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Eingeladener Vortrag
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Controlled oriented crystallization of glass surfaces is desired for high precision applications, since the uppermost crystal layer significantly influences the properties of the material. In contrast to previous studies, the data presented here deal with separated crystals growing at defect-free surfaces in four atmospheres with different degrees of humidity (ambient/dry air, argon and vacuum). A glass with the composition 2 BaO–TiO2–2.75 SiO2 was heat-treated at 825 °C until fresnoite (Ba2TiSi2O8) grew to a significant size. The crystal growth rate is found to increase with increasing humidity. The morphology of the crystals changes from highly distorted dendrites in the driest atmosphere (vacuum) to circular/spear-head-shaped crystals in the wettest atmosphere (ambient air), which we attribute to a decrease in viscosity of the glass surface due to water uptake. The least distorted crystals appear in the form of depressions of up to 6 µm. This has an influence on the observed crystal orientation, as measured by electron backscatter diffraction (EBSD). The pulled-in crystals change the orientation during growth relative to the flat glass surface due to an enrichment in SiO2 at the crystal fronts. This confirms that the orientation of crystals is not fixed following nucleation.
Quantitative Microstructural Analysis - VAMAS TWA 37 & Liaison with ISO/TC 202 Microbeam Analysis
(2023)
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the identification and launching corresponding VAMAS projects. The ongoing project "FIB sample processing for TEM" is presented in detail.
To visualize the varying tetragonal distortions in high carbon martensitic steels by EBSD, two different approaches have been applied on backscattered Kikuchi diffraction (BKD) patterns. A band-edge refinement technique called Refined Accuracy (RA) (Oxford Instruments) is compared with a technique called Pattern Matching (PM), which optimizes the fit to a simulated BKD signal. RA distinguishes between hypothetical phases of different fixed 𝑐∕𝑎, while PM determines a best fitting continuous 𝑐∕𝑎 by projective transformation of a master pattern. Both techniques require stored BKD patterns.
The sensitivity of the 𝑐∕𝑎-determination was tested by investigating the microstructure of a ferritic steel with an expected 𝑐∕𝑎 = 1. The influence of the Kikuchi pattern noise on 𝑐∕𝑎 was compared for a single or 40 averaged frames per measuring point, and turned out to be not significant. The application of RA and PM on the martensitic microstructure delivered qualitatively similar maps of 𝑐∕𝑎. The comparison of RA and PM shows that RA is suitably fast and precise during mapping the martensite 𝑐∕𝑎 ratio in analyses of high carbon martensite, especially for fast initial surveys. As RA leads quantitatively to higher noise in 𝑐∕𝑎, the PM analysis can be used for higher precision results.
(Pre)Standardisation and Metrology in Microbeam Analysis – Ongoing Activities and Opportunities
(2023)
The presentation addresses the current ongoing projects as well as the gaps and opportunities in microbeam analysis within ISO/TC 202 Microbeam Analysis standardisation body and in-liaison Technical Working Areas (TWAs) at the pre-standardization platform of VAMAS (Versailles Project on Advanced Materials and Standards).
The progress in the activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects/inter-laboratory comparisons. The recently started project FIB sample processing for TEM is presented. Next projects in the pipeline involving EBSD and TKD are shortly announced. The need of more promotion for the engagement of more experts from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed.
A paradigm shift in the description of creep in metals can only occur through multi-scale imaging
(2022)
The description of creep in metals has reached a high level of complexity; fine details are revealed by all sorts of characterization techniques and different theoretical models. However, to date virtually no fully microstructure-driven quantitative description of the phenomenon is available. This has brought to interesting inconsistencies; the classic description of (secondary) creep rests on the so-called power law, which however: a- has a pre-factor spanning over 10 orders of magnitude; b- has different reported exponents for the same material; c- has no explanation for the values of such exponents.
Recently, a novel description (the so-called Solid State Transformation Creep (SSTC) Model) has been proposed to tackle the problem under a different light. The model has two remarkable features: 1- it describes creep as the accumulation of elementary strains due to dislocation motion; 2- it predicates that creep is proceeding by the evolution of a fractal arrangement of dislocations. Such description, however, needs a great deal of corroborating evidence, and indeed, is still incomplete.
To date, we have been able to observe and somehow quantify the fractal arrangement of microstructures through Transmission Electron Microscopy (TEM), observe the accumulation of dislocations at grain boundaries by EBSD-KAM (Electron Back-Scattered Diffraction-Kernel Angular Misorientation) analysis, quantify the kinetic character (solid state transformation) of experimental creep curves, and estimate the sub-grain size of the fractal microstructure through X-ray refraction techniques. All pieces of the mosaic seem to yield a consistent picture: we seem being on the right path to reconstruct the whole elephant by probing single parts of it. What is still missing is the bond between the various scales of investigation.
Quantitative Microstructural Analysis - VAMAS TWA 37 & Liaison with ISO/TC 202 Microbeam Analysis
(2022)
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. The recently started project FIB sample processing for TEM is highlighted. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. Further, a short overview of the VAMAS areas of activities is given where Germany is involved. Planed regional VAMAS Workshops in Germany in 2023 are announced.
Tempered martensite-ferritic steels, such as the grade P92 steel studied in this contribution, exhibit pronounced macroscopic cyclic softening under isothermal low-cycle fatigue (LCF) and non-isothermal thermomechanical fatigue (TMF) conditions, which is considered to be the predominant degradation mechanism in high-temperature fatigue in this and other material groups. However, such softening processes are highly complex since microscopic (e.g., recovery) and macroscopic (e.g., crack initiation and growth), as well as global and local effects superimpose, especially under creep-fatigue conditions. In this contribution, we discuss the cyclic deformation and softening behavior of P92 in strain-controlled LCF, in-phase (IP) TMF, and out-of-phase (OP) TMF tests with and without dwell times in the temperature range from 300 °C to 620°C. EBSD-based dislocation analysis on various fatigued material states confirms the continuous redistribution and annihilation of geometrically necessary dislocations in all studied states, which can be quantitatively correlated with macroscopic softening despite different damage mechanisms for different test types. Deviations from this correlation are observed for OP TMF and LCF with dwell times, i.e., for conditions where optical microscopy reveals pronounced crack-oxidation interactions at the specimen surfaces.
Cast magnesium alloys welds produced by refill friction stir spot welding (refill FSSW) show low lap shear strength (LSS) and constantly fail in stirred zone (SZ) shear mode. The cause is most probably related to the heavily textured microstructure. Here, to re-engineer the resulting microstructure, we pro- pose a novel process variant, the differential rotation refill FSSW (DR-refill FSSW). DR-refill FSSW stim- ulates discontinuous dynamic recrystallization and produces a bimodal microstructure with weakened texture. Therefore, the deformation incompatibility between SZ and thermal-mechanically affected zone is avoided. The welds have 50% higher LSS than that of standard refill FSSW welds, and fail in a different failure mode, i.e., SZ pull-out mode. DR-refill FSSW provides a new and effective strategy for improving the performance of spot welds based on microstructural engineering.
The presentation is structured in the following three parts:
i) Report of the Working Group 4 X-Ray Spectroscopy including the publication of ISO 15632:2021 Microbeam analysis — Selected instrumental performance parameters for the specification and checking of energy-dispersive X-ray spectrometers for use in electron probe microanalysis,
ii) Liaison activities between ISO/TC202 Microbeam Anaylsis and VAMAS/TWA34 Quantitative Microstructural Analysis, and
iii) Liaison activities from ISO/TC202 Microbeam Analysis for ISO/TC229 Nanotechnologies.
Most relevant projects are highlighted for information and further discussions. New initiatives and better promotion of strategic projects are addressed.