5 Werkstofftechnik
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High-temperature corrosion is a widespread problem in various industries.
As soon as a hot and reactive gas (CO2, O2, H2O, SO2, NOx, etc.) is in contact with a solid, physico-chemical processes at the surface and interfaces lead to material degradation. The processes are dynamic and controlled by thermodynamic and kinetic boundary conditions. Whether a reaction product is protective or not depends on various factors, such as chemical composition of the solid and the reactive media, surface treatment as well as diffusion and transport paths of cations and anions. Resulting chemical and structural inhomogeneities with the corrosion layers are characterized by off stoichiometry within cationic and anionic sub lattices. The competitive processes can be studied by various techniques of applied crystallography.
This chapter gives an overview on the challenges of chemical-structural Analysis of reaction products by crystallographic methods such as X-ray diffraction and X-ray near-edge structure spectroscopy and scanning electron microscopy electron backscatter diffraction (SEM-EBSD) for corrosion science.
A variety of materials of technological interest change their properties through contact with reactive media. Solid-gas reactions lead to a variety of reaction products on the surfaces and internal interfaces. The observation of nucleation and growth processes in the environment where they occur (in situ) from a chemical-structural perspective is especially challenging for aggressive atmospheres. The talk presents innovative approaches to study corrosion mechanisms using advanced X-ray methods. Using energy dispersive X-ray diffraction and X-ray absorption spectroscopy in different tailor made environmental reaction chambers, valuable insights into high temperature oxidation and sulfidation processes were gained. Fe-based alloys were exposed to hot and reactive atmospheres containing gases like SO2, H2O and O2 at 650°C. During the gas exposure the tailor made reaction chambers were connected to a high energy diffraction end station at the synchrotron. The crystallization and growth of oxide and sulfide reaction products at the alloy surfaces were monitored by collecting full diffraction pattern every minute. Careful examination of shape and intensity of phase-specific reflections enabled to a detailed view on growth kinetics. These studies showed, oxides are the first phases occurring immediately after experimental start. As soon as reactive gas media enter the chamber, the conditions change and different reaction products, such as sulfides start to grow. A comparison of different gas environments applied, illustrated the differences in the type of reaction products. The in situ observation of high temperature material degradation by corrosion made it possible to study the contribution of phases, which are not stable at room temperature. For instance, wuestite (Fe1-xO), was frequently observed at high temperatures in humid gases on Fe with 2 wt.% and 9 wt.% chromium, but not at room temperature. The strength of the occurrence of this phase additionally explains why, despite a higher Cr content, ferritic alloys with 9 wt.% Cr in a challenging atmosphere prevent the intrinsic formation of protective layers. The in situ observations were supplemented by careful considerations of thermodynamic boundary conditions and detailed post characterization by classical metallographic analysis. Additionally, the structure and chemistry of the dominant oxide layers were evaluated using X-ray absorption near edge structure spectroscopy. The talk will give an overview about chances and challenges for studying high temperature corrosion phenomena by advanced X-ray methods.
Ferritic-austenitic chromia-forming alloys are frequently used as boiler tubes and heat exchanger materials for fossil-,biomass, and co-fired power plants. In all applied environments several strongly corrosive gaseous species such as CO2, SO2, SO3, H2O, O2 exist, causing materials degradation by high-temperature corrosion. The elucidation of degradation mechanisms introduced by multiple gases is challenging due to the presence of different oxidizing agents contributing to the competing reactions for oxidation, sulfurization or carburization. The degradation processes can be divided into initial stages, a transitional stage and the further proceeding steady-state oxidation reaction. Especially the long-term steady-state oxidation and further materials’ life-time are strongly dependent on the initial stages. The adsorption and absorption of the reactive species at the alloy surface and the growing oxide in the initial reaction is further influenced by dissociation and re-reactions of the gas phase molecules. To understand these mechanisms from a fundamental point of view in more detail, dedicated experiments and advanced characterization techniques on various length scale need to be applied. Real-time approaches using highly energetic synchrotron X-ray diffraction showed a high potential to enlighten competitively mechanisms by following the corrosion reactions in-situ in the environment they occur. Despite various other thin film characterization techniques, time of flight secondary ion mass spectroscopy (ToF-SIMS) is a powerful tool to visualize light atoms or labeled isotopes enabling the Differentiation between different oxidizing species. It was especially shown to be applicable in challenging atmospheres containing KCl deposits or in CO/CO2/O2 environments. The present study analyses the competing oxidation/sulfidation process in a humid atmosphere on two ferritic alloys with 2 and 9 % in weight chromium by in situ energy dispersive X-ray diffraction (EDXRD) and comparative tube furnace exposure using S16O2 and H2 18O atmosphere.
Latente Wärmspeicher auf der Basis von NaCl-KCl-MgCl2 Mischungen stellen eine kostengünstige Option für die Energiespeicherung von Prozesswärme dar. Der Beitrag gibt einen Überblick über die materialwissenschaftlichen Herausforderungen im System Salz-Legierung, welche gelöst werden müssen, um diese Speichertechnologie industriell zu etablieren.
Additive manufacturing (AM) processes allow a high level of freedom in designing and producing components for complex structures. They offer the possibility of a significant reduction of the process chain. However, the large number of process parameters influence the structure and the behavior of AM parts. A thorough understanding of the interdependent mechanisms is necessary for the reliable design and production of safe AM parts.
In this presentation we discuss the online monitoring of metallic AM parts produced by the Laser Powder Bed Fusion (LPBF) process by using optical, thermographic and electromagnetic methods. In a first approach we present the detection of defects generated during the process and discuss how to improve these methods for the optimization of design and production of metallic AM parts.