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Superior radiation tolerance via reversible disordering–ordering transition of coherent superlattices

Nature Materials volume 22, pages 442–449 (2023)Cite this article

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Abstract

Materials capable of sustaining high radiation doses at a high temperature are required for next-generation fission and future fusion energy. To date, however, even the most promising structural materials cannot withstand the demanded radiation environment due to irreversible radiation-driven microstructure degradation. Here we report a counterintuitive strategy to achieve exceptionally high radiation tolerance at high temperatures by enabling reversible local disordering–ordering transition of the introduced superlattice nanoprecipitates in metallic materials. As particularly demonstrated in martensitic steel containing a high density of B2-ordered superlattices, no void swelling was detected even after ultrahigh-dose radiation damage at 400–600 °C. The reordering process of the low-misfit superlattices in highly supersaturated matrices occurs through the short-range reshuffling of radiation-induced point defects and excess solutes right after rapid, ballistic disordering. This dynamic process stabilizes the microstructure, continuously promotes in situ defect recombination and efficiently prevents the capillary-driven long-range diffusion process. The strategy can be readily applied into other materials and pave the pathway for developing materials with high radiation tolerance.

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Fig. 1: Superior radiation tolerance of superlattice steel containing high-density Ni(Al,Fe) NPs. Comparison of b and c shows that the superlattice steel exhibits much stronger void swelling resistance than 9Cr ODS steel.
Fig. 2: Microstructural evolution of superlattice steel under ion irradiation.
Fig. 3: Mechanism of radiation-induced dissolution of NPs in superlattice steel.
Fig. 4: Fast formation kinetics of NPs during thermal aging.
Fig. 5: Schematic of the disordering and reordering process of NPs in superlattice steel as a function of time.
Fig. 6: Application of current strategy in fcc Fe35.8Ni37.6Cr22.9Ti1.7Al2 (wt.%) MEA.

Data availability

Source data are provided with this paper. All other data needed to evaluate the conclusions in the paper are present in the paper or Supplementary Information.

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Acknowledgements

We sincerely thank S. J. Zinkle, L. Shao, F. A. Garner and F. Gao for the fruitful and valuable discussions. We also thank J. Zhang, Z. J. Zhou, T. D. Shen, K. Y. Yu, Y. Liu, S. Y. Hu, P. Wang, S. D. Yao, H. H. Zhu, J. M. Zhang, Z. M. Wu, Z. Y. Hu, Y. B. Zhao, Z. F. Wu, S.K. Shen and L. Y. Hao for help in the experiments. This work was supported by the National Magnetic Confinement Fusion Energy Research Project from the Ministry of Science and Technology of China (grant nos. 2019YFE03120003 (E.F.), 2018YFE0307100 (E.F.) and 2022YEF03030000 (J.D.)), the National Natural Science Foundation of China (NSFC) (grant nos. 11921006 (E.F.), 11975034 (E.F.), 11375018 (E.F.), 51921001 (Z.L.), 51671018 (S.J.), 11790293 (Z.L.), U20B2025 (Z.L.), U21B2082 (C.X.) and 51871016 (Y.W.)) and Beijing Municipal Natural Science Foundation (grant no. 1222023 (E.F.)). E.F. acknowledges support from the Science Fund for Creative Research Groups (NSFC), the Ion Beam Materials Laboratory (IBML) at Peking University and Collaborative Innovation Center of Quantum Matter at Peking University. Z.L. and S.J. acknowledge financial support from the 111 Project (B07003 (Z.L.)), the Fundamental Research Fund for the Central Universities of China (FRF-MP_20-43Z (S.J.) and National Postdoctoral Program for Innovative Talents (BX20180035 (S.J.)).

Author information

Author notes

  1. These authors contributed equally: Jinlong Du, Suihe Jiang, Peipei Cao.

Authors and Affiliations

  1. State Key Laboratory of Nuclear Physics and Technology, Department of Technical Physics, School of Physics, Peking University, Beijing, People’s Republic of China

    Jinlong Du, Chuan Xu, Huaqiang Chen & Engang Fu

  2. Beijing Advanced Innovation Centre for Materials Genome Engineering, State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing, People’s Republic of China

    Suihe Jiang, Peipei Cao, Yuan Wu & Zhaoping Lu

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  1. Jinlong Du
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Contributions

E.F. and Z.L. conceived and designed the research. J.D. and S.J. performed the main experiments and data analysis. P.C. prepared the MEA alloy and performed its APT data analysis. J.D. performed the TEM characterization. J.D. and C.X. performed the ion radiation experiments. S.J. performed the synchrotron characterization. With inputs from Y.W., J.D. and S.J. performed the APT experiments and carried out the analysis. J.D. and H.C. performed the calculation. J.D., S.J., E.F. and Z.L. wrote the manuscript with inputs from all the authors.

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Correspondence to Engang Fu or Zhaoping Lu.

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Extended data

Extended Data Fig. 1 STEM and APT characterization of the superlattice steel before radiation.

a, STEM micrograph. b, High-resolution HAADF-STEM micrograph of the steel specimen taken along the 001 zone axis. The contrast in the HAADF imaging originates from different atomic numbers (Z), and dark columns arise from the partitioning of Al atoms. c, Combined elemental mapping of the APT datasets. d, NPs highlighted by an isoconcentration surface encompassing regions containing more than 50 at% of Al and Ni combined.

Extended Data Fig. 2 Safe analysis region for the 6 MeV Au ion irradiation.

a, SRIM simulation (using the Kinchin-Pease method56,57) showing the radiation damage (dpa) profile and injected ion distribution along the ion penetration depth for 6 MeV Au3+ with a dose of 3×1017 cm−2. Inset is the corresponding cross-sectional HAADF-STEM image of the Au ion-irradiated superlattice steel. b, Energy dispersive X-ray spectrometer (EDS) profiles along radiation depth of the samples subjected to 84, 840 and 2350 dpa at 500 °C. The error bars are the standard deviation of the mean. c, Enlarged EDS profiles’ image labeled by violet dashed rectangle. d, The temperature-dependent void denuded zone near the surface and the injected ion-affected region for the 6 MeV Au ion-irradiated superlattice steel. Safe analysis region for void swelling is shown between two regions.

Source data

Extended Data Fig. 3 Cross-sectional TEM images of the superlattice steel subjected to 2350 dpa at a, 400 °C and b, 600 °C under different objective lens (OL) focus conditions.

No voids were observed in both cases. (a1, b1) Cross-sectional TEM images showing the radiation damage along the radiation depth. The investigated layer (200 ~ 320 nm) was indicated by two vertical dashed lines. (a2-a4) Cross-sectional TEM images of the investigated layer (200 ~ 320 nm deep) of the superlattice steel irradiated at 400 °C taken at a2, underfocus, a3, in focus, and a4 overfocus conditions. (b2-b4) Cross-sectional TEM images of the investigated layer (200 ~320 nm deep) in the superlattice steel irradiated at 600 °C taken at b2, underfocus, b3, in focus, and b4, overfocus conditions. The defocus distance is ±2 μm.

Extended Data Fig. 4 Cross-sectional HAADF-STEM images of the superlattice steel irradiated with different dpa at varied temperatures.

a, 84 dpa, 400 °C. b, 84 dpa, 500 °C. c, 420 dpa, 500 °C. d, 84 dpa, 600 °C. e-f, 84 dpa, 700 °C. g, 84 dpa, 400 °C. Insets are the corresponding SAED or FFT images. h, NPs density and diameter evolution versus radiation temperature up to 84 dpa. i, NPs density and diameter evolution versus radiation damage at 500 °C. j, Composition evolution of NPs versus radiation damage at 500 °C. The error bars represent the standard deviation of the mean.

Source data

Extended Data Fig. 5 APT characterization of the superlattice steel subjected to 840 dpa at 500 °C.

a, NP labeled by the red arrow in Fig. 2b, which is highlighted by the isoconcentration surface encompassing regions containing more than a 50 at.% combination of Al and Ni. b, Proximity histogram showing the composition change across the selected NPs, especially the Mo profile. c, The solute-enriched region labeled by the blue arrow in Fig. 2b, which is highlighted by the isoconcentration surface encompassing regions containing more than a 50 at.% combination of Al and Ni; Additionally, more than 23 at.% Al and 28 at.% Ni show an inhomogeneous distribution of Ni and Al in the solute-enriched regions. d, Proximity histogram showing the composition change across the selected solute-enriched regions, revealing the rejection of Mo atoms out of the precipitates and reformation of NPs inside the solute-enriched regions. The error bars represent the standard deviation of the mean.

Source data

Extended Data Fig. 6 Radiation-induced dissolution and thermally activated reprecipitation of NPs in the superlattice steel.

a, The number density of NPs versus radiation damage at room temperature (RT). b, Cross-sectional STEM image of the specimen subjected to 5 dpa at room temperature. The inset is the corresponding SAED pattern. c, Cross-sectional STEM image of the specimen irradiated to 5 dpa at room temperature followed by aging at 500 °C for 3 h. d, APT characterization of the superlattice steel irradiated to 5 dpa at room temperature. e, Proximity histogram showing the composition profiles across the selected nanopreccipitates shown in 40 at.% Ni+Al isosurface image (labeled by the red rectangular box). f, Proximity histogram showing the composition profiles across the selected nanoprecipitate shown in 40 at.% Ni+Al isosurface image (labeled by the blue rectangular box). The error bars are the standard deviation of the mean.

Source data

Extended Data Fig. 7 Room temperature radiation induced disordering of NPs in the superlattice steel and MEA.

a-f, APT characterization of the superlattice steel for a, As-prepared, b, 1 dpa, c, 2 dpa, and d, 5 dpa of the ion-irradiated sample followed by aging. The steel was radiated by Fe ion with doses of 1, 2 and 5 dpa at room temperature. The ion-irradiated steel with a dose of 5 dpa was aged at 500 °C for 3 h. e, The nearest neighbor distribution of Ni. f, The nearest neighbor distribution of Al. g-i. APT characterization of the designed MEA experienced 5 dpa radiation at room temperature, indicating fully dissolution of the L12-ordered phase. g, The tomographic reconstruction from one of the APT datasets, revealing complete dissolution of NPs after 5 dpa radiation at room temperature. h, The corresponding Ni elemental mapping. i, The nearest neighbor distribution of Ni, Ti and Al. The error bars are the standard deviation of the mean.

Source data

Extended Data Fig. 8 Structural motif effect of NPs for the disordering-ordering process.

a-c, Schematic figures showing the atomic structures of a, α-iron, b, B2-Ni:(Fe,Al), and c, L21-Fe2AlV. d-f, Evolution of L21 nanoprecipitation in Fe-12Cr4Al10V0.7Nb0.01B alloy before and after ion irradiation. d, As-prepared sample, showing the L21 NPs. e, Irradiated by Au ions up to 10 dpa at 500 °C, and SAED patterns show the dissolution of L21 NPs. f, Irradiated by Au ions up to 50 dpa at 600 °C, and SAED pattern shows the dissolution of L21 NPs, accompanied with formation of voids.

Extended Data Fig. 9 Mechanical properties, STEM characterizations and dynamic evolution of NPs of the superlattice steels with different Al contents and density of NPs.

a, Nanoindentation hardness evolution of the superlattice steels with different density of NPs as a function of radiation damage at 500 °C. The value without NPs is plotted by yellow dashed line and the line width indicates the corresponding error bar. Detailed description of the NPs in the superlattice steels with different NP density is provided in Supplementary Table S3. b, Nanoindentation hardness evolution of the superlattice steels and solution-annealed steel subjected to ion irradiation at 500 °C. c-e, STEM characterization of the 2Al superlattice steel with lower NPs density before and after ion irradiation; c, As-prepared. d, 84 dpa, 500 °C. e, 840 dpa, 500 °C. No NPs were observed in the ion-irradiated samples. f, Atomic resolved cross-sectional HAADF-STEM image of the steel with low NP density (that is, the 2Al steel) after 840 dpa ion irradiation at 500 °C. The inset is the corresponding FFT image showing weak spots of B2 structure. g, Inverse FFT image showing the B2 reordered regions (several are circled). h, Vickers hardness versus aging time revealing nanoprecipitation kinetics of the superlattice steels with different Al contents.The error bars are the standard deviation of the mean.

Source data

Extended Data Fig. 10 Microstructure of the 9Cr ODS steel.

a, SEM image of 9Cr ODS steel. b, STEM image of 9Cr ODS steel containing nanoparticles labeled by red arrows and EDS mappings of one typical nanoparticle, in which rich Y and Ti can be detected.

Supplementary information

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Du, J., Jiang, S., Cao, P. et al. Superior radiation tolerance via reversible disordering–ordering transition of coherent superlattices. Nat. Mater. 22, 442–449 (2023). https://doi.org/10.1038/s41563-022-01260-y

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