RADIATION RESISTANT HIGH ENTROPY ALLOYS FOR FAST REACTOR CLADDING APPLICATIONS

Lead Research Organisation: University of Oxford
Department Name: Materials

Abstract

High entropy alloys are a recently developed novel class of materials in which no one element dominates. Instead four or more elements are used in near equal proportions. These alloys have been reported to have a wide range of attractive properties including high strengths at high temperatures, good corrosion resistance and ability to withstand irradiation damage. These properties make HEAs strong candidate materials for use as fuel cladding in sodium cooled fast reactors. These reactors can operate at higher temperatures, using less fuel and are safer than current water and gas cooled reactors.

However if HEAs are to be utilised in this highly aggressive environment there are two key needs that must be addressed. The first is to identify promising alloy compositions, manufacture them and characterise their mechanical behaviour. Secondly the mechanisms that lead to the excellent resistance to irradiation damage need to be understood. Through this we will establish whether the irradiation response is universal to all HEAs and devise strategies to predict other potentially better systems to investigate. This grant will use ion irradiations rather than neutrons as ion irradiations are cheaper and faster to carry out and allow for more rapid turn around in alloy development. How the structure of the alloys is changed by irradiation will be studied using advanced microscopy methods and the effect the irradiation has on the mechanical behaviour will be studied using novel micro-mechanical testing methods. Importantly these methods can be used to measure mechanical behaviour at temperatures over 900oC, so the mechanical properties at the operational temperature can be studied in both irradiated and unirradiated conditions.
Once the most promising alloys, with the best resistance to irradiation damage, have been identified their resistance to liquid sodium corrosion will be studied. In this way we will develop a novel alloy which can be used as fuel cladding in sodium cooled fast reactors.

Planned Impact

Sodium cooled fast reactor are a proven nuclear fission reactor design which are a leading candidate for the next generation of nuclear reactors (so called GEN IV). These reactors will be more efficient and safer than the current gas or water cooled systems. However they are currently held back by a lack of suitable materials to use as fuel cladding. Zirconium cannot be used as the operational temperatures are too high. Steels have been used in several test systems. However they suffer from swelling under irradiation and a decrease in mechanical properties after irradiation and exposure to liquid sodium. High entropy alloys are a series of novel systems where no single element dominates as is the case in traditional alloys. Instead 4 or more elements are used in near equal amounts. Recent preliminary work has shown they alloys can be almost immune to the irradiation damage which severally degrades conventional alloys. This grant will accelerate the development of high entropy alloys and assess their ability to act under the extreme environments envisaged for a sodium cooled fast reactor. This development of safer nuclear reactors will allow the further deployment of nuclear power plants in an effort to reduce greenhouse gas emissions, and minimise the effect of climate change. This will have a positive impact of the well being of the global population.
Within the UK, high entropy alloys are of interest to a wide range of end users across the nuclear, aerospace and automotive industries. In particular the Culham Centre For Fusion Energy is interested in using HEAs as structural materials in future nuclear fusion devices and Rolls Royce are studying them for potential jet turbine applications. These are groups we already have good links with and we will disseminate our key finding directly to them, through our regular meetings as well as larger public workshops. In this way we aim to find synergistic links across industries and accelerate alloy design in this nascent area of research.
We will work with Oxford University Innovation, the University of Oxford's Technology Transfer Department, to exploit any commercial potential of our research. The testing techniques and modelling methodologies developed for high temperature micro-mechanical testing of irradiated materials are of interest to leading UK companies such as NNL for validating life extensions of nuclear reactors, EdF who are leading the current new build at Hinkley point and SME's such as Tokamak Energy who are developing compact nuclear fusion reactors. These are companies who are already involved in supporting research into nuclear materials and systems at Oxford University and we will invite them or their representatives to our open meetings to ensure they are exposed to the latest techniques we are develop (see "academic beneficiaries" section)

Publications

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Carruthers A (2021) Novel reduced-activation TiVCrFe based high entropy alloys in Journal of Alloys and Compounds

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Pickering EJ (2021) High-Entropy Alloys for Advanced Nuclear Applications. in Entropy (Basel, Switzerland)

 
Description new HEA compositions - several of which should not be pursued further
Exploitation Route People should not study the poorer alloy compositions. We are now working to get neutron irradiation time for the better alloys.
Sectors Aerospace

Defence and Marine

 
Description HEAs are being used in irradiation campaign for joint USA UK project
First Year Of Impact 2024
Sector Energy
 
Title Research data for: Origin of age softening in the refractory high-entropy alloys 
Description This dataset contains the raw data used in the study on the "Origin of Age Softening in Refractory High-Entropy Alloys". It includes the 3D FIB/SEM dataset, nanoindentation datasets, Correlative SEM/EDX/EBSD dataset, APT dataset, STEM-EDX datasets, STEM-EELS dataset, and the TKD dataset.Description of the data and file structureThe raw data were collected using a series of advanced microscopy techniques and a nanoindenter from Ti-V-Nb-Ta high-entropy alloys. Details on the materials and the data acquisition parameters can be found in the paper "Origin of Age Softening in Refractory High-Entropy Alloys" by J. Liu et al. in Science Advances.Datasets include: 1. '3D FIB-SEM'Image stack.raw: This is a stack of two-dimensional scanning electron microscopy (SEM) images acquired by serially sectionning using a focused ion beam (FIB). The data can be accessed using commercial software Avizo or the open-source ImageJ software.Voxel size.txt: This file includes the voxel size information for the image stack.2. 'Nanoindentation' This folder contains the raw nanoindentation datasets from the four samples studied in the research. NanoSuite was used to extract the values of modulus and hardness.TiVNbTa_Wisc_700C_1day.mss: Nanoindentation data from the TiVNbTa sample after 1-day aging at 700°C.TiVNbTa_Wisc_700C_5days.mss: Nanoindentation data from the TiVNbTa sample after 5 days of aging at 700°C.TiVNbTa_Wisc_700C_40days.mss: Nanoindentation data from the TiVNbTa sample after 40 days of aging at 700°C.TiVNbTa_Wisc_homogenised.mss: Nanoindentation data from the homogenized TiVNbTa sample.3. 'APT' This folder contains the raw atom probe tomography (APT) data used to analyze the chemical composition at atomic resolution from the selected samples in the study. AP Suite was used to analyze and visualize the datasets.#1.HITS: Raw atom probe tomography data from the matrix of the Ti-V-Nb-Ta sample after 1-day aging at 700°C.#2.HITS to #6.HITS: Additional raw atom probe tomography datasets following the same description as #1.HITS.#7.HITS and #8.HITS: Raw atom probe tomography data from the matrix of the Ti-V-Nb-Ta sample after 40-day aging at 700°C.Precipitate.HITS: Raw atom probe tomography data containing a precipitate in the Ti-V-Nb-Ta sample after 40-day aging at 700°C.4. 'STEM-EDX' This folder contains the raw data of the energy-dispersive X-ray (EDX) line scan used for the chemical analysis of the Ti-V-Nb-Ta sample after 40-day aging at 700°C. Aztec version 4.2 was used to interpret and extract the quantification line scan.TiVNbTa_40dayProject 1data: This folder includes the raw EDX data.reports: This folder includes two line scanning data in CSV format.Project 1.oip: This is the shortcut to use Aztec to open.5. 'STEM-EELS' This folder contains the energy electron loss spectroscopy (EELS) data used to analyze the chemical composition and oxidation states of specific elements in the TiVNbTa sample after 40-day aging at 700°C. Digital Micrograph can be used to open and analyze the .dm3 file.Core loss O reconstructed with 3 components.dm3: This is the aligned EELS map.GB precipitate.msa: This is the EELS spectrum extracted from a precipitate at the grain boundary in the EELS map.intragrainular precipitate.msa: This is the EELS spectrum extracted from a precipitate in the metal matrix in the EELS map.matrix.msa: This is the EELS spectrum extracted from the metal matrix in the EELS map.6. 'TKD' This folder contains the on-axis transmission Kikuchi diffraction (TKD) data used to interpret the crystallographic orientation of nanoscale features in the Ti-V-Nb-Ta sample after 40-day aging at 700°C. The .ctf files can be accessed using the Oxford Instruments Channel 5 software or the open-source Matlab codes at https://mtex-toolbox.github.io/.On_axis_5nm_1p5nA.ctf: TKD data from the TiVNbTa sample aged at 700°C for 40 days.7. 'SEM-EDX-EBSD' This folder contains co-located energy-dispersive X-ray (EDX) chemical and electron backscatter diffraction (EBSD) orientation mapping from the selected samples, showing the chemical and crystallographic orientation information. Aztec version 4.2 was used to interpret the data and extract the maps.TiVNbTa_40dayProject 1data: This folder includes the raw EDX and EBSD data.Project 1.oip: This is the shortcut to use Aztec to open.TiVNbTa_homogenisedProject 1data: This folder includes the raw EDX and EBSD data.Project 1.oip: This is the shortcut to use Aztec to open.Methods3D FIB/SEM data were acquired with the Zeiss Crossbeam 540 dual-beam instrument.APT data were obtained using a CAMECA LEAP 5000XR instrument.SEM-EDX-EBSD data were collected using the Oxford Instruments XmaxN 150 EDX detector, and the Oxford Instruments Nordlys Max EBSD detector on a Zeiss Crossbeam 540 dual-beam instrument.STEM-EDX data were obtained with a Jeol JEM-3000F STEM equipped with an Oxford Instruments EDX detector.STEM-EELS data were collected on a Cs-corrected JEOL ARM 200F. .TKD data were acquired using a Zeiss Merlin FEG-SEM system equipped with a Bruker e-flash high-resolution EBSD detector and an OPTIMUSTM TKD head.Nanoindentation data were collected using an Agilent G200 nanoindenter with a Berkovich diamond indenter. 
Type Of Material Database/Collection of data 
Year Produced 2023 
Provided To Others? Yes  
URL https://figshare.com/articles/dataset/Research_data_for_Origin_of_age_softening_in_the_refractory_hi...