework of such compounds and their properties. As an example of this, I will show how advanced STEM techniques can elucidate key questions about the landscape of superconductivity in recently discovered nickelates. But many of these functional systems are most useful (and therefore interesting) away from the ambient conditions of most typical high-resolution STEM experiments, for instance at cryogenic or elevated temperatures or under an external bias. It is therefore imperative to expand the environmental compatibility of these methods through the parallel development of both hardware and data processing tools, key examples of which will be highlighted here. [more]

Atomistic Dynamics of Deformation, Fracture and GB Migration in Oxides

In order to clarify the deformation and fracture mechanism in oxides such as Al2O3 and STO, TEM in situ nanoindentation experiments were conducted for their single crystals and bicrystals. We successfully observed the dynamic behavior of twin formation, twin-GB interaction, pile-up dislocation, jog and kink formation and jog drag dynamics and so on. The mechanism of each dynamic behavior will be discussed in detail in this presentation. GB migration plays an important role in considering the high temperature mechanical properties. Recently, we have found that GB migration behavior in Al2O3 can be precisely controlled by the aid of the high-energy electron beam irradiation. This technique was applied to directly visualize the atomistic GB migration. It was revealed that the GB migration is processed by a cooperative shuffling of atoms in GB ledges along specific routes. References [1] S. Kondo, T. Mitsuma, N. Shibata, Y. Ikuhara, Sci. Adv., 2[11], e1501926(2016). [2] S. Kondo, A. Ishihara, E. Tochigi, N. Shibata, and Y. Ikuhara, Nat. Commun., 10, 2112 (2019). [3] J.Wei, B.Feng, R.Ishikawa, T.Yokoi, K.Matsunaga, N.Shibata and Y.Ikuhara, Nat. Mater.,20 (7), 951 [4] J.Wei, B.Feng, E.Tochigi, N.Shibata and Y.Ikuhara, Nat. Commun., 13(1), 1455, (2022) [more]

Local Phase Transformations: A New Creep Strengthening Mechanism in Ni-Base Superalloys

Polycrystalline Ni-based superalloys are vital materials for disks in the hot section of aerospace and land-based turbine engines due to their exceptional microstructural stability and strength at high temperatures. In order to increase operating temperatures and hold times in these engines, hence increasing engine efficiency and reduction of carbon emissions, creep properties of these alloys becomes increasingly important. Microtwinning and stacking fault shearing through the strengthening g’ precipitates are important operative mechanisms in the critical 600-800°C temperature range. Atomic-scale chemical and structural analyses indicate that local phase transformations (LPT) occur commonly during creep of superalloys. Furthermore, the important deformation modes can be modulated by LPT formation, enabling a new path for improving high temperature properties. [more]
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