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(1)WIR SCHAFFEN WISSEN – HEUTE FÜR MORGEN. Manuel A. Pouchon :: Laboratory Head :: Paul Scherrer Institut. LNM: Labor für Nukleare Materialien NES Information Event, 24.10.2017.

(2) Table of Contents o Introduction • LNM Mission • Background / Aspects of Nuclear Materials •  Research Programs in LNM o Examples from Research Programs • Pressure Boundary Components / RPV Internals (INTEGER) − SCC in Ni-Alloys and Weldments in LWRs − … effect of hydrogen on SCC initiation in Alloy 182 − … SCC resistance and fracture toughness on mock-up weld on Alloy 52M • Cladding & Fuel (Nuclear Fuels) − Hydride (Re-)Orientation − … under fatigue − … investigation using neutrons − … liner cladding and H distribution • Advanced Systems (Advanced Nuclear Materials) − Spallation material investigations (from STIP) − … material flow using new sample preparation box and FIB − … example using atom probe tomography. M.A. Pouchon, NES Information Event, 24.10.2017, Page 2 / 26.

(3) Table of Contents o Introduction • LNM Mission • Background / Aspects of Nuclear Materials •  Research Programs in LNM o Examples from Research Programs • Pressure Boundary Components / RPV Internals (INTEGER) − SCC in Ni-Alloys and Weldments in LWRs − … effect of hydrogen on SCC initiation in Alloy 182 − … SCC resistance and fracture toughness on mock-up weld on Alloy 52M • Cladding & Fuel (Nuclear Fuels) − Hydride (Re-)Orientation − … under fatigue − … investigation using neutrons − … liner cladding and H distribution • Advanced Systems (Advanced Nuclear Materials) − Spallation material investigations (from STIP) − … material flow using new sample preparation box and FIB − … example using atom probe tomography. M.A. Pouchon, NES Information Event, 24.10.2017, Page 3 / 26.

(4) Mission of LNM •. CENTRE OF EXCELLENCE: The LNM is national centre of excellence in Switzerland in the domains of (irradiated) materials behaviour and ageing in nuclear installations.. •. ACADEMIC R&D & SCIENTIFIC SERVICE Sustainability of current and future nuclear installations for electricity & heat generation as well as to the performance of nuclear facilities. A special emphasis is placed to the safety & safe long-term operation of the CH NPPs. • Material ageing in the primary circuit and its impact on integrity, safety & lifetime • Performance and safety of LWR core materials in service and storage • Radiation damage in structural and core/target materials of advanced nuclear and accelerator systems. • Material irradiation program at SINQ in co-operation with the Spallation Neutron Source Division. • Post-irradiation examinations and failure analysis in close cooperation with the Hotlab Division AHL.. M.A. Pouchon, NES Information Event, 24.10.2017, Page 4 / 26.

(5) Mission of LNM •. KNOWLEDGE MANAGEMENT: Academic teaching and education as well as in knowledge transfer  contributing to the education of the future nuclear specialists and  preservation of expertise & excellence. •. INDEPENDENT EXPERTISE: Independent expertise and excellence for  Swiss safety authority, e.g. for expertise’s and consulting (TSO)  industry, e.g., for material examinations and failure analysis.. •. STATE OF THE ART INFRASTRUCTURE: State-of-the-art lab & computing infrastructure and modelling tools for:  characterization of (radioactive) materials  analysis & prediction of the material behavior, integrity, safety & lifetime (strongly benefiting from PSI’s unique large scale facilities: hotlab, SLS, SINQ, SwissFEL). M.A. Pouchon, NES Information Event, 24.10.2017, Page 5 / 26.

(6) Background - Programs Today in CH. LWRs. High T Fast n. ADS Spallation. Nuclear Fuels. Component Structural Integrity. Advanced Nuclear Materials. M.A. Pouchon, NES Information Event, 24.10.2017, Page 6 / 26.

(7) Projects overview ANM: • MeAWaT - ETH competence center CCEM • 3D Printing - ETH scientific focus area – additive manufacturing • MatISSE, SOTERIA, INSPYRE, M4F - European projects • STIP irradiation program / PIE - CAS, JAEA, USTB, Beijing University, HFUT NF: • Cladding Mechanical Behavior and Influence of Hydrogen (dry storage, …) - swissnuclear, ESB • Hydrogen uptake - swissnuclear, MUZIC • ATF - CARAT, swissnuclear, KKG • Fuels - swissnuclear, Areva, Westinghouse, NFIR • FIB – R’Equip. INTEGER: • PISA-II & -ext, PARENT, NORA-II, SAFE-II  LEAD, PROBAB, NORA-III - ENSI • PLiM-VI - swissnuclear • Helium FM - fusion/STIP-V • SOTERIA, INCEFA+, NOMAD, MEACTOS, M4F - European projects • YUMOD (KKL), SCC Alloy 52 (KKL), BWRVIP-233(EPRI), EAF LAS (EPRI) M.A. Pouchon, NES Information Event, 24.10.2017, Page 7 / 26.

(8) Table of Contents o Introduction • LNM Mission • Background / Aspects of Nuclear Materials •  Research Programs in LNM o Examples from Research Programs • Pressure Boundary Components / RPV Internals (INTEGER) − SCC in Ni-Alloys and Weldments in LWRs − … effect of hydrogen on SCC initiation in Alloy 182 − … SCC resistance and fracture toughness on mock-up weld on Alloy 52M • Cladding & Fuel (Nuclear Fuels) − Hydride (Re-)Orientation − … under fatigue − … investigation using neutrons − … liner cladding and H distribution • Advanced Systems (Advanced Nuclear Materials) − Spallation material investigations (from STIP) − … material flow using new sample preparation box and FIB − … example using atom probe tomography. M.A. Pouchon, NES Information Event, 24.10.2017, Page 8 / 26.

(9) SCC in Ni-Alloys and Weldments in LWRs Current activities: •. SAFE-II (ENSI): Subproject-I: PhD thesis of J. Bai on the Effect of hydrogen on SCC initiation in Alloy 182 under BWR/HWC conditions @ 274 °C. •. MICRIN+ (EU-7 /NUGENIA+): Accelerated screening test method for SCC initiation studies. •. ICG-EAC Round Robin (in-kind): SCC initiation study in Ni-alloys under constant load. •. MEACTOS (H2020 EURATOM): Mitigating environmentally-assisted cracking through optimisation of surface condition. •. ECG-COMON Round Robin (in-kind): Effect of hydrogen on the corrosion behaviour and oxide films in Ni, Alloy 600 and Alloy 182. •. Overlay repair weld with Alloy 52M (KKL, service project): Characterization of SCC resistance and fracture toughness on mock-up weld. M.A. Pouchon, NES Information Event, 24.10.2017, Page 9 / 26.

(10) SAFE-II SP-I: SCC Initiation in Alloy 182 Dissimilar Metal Welds. PhD project of J. Bai: • Background: SCC incidents in Alloy 182 DMWs in BWRs • Effect of H2 on SCC initiation & short crack growth in Alloy 182 under BWR/HWC conditions @ 274°C • Identification of optimal mitigation conditions • Tentative mechanistic interpretation on mechanism. Maximum in SCC initiation susceptibility & SCC crack growth rate at Ni/NiO phase boundary! M.A. Pouchon, NES Information Event, 24.10.2017, Page 10 / 26.

(11) EBSD Analysis of IGSCC Initiation & Propagation. All grain boundaries in original material. • •. All cracked grain boundaries. Low angle grain boundaries seem to be resistant to SCC. Random high-energy, high-angle grain boundaries (HABs) with higher number of Schmid factor mismatch between the adjacent grains are prone to SCC → strain/deformation incompatibility plays a key role in crack initiation & propagation M.A. Pouchon, NES Information Event, 24.10.2017, Page 11 / 26.

(12) Material Characterization on Alloy 52 for KKL Axial SCC crack in N5 RPV FW nozzle ~ 93 % of wall thickness. Full structural overlay repair weld with Alloy 52M. • Request of ENSI for additional material tests with Alloy 52M to confirm the assumptions of the performed integrity assessment • Tensile and EPFM tests in air, SCC test in high-temperature water • Very high SCC resistance & high toughness confirmed • KKL & ENSI were highly satisfied by professional PSI work. M.A. Pouchon, NES Information Event, 24.10.2017, Page 12 / 26.

(13) Table of Contents o Introduction • LNM Mission • Background / Aspects of Nuclear Materials •  Research Programs in LNM o Examples from Research Programs • Pressure Boundary Components / RPV Internals (INTEGER) − SCC in Ni-Alloys and Weldments in LWRs − … effect of hydrogen on SCC initiation in Alloy 182 − … SCC resistance and fracture toughness on mock-up weld on Alloy 52M • Cladding & Fuel (Nuclear Fuels) − Hydride (Re-)Orientation − … under fatigue − … investigation using neutrons − … liner cladding and H distribution • Advanced Systems (Advanced Nuclear Materials) − Spallation material investigations (from STIP) − … material flow using new sample preparation box and FIB − … example using atom probe tomography. M.A. Pouchon, NES Information Event, 24.10.2017, Page 13 / 26.

(14) Transportation of spent fuels, dry storage Cladding fatigue risk. Credit: Zwilag. Credit: NAGRA. M.A. Pouchon, NES Information Event, 24.10.2017, Page 14 / 26.

(15) Hydride (Re-)Orientation – Impact on Fatigue H-free, as-received.  ‘Normal’ appearance. F In-plane hydrides. F.  Deep splits  No lifetime reduction detected. Reoriented hydrides. W. Gong, A. Brenin, R. Zubler, J. Bertsch, Hydrides Impact on Zircaloy Fatigue Properties, , WRFPM, Sep. 10-14, 2017, Jeju, Korea.  Facetted due to hydrides  Lifetime reduction unclear  Further tests needed. M.A. Pouchon, NES Information Event, 24.10.2017, Page 15 / 26.

(16) Neutron Radiography at PSI SINQ Spatial resolution. neutrons. Neutron microscope neutrons. SINQ spallation neutron source M.A. Pouchon, NES Information Event, 24.10.2017, Page 16 / 26.

(17) Ex-situ Measurements – H & Stress pre-test. post-test (350°C, 120 MPa nom., 10 h, 240 wppm H). Hydrides metallography. H concentration Calibration. 0.016 transmission increase. ~160wppm H elevated by stress. M.A. Pouchon, NES Information Event, 24.10.2017, Page 17 / 26.

(18) Liner Cladding – Quantification H content  DX-D4 outer liner cladding, ~200 wppm H  4.5 mm segment // neutron beam  POLDI thermal neutron beamline, exposure 3 min x 100. Further tests with different cooling rates already performed. hydrides free. hydrides present. Neutron image M.A. Pouchon, NES Information Event, 24.10.2017, Page 18 / 26.

(19) Table of Contents o Introduction • LNM Mission • Background / Aspects of Nuclear Materials •  Research Programs in LNM o Examples from Research Programs • Pressure Boundary Components / RPV Internals (INTEGER) − SCC in Ni-Alloys and Weldments in LWRs − … effect of hydrogen on SCC initiation in Alloy 182 − … SCC resistance and fracture toughness on mock-up weld on Alloy 52M • Cladding & Fuel (Nuclear Fuels) − Hydride (Re-)Orientation − … under fatigue − … investigation using neutrons − … liner cladding and H distribution • Advanced Systems (Advanced Nuclear Materials) − Spallation material investigations (from STIP) − … material flow using new sample preparation box and FIB − … example using atom probe tomography. M.A. Pouchon, NES Information Event, 24.10.2017, Page 19 / 26.

(20) STIP program – Materials in Spallation Target. Embrittlement of FM Steels (high He production) M.A. Pouchon, NES Information Event, 24.10.2017, Page 20 / 26.

(21) Analysis Tools – Connection Through FIB Spallation Materials. NPPs. Hot Cells. Hotlab Preparation box. Hotlab-FIB. nm Mechanical Testing. Microscopy / APT. μm - mm Beam Line Techniques. M.A. Pouchon, NES Information Event, 24.10.2017, Page 21 / 26.

(22) APT – Sample prep. lift out. Activity for a TEM sample: · 106 Bq. Pt pre-welding. Pre-tip. Sample Pt Pre-tip Sharpening Pt pre-welding. Pt welding Activity for APT sample: 1.4·10-3 Bq M.A. Pouchon, NES Information Event, 24.10.2017, Page 22 / 26.

(23) APT - Background. E ≈ 10...30. mass to charge ratio of the ions allows to determine their chemical nature. V nm. m t = 2 ⋅ e(VO + VP ) ⋅   n L t1. t2. 50000. 2. Number of atoms. electric field is induced at the apex of a tip. 40000. 57Fe2+. 20000 53Cr2+ 50Cr2+. 58Fe2+. 0 24. 25. 26. 27. Mass spectrum of Fe-Cr alloy +. 56Fe2+. 30000. 10000 +. 54Cr2+ 54Fe2+. 52Cr2+. 28. 29. 30. 30×30×100nm3. V 0 + VP. V0. few Mega atoms M.A. Pouchon, NES Information Event, 24.10.2017, Page 23 / 26.

(24) proton irradiation. APT Results - Example. Material: Fe-8Cr-2W-0.1C-0.2V-0.04Ta martensitic steel F82H Japanese reduced activation steel, fusion structural material, also candidate for GenIV Exposure: Irradiation in SINQ target (STIP II), to 20 dpa at 350°C CV>1at% CW>4at%. С-enriched clusters:. CCr>15at% 15×33×37 nm3. CTi>5at% 15×33×37 nm3. F82H, 20 dpa, 350°C. CC>2at%. С-enriched clusters:. • on the loops or in its neighborhood • (Cr, W, V, Ti and Fe) to C ratio ≈ 17 to 1, M18C carbide Chi (χ) -phase? • But: no data about such phases in F82H  radiation induced M.A. Pouchon, NES Information Event, 24.10.2017, Page 24 / 26.

(25) Wir schaffen Wissen – heute für morgen Nuclear Materials Research at PSI is active… … serving the authorities and industry with safety investigations. … helping the industry with performance optimizations. … contributing to education and training. … contributing to the next generation research..

(26) Wir schaffen Wissen – heute für morgen My thanks go to • All the members of LNM for their great efforts & performance • AHL / SU / NES / NUM • All external partners like ENSI, swissnuclear, CCEM, SNF, …. LNM & Friends.

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