質(zhì)子輻照對12Cr2W2Mn鐵素體/馬氏體鋼液態(tài)鉛鉍共晶合金腐蝕行為的影響

Effect proton irradiation on corrosion behavior 12Cr2W2Mn ferritic/martensiticsteelinliquidlead-bismutheutectic

ZHONGYu-Xin，SHI Ke² ，ZHANGFei-Fei，YANGJi-Jun （1. Education，InstituteNuclear Science ，Sichuan University，Chengdu 61Oo64，China；2.National Aerospace Chemical Power，Hubei Institute Aerospace Chemotechnology，Xiangyang 441Oo3，China; 3.China Nuclear Power Research Institute，Shenzhen 5l8O26，China）

Abstract：Ferritic/Martensitic（F/M） steel is regarded asa promising structural material for lead-cooled fast reactors due to its excellnt radiation resistance mechanical properties.However，its long-term service performance is significantly affected by two factors ：corrosion from high-temperature liquid lead-bismuth eutectic （LBE） iradiation damage caused by intense neutron flux.To systematically investigate the syner gistic effects irradiation corrosion on l2Cr2W2Mn F/M steel，this study evaluated the impact pro tonirrdiation on its corrosion behavior in liquidLBE.The samples were first iradiated with protons at

400^°C ，followed by exposure to liquid LBE at 400^°C for 500 hours.A comparative analysis was conducted on the corrosion products corrosion depth between irradiated non-irrdiated samples. The results showed that proton irradiation induced the formation a large amount M₂₃C₆ phases on the surface. During subsequent corrosion in LBE，Cr-rich oxides were observed to preferentially grow around the M₂₃C₆ particles along grain boundaries.Notably，iradiated samples exhibited fewer oxide particles than non-irradiated ones，indicating that proton irradiation improves the corrosion resistance 12Cr2W2MnF/M steel. This improvement is attributed to the M₂₃C₆ phase blocking the diffusion paths iron chromium atoms，thereby inhibiting corrosion progression.These findings provide valuable insights for the development irradiation corrosion-resistant structural materials for future lead-cooled fast reactors.

words： Liquid lead-bismuth eutectic；Proton irradiation;Corrosion; M₂₃C₆ phase;Cr-rich oxide

1 Introduction

Lead-Bismuth Eutectic（LBE） is widely recog nized as the most promising metallic coolant for the lead-cooledfastreactors[1.]，primarilydue toits unique combination advantageous properties： low melting point，high boiling point，low vapor pressure，low viscosity，excellent thermal conductivity， negligible structural damage under irra diation[3.4]. However， the corrosion structural materials in contact with LBE remains the primary challenge for its practical application as a reactor coolant[5.6].

Ferritic/martensitic （F/M） steels are recog nized as promising cidate structural materials for lead-cooled fast reactors，owing to their excellent corrosion resistance， high thermal conductivity， lowthermalexpansioncoefficient， costeffectiveness[7-0]. Extensive research has been conducted on the corrosion behavior F/M steels in liquid LBE，yielding significant findings. Kikuchi et al.[8] investigated the corrosion behavior F82H steel inacirculatingLBE loop at 450^°C 500^°C revealingthatthe corroded F82H steel exhibited a three-layer structure：an outer magnetite （Fe₃O₄） layer，a spinel-type FeCr₂O₄ intermediate layer， an oxygen diffusion layer.Weisenburger et al.[l] studied the corrosion T91 steel in flowing LBEunder varying flow velocities，demonstrating that the hydrodynamic effect flowing LBE induced delamination the outermagnetitelayer.Shi et al.[12] further explored the corrosion behavior SIMP T91 steels by exposing them to static oxygen-saturated liquid LBE at 600^°C for up to 1000 h.Their results showed that the corroded structure comprised an outer layer columnar plumberrite magnetite，aninnerlayer FeCrspinel， adiffusionlayerwith Cr/Si -richox ide precipitates.

Ontheotherh，structuralmaterialsinleadcooled fast reactors are subjected to irradiation， which induces damage such as voids，second-phase particles， dislocation loops[13-15]. Irradiation damagealters the internal microstructure materials， affecting theirperformance—including embrittlement，phaseinstability， irradiation-enhanced corrosion[16-18]. Researchers have investigated the effectirradiation onmaterialcorrosionbehavior，reportingboth irradiation-decelerated irradiationpromoted corrosion phenomena.

In general， the corrosion resistance most materials deteriorates after irradiation. Li et al.[17] found that Si-ion irradiation accelerated the corrosion SiC in FLiNaK molten salt. Kenik et al.[19] reported radiation-induced degradation stainless steel in light water reactors，while Ickes et al.[18] observed irradiation-assisted stress corrosion crackingin 3l6 steels irradiated in commercial pressur ized water reactors.Notably，some studies have indicated that irradiation can mitigate corrosion under specific conditions. Zhou et al.[2o] found that proton irradiation decelerated intergranular corrosion NiCr alloys in molten salt，while Hanbury et al.[21] suggested that proton irradiation could reduce the corrosion rate 316L stainless steel in hightemperature water. Dai et al.[22] also demonstrated good compatibility between FeCrAlY/TiN coatings LBE under proton irradiation.However，limitedresearch has investigated the effect irradiation on the corrosion behavior F/M steels in liq uid LBE^[23，24] ， whether irradiation exerts a positiveor negative effect remains unclear.Previous studies on the LBE corrosion behavior F/M steels have primarily focused on parameters such as temperature，time，flow rate， oxygen content8.11.2]. Therefore，clarifying how irradiation influences corrosion behavior is critical for the development LBE-cooled reactors in the future.

In our previous work， 12Cr2W2MnF/M steel wasdeveloped，itsirradiationperformancewas systematicallyinvestigated.In this study，a proton irradiation experiment was designed，followed by static oxygen-saturated liquid LBE corrosion tests， aiming to explore the effect proton irradiation on thecorrosion behavior12Cr2W2MnF/M steel in liquid LBE.

2 Experimental procedures

2.1 Materialssamples

The 12Cr2W2Mn F/M steel was prepared by vacuum inductionmelting， the sintered ingotwas forged into a plate with dimensions 335mm× mm×20mm .The steel was normalized at 1050^°C for 30min ，followed by tempering at 760^°C for 2h withaircoolingaftereachheattreatment step.The chemical composition 12Cr2W2MnF/M steel is listed in Tab.1.Prior to testing，the steel surface was sequentially ground with 80o，100o，200O 3000 gritssilicon carbide papers，followed by mechanical polishing with diamond powder. Finally，the samples were electrochemically polished using a solution 20% perchloric acid 80% ethanol to remove the surface stress caused by previous processing steps. The electrochemical polishing parameters were as follows： voltage 20V ，current 2A ，pol

ishingtime 20s

2.2 Protonirradiationexperiments

Proton irradiation experiments with 5 MeV protons were conducted at 400^°C usinga 3MV temaccelerator at the Institute Nuclear Science ，Sichuan University，Chengdu， China. The ion beam flux was 3.4×10¹²cm^-2?s^-1 the H⁺ irradiation fluence was 6.2×10¹⁷cm^-2 The total irradiation time was approximately 50h ， while the cumulative time at 400^°C （including heat ing cooling）was about 65h .Thedisplacement damage levels proton concentration prilesas a function depth were calculated by the Stopping Range Ions in Matter（SRIM） code，as shown in Fig.1.The fluencecorrespondstoapeak damage level O.27 dpa（displacement per atom） at 82μm below the surface.In the uniform damage areaextending from the surface to a depth 2O μm ，the damage level remains at approximately O.Oldpa，so that the influence irradiation damage changes with irradiation depth can be neglected.

2.3 CorrosionexperimentsinliquidLBE

The quartz tube with a thickness 2mm served as the corrosion container，following a de sign similarto that reported by Bian et al.[25].As shown inFig.2，proton-irradiated samples solid LBE alloy were placed inside the quartz tube， which was then evacuated to a vacuum better than 1×10^-2 Pa sealed by flame.The LBE consisted 44.5% （weight percentage） pure lead granules（Aladdin，purity 599.99% ） 55.5% （weight percentage） pure bismuth granules （Aladdin，puritygt; 99.999% ）.The sealed quartz tubes werevertically positioned in a vertical furnace maintained at 400^°C for 500h using a temperature controller. A quartz column ensured the samples werecompletelyimmersed in liquidLBE facilitatedtheir separation from theLBEafter the corro sion testing.Non-irradiation F/M steels samplesun derwent the same corrosion procedure as a control group.

2.4 Samplescharacterization

After the corrosion experiments，one subset samples was cleaned at room temperature using a fresh solution composed glacial acetic acid，absoluteethanol， hydrogen peroxide（volumeratio to remove adherent LBE from the surface^[26，27] . These samples were then prepared for sur face characterization. The remaining samples were face-mounted with epoxy adhesive（FP14420， USA）， their cross-sections were polished to a mirror finish using silicon carbide papers dia mond powder for cross-sectional analysis.

The composition phases the F/M steels were analyzed by X-ray diffraction （XRD，DX2700， Dong Fangyuan， China）. Foreach sample，the XRD 20 range was set from 20^° to 90^° ， diffractogram analysis was performed using Jade6.5stware.Surfacecross-sectionalmor phologies，alongwith elemental distribution，were characterized by field-emission scanning electron microscopy（FESEM，Hitachi S480O） equipped with energy-dispersiveX-rayspectroscopy（EDS）. Transmission electron microscopy（TEM，Titan Cubed Themis G2 3OO，F(xiàn)EI）was used to obtain selected area electron diffraction （SAED） patterns high-resolution （HR） images. Cross-sectional TEM specimens were prepared via ion thinning （Gatan69l）focusedionbeam（FIB，HELIOS Nano Lab 6OOi，F(xiàn)EI）milling，with Pt C pro tective layers deposited prior to processing.

3 Results

3.1 Surfacemorphologycorrosionsamples

Fig.3 illustrates the surface topography samples after liquid LBE corrosion testing at 400^° C for 500h .As shown in Fig.3a，the non-irradiated sample surface exhibited dense granular corrosion products that completely covered the metal matrix， with no exposed substrate visible.In contrast，the proton-irradiated sample（Fig.3b）displayed only a fewlarge particles numerous small particles after corrosion. The microstructure elemental composition these particleswillbe analyzed in the subsequent section.Notably， the non-irradiated sample showed significantly larger particle size higher density corrosion products compared to the proton-irradiated sample.This indicates that pro ton irradiation enhances the corrosion resistance 12Cr2W2MnF/M steel in liquid LBE.

3.2XRD patterns corrosion samples

Fig.4 presents XRD patterns samplesafter liquidLBE corrosionat 400^°C for 500h ，withthe black curve representing the non-irradiated sample the red curve the proton-irradiated sample.Diffraction peaks corresponding to cubic Fe-Cr oxide （PDF #34-0140） Cr₃O₈ （PDF#36-1330）were detected on both sample surfaces.Characteristic peaks the body-centered cubic（bcc）structure F/Msteel—（11O），（20O），（211）—were also identified in all XRD spectra.

These results indicate that the surfaces both samples were covered by Fe-Cr oxides （e. g.， （202 Fe₃O₄ （Fe，Cr）₃O₄ spinel）[26.28] Cr-rich oxides（e.g.， Cr₃O₈. ）afterLBE corrosion.Notewor thy，thediffraction peak positions intensities differed between samples，suggesting that the protonirradiated sample had fewer corrosion products than the non-irradiated one. This finding aligns with the SEMobservationsin Fig.3，further confirming that proton irradiation enhances the corrosion resistance 12Cr2W2MnF/M steel in liquid LBE.

3.3Cross-sectional micrographs EDSanalysis corrosion samples

As shown in Fig. 5， the cross-sectional morphology composition the samples after liquid LBEcorrosion were characterized in detail by SEM EDS.Ascanbeseen from Fig.5a Fig.5b， the corrosion layer the non-irradiated sampleis mainly divided into two layers：an oxide layer an internal oxidation zone（IOZ）. According to the results XRD EDSanalysis，the oxide layer is about 3.6μm thick，mainly composed Fe-Cr oxides（such as Fe₃O₄ （Fe， Cr）₃O₄ spinel）；the IOZ is about 0.9μm thick， its main component is Cr-rich oxides（such as Cr₃O₈， .The crosssectional area photon-irradiated sample（Fig.5c Fig.5d）exhibits a corrosion layerwith a thickness approximately 0.8μm ，containing Fe，Cr O element. Combining the XRD EDS results，this region can be attributed to Fe-Cr oxide Cr₃O₈ .Notably，the thicknesscorrosion layer issignificantly reduced after proton irradiation. These cross-sectional analysis results are consistent withthepreviousresultsin Fig.3 Fig.4，fur ther confirming that proton irradiation enhances the corrosion resistance 12Cr2W2Mn F/M steel in liquid LBE.

4 Discussion

Based on the above study，it was found that proton irradiation can enhance the corrosion resistance12Cr2W2MnF/M steel inliquid LBE. To explore the mechanism， technologiessuchas SEM，EDS，XRD TEM were used to analyze theoriginal samples，proton-irradiated samples， LBE-corroded samples， samples under the syn ergistic effect proton irradiation LBE corrosion.

4.1The M₂₃C₆ phase induced byproton irradiation

Fig.6 shows the surface morphology ele ments distribution samples before after pro ton irradiation using SEM EDS.In Fig. 6a， thereisno special matters on the sample surface except some micro scratches.In contrast，F(xiàn)ig.6b shows that a large number particulate precipitates adhere to the surface 12Cr2W2Mn F/M steel， theirmorphologyissimilarto thesmallparticles inFig.3b，indicating thatproton irradiation induces the formation numerous precipitated phases in the steel.EDS analysis Areas 1 2（Figs. 6c～6d ） shows that the carbon content significantly increases from 4.60% to 19.16% （atomic percentage）， whilethecontents otherelements show no obvious changes. This indicates that the precipitates are carbides.Combined with the atomic percentage carbon content （ 19.16% atomic percentage），they are speculated to be M₂₃C₆ phase（Fe，Cr，W-rich carbide）.The signals elements such as Cr ，Mn， W，Ni， Ta do not change，which is attributed to the fact that the matrix signal 12Cr2W2MnF/ M steel is too strong to reveal the real signal the precipitated phase.

Fig.7shows XRD patterns samples before after proton irradiation，exhibiting diffraction peaks the Fe-Cr bcc structure.The （11O）， （200），（21l）peaks shift rightward after proton irradiation，which can be attributed to the change in lattice parameter 12Cr2W2Mn ferritic/martensitic steel induced by proton irradiation[29.30]. Magnified（21l） peaks the samples are inset in the toprightcornerFig.7.Notably，an impuritypeak emerges near the （2ll）peak in the irradiated sample，assigned to the M₂₃C₆ phase（PDF ?35 1 0783）.This finding is consistent with the EDS results in Fig. 6， subsequent TEM analysis was conducted to confirm the M₂₃C₆ precipitates.

Fig. 8 shows TEM micrographs protonirradiated sample in different areas where M₂₃C₆ pre cipitates（white arrows）are observed.The SAED pattern in Fig.8b shows that the（20O），（111）， （11I） reflections correspond to a [Oll] zone axisinthered-circledarea，characteristicthefacecentered cubic（fcc）structure M₂₃C₆ precipitates. The EDS results（Fig. 8c） the red-circled area in Fig.8b confirm that it is a Cr-rich carbide precipitate，such as Cr₂₃C₆

The M₂₃C₆ phase is one the common precipi tatesin F/M steels，typically distributed at grain boundaries rich in Fe，Cr，W elements[31.32]. The M₂₃C₆ precipitate was confirmed by SAED EDS analysis observed in various regions via TEM micrographs.By integrating the SEM，XRD， TEM results from Figs.6～8，it can be concludedthattheprecipitate inducedbyproton irradiationon the surface 12Cr2W2MnF/M steel is the M₂₃C₆ （Cr-rich carbide）phase.

4.2Analysis corrosion products in samples after LBE corrosion testing

Fig.9 presents surface micrographs EDS analysis samples after LBE corrosion testing. Figs.9a 9b are high-magnification images Fig.3.Fig.9c shows the EDS results Area A in Fig.9a，where the detected main elements are Fe， Cr ， O.Based ontheXRD（Fig.4） EDS results，AreaAisinferred to be Cr-richoxides，such as Fe-Cr mixed oxides Cr₂O₃ .Area B corresponds to one the large particles（white arrows） onthe surface the proton-irradiated sampleafter

LBE corrosion， EDS analysis confirms it as a Cr-rich oxide.ForArea C inFig.9b，the small par ticlesresemble those observed in the morphology Fig.6b.Fig. 9e reveals the main components Area C，which is presumed to be the M₂₃C₆ phase due to the high C content （22.68% atomic percentage）.These results indicate that the large particles （Area B）in Fig.9b are Cr-rich oxidesformed dur ing LBE corrosion，whereas the small particles （Area C）are M₂₃C₆ phases induced by proton irra diation prior to LBE testing.It can be inferred that theproton irradiation-induced M₂₃C₆ phase enhances the corrosion resistance 12Cr2W2Mn F/M steel in liquid LBE.

4.3 Cr-rich oxideanalysisin proton-irradiated sample after LBE corrosion testing

Fig.1O presents cross-sectional TEM micrographs HAADF image proton-irradiated sample afterLBE corrosion testing.Fig.lOa shows the overall perspective the cross-sectional sample prepared by FIB system，where Pt C were deposited as protective layers. The HAADF image the region outlined by the yellow dashed line clearly reveals the cross-sectional morphology，with dis tinct microscopic contrast enabling the observation M₂₃C₆ phases （marked by red arrows） Crrich oxides. These TEM observations are in good 920

agreement with SEM results shown in Fig. 9b.

Fig.11 displays an amplified HAADF image the area in Fig.1Ob，along with EDS mapping re sultsforFe，Cr，O，C，Welements.TheEDS mapping the black particulates on the sample sur face exhibits strong signals for oxygen chro mium，confirming that these particulates in Fig.10b （markedbyblue arrows） Fig.1lareCr-rich ox ides.Notably，the Cr-rich oxide particulates are sparsely distributed，with M₂₃C₆ particles acting as separators.The growth Cr-rich oxide particles is inhibited because M₂₃C₆ particles occupy the prefer ential growth sites.

4.4Growth process cr-rich oxides in protonirradiated samples after Ibe corrosion testing

Fig.12 shows a cross-sectional TEM micro graph a proton-irradiated sample afterLBE corrosion，with three typical areas selected for EDS analysis.Based on the particle size C content （21. 65% atomic percentage），the particle in Area A was identified as an M₂₃C₆ phase.Similarly，Area Bwas characterized as Cr-rich oxide.In Area C， EDSanalysis detected higher contents C （204號 （9.34% atomicpercentage）O（ 19.19% （204號 atomic percentage）.Additionally，TEM observations revealed a smaller particle encapsulated by a larger one，indicating that the larger particle is Crrich oxide while the smaller one is an M₂₃C₆ precipitate.The Cr-rich oxide growsaround the M ₂₃C₆ par ticle eventually wraps it up. As reported in Refs.[31，32]， M₂₃C₆ precipitates preferentially format martensitic lath boundaries grain boundaries.Concurrently，diffusionFe Crelements occurs primarily at grain boundaries[7.26]. Thus，F(xiàn)e Cr atoms diffuse around M₂₃C₆ particles reactwith oxygen from LBE，leadingtothe formation Cr-rich oxides.

Fig.13 shows the corrosion mechanism proton-irradiated samplesafterLBE corrosion.The growth mechanism the Cr-rich oxides in these samples during liquid LBE corrosion testing can be inferred as follows ：

（1）As shown in Fig.13a， M₂₃C₆ precipitates cover the steel matrix surface after proton irradiation，as confirmed by Figs. 6～8

（2）In the LBE corrosion experiment，F(xiàn)e atoms first diffuse into LBE liquid through gaps in the M₂₃C₆ precipitate layer.Concurrently，O atoms contacted with steel matrix via these gaps.However， dense M₂₃C₆ precipitates interdict most diffusion paths forFe Cr ，as depicted inFig.13b.

（3）With Cr atoms diffusing more slowly than Fe，O atoms infiltrate the metal matrix along Fediffusionpathways react with diffused Cr to form oxides. Cr-rich oxides grow around M₂₃C₆ particles atnarrow gaps along the sample surface at widergaps（Fig.13b），as validatedbyFigs. 9～12 業(yè)

（4）As Cr-rich oxides further fill the gaps be tween M₂₃C₆ particles，they block diffusion Fe Cr atoms the permeation Pb/Bi atoms， therebyenhancingLBEcorrosionresistance （Fig.13d supported by Figs. 1～5） ：

Additionally，theoxidelayernon-irradiated sample（Figs. 5a～5b ）is consistent with previous studies[7.26]. There is no obvious boundary between theF e₃O₄ layer （Fe，Cr）₃O₄ layer，whichcan beattributed to the relatively thin thickness the Fe （Cr）oxide layer，making it difficult for EDS line scanning to distinguish them clearly.By the way， Frazer et al.[24] found that the corrosion resistance HT-9 steel degrades under the combined action ion beam irradiation liquid metal corrosion. Ourstudy differs from theirs in that the irradiation LBE corrosion experiments were conducted step-by-step（as inferred from simultaneousion irradiation liquid metal corrosion experiments）. Investigatingthebehavior 12Cr2W2Mn F/M steel undersimultaneous irradiation corrosionwillbe ournext research focus.

5 Conclusions

Based on the study 12Cr2W2Mn F/M steel subjected to 5 MeVproton irradiation at 400^°C in LBEliquid at 400^°C for 500h ，the main conclu sions are summarized as follows ：

（1）Proton irradiation induced the formation abundant M ₂₃C₆ precipitates on the sample sur face.

（2）In the LBE corrosion experiment，the nonirradiatedsampleformedtwoCr-richoxidelayersafter corrosion：The outer oxide layer （3.6μm ）was mainlycomposedFe-CroxidessuchasF e₃O₄ （Fe， Cr）₃O₄ spinel，while the inner oxide layer （204號 （0.9μm ）was primarily composed Cr-rich oxides with numerous oxideparticles. Theprotonirradiated sample only formed one Cr-rich oxide layer （0.8μm ）small amount oxide particles after corrosion.

（3）The Cr-rich oxide grow along the periph ery within the gaps M₂₃C₆ particles.

（4）The M₂₃C₆ phase Cr-rich oxides inter dictthediffusionpathsFe Cratoms，deceler ateLBE corrosion， enhance the LBE corrosion resistance 12Cr2W2Mn ferritic-martensitic steel afterproton irradiation.

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