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UC Berkeley UC Berkeley Electronic Theses and Dissertations UC Berkeley UC Berkeley Electronic Theses and Dissertations Title Development of Novel Small Scale Mechanical Tests to Assess the Mechanical Properties of Ex-Service Inconel X-750 CANDU Reactor Components Permalink https://escholarship.org/uc/item/99k9w508 Author Howard, Cameron Publication Date 2018 Peer reviewed|Thesis/dissertation eScholarship.org Powered by the California Digital Library University of California Development of Novel Small Scale Mechanical Tests to Assess the Mechanical Properties of Ex-Service Inconel X-750 CANDU Reactor Components by Cameron Boyd Howard A dissertation in partial satisfaction of the requirements for the degree of Doctor of Philosophy in Engineering – Nuclear Engineering in the Graduate Division of the University of California, Berkeley Dissertation Committee: Professor Peter Hosemann, Chair Professor Per Peterson Professor Andrew M. Minor Spring 2018 Abstract Development of Novel Small Scale Mechanical Tests to Assess the Mechanical Properties of Ex-Service Inconel X-750 CANDU Reactor Components by Cameron Boyd Howard Doctor of Philosophy in Nuclear Engineering University of California, Berkeley Professor Peter Hosemann, Chair Inconel X-750 is a precipitation hardened nickel superalloy designed to have high strength and creep resistance at elevated temperatures. In Canada Deuterium Uranium (CANDU) reactors, this material serves as tight fitting fuel channel annulus spacers in the form of springs separating the cold calandria tube from the hot pressure tube. Unlike light water reactors (LWRs), CANDU reactors have an elevated thermal neutron flux spectrum which amplifies nickel transmutation reactions, producing more radiation damage and increased amounts of internal hydrogen and helium compared to all other current generation reactors. Bulk component testing performed over the last few years indicates that these spacers are losing ductility and strength after time in service, and that the quantity of this loss is dependent on the irradiation temperature and dose. In addition, observations of fracture surfaces reveal intergranular failure and transmission electron microscopy (TEM) shows that helium bubbles preferentially align along grain boundaries. However, a dearth of knowledge on the mechanical properties of these components at high dose exists because only one to three component tests are performed at each irradiation condition inside hot cells, and these component tests produce complicated stress states, making the extraction of yield stresses and failure stresses challenging. Thus, two first of their kind, in-situ, small scale mechanical tests (SSMTs) employing scanning electron microscopy (SEM) and focused ion beam (FIB) techniques were developed to test components irradiated to doses of 53, 67, and 81 dpa in CANDU reactors at average irradiation temperatures of 180 oC and 300 oC. The first, a lift-out, three-point bend test quantified the yield stresses of the components as a function of irradiation temperature and dose. Material irradiated at the higher temperature undergoes significant yield strength increases up to 1 GPa, whereas this is negligible for material irradiated at the lower temperature (≤ 310 MPa). Grain boundary cracking after yielding was observed in specimens irradiated to 67 dpa at 180 oC. The second new SSMT is a push-to-pull, micro-tensile test 1 quantifying the yield strengths, failure strengths, and total elongations of the components as a function of irradiation temperature and dose. For specimens irradiated to 81 dpa, intergranular failure was directly observed, so failure stresses quantify grain boundary strengths. Both novel SSMTs also revealed significant regional differences in mechanical properties between the inner diameter, center, and outer diameter due to variations in the cold working and grinding of the component that went undetected in bulk component testing. The conclusion of this work is a detailed analysis of the degradation of an Inconel X- 750 CANDU component in terms of its quantitative mechanical properties through the invention of two novel SSMTs. These new testing methods and analyses are applicable for assessing the mechanical ageing of other reactor core components. 2 Contents Dedication List of tables List of figures Acknowledgements Publications 1 Motivation 1.1 The Need for Current and Future Clean Nuclear Energy 1.2 CANDU Life Management Surveillance Programs 1.3 Relevance to Reactor Lifetime Extension Programs 1.4 The Need for SSMTs 1.5 Research Goals 2 Background: A Review of Small Scale Mechanical Testing (SSMT) Applied to Nuclear Materials 2.1 Introduction 2.2 Small Shear Punch Test (SPT)/Miniaturized Disk Bend Test (MDBT) 2.3 Miniaturized Charpy Subsize Fracture Tests 2.4 Microhardness Tests 2.5 Nanoindentation Tests 2.6 Micro-pillar Compression Tests 2.7 Micro-tensile Tests 2.8 Micro-Bend Tests 2.8.1 Micro-Cantilever Tests 2.8.2 Micro-Fatigue Tests 2.9 In-Situ Transmission Electron Microscope (TEM) Tests 3 Materials and Radiation Effects Theory 3.1 Nickel-Based Superalloys 3.2 Nickel-Based Superalloys in Nuclear Reactors i 3.2.1 Inconel X-750 in CANDU Reactors 3.3 Radiation Damage Basics 3.3.1 Radiation Damage in the CANDU Core 3.3.1.1 Fast Neutron Damage 3.3.1.2 Thermal Neutron Damage: (n,p) and (n,α) Transmutations 3.3.1.3 Point Defects 3.3.1.4 Helium and Hydrogen Gas Production 3.3.1.5 Helium Bubble Nucleation and Growth 3.3.1.6 Helium Bubble Pressure 3.3.2 Mechanical Properties Evolution of Irradiated Nickel Superalloys 3.3.2.1 Radiation Hardening Mechanisms 3.3.2.2 γ’ Disordering and Dissolution 3.3.2.3 Dose Evolution of Mechanical Properties 3.3.2.4 Mechanisms for Grain Boundary Embrittlement 4 Experimental Procedures 4.1 Inconel X-750 Coils 4.1.1 Ex-Service Neutron Irradiated Inconel X-750 4.2 Sample Preparation 4.2.1 Sample Preparation of Non-Irradiated Inconel X-750 4.2.2 Sample Preparation of Neutron Irradiated Inconel X-750 4.3 Bulk Component Crush Testing 4.4 Microhardness Testing 4.5 In-Situ Micro-Three-Point Bend Testing 4.5.1 Micro-Three-Point Bend FIB Specimen Preparation 4.5.2 Electron Backscattered Diffraction Pre-Test Analysis 4.5.3 Testing Procedures 4.6 In-Situ Micro-Push-to-Pull Tensile Testing ii 4.6.1 Push-to Pull Device 4.6.2 Tensile Specimen Sample Preparation 4.6.3 Electron Backscattered Diffraction Pre-Test Analysis 4.6.4 Testing Procedures 4.7 Nanoindentation: Non-Irradiated Inconel X-750 4.8 Room Temperature Ion Irradiation Studies 4.8.1 Nanoindentation: Ion Irradiated Inconel X-750 4.8.2 In-Situ Gripper Micro-Tensile Testing 5 Results 5.1 Bulk Component Crush Testing 5.2 Microhardness Testing 5.3 In-Situ Micro-Three-Point Bend Testing 5.3.1 Non-Irradiated Outer Edge Specimens 5.3.2 Non-Irradiated Center Specimens 5.3.3 54 dpa Low Irradiation Temperature Specimens 5.3.4 54 dpa High Irradiation Temperature Specimens 5.3.5 67 dpa Low Irradiation Temperature Specimens 5.3.6 67 dpa High Irradiation Temperature Specimens 5.3.7 Summary 5.4 In-Situ Micro-Push-to-Pull Tensile Testing 5.4.1 Non-Irradiated Outer Edge Specimens 5.4.2 Non-Irradiated Center Specimens 5.4.3 Non-Irradiated Inner Edge Specimens 5.4.4 67 dpa Low Irradiation Temperature Specimens 5.4.5 67 dpa High Irradiation Temperature Specimens 5.4.6 81 dpa Low Irradiation Temperature Specimen 5.4.7 81 dpa High Irradiation Temperature Specimens iii 5.4.8 Summary 5.5 Nanoindentation: Non-Irradiated Inconel X-750 5.6 Room Temperature Ion Irradiation Studies 5.6.1 Nanoindentation: Ion Irradiated Inconel X-750 5.6.2 In-Situ Gripper Micro-Tensile Testing 5.6.3 Summary 6 Discussion 6.1 In-Situ Micro-Three-Point Bend Testing 6.1.1 Testing Limitations 6.2 In-Situ Micro-Push-to-Pull Tensile Testing 6.2.1 Quantifying Cold Working Effects from Material Processing 6.2.2 Critical Resolved Shear Stress 6.2.3 Yield Strengths 6.2.4 Failure Strengths and Total Elongations 6.2.5 Grain Boundary Strengths 6.2.6 Resolved Normal Stresses on High Angle Grain Boundaries 6.2.7 Deformation Mechanisms 6.2.8 Testing Challenges 6.3 Room Temperature Ion Irradiation Studies 6.3.1 Nanoindentation: Ion Irradiated Inconel X-750 6.3.2 In-Situ Gripper Micro-Tensile Testing 6.4 Future Work with SSMT Tensile Testing 7 Conclusions 8 References iv Dedication This work is dedicated to my parents, Michelle Howard and Dewey Howard Jr. Without their love and incredible work ethic and sacrifice throughout my entire life, this journey would not have been possible. v List of Tables Table 1. Ratio of Yield Strength to Shear Strength for Alloys with Indicated Base Element Table 2. Room Temperature Properties of Commercially Pure (99.6%) Ni 58 59 Table 3. Ni and Ni transmutation reactions and their associated σa-th and displacement damage Table 4. Chemical composition in wt. % and heat treatments for Inconel X-750 coils [191] Table 5. Room Temperature Properties of Inconel X-750 [191] Table 6. Ex-Service Neutron Irradiated Inconel X-750 Table 7. Struers Polishing Formula for Preparing Ni-Based Superalloys Table 8. Root-Mean-Squared Absolute and Normalized Grain Interior Misorientations of Inconel X-750 Table 9. He2+ Ion Energies Exiting the Degrader Wheel and Their Associated Stopping Peak Depths in the Inconel X-750 Spacers Table 10: Micro Three-Point Bend Yield Strength and Critical Resolved Shear Stress (CRSS) of Inconel X-750 Spring Material Table 11. Mechanical Data Summary Table for Push-to-Pull Inconel X-750 Micro-tensile Specimens Table 12. Mechanical Properties of Outer Edge Bulk Micro-Tensile Specimens vi List of Figures Figure 1. The temperature and dose range requirements for in-core structural materials that will operate in each of the 8 next generation reactor design concepts [8]. Figure 2.
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