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The application of in-situ 3D X-ray Diffraction in annealing experiments: First interpretation of substructure development in deformed NaCl
Stockholm University, Faculty of Science, Department of Geological Sciences. (Petrotectonics)
Stockholm University, Faculty of Science, Department of Geological Sciences. (Petrotectonics)
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2010 (English)In: Recrystallization and Grain Growth: Proceedings of the fourth Joint International Conference of Recrystallization and Grain Growth, 2010Conference paper (Refereed)
Abstract [en]

In-situ 3D X-ray diffraction (3DXRD) annealing experiments were conducted at the ID-11 beamline at the European Synchrotron Radiation Facility in Grenoble. This allowed us to non-destructively document and subsequently analyse the development of substructures during heating, without the influence of surface effects. A sample of deformed single crystal halite was heated to between 260-400 ºC. Before and after heating a volume of 500 by 500 by 300 mm was mapped using a planar beam, which was translated over the sample volume at intervals of 5-10 µm in the vertical dimension. In the following we present partially reconstructed orientation maps over one layer before and after heating for 240min at 260 ºC. Additional small syn-heating “maps” over a constrained sample rotation of 12-30º. The purpose of this was to illuminate a few reflections from 1 or 2 subgrains and follow their evolution during heating.

Preliminary results show that significant changes occurred within the sample volume, for which, surface effects can be excluded. Results show a number of processes, including: i) change in subgrain boundary misorientation angle and ii) subgrain subdivision into areas of similar lattice orientation with new subgrain boundary formation. These results demonstrate that 3DXRD coupled with in-situ heating is a successful non-destructive technique for examining real-time post-deformational annealing in strongly deformed crystalline materials with complicated microstructures.

Place, publisher, year, edition, pages
Keyword [en]
halite, annealing, X-ray diffraction, substructure, in-situ
Research subject
URN: urn:nbn:se:su:diva-45688OAI: diva2:369341
Recrystallization and Grain Growth
Available from: 2010-11-10 Created: 2010-11-10 Last updated: 2010-11-12Bibliographically approved
In thesis
1. Fundamentals of substructure dynamics: In-situ experiments and numerical simulation
Open this publication in new window or tab >>Fundamentals of substructure dynamics: In-situ experiments and numerical simulation
2010 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Substructure dynamics incorporate all features occurring on a subgrain-scale. The substructure governs the rheology of a rock, which in turn determines how it will respond to different processes during tectonic changes. This project details an in-depth study of substructural dynamics during post-deformational annealing, using single-crystal halite as an analogue for silicate materials. The study combines three different techniques; in-situ annealing experiments conducted inside the scanning electron microscope and coupled with electron backscatter diffraction, 3D X-ray diffraction coupled with in-situ heating conducted at the European Radiation Synchrotron Facility and numerical simulation using the microstructural modelling platform Elle. The main outcome of the project is a significantly refined model for recovery at annealing temperatures below that of deformation preceding annealing. Behaviour is highly dependent on the temperature of annealing, particularly related to the activation temperature of climb and is also strongly reliant on short versus long range dislocation effects. Subgrain boundaries were categorised with regard to their behaviour during annealing, orientation and morphology and it was found that different types of boundaries have different behaviour and must be treated as such. Numerical simulation of the recovery process supported these findings, with much of the subgrain boundary behaviour reproduced with small variation to the mobilities on different rotation axes and increase of the size of the calculation area to imitate long-range dislocation effects. Dislocations were found to remain independent to much higher misorientation angles than previously thought, with simulation results indicating that change in boundary response occurs at ~7º for halite. Comparison of 2D experiments to 3D indicated that general boundary behaviour was similar within the volume and was not significantly influenced by effects from the free surface. Boundary migration, however, occurred more extensively in the 3D experiment. This difference is interpreted to be related to boundary drag on thermal grooves on the 2D experimental surface. While relative boundary mobilities will be similar, absolute values must therefore be treated with some care when using a 2D analysis.

Place, publisher, year, edition, pages
Stockholm: Department of Geological Sciences, Stockholm University, 2010. 23 p.
Meddelanden från Stockholms universitets institution för geologiska vetenskaper, 342
halite, in-situ, X-ray diffraction, EBSD, annealing, substructure, modelling
National Category
Earth and Related Environmental Sciences
Research subject
urn:nbn:se:su:diva-45811 (URN)978-91-7447-187-8 (ISBN)
Public defence
2010-12-20, De Geersalen, Geovetenskapens hus, Svante Arrhenius väg 14, Stockholm, 10:30 (English)
At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 3: Manuscript. Paper 4: Manuscript.Available from: 2010-11-28 Created: 2010-11-11 Last updated: 2010-12-03Bibliographically approved

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