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FTP/4-5Rb: LOW ACTIVATION VANADIUM ALLOYS FOR FUSION POWER REACTORS - THE RF RESULTS

This presentation discusses the RF results of using low activation vanadium alloys for fusion power reactors, including the R&D approaches, reactor tests, and future developments.

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FTP/4-5Rb: LOW ACTIVATION VANADIUM ALLOYS FOR FUSION POWER REACTORS - THE RF RESULTS

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  1. FEC-2012 USA, San-Diego, 9-13 October, 2012 9/18/2012 FTP/4-5Rb: LOW ACTIVATION VANADIUM ALLOYS FOR FUSION POWER REACTORS - THE RF RESULTS V.M.Chernov, M.M.Potapenko, V.A.Drobyshev, D.A.Blokhin, N.I.Budylkin, E.G.Mironova, I.E.Kostrovskaya, N.A.Degtyarev, I.N.Izmalkov, A.N.Tyumentsev, I.A.Ditenberg, K.V.Grinyaev, B.K.Kardashev, A.I.Blokhin, N.A.Demin, N.I.Loginov, V.A.Romanov, A.B.Sivak, P.A.Sivak, S.G.Psakhie, K.P.Zolnikov Bochvar High Technology Research Institute of Inorganic Materials (JSC “VNIINM”), Moscow, Russia, Tomsk State University, Tomsk, Russia, Ioffe Physical-Technical Institute, RAS, S.-Petersburg, Russia, Leypunsky Institute of Physics and Power Engineering, Obninsk, Russia, NRC “Kurchatov Institute”, Moscow, Russia , Institute of Physics Strength and Material Science, SB RAS, Tomsk, Russia

  2. Low Activation Structural Materials (LAMA-SMs) are the backbone of cores for all Fusion reactors (DEMO-FPP) and Fast Breeder reactors (FBR). Substantial improvement in the performance of LAMA-SMs can be rapidly achieved with R&D approaches using the RF nuclear way to the FBRs and the possibilities of the RF FBRs for the reactor tests of LAMA-SMs: under operation: BOR-60(Na), BN-600(Na), under construction: BN-800(Na), MBIR(Na), BN-1200(Na), BREST(Pb). The RF attention is currently focused on the LAMA-SMs: - (12-14)Cr RAFMS. RUSFER-EK-181 (Fe-12Cr-2W-V-Ta-B-C), - Vanadium alloys. V-4Ti-4Cr , V-Cr-W-Zr, V-Cr-Zr. The R&Ds and Technologies: LARGE HEATS AND ARTICLES, WIDENING OF THE TEMPERATURE-WINDOWS OF APPLICATIONS, INCREASING HEAT-STRENGTH-CORROSION-RADIATION RESISTANCES, OPTIMIZATION OF THE CHEMICAL COMPOSITIONS, MINIMIZATION OF TECHNOLOGICAL CONCENTRATIONS OF IMPURITIES, OPTIMIZATION OF THERMAL-MECHANICAL-CHEMICAL TREATMENTS, THEORY AND MODELLING OF DEFECTS AND PROPERTIES, INTERACTIONS WITH LIQUID METALS (Li, Na, Pb, Pb-Li), FBR BN-600 TESTS: doses 10-160 dpa-Fe, Tirr = (≈380 - 700) 0C.

  3. The RF Low Activation Vanadium Alloys for fusion and fission reactor applications (coolants Li, Na, Pb, Pb-Li). <2012: Referenced alloy V-4Ti-4Cr: Heats up to 110 kg. Any articles. Recommendations for the nuclear applications: <100 dpa-Fe, T-window (300)350 – 750(800) ºC. Applications: TBM DEMO in ITER, DEMO-FPP (Li, Pb-Li), FBRs: BN-1200(Na), MBIR(Na), BREST (Pb). The alloy V-4Ti-4Cr is the best alloy of the V-Ti-Cr system (USA, Japan, Russia). The alloy V-4Ti-4Cr is the real alternative to all types of ferritic-martensitic steels. It is possible mainly small structure modifications of the alloy V-4Ti-4Cr with small improvements of the functional properties of large articles via thermo-mechanical treatments and the improvements of the quality of the heats and articles (more impurity cleaning, more homogeneous, plates, multilayer tubes, welding). < 2020. Optimism up to 170 dpa-Fe, T-window < 300 – 850(900) ºC. Referenced V-4Ti-4Cr: Large heats (150-300 kg) and articles. Reactor tests: BN-600, 10-160 dpa-Fe, Tirr = 380ºC – 700 ºC. Corrosion tests (Li, Na, Pb, Pb-Li). Advanced alloys V-Cr-W-Zr-C-O: - optimizations of chemical compositions and regimes of thermal-mechanical-chemical treatments of heats and articles, higher the thermal stability of solid solutions, nanoparticles, substructures, grain boundaries, precipitation strengthening, - heats, articles and reactor properties.

  4. The RF vanadium alloys: V-4Ti-4Cr, V-Cr-W-Zr. Heats and articles (JSC “VNIINM”): <2014. V-4Ti-4Cr heats: 300 kg 2009-2011. V-4Ti-4Cr heats: 100-110 kg 2010-2011,V-Cr-W-Zr V-(4-9)Cr-(0.1-8)W-(1-2)Zr heats of 0.5-2 kg, welds (plates 2-6 mm) - platesup to 1930х367х15 mm, 1500х257х80mm,- tubesup to 67x6 mm

  5. VANADIUM ALLOYS - CHEMICAL COMPOSITIONS. MICROSTRUCTURES AND PROPERTIES AFTER DIFFERENT TMTs (NEXT SLIDES)

  6. Neutron spectrum, Radiation Damage, Activation, Cooling (ACDAM) 79.6 dpa-V/y (BN-600) 60.1 dpa-Fe/y (BN-600) 15.3 dpa-V/y (DEMO) 15.2 dpa-Fe/y (DEMO) V-4Ti-4Cr (VV1), V4Ti4Cr( noimpurities), Irradiation during 30-50 years NEUTRON FLUX (n/cm2/s, E > 0): DEMO: 9.00·1014 , BN-600: 6.50·1015 (BN-800:2.0x1016) , IFMIF: 6.71·1014 , GDT: 5.18·1014 , BOR-60: 3.00·1015, IVV-2M : 5.29·1014 V-4Ti-4Cr (VV1) Without impurities, V4Ti4Cr

  7. Alloy V-4Ti-4Cr(VV1) AND RAFMS RUSFER-EK-181. NUCLEAR ABSORPTION OF NEUTRONS (DEMO-RF and BN-600 ) Absorption of neutrons (%) for the nuclear generations of H and He and total neutron absorption (all nuclear reactions) under the neutron irradiation in DEMO-RF (neutron flux 9.0·1014 n/cm2/s) and BN-600 (neutron flux 6.5·1015n/cm2/s)

  8. ACDAM: H, He concentrations and H/DPA and He/DPA ratios for V-4Ti-4Cr (VV1) alloy irradiated in the BN-600 and DEMO reactors H DEMO He DEMO H/dpa DEMO He/dpa DEMO H BN-600 H/dpa BN-600 He BN-600 He/dpa BN-600 How to compare and to predict the degradations of the radiation properties via H, He and dpa formations ?

  9. VANADIUM ALLOYS: THE THERMAL-MECHANICAL-CHEMICAL TREATMENTS TO IMPROVE THEIR FUNCTIONAL PROPERTIES • The treatments allow to form the multiphase structure states with high degree of dispersity and thermal stability, to elevate the recrystallization temperature by (100–200) C, and to improve the low-high temperature strength characteristics of alloys with their high plasticity preserved. • 2. The promising way for developing radiation-proof vanadium alloys and improving their high-temperature strength and corrosion resistances iscontrollable interstitial alloying (C, N,O) followed by the treatments to produce structural states with highly homogeneous high-dispersion nonmetallic nanostructured phases and thermally stable multiphase and defect substructures (PRECIPITATION HARDENING VANADIUM ALLOYS).

  10. FEATURES OF VANADIUM ALLOYS WHICH ARE OF GREAT IMPORTANCE FOR THE FORMATION OF THE ALLOY MICROSTRUCTURE AND SERVICE PERFORMANCE • High chemical activity to interstitial impurities (O, C, N) resulting in saturation of alloys with these impurities during the production of ingots and articles and the subsequent thermo-mechanical (TMT) and chemico-thermal (CTT) treatments. • Low solubility of carbon. • Low activation energy of the diffusion of carbon and, as a consequence, high rate of formation of vanadium carbides. • As a result, even a rather low carbon concentration transforms vanadium alloys to the category of precipitation-hardening alloyswith a complex sequence of phase transformations, whose degree of dispersity and secondary phase distribution are highly sensitive to the parameters of the technological TMT-CTT cycles. • Minor variations in these parameters may strongly affect: • - the thermal stability of the microstructure of the alloys; • - the grain size; • the phase composition of grain boundaries; • the levels of heat-strength and heat-corrosion resistances; • - their propensity to low-temperature radiation embrittlement; • - other structure-sensitive properties of alloys.

  11. VANADIUM ALLOYS: TMT AND CTT.V-4Ti-4Cr, V-Cr-Zr-C, V-Cr-W-Zr-C: Promising ways to improve high-temperature strength-corrosion-radiation resistance are the methods of thermo-mechanical (TMT) and chemico-thermical (CTT) treatments using the combined methods of formation and modification of heterophase and defect substructures: 1. The uniform distribution of the stable phases nanoparticles during VXC → TiV (C, O, N) and VXC → ZrC transformations by changing (controlling) mechanism of such transformations – from “in situ transformation” to the mechanism of dissolution of VXC phase, followed by separation of fine carbides TiV (C, O, N) or ZrC from a supersaturated solid solution. 2. Microcrystalline structure under using of large plastic deformation in the intermediate stages of TMT and formation of defect substructures with high stored energy of deformation. 3. Ultra-fine particles of ZrO2 (CTT) in low-temperature diffusion alloying of oxygen (internal oxidation) which have a higher thermal stability and provide a significant (200 – 300 deg.) increase of the recrystallization temperature of alloys. 4. Structural states with both dispersed and substructure (by the elements of the dislocation, polygonal or microcrystalline structure) hardenings (TMT, CTT, TMT+CTT).

  12. VANADIUM ALLOYS: formation of stable phase particles with a high content of titanium or zirconium. 1. Formation of stable phase particles on the coarsemetastable vanadium carbide precipitates by substitution of vanadium by titanium or zirconium without dissolution of the initial metastable phase or with its partial dissolution – in situ transformation. TiV(C,N,O); ZrC jC CCDC jC CCDC jTi(Zr) CTi(Zr)DTi(Zr) The contribution of these mechanisms is determined by kinetic conditions of dissolution and precipitation, respectively, of stable and metastable phases – by the value of the kinetic parameter К = СcDc/CTi(Zr)DTi(Zr) V2C V2C 2. Dissolution of metastable vanadium carbides, followed by separation of the stable phase from a supersaturated solid solution and the formation of a spatially homogeneous distribution of fine particles of this phase. TiV(C,N,O); ZrC

  13. VANADIUM ALLOYS: THERMO-MECHANICAL (TMT) AND CHEMICO-THERMAL (CTT) TREATMENTS 0. TMT-0: as received plates, roads and tubes (JSC “VNIINM”). 1. TMT-I : TMT-0 + annealing at (1000 – 1100) ºC, (40 – 60) min (vac). 3. TMT-III : TMT-I + annealing 1400 ºC, 1h (vac) + 3 cycles “deformation 30 % at RT and annealing at 600 ºC, 1h (vac)” + 16 cycles with the changing of the deformation axis after each cycle “deformation 30 % at RT and annealing at 1000 ºC, 1 h (vac)”. 4. TMT-IV: TMT-I + annealing 1400 ºC (vac), 1h, + 3 cycles with the changing of the deformation axis after each cycle “deformation 30 % at RT and annealing at 600 ºC, 1 h (vac)” + 16 cycles with the changing of the deformation axis after each cycle “deformation 30 % at RT and annealing at 900 ºC, 1 h (vac)”. 2. TMT-II : TMT-I + annealing 1400 ºC (vac), 1h, + 3 cycles “deformation 30 – 50 % at RT, annealing at (600 – 700) ºC, 1h (vac)” + deformation (30-50) % at RT and annealing at (950 – 1100) ºC, 1h (vac). 5. CTT-I (Chemico-Thermal Treatment with oxygen saturation of the alloy): TMT-0 + annealing at ≈ 600 ºC, ≈1h (air, oxidation saturation) + annealing at (800 – 1200) ºC, (1 – 2) h (vac). Annealing time and temperature are depended from the final oxygen concentration in alloy. 6. CTT-II: TMT-II + CTT-I.

  14. VANADIUM ALLOYS V-4Ti-4Cr: TMT-III. THE TMT-III is based on the phenomenon of ultra-high technological plasticity of alloy that shows up in their high (practically unlimited) plastic strains at room temperature. Microstructure ofV-4Ti-4Cr alloy subjected toTMT III In the TMT case, under the conditions of high stored strain energy, a possibility arises to increase the recrystallization nucleus density and to reduce the grain size after TMT-III. After TMT-III the fine-crystal structures with less than 10-µm grain sizes are formed.

  15. VANADIUM ALLOYS: MULTI-DIRECTIONAL FORGE MOLDING AS A PROMISING METHOD OF ENHANCEMENT OF THEIR FUNCTIONAL PROPERTIES (TMT-III, TMT-IV).

  16. V-4Ti-4Cr: TMT-I, TMT-II.Fine particles of the second phase can show rather high thermal stability, strengthening the elements of the defect substructure andincrease the recrystallization temperature. The recrystallization temperature of an alloy can be over the temperature of the final stabilizing annealing at the ТMT-II. After the TMT-II, either polygonization of the alloy or the formation of structural states with high (about 1010 cm–2) density of chaotically distributed dislocations fixed by second phase particles is observed. 1 µm 1 µm 0.3 µm 1 µm 40 µm 40 µm TMT-II TMT-I

  17. Combined dispersion and substructure strengthening , % 30 Produced in Russia 0.2, MPa Produced in the USA 25 400 Produced in Japan 20 300 15  =90MPa 10 200  =160MPa 0 200 400 600 800 1000 Т, 0С 100 600 800 400 200 1000 Т, 0С V-4Ti-4Cr: TMT-I, TMT-II. An increase of volumetric content of finely dispersed (nano-) phases and suppression of recrystallization substantially increase the yield strength at Т = 20 – 1000 C. The maximum hardening is achieved in the temperature range, Т = 600 – 800 C, the gain in yield point after TMT-II reaches values of about ≈90MPa. TMT-I TMT-II TMT-II TMT-I The temperature dependence of the relative elongations after TMT-Iand TMT-II regimes A substantial increase in strength is achieved with a high margin of plasticity preserved after TMT-II regime

  18. c b a 2 µm ТМT-I 0.3 µm 1 µm 0.3 µm 0.3 µm ТМT-II d f e 1 µm V-4Ti-4Cr: TMT-I, TMT-II. MICROSTRUCTURES

  19. 0.5 μm 50μm 50μm 2.5 μm 20 μm 0.09 0.06 N/N Opticalmetallography Disorientation angles (degrees) 0.03 ТМT- I ТМT-III 0.00 60 20 40 0.15 N/N 0.10 Transmission electronmicroscopy Grain sizes, μm 0.05 ТМT-III ТМT-I 0.00 5 15 10 1 V-4Ti-4Cr: ТМT-I AND TMT-III. MICROSTRUCTURES AND GRAIN BOUNDARIES Electron backscatteringdiffraction ТМT-III:formation of high stored energy of deformation leads to an increase in the number of centers of nucleation of new grains and to a significant decrease of the grain sizes. The average grain size (EBSD-analysis) afterТМT-IIIis d  3–5 μm, which isan order lower than afterТМT-I (d  30–50 μm). ТМО III

  20. 150 nm 1000 nm V-4Ti-4Cr: TMT-IV. The formation of a high uniformity and dispersity of particles of the second phase, the control parameters of the polygonal substructure and the thermal stability of heterophase and defect substructure is essentially facilitated. ТМT-IV Particles of the second phase with sizes less than 10 nmwithelements ofpolygonal substructure, which are stable up to Т = 900С.

  21. ТМT-III ТМT-III ТМT-I ТМT-I 800С 20С V-4Ti-4Cr: TMT-I AND TMT-III. MECHANICAL PROPERTIES s, MPa s, MPa Structure and phase modifications (TMT-III) lead to a significant increase in the strength of the alloy in a wide temperature range (up to 800 ºC). The absolute value of hardening ( 100 MPa) is weakly dependent on temperature.

  22. V-4Ti-4Cr: TMT-I – TMT-IV. MECHANICAL PROPERTIES

  23. c b а 35 μm 35 μm 100 μm V-ALLOYS: TMT-I. MICROSTRUCTURE AND MECHANICAL PROPERTIES: V-4Ti-4Cr V-Cr-Zr-C V-Cr-W-Zr-C

  24. b a 120 μm СO  1.2 at. % СO  2.1 at. % 120 μm 35 μm 35 μm b a V-Alloys: TMT-II, CTT-I. RECRYSTALLIZATION. V-Cr-W-Zr V-Cr-Zr TMT-II. Collective recrystallization. CTT-I. Suppression of the collective recrystallization

  25. 200 μm 250μm 2 μm VANADIUM ALLOY: V-Cr-W-Zr. CTT-I. NANOPARTICLES ZrO2 (SIZES < 10 nm) CO 2.1 at. % NANOPARTICLES ZrO2 CO 2.1 at. %

  26. VANADIUM ALLOYS: V-Cr-Zr-C andV-Cr-W-Zr-C: TMT-I, CTT-I. Mechanical properties

  27. VANADIUM ALLOYS: V-Cr-Zr-C andV-Cr-W-Zr-C: TMT-I, CTT-II. Mechanical properties

  28. Vanadium-crystallite: THEORY AND MODELLING OF THE SELF DEFECTS (SIA-self interstitial atom, Vac-vacancy). CALCULATED AND EXPERIMENTAL RESULTS (SUMMARY) VANADIUM CRYSTAL MODEL (CONCEPTION): - vacancies migration takes place at stage III (170 – 200 K) of annealing of irradiated specimens with the activation energyEMVac =(0.45±0.05) eV; - the formation energy of vacancyEFVac =(2.6 ±0.2) eV; - free migration of SIAtakes place at stageIE of annealing(70–90 K) with the activation energyEMSIA =(0.19 ±0.03) eV; - the most probable stable SIA configuration is <110>-dumbbell.

  29. Vanadium-crystallite: THEORY AND MODELLING OF THE SELF DEFECTS. MOLECULAR STATICS AND DYNAMICS • Semi-empirical many-body interatomic interaction potential has been proposed (V.A. Romanov, 2012). • Self-point defects characteristics have been obtained by molecular statics and molecular dynamics methods: Vacancy: EFVac= 2.785 eV, EMVac= 0.423 eV, SIA: EFSIA = 3.165 eV, EMSIA = 0.168 eV. • SIA diffusion mechanism is mixed at temperatures above 550 K(1d–crowdion migration + 3d <110>-dumbbell migration). • Under lowering the temperature from the melting temperature (2188 K) to 300 K, the SIA effective migration energy increases from 0.1 to 0.2 eV. • 3d -<110>-dumbbell diffusion mechanism with the activation energy 0.2 eV dominates at temperatures below 550 K. • Stable <110>-dumbbell SIA configuration migration takes place at annealing stage IE(80 K). • Metastable <100>- and <111>-dumbbells can migrate at temperatures below 10 K with the activation energy < 0.02 eV.

  30. d =1 nm d =3.2 nm VANADIUM -CRYSTALLITE WITH INTERNAL STRUCTURE (GBs). 450 000 atoms,FS potential by M.I. Mendelev . MD simulation of atomic collision cascades, [320] EPKA = 1 keV Grain Boundary Σ13 Ideal structure t = 0.2 ps The end of the stage 1 GB Σ 13. The distance between PKA and GB = 1,81nm. Time dependence on the number of point defects n (τ). d - the distance from the PKA initial position to the GB EPKA = 1 keV ┴ to the GB

  31. VANADIUM CRYSTALLITE: THE INFLUENCE OF GRAIN BOUNDARIES ON THE CASCADE FORMATIONS The GB exerts the essential influence on the cascade evolution. The GB accumulates the considerable part of point defects. The large size clusters arise inside the GB area. Developmental character of the displacement cascades is determined in many respects by the presence of extensive interfaces in materials. The GB hinders the cascade propagation on its other side. The GB impenetrability depends from its type, PKA energy and distance between PKA and GB.

  32. VANADIUM ALLOYS: V-4Ti-4Cr, V-Cr-Zr-C and V-Cr-W-Zr-C Thermo-mechanical (TMT) and chemico-thermal (CTT) treatments: possibilities and prospects • For alloys there are promising effective new methods to improve their functional properties: • –radical modification of the heterophase structures (TMT-I – TMT-IV) for a significant increase of dispersity and uniformity of the spatial distribution of the particles of carbide phases; • –chemical thermal treatments (CTT-I - CTT-II)for disperse and substructure hardening. • 2. Hybrid methods that combine the different ways to modify the phase-structural state are promising: • – nanostructuring of heterophase structure by controlling mechanisms of VXC→TiV(C,O,N) orVXC→ZrCtransformations; • – formation of substructures with both disperse and substructure (by the elements of the dislocation, polygonal or microcrystalline structure) hardening.

  33. VANADIUM ALLOYS: Thermo-mechanical (TMT) and chemico-thermal (CTT) treatments: possibilities and prospects (cont.) • The CTT regimes for the alloys V-Cr-Zr-C and V-Cr-W-Zr-C are found. This treatment leads to a higher (compared to standard TMT-I regime) thermal stability of nanoparticles ZrO2, to increase of recrystallization temperature by 300 – 400 C and to more than twofold increase of yield stress in the range of high temperatures. • Optimizing the composition of alloys (V-4Ti-4Cr, V-Me-Zr-C) with carbidehardening and the TMT regimes can provide a range of operating temperatures of these alloys up to (700 – 800) ºC.The CTT regimes can be used to create products that operate at higher temperatures: (800 – 900) C. • High thermal stability of the microstructure of the alloys with internal oxidation indicates that CTT regimes to improve their long-term performance of high-temperature strength are promising.

  34. VANADIUM ALLOYS: BN-600 Tests (2012 – 2018): FBR BN-600: Neutron flux: 6.5·1015 n/cm2/s (E > 0), Primary damage: 60 dpa-Fe/year, 80 dpa-V/year. Irradiation start: 2015. Irradiation Time 592(1) + 196(2) = 888 (1+2) eff. days. Irradiation Temperature : 375 – 715 ºС ±(15 – 25) ºC. Doses: (1) 10–110 dpa-Fe (2015–2017, 592 ef.days), Results–2017-2018. (2) 15–160 dpa-Fe (2015–2018, ≈888 ef.days), Results–2018-2019. Environment: flowing and static sodium, static argon. Total number of specimens of various types is ≈ 280 (SSTT, pressure tubes). RADIATION PROPERTIES (Data Base): elastic and micro-plastic; mechanical;swelling; creep (pressure tubes); impact ductility;DBTT, crack-resistance; corrosion; structural and phase transformations.

  35. CONCLUSION: The RF Low Activation Vanadium Alloys for Nuclear Applications (coolants Li, Na, Pb, Pb-Li).Potential of recycling vanadium alloys can make structure waste manageable.VANADIUM ALLOYS ARE THE REAL ALTERNATIVE TO ALL TYPES OF RAFMS. <2012: Referenced alloy V-4Ti-4Cr: Heats up to 110 kg. Any articles. Recommendations for the nuclear applications: <100 dpa-Fe, T-window (300)350 – 750(800) ºC. Applications: TBM DEMO in ITER, DEMO-FPP (Li, Pb-Li), FBRs: BN-1200(Na), MBIR(Na), BREST (Pb). The alloy V-4Ti-4Cr is the best alloy of the V-Ti-Cr system (USA, Japan, Russia). The RF Knowledge Data Bases seem to be appropriate for the V-4Ti-4Cr alloy butfurther progress is anticipated for the advanced alloys of the system V-Cr-W-Zr-C-O. < 2020: OPTIMISM UP TO 170 dpa-Fe, T-window <300 – 850(900) ºC. REFERENCED V-4Ti-4Cr: Large heats (150-300 kg) and articles. Optimization (minimization) of the technological concentration of impurities. Reactor tests: BN-600, 10-160 dpa-Fe, Tirr = 380 ºC – 700 ºC. Corrosion tests (Li, Na, Pb, Pb-Li). ADVANCED V-Cr-W-Zr-C-O (heats up to 40 kg): - further optimizations of chemical compositions and regimes of thermal-mechanical-chemical treatments (TMT&CTT) of heats and articles, higher the thermal stability of solid solutions, nanoparticles, substructures and grain boundaries, - heats, articles and reactor properties. 36

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