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Alumina-forming stainless steels in liquid lead and lead-bismuth eutectic
KTH, School of Engineering Sciences in Chemistry, Biotechnology and Health (CBH), Chemistry, Surface and Corrosion Science. KTH, School of Engineering Sciences (SCI), Physics, Nuclear Science and Engineering.ORCID iD: 0000-0001-5645-5838
2024 (English)Doctoral thesis, comprehensive summary (Other academic)
Sustainable development
SDG 7: Affordable and clean energy
Abstract [en]

This work focuses on mechanical properties, susceptibility to liquid metal embrittlement (LME), and erosion-corrosion of alumina-forming steels using a Slow Strain rate testing rig (SSRT) and an Erosion Corrosion-rig (ECO) developed at KTH. The environments investigatedare liquid lead and lead-bismuth eutectic (LBE) intended for use in high-temperature energy applications such as generation IV nuclear power or fast nuclear reactors. The lead and LBEare intended to serve as a heat-transfer medium in the reactor. These higher temperature sand harsher environments put new demands on the construction materials used. The work has been mainly focused on mechanical testing using slow strain rate testing (SSRT) to evaluate susceptibility to LME. However, since other properties, such as oxidation, are intimately intertwined with the LME phenomenon, liquid metal corrosion and erosion are also part of this work. The tested materials include a ferritic FeCrAl steel designated EF100, three alumina-forming austenitic (AFA) steels and an alumina-forming martensitic (AFM) steel. The temperature range of the tests in liquid Pb was 340-600 °C and in LBE 140-600 °C with varying oxygen activities. Microstructure analyses were performed to underst and theunderlying mechanisms responsible for LME. The ferritic EF100 showed excellent performance in liquid Pb, exhibiting no signs of being affected by LME. However, in liquid LBE, it was severely affected by LME. The effects of Bi were investigated by stepwise additions of Bi to pure Pb, and signs of LME were observed already at 3-5 wt.% Bi. The AFM alloy suffered from severe LME in both liquid Pb and LBE, starting at the melting point of the liquid metal. The AFA alloys showed no signs of LME in either liquid Pb or LBE in the temperature range of 350-550 °C and 140-550 °C, respectively. However, above 570 °C, signs of LME were observed in all three alloys. Erosion-corrosion was found to have the largest impact on steels containing Ni (e.g., 316L and AFA 3), while the steels with a higher hardness and that were able to form a protective oxide scale remained largely unaffected (Kanthal AF, APMT, EF100, Alkrothal 14, coated 316L PC/DG, and AFM).

Abstract [sv]

Denna avhandling fokuserar på aluminiumoxidbildande ståls mekaniska egenskaper och deras påverkan av flytande metallförsprödning (LME) i smält bly och bly-vismut eutectiska (LBE) miljöer. Dessa smälta metaller är tänkta att kunnas användning som värmetransportertmedium inom högtemperatur- energiapplikationer så som generation IV kärnkraftsreaktorer. Dessa höga temperaturer och miljöer ställer nya krav på dekonstruktionsmaterial som ska användas. Avhandlingsarbetet har framför allt gått ut på att utvärdera de olika ståltypernas mekaniska egenskaper genom ”Slow strain rate testing” föratt utvärdera effekter av LME- påverkan. Eftersom även andra materialegenskaper spelar också stor roll för hur de de olika ståltyperna beter sig, är både oxidation och erosionskorrosion en del av detta arbete. De undersökta stålen inkluderade ett ferritiskt stål-EF100, tre olika typer av aluminiumoxidbildande autentiska stål-AFA, samt ett martensitiskt stål benämnt AFM. Dessa stål undersöktes inom temperaturintervallet 350-600 °C för blysamt 150-600 °C för LBE. Stålens mikrostrukturer analyserades för att öka förståelsen för de mekanismer som styr LME. Det ferritiska EF100-stålet visade inga tecken av att påverkas av LME i flytande Pb men var dock påverkat av LME in LBE. AFM-stålet betedde sig på ett liknande sätt som AF100-stålet men var påverkat av LME i både flytande Pb och LBE. AFA stålen påverkades varken av LME i Pb eller LBE men visade tecken på LME vid entemperatur av 570 °C. Omfattningen av erosions-korrosion undersöktes också vilken visade sig hastor påverkan hos stål innehållande nickel - Ni (316L och AFA3). Stål med en högre hårdhet och som bilade skyddande ytoxider påverkades väldigt lite (Kanthal AF, APMT, EF100,Alkrothal 14, aluminiumoxid belagd 316L, och AFM).

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2024. , p. 121
Series
TRITA-CBH-FOU ; 2024:61
Keywords [en]
Liquid metal embrittlement (LME), Liquid metal corrosion, Lead, Lead-bismuth eutectic (LBE), EF100, Alumina-forming austenitic steel, Alumina-forming ferritic/martensitic steel, Erosion-corrosion, ANSYS FLUENT modelling
Keywords [sv]
Nyckelord: Flytande metallförsprödning (LME), Flytande metallkorrosion, Bly, Bly-vismut eutektisk (LBE), EF100, Aluminiumoxidbildande austenitiskt stål, Aluminabildande ferritiskt/martensitiskt stål, Erosionskorrosion, ANSYS FLUENT modellering.
National Category
Metallurgy and Metallic Materials
Research subject
Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-356551ISBN: 978-91-8106-145-1 (print)OAI: oai:DiVA.org:kth-356551DiVA, id: diva2:1914011
Public defence
2024-12-20, F3, Lindstedtsvägen 26, via Zoom: https://kth-se.zoom.us/j/67833310452, Stockholm, 10:00 (English)
Opponent
Supervisors
Funder
Swedish Foundation for Strategic Research, Lindstedtsvägen 26
Note

QC 2024-11-19

Available from: 2024-11-19 Created: 2024-11-18 Last updated: 2024-12-17Bibliographically approved
List of papers
1. Slow strain rate testing of Fe-10Cr-4Al ferritic steel in liquid lead and lead-bismuth eutectic
Open this publication in new window or tab >>Slow strain rate testing of Fe-10Cr-4Al ferritic steel in liquid lead and lead-bismuth eutectic
2023 (English)In: Nuclear Materials and Energy, E-ISSN 2352-1791, Vol. 34, article id 101403Article in journal (Refereed) Published
Abstract [en]

The susceptibility of Fe-10Cr-4Al steel to liquid metal embrittlement (LME) in low oxygen liquid lead and lead-bismuth eutectic (LBE) environments has been investigated using a newly developed slow strain rate testing (SSRT) technique that can be employed at elevated temperatures. This study showed that the Fe-10Cr-4Al steel suffered embrittlement when exposed to LBE over a wide temperature range. The embrittlement, here measured as a reduction in fracture strain, was observed at the melting temperature of LBE and reached a maximum at approximately 375 degrees C. At temperatures above 425 degrees C, the material's ductility regained its original levels. The exposures in liquid lead showed no indications of embrittlement, but a ductile behavior over the entire tem-perature range studied (340-480 degrees C).

Place, publisher, year, edition, pages
Elsevier BV, 2023
Keywords
Liquid metal embrittlement (LME), Lead, Lead-bismuth eutectic (LBE), Fe-10Cr-4Al
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:kth:diva-328302 (URN)10.1016/j.nme.2023.101403 (DOI)000990107900001 ()2-s2.0-85149320816 (Scopus ID)
Note

QC 20231122

Available from: 2023-06-07 Created: 2023-06-07 Last updated: 2024-11-18Bibliographically approved
2. Negative effect of bismuth in lead on liquid metal embrittlement of a ferritic steel
Open this publication in new window or tab >>Negative effect of bismuth in lead on liquid metal embrittlement of a ferritic steel
2024 (English)In: Journal of Nuclear Materials, ISSN 0022-3115, E-ISSN 1873-4820, Vol. 588, article id 154829Article in journal (Refereed) Published
Abstract [en]

Liquid metal embrittlement (LME) of a Fe-10Cr-4Al ferritic steel was studied at 375 degrees C in liquid Pb-Bi alloys. Slow strain rate testing (SSRT) in low oxygen conditions was used to evaluate the ductility as a function of Bi concentration. It was found that susceptibility to LME increased strongly with the Bi concentration. The steel showed a reduction in its total strain to failure, which started at 3-5 wt.% Bi. The alloying elements (Fe, Cr, and Al) have a higher solubility in Bi than pure lead (Pb), so they are expected to dissolve more readily when Bi is added to the Pb. This is believed to be part of the explanation for the observed increase of LME. Lead with up to 3 wt.% Bi induced no LME in the studied corrosion resistance FeCrAl alloy.

Place, publisher, year, edition, pages
Elsevier BV, 2024
Keywords
Liquid metal embrittlement (LME), Lead, Lead-bismuth eutectic (LBE Fe-10Cr-4Al)
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:kth:diva-342290 (URN)10.1016/j.jnucmat.2023.154829 (DOI)001127691300001 ()2-s2.0-85182236696 (Scopus ID)
Note

QC 20240124

Available from: 2024-01-24 Created: 2024-01-24 Last updated: 2024-11-18Bibliographically approved
3. Influence of liquid lead and lead-bismuth eutectic on three alumina forming austenitic (AFA) steels through slow strain rate testing
Open this publication in new window or tab >>Influence of liquid lead and lead-bismuth eutectic on three alumina forming austenitic (AFA) steels through slow strain rate testing
2025 (English)In: Journal of Nuclear Materials, ISSN 0022-3115, E-ISSN 1873-4820, Vol. 603, article id 155415Article in journal (Refereed) Published
Abstract [en]

Liquid metal embrittlement (LME) in three newly developed alumina-forming austenitic (AFA) alloys, two 50 kg batches and one 5-ton heat, was studied in the temperature range 350–600 °C in liquid Pb and 140–600 °C in LBE using slow strain rate testing (SSRT) in a low-oxygen environment. No significant decrease in the engineering strain was observed in either environment. However, the presence of secondary cracks along the length of the specimen and brittle intergranular areas on the fracture surfaces indicates that the AFA alloys do show a minor degree of embrittlement above 570 °C. This appears to be related to grain boundary wetting by Pb/LBE. At temperatures below 570 °C, this wetting effect does not seem to be strong enough to induce LME in the alloys, and their ability to form a sufficiently protective oxide means that they remain unaffected by LME. The results indicate that the AFA alloy group can perform sufficiently well in liquid Pb/LBE environments, and long-term testing should be carried out to determine their viability as candidate materials for use in Pb- and LBE-based cooling systems.

Place, publisher, year, edition, pages
Elsevier BV, 2025
Keywords
Alumina forming austenitic steel, Lead, Lead-bismuth eutectic (LBE), Liquid metal embrittlement
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:kth:diva-354647 (URN)10.1016/j.jnucmat.2024.155415 (DOI)001329599300001 ()2-s2.0-85205268583 (Scopus ID)
Funder
Swedish Foundation for Strategic Research, Grant No. ARC19-0043
Note

QC 20241023

Available from: 2024-10-09 Created: 2024-10-09 Last updated: 2024-11-18Bibliographically approved
4. A combined modelling and experimental investigation of erosion-corrosion of chromia- and alumina-forming steels in liquid lead
Open this publication in new window or tab >>A combined modelling and experimental investigation of erosion-corrosion of chromia- and alumina-forming steels in liquid lead
2025 (English)Manuscript (preprint) (Other academic)
Abstract [en]

Erosion-corrosion experiments were carried out a chromia-forming steel (316L) alumina-forming ferritic, austenitic and martensitic steels and coated 316L at 480-520 °C in liquid lead. Testing was done under low oxygen conditions (10-7-10-8 wt.% O) for times up to 1392 hours using a purpose-built Erosion Corrosion rig (ECO). It was found that uncoated 316L suffered from Ni dissolution to a depth of 140 µm and severe erosion-corrosion attack. After coating with alumina oxide via Detonation Gun (DG) and Pack Cementation (PC) methods, the 316L remained unaffected. The commercial alumina forming alloys containing multiple reactive elements, Kanthal EF 100, Alkrothal 14 and Kanthal APMT, performed well and were minimally affected by erosion-corrosion. However, Kanthal AF, which contains only the single reactive element Y, lost a similar amount of mass as the 316L sample. The experimental alumina forming austenitic alloy denoted AFA 3 showed very poor resistance to erosion-corrosion, suffering from severe mass loss and with signs of Ni dissolution to a depth of 25 µm. The experimental alumina-forming martensitic steel, AFM, on the other hand, remained unaffected by erosion-corrosion. Hydrodynamic simulations were carried out using ANSYS FLUENT to determine the relative velocity between the HLM and the samples, calculating the highest velocity to be 9.9 m/s. It also demonstrated a good qualitative alignment between the experimental result and the simulations. This indicates that the erosion damage originated from a combination of the turbulence created inside the ECO-rig and particle erosion.

National Category
Materials Engineering
Research subject
Physics, Nuclear Engineering
Identifiers
urn:nbn:se:kth:diva-356548 (URN)
Funder
Swedish Foundation for Strategic Research, ARC19-0043
Note

Manuscript under review in Nuclear Materials and Energy

QC 20241118

Available from: 2024-11-18 Created: 2024-11-18 Last updated: 2024-11-18Bibliographically approved
5. Effects of Liquid metal embrittlement on an Alumina forming Martensitic steel
Open this publication in new window or tab >>Effects of Liquid metal embrittlement on an Alumina forming Martensitic steel
2025 (English)Manuscript (preprint) (Other academic)
Abstract [en]

Liquid metal embrittlement was observed in an alumina-forming martensitic (AFM) steel tested in both liquid Pb and lead-bismuth eutectic (LBE) in the temperature range 350-550 °C and 150-550 °C, respectively, using slow strain rate testing (SSRT) in a low oxygen environment ( ~10-11 wt.% O dissolved in Pb). A significant decrease in the total elongation to failure (TEF) could be observed in both environments, with LBE yielding the lowest measured TEF of 0.9% strain at 150 °C. The elongation to failure followed the classic pattern of a ductility dip, gradually recovering with increasing testing temperature so that fully ductile behaviour was restored at 550°C. There may be a potential to improve the performance of the AFM alloy by optimizing the microstructure through adjustments to the austenitizing, quenching and tempering conditions. 

National Category
Metallurgy and Metallic Materials
Research subject
Physics, Nuclear Engineering
Identifiers
urn:nbn:se:kth:diva-356549 (URN)
Funder
Swedish Foundation for Strategic Research, No. ARC19-0043
Note

Submitted version to Nuclar Matrials and Energy

QC 20241118

Available from: 2024-11-18 Created: 2024-11-18 Last updated: 2024-11-18Bibliographically approved

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