STRENGTH OF STEELS EXPOSED TO HEAVY LIQUID METALS
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1 IAEA INPRO COOL project Activity 6: Components for service in intimate contact with high temperature coolants (LM and MS) 6.1 Experimental study on components and various materials that are in contact during operation with LM and MS IMPROVING THE CORROSION RESISTANCE AND CREEP STRENGTH OF STEELS EXPOSED TO HEAVY LIQUID METALS BY SURFACE MODIFICATION USING PULSED E-BEAMS Adrian Jianu with the support of KIT-Program of Nuclear Safety Research and the KIT Campus Nord Institutes: INR, IKET, IHM, IMF III 1 A. Jianu IAEA COOL Project, May 2011
2 Overview of material compatibility with HLM Protective approache: surface modification/alloying by pulsed electron beam (GESA) Mechanical properties of materials exposed to HLM: creep-to-rupture experiments Conclusions 2 A. Jianu IAEA COOL Project, May 2011
3 Nuclear facilities cooled with liquid lead alloys Future GEN IV reactors Subcritical systems for transmutation Neutron source - spallation LEADER, ALFREDO - Pb, SVBR-100 PbBi EFIT, XT-ADS, MYRRHA Coolant + target: Pb, PbBi MEGAPIE Coolant +Target: Pb, PbBi 3 A. Jianu IAEA COOL Project, May 2011
4 Reference structural materials for HLM systems 9Cr ferritic/martensitic (FM) steel T91 for high loaded components (Heat, stress and irradiation) like spallation target and fuel cladding as alternative cladding from (15-15Ti) developed for fast Na cooled breeder alternative materialies for pumps Maxthal, SiSiC, Noriloy Austenitic steel AISI 316L for reactor vessel and components Targeted operation temperature for T91 and 316L : 200 C < T91, 316L < 550 C - at incidents shortly higher Flow velocity of coolant : < 2m/s; in pump region up to 10m/s 4 A. Jianu IAEA COOL Project, May 2011
5 Solubility in Pb [wt.%] oxide Materials compatibility problems in HLM Materials: F/M steels (T91-type), austenitic steels (316L-type) Problem: Dissolution of steel alloys (Fe<Cr<Ni) E-08 1E-10 1E-12 1E-14 1E-16 Solubility in Pb Temperature [ C] Ni Cr Fe Corrosion counter measure: Thin oxide scales as corrosion barrier! steel HLM + O Tasks: Precise oxygen control in HLM Investigation of corrosion / oxidation properties of steels Additional measures to minimize corrosion/oxidation rate (surface alloying by GESA process) 5 A. Jianu IAEA COOL Project, May 2011
6 Austenitic steel (316L-type) Temperature limits at optimal oxygen concentration 10-6 wt% 420 C / 4000 h 550 C / 4300 h 600 C / 4000 h 30µm 30µm 60µm onset of corrosion 500 C 550 C 600 C Austenitic steels operable without protection for temperatures below 500 C Above 500 C: severe dissolution of alloying elements (dissolution rate up to 1 µm/h) 6 A. Jianu IAEA COOL Project, May 2011
7 F/M steel (HCM12a -type) Temperature limits at optimal oxygen concentration 10-6 wt% oxide scale oxide scale LBE 500 C 10000h 550 C 10000h 600 C 2000h 30µm 30µm 30µm C 550 C 600 C 650 C onset of corrosion Oxidation F/M steels are operable below 550 C but Problematic is the huge oxidation rate: up to µm/ h and frequent spallation of oxide scale. contamination of liquid metal reduced heat removal capability (KM 3 O 4 1W/mK) 7 A. Jianu IAEA COOL Project, May 2011
8 Impact of oxidation and dissolution Austenitic steel F/M steel Temperature limits for: - Austenitic steels 316 type: 500 C 10000h start of dissolution attack - F/M steels up to 550 C - but severe oxidation Two main effects: - Structure integrity metal loss (dissolution & oxidation) - Reduced heat dissipation (oxidation): 10 µm of oxide scale (spinel or magnetite type) increase the inner clad temperature by 10K (Struwe, Pfrang) 8 A. Jianu IAEA COOL Project, May 2011
9 Overview of material compatibility with HLM Protective approache: surface modification/alloying by pulsed electron beam (GESA) Mechanical properties of materials exposed to HLM: creep-to-rupture experiments Conclusions 9 A. Jianu IAEA COOL Project, May 2011
10 Solution for corrosion and severe oxidation: thin protective surface layers Alumina as an example for protective slow growing oxide scales Al 2 O 3 layer Fe(Cr,Al)-phase Steel Oxide map of FeCrAl - oxide Requirements Corrosion resistant in HLM up to ca. 650 C Self healing of mechanically damaged layers No negative influence on mechanical properties Irradiation stability under relevant fluxes Coating / alloying process must be of industrial relevance. Alumina thermal conductivity: 400 C : 8-12 W/mK 500 C : 14 W/mK 10 A. Jianu IAEA COOL Project, May 2011
11 Corrosion barrier for T91 The procedure consists in two steps: - coating the steel surface with an Al-containing alloy layer - melting the coating layer and the steel surface layer using intense pulsed electron beam. LPPS=Low Pressure Plasma Spraying FeCrAlY coating The coating is porous, with variable thickness and reduced adherence to the substrate 11 A. Jianu IAEA COOL Project, May 2011
12 Surface alloying by pulsed E-beam (GESA) e - - beam LPPS FeCrAl coating cathode Volumetric Heating: rate: < 10 9 K/s time: < 40 µs Melt layer: depth: < 100 µm cooling: 10 7 K/s (heat conduction) restructured surface layer Substrate temperature remains relatively low no micro-structural changes observed The process is suitable for surface alloying by melting the material surface layer. Magnetic - coils anode target Electron beam Parameter: Electron Energy: 125 kev Power density : 2 MW/Cm² Pulse duration controllable: < 40 µs Beam diameter: ~ 4cm GESA I Treatable length ~ 32 cm GESA IV 12 A. Jianu IAEA COOL Project, May 2011
13 GESA IV 13 A. Jianu IAEA COOL Project, May 2011
14 FeCrAlY coating before and after GESA treatment As deposed After GESA treatment Re-melted layer 14 A. Jianu IAEA COOL Project, May 2011
15 Corrosion tests in stagnant HLM The COSTA facility is dedicated to investigate: COSTA - corrosion mechanisms, - influence of protective coatings on the corrosion behavior The program COSTA has been in continuous operation since COSTA stands are equipped with the Karlsruhe Oxygen Control System (OCS). 15 A. Jianu IAEA COOL Project, May 2011
16 Normalized Intensity T91+GESA after exposure to Pb-Bi at 550 C (10-6 wt.% oxygen) XPS Fe EDX m Cr Al m O Re-melted layer m m 16 A. Jianu IAEA COOL Project, May 2011 Al2O3 Outer scale of Al oxide No diffusion of Al into the bulk Thin stable oxide layer protects the T91 Al 2p Al3+ -O Al Energy (ev) 69
17 Background of the work Overview of material compatibility with HLM Protective approache: surface modification/alloying by pulsed electron beam (GESA) Mechanical properties of materials exposed to HLM: creep-to-rupture experiments Conclusions 17 A. Jianu IAEA COOL Project, May 2011
18 Creep-to-rupture tests in PbBi & Air Samples made out of T91 with and without GESA modification of Fe-Cr-Al coating T91 original T91 coated with Fe-Cr-Al-Y (LPPS) T91 + Fe-Cr-Al-Y + GESA treatment 18 A. Jianu IAEA COOL Project, May 2011
19 Comparison of creep-to-rupture tests on T91 in air and PbBi Strain and strain rate increase and time-to-rupture decreases: all creep stages are shorter for samples exposed in LBE 19 A. Jianu IAEA COOL Project, May 2011
20 Time-to-rupture of T91 samples tested in air and Pb-Bi at 550 C Decrease of time-to-rupture: -Oxide scale breaking and crack propagation -Liquid-metal-steel interaction at the crack tips -Dissolution of steel components 20 A. Jianu IAEA COOL Project, May 2011
21 Secondary creep rate of T91 tested in air and Pb-Bi at 550 C Stress [MPa] Ratio of 2 nd creep rates, LBE/air Pb-Bi penetration Strain rate up to a factor of 53 Strain rate depends on applied stress At low stress and low strain no oxide scale cracks no contact between steel and Pb-Bi no influence on the strain threshold stress 21 A. Jianu IAEA COOL Project, May 2011
22 The effect of protective coating on the creep behavior at 550 C Air 22 A. Jianu IAEA COOL Project, May 2011
23 The effect of protective coating on the creep behavior at 550 C After completion of these experiments a important improvement (comparing with original T91) can be seen. Surface modified samples using GESA process shown a decrease of creep strength (in Pb-Bi); however this is much lower comparing to original T91 2nd creep rate in Pb-Bi almost similar with original T91 in air Negative impact of Pb-Bi is reduced at 550 C 23 A. Jianu IAEA COOL Project, May 2011
24 T91+GESA creep tested in PbBi (200 MPa, 550 C) High Al- concentration Alumina Al-concentration < 2wt% Spinel und Magnetite Small cracks without Pb-Bi Cracks in magnetite and spinel, with Pb-Bi penetration Samples are not covered all over with alumina scale further optimization of GESA better results 24 A. Jianu IAEA COOL Project, May 2011
25 Conclusions The alloying of steel surface with aluminum using microsecond-pulsed intense electron beams was developed and optimized in order to be used for improving the corrosion resistance and creep strength of steels, exposed to liquid Pb and Pb-Bi-eutectic. The procedure consists in two steps: (i) coating the steel surface with an Al-containing alloy layer and (ii) melting the coating layer and the steel surface layer using intense pulsed electron beam. Using the mentioned procedure, the corrosion resistance and creep strength of the F/M 9Cr T91 steel, exposed to Pb and Pb-Bi-eutectic with different oxygen concentrations and under different temperatures, were considerably improved due to the formation of a thin alumina layer, whose thickness is lower than 1µm for all the tested temperatures and durations. This slowly growing alumina layer acts as an anti-corrosion barrier and is less susceptible to crack formation and therefore to lead alloy enhanced creep. First indications on the tolerable creep strain were evaluated. However, further detailed experiments would be required at higher operating temperatures, which are expected usually in pure Pb-cooled systems. 25 A. Jianu IAEA COOL Project, May 2011
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