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Fundamentals of Substructure Dynamics In-Situ Experiments and Numerical Simulation

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Fundamentals of Substructure Dynamics In-Situ Experiments and Numerical Simulation Meddelanden fr˚an Stockholms Universitets Institution f¨or Geologiska Vetenskaper No. 342 Fundamentals of substructure dynamics In-situ experiments and numerical simulation Verity Borthwick Stockholm 2010 Department of Geological Sciences Stockholm University S-106 91 Stockholm Sweden A Dissertation for the degree of Doctor of Philosophy in Natural Science Department of Geological Sciences Stockholm University S-106 91 Stockholm Sweden Abstract 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 with 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. c Verity Borthwick ISBN 978-91-7447-187-8, p 1{23 Cover: Printed by US-AB SU, Stockholm 2010 Fundamentals of substructure dynamics In-situ experiments and numerical simulation Verity Borthwick This doctoral thesis consists of a summary and four manuscripts. The presented manuscripts are referred to as Manuscript I { IV in the text. Manuscript I | Borthwick, V.E. and Piazolo, S. (2010) Post-deformational annealing at the subgrain scale: temperature dependent behaviour revealed by in-situ heating experiments on deformed single crystal halite. Journal of Structural Geology, 32, 982-996. Reprinted with permission from Elsevier Manuscript II | Borthwick, V.E., Schmidt, S., Piazolo, S., Gundlach, C., Griera, A., Bons, P.D. and Jessell, M.W. (2010) The application of in-situ 3D X-ray Diffraction in annealing experiments: First interpretation of substructure development in deformed NaCl. Recrystallization and Grain Growth, Proceedings of the International Conference of Recrystallization and Grain Growth. In press. Manuscript III | Borthwick, V.E., Schmidt, S., Piazolo, S. and Gundlach, C. In-situ 3DXRD annealing of a geological material: Evaluating the validity of 2D. To be submitted to Nature Geoscience. Manuscript IV | Borthwick, V.E., Piazolo, S., Evans, L., Griera, A. and Bons, P.D. Numerical simulation coupled with in-situ annealing experiments: A new model for recovery. To be submitted to Acta Materialia. The work of this thesis has principally been carried out by the author. All four manuscripts were predom- inantly written by the author with support, suggestions and extensive discussion from Sandra Piazolo. Experiments for Manuscript I were designed by Piazolo, and carried out with initial supervision by her and continued advice and assistance throughout the experimental process. Post-experimental processing and analysis was conducted by the author. For Manuscripts II and III the data reconstruction of full crystal diffraction patterns was conducted by Søren Schmidt. The six day experiment was run with the support of the other co-authors on II. Data analysis for both papers was conducted by the author. The numerical simulation in Manuscript IV was written by the author in close collaboration with the co-authors. Testing of the simulation and interpretation were conducted by the author with assistance from Sandra Piazolo. Stockholm, October 2010 Verity Borthwick To Mumedean and Grandpa Ronald, I know you would have been proud Contents 1 Project aim 1 1.1 Why study substructure dynamics?...............................1 1.2 Overall approach.........................................1 1.3 Mineral Substructure Dynamics { a European wide-network.................1 2 Background 2 2.1 The deformed state........................................2 2.2 Post-deformational annealing..................................2 2.3 Halite as an analogue......................................4 2.4 2D In-situ annealing experiments................................5 2.5 3D X-ray diffraction.......................................5 2.6 Numerical simulation.......................................6 3 Methods 6 3.1 2D in-situ annealing and EBSD.................................6 3.1.1 Data processing......................................6 3.2 3D X-ray diffraction.......................................7 3.2.1 Data analysis.......................................9 3.3 Numerical modelling.......................................9 3.3.1 Data analysis....................................... 11 4 Results and discussion 11 4.1 Manuscript I........................................... 11 4.2 Manuscript II........................................... 12 4.3 Manuscript III.......................................... 12 4.4 Manuscript IV.......................................... 13 5 Summary and conclusions 13 6 Main outcomes 14 7 Future work 16 8 Acknowledgements 16 1 Project aim behaviour dependent on these types of dislo- cations? 1.1 Why study substructure dynam- ics? 4. Can we predict subgrain boundary be- haviour? Microstructures hold the key to understanding tec- tonic behaviour on the most fundamental of scales. 5. Can we use substructure and subgrain bound- Deformation of rocks in the crust and mantle ary behaviour to derive deformation and/or mostly occurs by crystal-plastic mechanisms such annealing conditions? as dislocation creep. Individual crystals within a rock respond to strain by forming defects in the crystal lattice. These form a microscale sub- 1.2 Overall approach structure of dislocation arrays, free dislocations The project involves a three-technique approach. and a network of subgrain boundaries (Humphreys The starting point for this work began with 2D and Hatherly, 2004 and references therein). On in-situ annealing experiments conducted inside the a macroscale these substructures effect the rheol- scanning electron microscope (SEM) and coupled ogy of a rock (Ashby, 1969; Means and Xia, 1981; with electron backscatter diffraction (EBSD). A Ranalli, 1995; Passchier and Trouw, 2005). Thus, comparison experiment was conducted using 3D X- in order to investigate behaviour on a macroscale it ray diffraction (3DXRD) at the synchrotron facil- is essential to understand substructure dynamics. ity in Grenoble in order to rule out the potential of As a rock is exhumed to the crust it is affected by a surface effects in 2D experiments. Numerical simu- complex series of processes which change the sub- lation directly accessing results from the 2D exper- structure. In order to reconstruct this temperature- iments allowed development of theories and itera- time path it is necessary to predict the results of tive improvement of a new deterministic recovery these various changes. Post-deformational anneal- model. This thesis discusses aspects of the above ing is of particular interest, as this is often the last questions that we have answered throughout the process to affect a rock, occurring when pressure project period as well as highlighting areas which is removed but the system still retains a high tem- need further research. perature. It can still have a significant effect on the arrangement of the substructure. If we under- stand this process than we can potentially create 1.3 Mineral Substructure Dynamics a \window" through to the previous deformation { a European wide-network conditions (Fig.1). The precursor studies to this project were con- This PhD project is part of a European Science ducted by Bestmann et al. (2005) and Piazolo Foundation EUROCORES funded collaborative, et al. (2006). They conducted in-situ annealing EuroMinScI (European Mineral Science Initiative), experiments on a polycrystalline synthetic halite. which involves nine projects with researchers from Though substructural dynamics were not the focus twelve different countries. The purpose of the Eu- of these papers,
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