基于深度神经网络的ODS合金辐照硬化预测

氧化物弥散强化(ODS)合金作为第4代先进堆结构材料和聚变堆第一壁结构材料的候选材料,其抗辐照性能仍是制约其在快堆和聚变堆领域应用的关键技术难题。本文通过收集ODS合金的成分、固化和热处理工艺、辐照条件、测试条件（包括温度等）及屈服强度等数据约570条,并对数据进行清洗及重要属性的筛选,采用机器学习中反向传播的深度神经网络方法,尝试构建了Cr、Y₂O₃等关键成分与ODS合金中子辐照硬化的关联性,获得针对ODS合金辐照硬化的性能预测。结果表明：Cr含量约为6%、Y₂O₃添加量约为0.2%时,ODS合金的辐照硬化程度降低,同时Ti的添加有利于ODS合金辐照硬化程度的降低,而添加Al则会加剧其辐照硬化。据此,后续可得出一定辐照条件下,辐照硬化程度更低的ODS合金成分设计方案。     

氦对低活性Fe-Cr-Mn(W,V)合金辐照损伤影响

采用低能离子加速器和超高压电镜相连接复合辐照装置,研究注入He后经电子束辐照,观察低放射性Fe-Cr-Mn（W,V）合金的辐照损伤特征;研究He对辐照过程中产生二次缺陷,空洞肿胀,诱起晶界偏析的影响。实验结果证明He的存在,增加辐照初期位错密度,促进空洞核心形成及空洞肿胀增加,抑制晶界近旁溶质元素偏析。     

12Cr-ODS钢中氧化物强化相（Y2O3）辐照损伤行为研究

本文采用电子束（e^－） 氦离子（He⁺）、氢离子（H⁺）束同时复合辐照方式研究12Cr-ODS铁素体钢中氧化物弥散强化相（Y₂O₃）辐照损伤行为,对不同辐照方式下辐照区内的氧化物形貌变化进行原位观察。研究结果表明,15dpa辐照后,氧化物周围出现微小高密度空洞,相界面变得不规则,氧化物在此特定条件下发生体积收缩或长大,尺寸有少量变化,但无明显溶解现象,对钢的性能不会产生影响。     

基于机器学习的高强度ODS合金成分设计

针对200~300组氧化物弥散强化（ODS）合金成分、工艺及力学性能数据，尝试借助机器学习的方法，建立了ODS合金中关键成分与拉伸性能的关联性。研究结果发现，在Cr、Y2O3、W和Ti含量与ODS合金抗拉强度的变化趋势中，均存在对应着抗拉强度极值的最优值，而添加Al对抗拉强度的提升无明显作用。获得了几种抗拉强度优化的ODS合金关键成分配比，预测出的室温抗拉强度均在1 400 MPa以上，这将为快堆结构材料用ODS合金优化设计提供技术支持，加速推进ODS合金的材料优化。     

双束同时辐照低活性Fe-Cr-Mn(W、V)合金微观组织损伤的影响

研究了时效热处理低活性Fe Cr Mn(W、V)钢双束同时辐照损伤行为 ,结果表明 :92 3K/ 3 0 0 0h时效合金 ,经单独电子辐照 (1 0a- 1)出现低密度空洞 ,而经双束同时辐照的时效合金 ,在辐照初期就形成间隙型位错环和微小空洞。与无时效合金相比 ,随时效温度增加 ,空洞尺寸、空洞密度和空洞肿胀量增大。随时效温度的提高碳化物析出数量增多 ,奥氏体中合金元素Cr、Mn、W、V降低 ,He的存在有效地促进空洞肿胀量增大。     

氢对12Cr-ODS钢中强化相(Y_2O_3)辐照稳定性影响研究

通过离子束-电子束(H++e-)双束同时辐照,原位观察氧化物在辐照过程中的组织损伤变化,研究了(H++e-)双束辐照对乙二胺四乙酸(EDTA)络合溶胶-凝胶法制备的12Cr-ODS铁素体钢中氧化物(Y2O3)稳定性的影响。实验结果表明:电子辐照剂量达15 dpa后,再进行(H++e-)双束辐照15 dpa,在此条件下,Y2O3氧化物会发生尺寸减小或溶解,辐照诱发点缺陷和合金元素界面化学反应是导致氧化物不稳定性的重要原因。     

双束(H~+/e~-)同时辐照对12Cr-ODS钢氧化物稳定性影响

利用氢离子和电子双束(H~+/e~-)对用化学浸润法制备的新型12cr-ODS铁素体钢进行辐照,研究了辐照对12Cr-ODS钢氧化物稳定性的影响.对不同辐照剂量下原位观察辐照区内氧化物形貌的变化过程发现:辐照前和15 dpa辐照后,约10～20nm氧化物的尺寸并没有明显变化,而氧化物周围出现微小高密度空洞并没有影响氧化物的稳定性;当辐照温度升高至823 K时,大尺寸的氧化物Y_2O_3与基体的相界面变得不规则,但氧化物颗粒尺寸并不发生明显变化.实验结果表明:弥散强化相Y_2O_3尺寸稳定,无明显溶解现象.     

双束同时辐照对低活性Fe-Cr-Mn(W,V)合金相稳定性影响

采用电子束 /He+ ion束同时复合辐照方式 ,研究了低活性Fe Cr Mn(W ,V)合金高温长时时效后组织稳定性 ,评价了He对辐照相稳定性影响。结果表明 ,单独电子辐照 ( 10a-1 )只引起相界面低密度空洞形成。而双束同时辐照对组织损伤具有协同效果 ,加剧相稳定性发生变化 ,如 :促进相间溶质原子扩散 ,导致析出相长大 ;新相的形成 ;发生结构无序化 ,促进析出相改性。从He原子与晶体辐照点缺陷与溶质原子相互作用和扩散等机制 ,讨论了辐照相稳定性发生变化的原因。     

He/H离子辐照损伤及其对ODS钢显微硬度的影响研究

为研究氧化物弥散强化铁素体钢(ODS钢)中的He/H离子协同辐照效应,本文开展了室温条件下ODS钢的He/H离子单一及复合辐照实验,并研究了辐照损伤对其显微硬度的影响。实验结果表明:He/H离子主要分布在损伤峰值附近;H离子辐照对ODS钢显微硬度的影响大于He离子;H离子的引入导致He离子低温解吸峰消失,而He离子的注量减半则使其热解吸起始温度升高;He、H离子与材料中缺陷相互作用不同是影响显微硬度及正电子寿命结果的主要因素。     

氦对低活性Fe-Cr-Mn(W,V)合金焊接热影响区辐照损伤的影响

采用高能离子加速器和超高压电镜连接装置 ,研究注入He后电子辐照和同时辐照 (He+ e-)低活性Fe Cr Mn(W ,V)合金焊接热影响区 (HAZ)损伤组织特点 ,测定He对损伤组织内晶界附近合金元素浓度变化的影响。实验结果表明 :He强烈促进辐照初期位错环和位错密度增加 ,促进HAZ辐照空洞核心形成及空洞肿胀增大。He有效抑制HAZ内晶界附近Cr、Mn浓度降低 ,对Ni,Si,V ,W元素浓度变化也有抑制作用。Fe Cr Mn(W ,V)合金焊接HAZ具有优良抗He气氛下的辐照损伤性能     

Development and characterization of advanced 9Cr ferritic/martensitic steels for fission and fusion reactors

This paper presents the results on the physical metallurgy studies in 9Cr Oxide Dispersion Strengthened (ODS) and Reduced Activation Ferritic/Martensitic (RAFM) steels. Yttria strengthened ODS alloy was synthesized through several stages, like mechanical milling of alloy powders and yttria, canning and consolidation by hot extrusion. During characterization of the ODS alloy, it was observed that yttria particles possessed an affinity for Ti, a small amount of which was also helpful in refining the dispersoid particles containing mixed Y and Ti oxides. The particle size and their distribution in the ferrite matrix, were studied using Analytical and High Resolution Electron Microscopy at various stages. The results showed a distribution of Y₂O₃ particles predominantly in the size range of 5-20 nm. A Reduced Activation Ferritic/Martensitic steel has also been developed with the replacement of Mo and Nb by W and Ta with strict control on the tramp and trace elements (Mo, Nb, B, Cu, Ni, Al, Co, Ti). The transformation temperatures (A_c1, A_c3 and M_s) for this steel have been determined and the transformation behavior of the high temperature austenite phase has been studied. The complete phase domain diagram has been generated which is required for optimization of the processing and fabrication schedules for the steel.     

Microstructure and oxidation properties of 16Cr–5Al–ODS steel prepared by sol–gel and spark plasma sintering methods

The 16Cr–5Al oxide dispersion strengthened (ODS) ferritic steel was fabricated by sol–gel method in combination with hydrogen reduction, mechanical alloying (MA) and spark plasma sintering (SPS) techniques. The phase characterization, microstructure and oxidation resistance of the 16Cr–5Al–ODS steel were investigated in comparison with the Al free 16Cr–ODS steel. X-ray diffraction (XRD) patterns showed that the Al free and Al added 16Cr–ODS steels exhibited typical ferritic characteristic structure. The microstructure analysis investigated by transmission electron microscopy (TEM) and energy dispersive spectrometry (EDS) revealed that Y–Ti–O complexes with particle size of 10–30 nm were formed in the Al free matrix and Y–Al–O complexes with particle size of 20–100 nm were formed in the Al contained high-Cr ODS steel matrix. These complexes are homogeneously distributed in the matrices. The fabricated 16Cr–5Al–ODS steel exhibited superior oxidation resistance compared with the Al free 16Cr–ODS steel and the commercial 304 stainless steel owing to the formation of continuous and dense Al₂O₃ film on the surface.     

氧化物弥散强化低活化合金的微观组织及力学性能

为了强化低活化合金(CLF-1)的高温性能,将采用Ar气超声雾化方法制备的CLF-1粉末与纳米Y₂O₃粉末混合后,经高能球磨和热等静压处理,获得氧化物弥散强化（ODS）CLF-1样品。对样品进行不同制度的热处理,并进行了微观组织分析和力学性能测试。分析结果表明,经过正火和回火处理,ODS CLF-1组织为回火马氏体,当正火温度为1 100 ℃时晶粒尺寸最为均匀。回火温度对显微组织影响不明显,但回火温度升高,维氏硬度下降。热处理后样品中观察到明显的弥散分布的Y₂O₃颗粒和位错塞积,证实了弥散强化的作用。Y₂O₃颗粒尺寸不均匀,100 nm左右的大颗粒倾向于沿晶界分布,而较小的颗粒则在晶内分布。ODS CLF-1样品具有良好的高温拉伸性能,600 ℃时抗拉强度为370 MPa,延伸率为18.5%。屈服强度和抗拉强度随热处理温度的升高而降低。     

Nanoscale characterization and formation mechanism of nanoclusters in an ODS steel elaborated by reactive-inspired ball-milling and annealing

Reactive-inspired ball-milling is proposed as a new production route for oxide dispersion strengthened (ODS) steels. So a Fe-14Cr-2W-1Ti-0.8Y-0.2O (wt.%) ODS steel is elaborated by ball-milling of FeCrWTi and YFe₃ plus Fe₂O₃ powders instead of Y₂O₃ and then by annealing at 800 °C for 5 min. Characterizations by Electron Probe MicroAnalysis and Atom Probe Tomography (APT) are performed after milling and after annealing. For the very first time, nanoclusters are observed after ball-milling by APT. Those nanoclusters are enriched in titanium, yttrium and oxygen and their mean radius is 0.8 nm. With annealing, the mean radius rises up to 1.4 nm and the number density as well as the enrichment factor in O, Ti and Y increase. So a new formation mechanism of nanoclusters is observed in those conditions of synthesis: ball-milling initiates the nanoclusters nucleation and during annealing, nucleation continues, accompanied by a slight growth of nanoclusters. Thus reactive-inspired ball-milling appears as a promising route for synthesizing ODS steels with a fine and dense dispersion of oxides.     

Creep behavior of oxide dispersion strengthened 8Cr-2WVTa and 8Cr-1W steels

Microstructures and creep behavior of two martensitic oxide dispersion strengthened (ODS) steels 8%Cr-2%W-0.2%V-0.1%Ta (J1) and 8%Cr-1%W (J2) with finely dispersed Y₂Ti₂O₇ have been investigated. Creep tests have been carried out at 670, 700 and 730 °C. Creep strength of J1 is stronger than that of any other ODS martensitic steels and the hoop strength of the ferritic ODS steel cladding. At the beginning of creep test, shrinkage was frequently observed for J1. This is one of the reasons for high creep strength of J1. The δ-ferrite, which is untransformed to austenite at hot isostatic press and hot rolling temperatures, was elongated along the rolling direction, and volume fraction of δ-ferrite in J1 is larger than J2. Although the elongated δ-ferrite affects the anisotropy of creep behavior, the extent of anisotropy in J1 is not so large as that of the ferritic ODS steel.     

先进反应堆用ODS F/M钢的强韧性匹配研究进展

氧化物弥散强化（ODS）铁素体/马氏体（F/M）钢具有极高的缺陷阱密度，加之体心立方结构基体，使其具有优异的抗辐照性能，被确定为包括聚变堆和第4代裂变堆在内的先进核能系统关键部件候选材料，成为核材料领域的研究热点。有利于ODS钢抗辐照性能的显微组织特点同时也赋予了ODS钢优异的室温和高温强度。但和其他高强度材料类似，ODS钢也存在强度高，而塑韧性不足的矛盾，不利于复杂部件的加工，因此，实现ODS F/M钢的高强高韧成为面向工程应用的ODS F/M钢研究的一大热点和难点。目前，针对ODS F/M钢强韧化的研究还较少，已有的相关研究也不够系统和深入，本文主要对抗辐照ODS F/M钢的显微组织结构要求及其强韧化研究现状进行总结和分析，为先进反应堆用抗辐照ODS F/M钢的强韧化设计提供思路和参考。     

奥氏体ODS钢在超临界水中的腐蚀行为

研究了奥氏体ODS钢（316-ODS）在600 ℃/25 MPa超临界水（SCW）中的腐蚀特性。采用腐蚀增重法、SEM、EDS和XRD分析了材料的氧化动力学、氧化膜的形貌、合金元素分布和组织结构。研究结果表明,316-ODS钢在SCW中出现了疖状腐蚀,同时还出现了敏化,其腐蚀增重服从幂指数生长规律。316-ODS钢表面氧化膜为双层结构,内层氧化膜富Cr贫Fe,其主要成分为FeCr₂O₄,而外层氧化膜富Fe贫Cr,其主要成分为Fe₃O₄。     

Fabrication and characterization of He-charged ODS-FeCrNi films deposited by a radio-frequency plasma magnetron sputtering technique

He-charged oxide dispersion strengthened(ODS)FeCrNi films were prepared by a radiofrequency(RF)plasma magnetron sputtering method in a He and Ar mixed atmosphere at150℃.As a comparison,He-charged FeCrNi films were also fabricated at the same conditions through direct current(DC)plasma magnetron sputtering.The doping of He atoms and Y_2O_3 in the FeCrNi films was realized by the high backscattered rate of He ions and Y_2O_3/FeCrNi composite target sputtering method,respectively.Inductive coupled plasma(ICP)and x-ray photoelectron spectroscopy(XPS)analysis confirmed the existence of Y_2O_3 in FeCrNi films,and Y_2O_3 content hardly changed with sputtering He/Ar ratio.Cross-sectional scanning electron microscopy(SEM)shows that the FeCrNi films were composed of dense columnar nanocrystallines and the thickness of the films was obviously dependent on He/Ar ratio.Nanoindentation measurements revealed that the FeCrNi films fabricated through DC/RF plasma magnetron sputtering methods exhibited similar hardness values at each He/Ar ratio,while the dispersion of Y_2O_3 apparently increased the hardness of the films.Elastic recoil detection(ERD)showed that DC/RF magnetron sputtered FeCrNi films contained similar He amounts(~17 at.%).Compared with the minimal change of He level with depth in DC-sputtered films,the He amount decreases gradually in depth in the RF-sputtered films.The Y_2O_3-doped FeCrNi films were shown to exhibit much smaller amounts of He owing to the lower backscattering possibility of Y_2O_3 and the inhibition effect of nano-sized Y_2O_3 particles on the He element.