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Irradiated Graphite Waste - Stored Energy Irradiated Graphite Waste - Stored Energy A thesis submitted to the University of Manchester for the degree of Doctor of Philosophy in the Faculty of Engineering and Physical Sciences 2012 Michael Lasithiotakis School of Materials Materials Performance Centre 1 2 List of Contents List of Contents List of Contents 3 List of Figures 5 List of Tables 8 Abstract 9 Declaration 10 Copyright Statement 11 Rationale for Submitting the Thesis in Alternative Format 12 Acknowledgements 13 Dedication 14 Chapter 1 - Introduction and Context of Research 15 Graphite 15 Nuclear reactors 17 Decommissioning of a Nuclear Facility 17 Radioactive Waste-Disposal of Radioactive Waste 17 Wigner Energy – An additional hazard during decommissioning. 21 The Windscale fire event – A nuclear accident that directly involved Wigner energy release 23 Chapter 2 - Literature Review 25 Stored Energy Release 25 Defects 27 Annealing of Defects 32 Kinetics of Stored Energy Release 37 Ion irradiation : A Method to Simulate Irradiation Damage. 48 Chapter 3- Methods 51 Differential Scanning Calorimetry 51 X-ray Diffraction 55 Raman Spectroscopy 62 Chapter 4 - Publication I: Application of an Independent Parallel Reactions Model to the Annealing Kinetics on BEPO Irradiated Graphite 67 3 List of Contents Chapter 5 - Publication II: Annealing of ion irradiation damage in nuclear graphite 68 Chapter 6 - Publication III: Application of an Independent Parallel Reactions Model on the Annealing Kinetics of BEPO Irradiated Graphite 69 Chapter 7 - General Conclusions and Future Work 70 Bibliography 73 Total Word Count : 43,227 words 4 List of Figures List of Figures Figure 1.1. Pg 16. A scheme of the manufacturing stages of nuclear graphite. Figure 1.2. Pg 18. SRF. Schematic of the Swedish Geological Repository for radioactive operational waste. It is the Swedish central disposal facility for all short lived low-and intermediate level waste from the operation of the nuclear power plants. It is located in granitic rock under the sea close to the Forsmark nuclear power plant, around 1 km offshore and 50 m below the seafloor. Figure 1.3. Pg 19. Examples of dry cask storage containers. Left: Vertical stand alone dry cask storage containers. Right dry cask storage containers in bunkers. Figure 1.4. Pg 19. Example of a penetration device used in deep sea experiments. Chapter 2 Figure 2.1. Pg 28. Schematic of the single vacancy (A, unreconstructed and B, reconstructed.) Figure 2.2. Pg 28. The Stone Wales topological defect, showing the exchange of positions of interstitial atoms. Figure 2.3. Pg 28. The metastable intimate Frenkel pair defect symbolised by I+V*. Figure 2.4. Pg 29. Prismatic (left) and basal (right) dislocation. Figure 2.5. Pg 29. Transmission Electron Micrographs of pyrolytic graphite. The dislocation network shown above, although not created by neutron irradiation, clearly depict dislocation networks lying in the basal planes. Figure 2.6. Pg 31. Configurations of the interstitials at the various sites A to E and for the free (F) interstitial as obtained with the first principles calculation package CASTEP and GGA. In Figure the light gray atoms are part of graphite; the interstitial is shown in red. For the high symmetry positions D and the free interstitial the top view is given as well. The inset at the top shows the high symmetry sites for an interstitial in graphite. 5 List of Figures Figure 2.7 . Pg 33. Migration of a single vacancy. Figure 2.8. Pg 33. A description of the annealing process by Telling et al. Figure 2.9. Pg 37. Stored energy accumulation as a function of effective dose. Figure 2.10. Pg 44. Fitting of energy distribution to data from a Windscale Pile 2 dowel graphitic sample at 10oC/min Figure 2.11. Pg 44. Comparison of constant activation energy models fitted to Iwata’s experimental date using the variable frequency factors from Iwata’s paper and using a constant frequency factor. Chapter 3 Figure 3.1. Pg 52. (a) Heat flux DSC; (b) power-compensated DSC. Figure 3.2. Pg 53. The rate of release of stored energy. Hanford cooled test hole graphite 30oC . Figure 3.3. Pg 53. The effect of irradiation temperature on the shape of DSC curves. In the diagram above three DSC curves at different irradiation temperatures (150oC, 200oC and 250oC)are depicted (heating rate was 10oC/min). Figure 3.4. Pg 54. A - Layout of a graphite reactor stack (left) and arrangement of sampling points along height of stack (right, a-m are sampling points) from bricks removed during dismantling of the reactor (single-hatched) and cut out from the stack with the aid of remote controlled drill cutter (double-hatched). Figure 3.5. Pg 54. Curves of behaviour of stored-energy release: Images 1 to 4: Curves for samples cut out of bricks removed during dismantling of a graphite pile; Images 5 to 8: curves for samples cut from stack with drill cutter. Image 1 to 3: Three samples a,b,c (see previous figure) from brick No. 4 in lattice cell 10-03; Image 4: Sample c from brick No. 7 in cell 06-10; Images 5-8: Samples c, d, e, g from cell 09-03. Depiction [--------] refers to sample adjacent to channel. Depiction [-∙-∙-∙-∙-∙-] refers to sample remote from channel; C is the specific heat of unexposed graphite. 6 List of Figures Figure 3.6. Pg 56. Phase identification between two allotropes of carbon, diamond and graphite[109]. A-The X-ray diffraction intensity for diamond nanoparticles B-The diffraction intensity of diamond nanoparticles with a coating of graphite after heat treatment at 1400°C.C- The diffraction intensity for spherical carbon onions after heat treatment at 1700°C. D-The diffraction intensity for polyhedral carbon onions after heat treatment at 2000°C. Figure 3.7. Pg 57.X-ray powder diffraction patterns of SP-1 pyrolytic graphite and nuclear graphite sample along with silicon standard. Some of the peaks that appear refer to the graphites while others to the silicon standard. Figure 3.8. Pg 59.Calculation of Integral Breadth β and Full Width Half Maximum of a specific peak of an XRD pattern. Figure 3.9. Pg 60. Normalised after Ka2 instrumental broadening subtraction of X-ray diffraction patterns of graphite milled in n-dodecane. Figure 3.10. Pg 61. Photograph of the open (left) and closed (right) DSC/XRD measuring head. The Pt sample and reference cups are occupied by empty graphite pans. Remnants of a sample are visible on the graphite pan and the sample itself can be seen on the support bracket. Figure 3.11. Pg 62. Schematic diagram of a Raman spectroscoper. Figure 3.12. Pg 64. Schematic diagram of the E2g and A1g modes. Carbon motions in the (a) G and (b) D modes. The G mode is just due to the relative motion of sp2 carbon atoms and can be found in chains as well. Figure 3.13. Pg 65. Two characteristic types of spectra from two graphitic materials.[127] On top, Highly Oriented Pyrolytic Graphite (HOPG) undisturbed, without defects, and glassy carbon, containing defects. The peak at the range of 1340cm-1 is indicative of the presence of defects. 7 List of Tables List of Tables Chapter 2 Table 2.1. Pg 27. A summation of various types of defects of graphite, and their symbolism. Table 2.2. Pg 34. A supposed mechanism of the Wigner energy release in irradiated graphite. C, means interstitial carbon molecules. and V means vacancies. Most energy is released by the annihilation of interstitial C2 molecules and vacancies Table 2.3. Pg 43. Activation Energy and Pre-exponential factors as calculated by various researchers Table 2.4. Pg 46. Activation Energy and Pre-exponential factors as calculated by Iwata [4] [2] [54] [45] , Simmons , Lexa et al , and Kelly et al, Chapter 3 Table 3.1. Pg 58. Lattice parameter of SP-1 and nuclear graphite samples. Table 3.2. Pg 58. Lattice parameter a, c, as correlated with the degree of graphitization (DOG: g) of the as received IG-110 and IG-430 Japanese types of nuclear graphite. Table 3.3. Pg 63. A collection of characteristic graphitic peaks. 8 Abstract The University of Manchester Michael Lasithiotakis Doctor of Philosophy in Materials Science Irradiated Graphite Waste - Stored Energy March 2012 Abstract The cores of early UK graphite moderated research and production nuclear fission reactors operated at temperatures below 150°C. Due to this low temperature their core graphite contains significant amounts of stored (Wigner) energy that may be released by heating the graphite above the irradiation temperature. This exothermic behavior has lead to a number of decommissioning issues which are related to long term "safe-storage", reactor core dismantling, graphite waste packaging and the final disposal of this irradiated graphite waste. The release of stored energy can be modeled using kinetic models. These models rely on empirical data obtained either from graphite samples irradiated in Material Test Reactors (MTR) or data obtained from small samples obtained from the reactors themselves. Data from these experiments is used to derive activation energies and characteristic functions used in kinetic models. This present research involved the development of an understanding of the different grades of graphite, relating the accumulation of stored energy to reactor irradiation history and an investigation of historic stored energy data. The release of stored energy under various conditions applicable to decommissioning has been conducted using thermal analysis techniques such as Differential Scanning Calorimetry (DSC). Kinetic models were developed, validated and applied, suitable for the study of stored energy release in irradiated graphite components. A potentially valid method was developed, for determining the stored energy content of graphite components and the kinetics of energy release.
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