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3DXRD – a New Probe for Materials Science Downloaded from orbit.dtu.dk on: Oct 09, 2021 3DXRD – a new probe for materials science Poulsen, Henning Friis Publication date: 2004 Document Version Publisher's PDF, also known as Version of record Link back to DTU Orbit Citation (APA): Poulsen, H. F. (2004). 3DXRD – a new probe for materials science. Risø National Laboratory. General rights Copyright and moral rights for the publications made accessible in the public portal are retained by the authors and/or other copyright owners and it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights. Users may download and print one copy of any publication from the public portal for the purpose of private study or research. You may not further distribute the material or use it for any profit-making activity or commercial gain You may freely distribute the URL identifying the publication in the public portal If you believe that this document breaches copyright please contact us providing details, and we will remove access to the work immediately and investigate your claim. 3DXRD – a new probe for materials science 3DXRD – a new probe for materials science by Henning Friis Poulsen Centre for Fundamental Research: Metal Structures in Four Dimensions, Materials Research Department, Risø National Laboratory, Roskilde, Denmark. Denne afhandling er af Danmarks Tekniske Universitet antaget til forsvar for den tekniske doktorgrad. Antagelsen er sket efter bedømmelse af den foreliggende afhandling. Kgs. Lyngby, den 5. februar 2004 Lars Pallesen Rektor /Kristian Stubkjær Forskningsdekan This dissertation has been accepted by the Technical University of Denmark for public defence in fulfilment of the requirements for the degree of Doctor Technices. The acceptance is based on the present dissertation. Kgs. Lyngby, 5 February 2004 Lars Pallesen Rector /Kristian Stubkjær Dean of Research Contents: Preface............................................................................................................................3 1. Introduction................................................................................................................5 2. Methods for structural characterisation in materials science...................................11 2.1 Electron and optical microscopy........................................................................11 2.2 X-ray diffraction with low energy x-rays. .........................................................13 2.3 Conventional bulk-sensitive methods................................................................14 2.4 Hard x-rays: properties ......................................................................................15 2.5 Hard x-ray work using synchrotron sources ......................................................18 3. 3DXRD: geometric principles .................................................................................21 3.1 The basic 3DXRD set-up...................................................................................22 3.2 GRAINDEX: Indexing distinct diffraction spots................................................25 3.3 Analysis of single grains based on GRAINDEX ................................................28 3.4 The conical slit...................................................................................................31 3.5 Characterisation of large volumes .....................................................................33 3.6 Dynamic experiments ........................................................................................34 3.7 Conclusions and outlook....................................................................................35 4. Reconstruction .........................................................................................................37 4.1 The ART routine for undeformed grains and a line beam..................................38 4.2 The FBP routine for undeformed grains and a box beam..................................39 4.3 The general 6D case...........................................................................................42 4.4 Conclusions and outlook....................................................................................43 5. The 3DXRD Microscope .........................................................................................45 5.1 Optics .................................................................................................................46 5.2 Diffractometer....................................................................................................48 6. Combining 3DXRD and absorption contrast tomography.......................................51 6.1 A study of wetting..............................................................................................52 6.2 Plastic strain.......................................................................................................53 6.3 Outlook ..............................................................................................................55 7. Applications .............................................................................................................57 7.1 Polycrystalline deformation...............................................................................57 7.2 Recrystallization ................................................................................................63 7.3 Recovery and nucleation....................................................................................70 7.4 Peak shape analysis............................................................................................77 7.5 Phase transformations ........................................................................................80 7.6 Grain size distributions ......................................................................................86 7.7 Crystallography..................................................................................................89 8. Outlook ....................................................................................................................93 8.1 Hardware improvements....................................................................................94 8.2 Applying 3DXRD methods to other sources .....................................................96 8.3 Other 3D resolved x-ray diffraction work .........................................................97 9. Conclusions..............................................................................................................99 Acknowledgments......................................................................................................101 References..................................................................................................................102 Dansk Resume (Summary in Danish)........................................................................111 List of abbreviations ..................................................................................................113 APPENDIX................................................................................................................115 2 Preface 3-Dimensional X-Ray Diffraction (3DXRD) is a novel experimental method for structural characterisation of polycrystalline materials. It is based on two principles: the use of highly penetrating hard x-rays from a synchrotron source and a “tomographic” approach to the acquisition of diffraction data. Uniquely, the method enables a fast and non-destructive characterization of the individual microstructural elements (grains and sub-grains) within mm-cm sized specimens. The position, morphology, phase, and crystallographic orientation can be derived for hundreds of elements simultaneously as well as their elastic and plastic strains. Furthermore, the dynamics of the individual elements can be monitored during typical processes such as deformation or annealing. Hence, for the first time information on the interaction between elements can be obtained directly. The provision of such data is vital in order to extend beyond state-of-art models in metal and ceramic science. The 3DXRD methodology has developed over a period of 7 years, as the result of work by a group at Risø National Laboratory, with the author of this thesis as project leader. The work has lead to the establishment of a dedicated instrument, the so-called 3DXRD microscope. The microscope was installed at the European Synchrotron Facility (ESRF) in Grenoble at the end of 1999. The aim of this thesis is to give a comprehensive account of 3DXRD microscopy, with focus both on methodology and applications. At the time of writing, the technique has reached a natural 1st stage in its development. A geometric formalism has been established, and implemented in terms of a set of experimental routines and analysis programs. Likewise, a number of prime applications have been identified, from which major results have emerged. The work is presented partly in this thesis itself, partly in 15 selected publications, which are attached. The thesis is written for a general reader who has a background in the natural sciences and a basic understanding of diffraction. To ease the presentation the methodology is introduced without the use of equations and with a minimum of materials science specific conventions. For a mathematical treatment and details of the algorithms please refer to the attached publications. Likewise, the main applications are introduced by a short preamble, written in
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