Response of 11B enriched ZrB2 ultra-high temperature ceramic to neutron irradiation at elevated temperatures

Lin, Yan-Ru; Koyanagi, Takaaki; Sprouster, David J.; Petrie, Christian M.; Fahrenholtz, William; Hilmas, Greg E.; Katoh, Yutai

doi:10.1016/j.actamat.2024.120111

Title: Response of ¹¹B enriched ZrB₂ ultra-high temperature ceramic to neutron irradiation at elevated temperatures

Journal Article · 13 June 2024 · Acta Materialia

DOI: https://doi.org/10.1016/j.actamat.2024.120111 · OSTI ID:2376345

^[1];

^[2];

^[1];

^[3];

^[1]

Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
State University of New York, Stony Brook, NY (United States)
Missouri University of Science and Technology, Rolla, MO (United States)

ZrB₂, an ultra-high temperature ceramic (UHTC) is being considered for use in fusion reactor first-wall structures, yet its response to irradiation remains poorly understood. This study employed scanning/transmission electron microscopy (S/TEM), synchrotron X-ray diffraction (XRD), finite element calculations, and thermal property measurements to thoroughly investigate the neutron-irradiation effects on ¹¹B-enriched ZrB₂. Neutron irradiations were conducted at 220 °C and 620 °C, with a neutron fluence of 2.2 × 10²⁵ neutron/m² (energy > 0.1 MeV), resulting in 3.9 dpa and 4200 appm He. The study revealed the unusual prevalence of prism loops and a > c anisotropic lattice swelling, likely linked to the low c/a ratio of ZrB₂, leading to grain boundary microcracking. Reducing the grain sizes was effective in reducing intergranular cracking and macroscopic swelling. The observation of cavities in ZrB₂ irradiated at 620 °C, as opposed to 220 °C, prompts questions about the temperature at which vacancies in ZrB₂ become mobile, and the role of neutron absorption by ¹⁰B in elevating irradiation temperatures. Isotopic enrichment in ¹¹B proves to be a viable strategy for mitigating helium production in transition-metal diborides, which is a critical consideration for nuclear applications. Irradiation-induced defects reduce the thermal diffusivity and conductivity of ZrB₂ by a factor of 4–9, which has important implications for its role as a plasma-facing material in fusion reactors that drive high heat fluxes through first-wall materials. Here, this comprehensive study lays the foundation for understanding ZrB₂ behavior under neutron irradiation and highlights important phenomena to consider for various material applications.

View Accepted Manuscript (DOE)

Cite

Export

Save

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Fusion Energy Sciences (FES); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: AC05-00OR22725; SC0018322; SC0012704

OSTI ID:: 2376345

Alternate ID(s):: OSTI ID: 2373286

Journal Information:: Acta Materialia, Journal Name: Acta Materialia Vol. 276; ISSN 1359-6454

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

References (71)

Effect of neutron irradiation on defect evolution in Ti3SiC2 and Ti2AlC Tallman, Darin J.; He, Lingfeng; Garcia-Diaz, Brenda L. Journal of Nuclear Materials, Vol. 468 https://doi.org/10.1016/j.jnucmat.2015.10.030	journal	January 2016
Infrastructure development for radioactive materials at the NSLS-II Sprouster, D. J.; Weidner, R.; Ghose, S. K. Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 880 https://doi.org/10.1016/j.nima.2017.10.053	journal	February 2018
Scratch-induced microplasticity and microcracking in zirconium diboride–silicon carbide composite Ghosh, Dipankar; Subhash, Ghatu; Radhakrishnan, Ramachandran Acta Materialia, Vol. 56, Issue 13 https://doi.org/10.1016/j.actamat.2008.02.038	journal	August 2008
Nature and thermal stability of radiation defects in single-crystal tungsten Bykov, V. N.; Birzhevoi, G. A.; Zakharova, M. I. Soviet Atomic Energy, Vol. 33, Issue 4 https://doi.org/10.1007/BF01666749	journal	October 1972
Structural integrity and damage of ZrB2 ceramics after 4 MeV Au ions irradiation Bao, Weichao; Robertson, Stuart; Zhao, Jia-Wei Journal of Materials Science & Technology, Vol. 72 https://doi.org/10.1016/j.jmst.2020.09.019	journal	May 2021
Evaluation of ultra-high temperature ceramics foraeropropulsion use Levine, Stanley R.; Opila, Elizabeth J.; Halbig, Michael C. Journal of the European Ceramic Society, Vol. 22, Issue 14-15 https://doi.org/10.1016/S0955-2219(02)00140-1	journal	January 2002
Materials for the plasma-facing components of fusion reactors Bolt, H.; Barabash, V.; Krauss, W. Journal of Nuclear Materials, Vol. 329-333 https://doi.org/10.1016/j.jnucmat.2004.04.005	journal	August 2004
Densification, mechanical and thermal properties of ZrC1− ceramics fabricated by two-step reactive hot pressing of ZrC and ZrH2 powders Wei, Boxin; Chen, Lei; Wang, Yujin Journal of the European Ceramic Society, Vol. 38, Issue 2 https://doi.org/10.1016/j.jeurceramsoc.2017.09.027	journal	February 2018
Temperature-dependent cavity swelling in dual-ion irradiated Fe and Fe-Cr ferritic alloys Lin, Yan-Ru; Bhattacharya, Arunodaya; Chen, Da Acta Materialia, Vol. 207 https://doi.org/10.1016/j.actamat.2021.116660	journal	April 2021
Thermal Properties of Hf-Doped ZrB ₂ Ceramics Lonergan, Jason M.; McClane, Devon L.; Fahrenholtz, William G. Journal of the American Ceramic Society, Vol. 98, Issue 9 https://doi.org/10.1111/jace.13717	journal	June 2015
Radiological analysis and transmutation calculation of representative castable nanostructured alloys Zhong, Weicheng; Tan, Lizhen Fusion Engineering and Design, Vol. 160 https://doi.org/10.1016/j.fusengdes.2020.111899	journal	November 2020
Neutron irradiation-induced microstructure damage in ultra-high temperature ceramic TiC Agarwal, S.; Koyanagi, T.; Bhattacharya, A. Acta Materialia, Vol. 186 https://doi.org/10.1016/j.actamat.2019.12.022	journal	March 2020
Separate effects irradiation testing of miniature fuel specimens Petrie, Christian M.; Burns, Joseph R.; Raftery, Alicia M. Journal of Nuclear Materials, Vol. 526 https://doi.org/10.1016/j.jnucmat.2019.151783	journal	December 2019
JANIS 4: An Improved Version of the NEA Java-based Nuclear Data Information System Soppera, N.; Bossant, M.; Dupont, E. Nuclear Data Sheets, Vol. 120 https://doi.org/10.1016/j.nds.2014.07.071	journal	June 2014
Grain boundary energy anisotropy: a review Rohrer, Gregory S. Journal of Materials Science, Vol. 46, Issue 18 https://doi.org/10.1007/s10853-011-5677-3	journal	September 2011
High temperature surface effects of He+ implantation in ICF fusion first wall materials Zenobia, Samuel J.; Radel, R. F.; Cipiti, B. B. Journal of Nuclear Materials, Vol. 389, Issue 2 https://doi.org/10.1016/j.jnucmat.2009.02.004	journal	May 2009
Swelling of ion-irradiated 3C–SiC characterized by synchrotron radiation based XRD and TEM Lin, Yan-Ru; Ho, Chun-Yu; Chuang, Wei-Tsung Journal of Nuclear Materials, Vol. 455, Issue 1-3 https://doi.org/10.1016/j.jnucmat.2014.06.061	journal	December 2014
Densification of ZrB2-based composites and their mechanical and physical properties: A review Guo, Shu-Qi Journal of the European Ceramic Society, Vol. 29, Issue 6 https://doi.org/10.1016/j.jeurceramsoc.2008.11.008	journal	April 2009
The EUROfusion materials property handbook for DEMO in-vessel components—Status and the challenge to improve confidence level for engineering data Gorley, Michael; Diegele, Eberhard; Gaganidze, Ermile Fusion Engineering and Design, Vol. 158 https://doi.org/10.1016/j.fusengdes.2020.111668	journal	September 2020
Part II: Experimental verification of computationally predicted preferential oxidation of refractory high entropy ultra-high temperature ceramics Backman, Lavina; Gild, Joshua; Luo, Jian Acta Materialia, Vol. 197 https://doi.org/10.1016/j.actamat.2020.07.004	journal	September 2020
Vacancy migration in high-temperature neutron-irradiated molybdenum Kulcinski, G. L.; Kissinger, H. E. Physica Status Solidi (a), Vol. 2, Issue 2 https://doi.org/10.1002/pssa.19700020212	journal	June 1970
Effect of neutron irradiation on select MAX phases Tallman, Darin J.; Hoffman, Elizabeth N.; Caspi, El’ad N. Acta Materialia, Vol. 85 https://doi.org/10.1016/j.actamat.2014.10.068	journal	February 2015
Nuclear Applications for Ultra-High Temperature Ceramics and MAX Phases Lee, William E.; Giorgi, Edoardo; Harrison, Robert Ultra‐High Temperature Ceramics: Materials for Extreme Environment Applications https://doi.org/10.1002/9781118700853.ch15	book	October 2014
Neutron irradiation damage in MgO, Al2O3 and MgAl2O4 ceramics Clinard, F. W.; Hurley, G. F.; Hobbs, L. W. Journal of Nuclear Materials, Vol. 108-109 https://doi.org/10.1016/0022-3115(82)90538-4	journal	July 1982
Designing Radiation Resistance in Materials for Fusion Energy Zinkle, S. J.; Snead, L. L. Annual Review of Materials Research, Vol. 44, Issue 1 https://doi.org/10.1146/annurev-matsci-070813-113627	journal	July 2014
Structural Tolerance of Zirconium Diboride under Electron Irradiation through in-situ Convergent Beam Electron Diffraction and Energy-dispersive X-ray Spectroscopy Lan, Yucheng; Farrell, Grace; Merritt, Mia Microscopy and Microanalysis, Vol. 29, Issue Supplement_1 https://doi.org/10.1093/micmic/ozad067.784	journal	July 2023
Limits on irradiation-induced thermal conductivity and electrical resistivity in silicon carbide materials Snead, L. L. Journal of Nuclear Materials, Vol. 329-333 https://doi.org/10.1016/j.jnucmat.2004.04.294	journal	August 2004
Handbook of SiC properties for fuel performance modeling Snead, Lance L.; Nozawa, Takashi; Katoh, Yutai Journal of Nuclear Materials, Vol. 371, Issue 1-3 https://doi.org/10.1016/j.jnucmat.2007.05.016	journal	September 2007
Comparative Assessment of Material Performance in DEMO Fusion Reactors Gilbert, M. R.; Zheng, S.; Kemp, R. Fusion Science and Technology, Vol. 66, Issue 1 https://doi.org/10.13182/FST13-751	journal	August 2014
Thermal and electrical transport in ZrB2-SiC-WC ceramics up to 1800 °C Ma, Hai-Bin; Zou, Ji; Zhu, Jing-Ting Acta Materialia, Vol. 129 https://doi.org/10.1016/j.actamat.2017.02.052	journal	May 2017
ENDF/B-VII.1 Nuclear Data for Science and Technology: Cross Sections, Covariances, Fission Product Yields and Decay Data Chadwick, M. B.; Herman, M.; Obložinský, P. Nuclear Data Sheets, Vol. 112, Issue 12 https://doi.org/10.1016/j.nds.2011.11.002	journal	December 2011
Thickness measurements with electron energy loss spectroscopy Iakoubovskii, K.; Mitsuishi, K.; Nakayama, Y. Microscopy Research and Technique, Vol. 71, Issue 8 https://doi.org/10.1002/jemt.20597	journal	August 2008
Thermal conductivity degradation of ceramic materials due to low temperature, low dose neutron irradiation Snead, L. L.; Zinkle, S. J.; White, D. P. Journal of Nuclear Materials, Vol. 340, Issue 2-3 https://doi.org/10.1016/j.jnucmat.2004.11.009	journal	April 2005
Mechanisms of irradiation-induced growth and cracking in beryllia Clarke, F. J. P.; Wilks, R. S.; Bowen, D. H. Journal of Nuclear Materials, Vol. 14 https://doi.org/10.1016/0022-3115(64)90179-5	journal	January 1964
Residual strain and the fracture stress-grain size relationship in brittle solids Clarke, F. J. P. Acta Metallurgica, Vol. 12, Issue 2 https://doi.org/10.1016/0001-6160(64)90181-6	journal	February 1964
Neutron cross sections of the boron isotopes for energies between 10 and 500 keV Mooring, F. P.; Monahan, J. E.; Huddleston, C. M. Nuclear Physics, Vol. 82, Issue 1 https://doi.org/10.1016/0029-5582(66)90520-7	journal	July 1966
Swelling of SiC at intermediate and high irradiation temperatures Snead, L. L.; Katoh, Y.; Connery, S. Journal of Nuclear Materials, Vol. 367-370 https://doi.org/10.1016/j.jnucmat.2007.03.097	journal	August 2007
In situ study on enhanced heavy ion irradiation tolerance of porous Mg Li, Jin; Chen, Y.; Wang, H. Scripta Materialia, Vol. 144 https://doi.org/10.1016/j.scriptamat.2017.09.018	journal	February 2018
Thermal Conductivity of ZrB₂ and HfB₂ Harrington, Gregory J. K.; Hilmas, Greg E. Ultra‐High Temperature Ceramics: Materials for Extreme Environment Applications https://doi.org/10.1002/9781118700853.ch9	other	October 2014
Evaluation of the continuous dilatometer method of silicon carbide thermometry for passive irradiation temperature determination Field, Kevin G.; McDuffee, Joel L.; Geringer, Josina W. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, Vol. 445 https://doi.org/10.1016/j.nimb.2019.02.022	journal	April 2019
High temperature ion irradiation effects in MAX phase ceramics Clark, D. W.; Zinkle, S. J.; Patel, M. K. Acta Materialia, Vol. 105 https://doi.org/10.1016/j.actamat.2015.11.055	journal	February 2016
Nano-scale microstructure damage by neutron irradiations in a novel Boron-11 enriched TiB2 ultra-high temperature ceramic Bhattacharya, A.; Parish, C. M.; Koyanagi, T. Acta Materialia, Vol. 165 https://doi.org/10.1016/j.actamat.2018.11.030	journal	February 2019
High-resolution electron microscopy of neutron-irradiation-induced dislocations in SiC Yano, Toyohiko; Iseki, Takayoshi Philosophical Magazine A, Vol. 62, Issue 4 https://doi.org/10.1080/01418619008244788	journal	October 1990
Fracturing of borides under neutron irradiation Grinik, E. U.; Ogorodnikov, V. V.; Krainy, A. G. Journal of Nuclear Materials, Vol. 233-237 https://doi.org/10.1016/S0022-3115(96)00293-0	journal	October 1996
The response of ZrB2 to simulated plasma-facing material conditions of He irradiation at high temperature Garrison, Lauren M.; Kulcinski, Gerald L.; Hilmas, Greg Journal of Nuclear Materials, Vol. 507 https://doi.org/10.1016/j.jnucmat.2018.04.016	journal	August 2018
Microstructure of Al2O3 and MgAl2O4 preimplanted with H, He, C and irradiated with Ar+ ions Yamada, Reiji; Zinkle, Steven J.; Philip Pells, G. Journal of Nuclear Materials, Vol. 209, Issue 2 https://doi.org/10.1016/0022-3115(94)90295-X	journal	April 1994
Thermophysical Properties of ZrB ₂ and ZrB ₂ –SiC Ceramics Zimmermann, James W.; Hilmas, Gregory E.; Fahrenholtz, William G. Journal of the American Ceramic Society, Vol. 91, Issue 5 https://doi.org/10.1111/j.1551-2916.2008.02268.x	journal	May 2008
Ultra-high temperature ceramics: Materials for extreme environments Fahrenholtz, William G.; Hilmas, Greg E. Scripta Materialia, Vol. 129 https://doi.org/10.1016/j.scriptamat.2016.10.018	journal	March 2017
Effects of fast neutron irradiation on zirconium carbide Snead, Lance L.; Katoh, Yutai; Kondo, Sosuke Journal of Nuclear Materials, Vol. 399, Issue 2-3 https://doi.org/10.1016/j.jnucmat.2010.01.020	journal	April 2010
Pushing the limits of atomistic simulations towards ultra-high temperature: A machine-learning force field for ZrB2 Zhang, Yanhui; Lunghi, Alessandro; Sanvito, Stefano Acta Materialia, Vol. 186 https://doi.org/10.1016/j.actamat.2019.12.060	journal	March 2020
A new type of defect on {1120} planes in ß-Si ₃ N ₄ produced by neutron irradiation Akiyoshi, Masafumi; Yano, Toyohiko Philosophical Magazine Letters, Vol. 81, Issue 4 https://doi.org/10.1080/09500830010024657	journal	April 2001
Refractory Diborides of Zirconium and Hafnium Fahrenholtz, William G.; Hilmas, Gregory E.; Talmy, Inna G. Journal of the American Ceramic Society, Vol. 90, Issue 5 https://doi.org/10.1111/j.1551-2916.2007.01583.x	journal	May 2007
Microstructure evolution in h.c.p. metals during irradiation Griffiths, M. Philosophical Magazine A, Vol. 63, Issue 5 https://doi.org/10.1080/01418619108213917	journal	May 1991
Experimental design and analysis for irradiation of SiC/SiC composite tubes under a prototypic high heat flux Petrie, Christian M.; Koyanagi, Takaaki; McDuffee, Joel L. Journal of Nuclear Materials, Vol. 491 https://doi.org/10.1016/j.jnucmat.2017.04.058	journal	August 2017
Bubble formation in helium-implanted nanostructured ferritic alloys at elevated temperatures Lin, Yan-Ru; Chen, Wei-Ying; Tan, Lizhen Acta Materialia, Vol. 217 https://doi.org/10.1016/j.actamat.2021.117165	journal	September 2021
Microstructure of Al2O3 and MgAl2O4 irradiated at low temperatures Zinkle, S. J.; Pells, G. P. Journal of Nuclear Materials, Vol. 253, Issue 1-3 https://doi.org/10.1016/S0022-3115(97)00323-1	journal	March 1998
Material property requirements for analysis and design of UHTC components in hypersonic applications Squire, Thomas H.; Marschall, Jochen Journal of the European Ceramic Society, Vol. 30, Issue 11 https://doi.org/10.1016/j.jeurceramsoc.2010.01.026	journal	August 2010
Evolution of microstructure in hcp metals during irradiation Griffiths, M. Journal of Nuclear Materials, Vol. 205 https://doi.org/10.1016/0022-3115(93)90085-D	journal	October 1993
Thermal conductivity degradation induced by point defects in irradiated silicon carbide Crocombette, Jean-Paul; Proville, Laurent Applied Physics Letters, Vol. 98, Issue 19 https://doi.org/10.1063/1.3589358	journal	May 2011
The effect of helium on cavity swelling in dual-ion irradiated Fe and Fe-10Cr ferritic alloys Lin, Yan-Ru; Bhattacharya, Arunodaya; Zinkle, Steven J. Journal of Nuclear Materials, Vol. 569 https://doi.org/10.1016/j.jnucmat.2022.153907	journal	October 2022
Defect clustering and self-healing of electron-irradiated boron-rich solids Carrard, M.; Emin, D.; Zuppiroli, L. Physical Review B, Vol. 51, Issue 17 https://doi.org/10.1103/PhysRevB.51.11270	journal	May 1995
A comparative study of low energy radiation responses of SiC, TiC and ZrC Jiang, M.; Xiao, H. Y.; Zhang, H. B. Acta Materialia, Vol. 110 https://doi.org/10.1016/j.actamat.2016.03.011	journal	May 2016
Helium induced microstructure damage, nano-scale grain formation and helium retention behaviour of ZrC Agarwal, Shradha; Bhattacharya, Arunodaya; Trocellier, Patrick Acta Materialia, Vol. 163 https://doi.org/10.1016/j.actamat.2018.09.062	journal	January 2019
Methods for Processing ENDF/B-VII with NJOY MacFarlane, R. E.; Kahler, A. C. Nuclear Data Sheets, Vol. 111, Issue 12 https://doi.org/10.1016/j.nds.2010.11.001	journal	December 2010
Transmission electron microscope studies of neutron irradiated beryllium oxide Rau, R. C. Journal of Nuclear Materials, Vol. 20, Issue 2 https://doi.org/10.1016/0022-3115(66)90002-X	journal	August 1966
Solute segregation in metals under irradiation Johnson, Robert A.; Lam, Nghi Q. Physical Review B, Vol. 13, Issue 10 https://doi.org/10.1103/PhysRevB.13.4364	journal	May 1976
An F82H steel pressurized tube creep capsule for irradiation in HFIR Mulligan, Padhraic L.; Sakasegawa, Hideo; Tanigawa, Hiroyasu Nuclear Materials and Energy, Vol. 15 https://doi.org/10.1016/j.nme.2018.05.011	journal	May 2018
Design, Preparation and Properties of Carbon Fiber Reinforced Ultra-High Temperature Ceramic Composites for Aerospace Applications: A Review Tang, Sufang; Hu, Chenglong Journal of Materials Science & Technology, Vol. 33, Issue 2 https://doi.org/10.1016/j.jmst.2016.08.004	journal	February 2017
Neutron Sources Kumada, H. Comprehensive Biomedical Physics, Vol. 8, p. 197-217 https://doi.org/10.1016/B978-0-444-53632-7.00613-4	book	August 2014
Limiters for DEMO wall protection: Initial design concepts & technology options You, J. H.; Bachmann, C.; Belardi, V. G. Fusion Engineering and Design, Vol. 174 https://doi.org/10.1016/j.fusengdes.2021.112988	journal	January 2022
Response of isotopically tailored titanium diboride to neutron irradiation Koyanagi, Takaaki; Katoh, Yutai; Ang, Caen Journal of the American Ceramic Society, Vol. 102, Issue 1 https://doi.org/10.1111/jace.16036	journal	September 2018

Similar Records

Effects of thermal annealing and ion irradiation on the microstructures of HT-9 ferritic steel

Thesis/Dissertation · 1986 · OSTI ID:7131331

Kai, J J

Structural Tolerance of Zirconium Diboride under Electron Irradiation through in-situ Convergent Beam Electron Diffraction and Energy-dispersive X-ray Spectroscopy

Journal Article · 2023 · Microscopy and Microanalysis · OSTI ID:1992012

Lan, Yucheng; Farrell, Grace; Merritt, Mia; +3 more

Temperature and fluence limits for a type 316 stainless-steel controlled thermonuclear reactor first wall

Journal Article · 1976 · Nucl. Technol.; (United States) · OSTI ID:7142779

Bloom, E E; Wiffen, F W; Maziasz, P J; +1 more

Related Subjects

36 MATERIALS SCIENCE
Ultra-high temperature ceramic (UHTC)
Intergranular fracture
synchrotron X-ray diffraction
Scanning/transmission electron microscopy
Radiation effects
Helium effects

Title: Response of 11B enriched ZrB2 ultra-high temperature ceramic to neutron irradiation at elevated temperatures

Citation Formats

References (71)

Similar Records

Related Subjects

Title: Response of ¹¹B enriched ZrB₂ ultra-high temperature ceramic to neutron irradiation at elevated temperatures