高能重离子辐照的ODS铁素体钢脆化效应研究

与传统的铁素体钢相比,氧化物弥散强化(ODS) 的铁素体钢具有更优的耐高温和抗辐照性能,近年来成为先进核能装置重要的候选结构材料。在HIRFL 的扇聚焦型回旋加速器(SFC) 材料辐照终端,对一种氧化物弥散强化(ODS) 铁素体钢MA956 进行了高能Ne 离子辐照实验,旨在研究级联碰撞损伤和惰性气体原子注入条件下该材料力学性能的变化。利用辐照终端的能量衰减装置将SFC出口123.4 MeV的离子能量分解为介于38.5~121.0 MeV之间的30 个入射能量值,并通过双面辐照在厚度60 μm的样品中均匀产生了损伤。辐照剂量为9x1016 ions/cm2,在样品中的平均位移损伤为0.7 dpa,注入的Ne原子浓度为350 appm。辐照期间样品温度保持在440 ℃附近。对辐照前后的样品分别在室温和500 ℃下进行了小冲杆试验(Small-punchTest),获得了辐照前后样品的加载位移曲线,由此得到该辐照条件下样品的延性损失为18%~26%。通过扫描电子显微镜观察了断口形貌和厚度变化,估算了样品的等效断裂应变和断裂韧性。结果表明,MA956 钢经过高能Ne离子辐照后等延伸率减小,断裂韧性降低,样品发生了一定的脆化。透射电镜结果说明氧化物弥散相界面处微空洞的形成可能是导致脆化的原因。Oxide dispersion strengthened (ODS) ferritic steels have better high-temperature creep rupture strength and higher irradiation resistance than conventional ferritic steels, and show high prominence of application in advance nuclear reactors. Their stability under high-dose radiation conditions needs to be clarified. In the present study, a commercial ODS ferritic steel MA956 were irradiated with high 20Ne ions at a terminal chamber of the Sector-focused Cyclotron (SFC) at HIRFL (Heavy-ion Research Facility in Lanzhou). With the energy gradient degrader of the irradiation chamber, the primary energy (123.4 MeV) of the Ne-ion was dispersed into 30 different energies between 38.5~ 121.0 MeV, which resulted in a plateau distribution of lattice damage in the specimens. The specimens were irradiated from both sides so that the whole 60 m thickness was nearly uniformly damaged. The specimen temperature was maintained around 440 ℃ during the irradiation. The irradiation dose is about 9x1016 ions/cm2, corresponding to a damage level of 0.7 dpa and a Ne concentration of 350 appm. The specimens before and after irradiation were tested with the Small-punch Test technique, at room temperature and 500 ℃, respectively. The fracture morphology was observed by scanning electron microscopy.The results show that MA956 underwent some loss of ductility and fracture toughness after the irradiation with high-energy 20Ne ions. It may be ascribed to the formation of nano-scale cavities at the oxides/matrix interfacesin the ODS steel specimens under irradiation .     

碳化硅中氦离子高温注入引入的缺陷及其退火行为的光谱研究

对氦（He）离子高温（600 K）注入6H-SiC中的辐照缺陷,在阶梯温度退火后演化行为的拉曼光谱和室温光致发光谱的特征进行了分析.这两种方法的实验结果表明,离子注入所产生晶格损伤的程度与注入剂量有关;高温退火导致损伤的恢复,不同注入剂量造成的晶格损伤需要不同的退火温度才可恢复.在阶梯温度退火下呈现出了点缺陷的复合、氦-空位团的产生、氦泡的形核、长大等特性.研究表明：高温（600 K）注入在一定剂量范围内是避免注入层非晶化的一个重要方法,为后续利用氦离子注入空腔掩埋层吸杂或者制备低成本、低缺陷密度的绝缘层 关键词： 6H-SiC 离子注入 拉曼光谱 光致发光谱     

两种国产低活化的铁素体/马氏体钢的He离子辐照硬化研究

低活化的铁素体/马氏体钢（RAFM）以其高导热率、低热膨胀率、高抗辐照肿胀能力成为未来核聚变堆重要的候选结构材料,在聚变堆高能中子辐照环境由于（n,α）核反应产生的高浓度He在材料中的积累对于材料微观结构和宏观性能的影响是关系这类材料服役寿命的重要问题。本工作研究了面向聚变反应堆应用的两种国产低活化钢（CLF、CNS）的辐照硬化效应,利用中国科学院近代物理研究所320 kV高压实验平台提供的4He离子束进行辐照实验,辐照剂量6×10-3,6×10-2,6×10-1 dpa （辐照损伤/原子平均离位）,对应注He浓度分别为100,1 000,10 000 appm （氦离子浓度/百万分之一）。采用多能注入方法,在样品表面至1微米深度形成He浓度和离位损伤的坪区分布。利用纳米压痕仪对参比样品和注入He的样品进行了连续刚度测试。基于NIX-GAO模型对纳米硬度数据进行分析,获得了注入He的区域样品纳米硬度的数据。研究表明,注入He区域的纳米硬度与辐照损伤水平之间存在着1/2次幂函数的关系。未辐照CLF钢比CNS钢的纳米硬度略低,随着辐照剂量的增加,CLF钢呈现的辐照硬化现象更明显。Reduced activation ferritic/martensitic steels (RAFM) are important candidate materials for future fusion nuclear reactors because of their high thermal conductivity, low thermal expansion rate and high resistance to irradiation swelling performance. The influence of high concentration helium produced by nuclear reaction (n,α) on the micro-structure and macro-properties is an important issue limiting the service lifetime of the materials. In the present work, helium implantation to three different doses (100, 1 000, 10 000 appm helium, corresponding to 6×10-3, 6×10-2, 6×10-1 dpa) was carried out to investigate irradiation hardening of two RAFM Steels. Multi-energy He ion-beams at 320 kV high-voltage platform were used to get a damage plateau from surface to 1 μm depth in specimens. The continuous-stiffness test by a Nano-indentor G2000 was carried out Data of nano-hardness were analyzed based on Nix-Gao model. It is shown that there is a 1/2-power law relationship between the hardening and the irradiation damage level. Before helium implantation, the hardness of the CLF steel is slightly lower than that of the CNS steel. However, with the increase of helium-implantation dose, the hardening is more obvious in CLF steel. Further investigation of microstructures is needed to get a deeper understanding of the hardening mechanism.     

注氦尖晶石的红外光谱研究

利用傅立叶变换红外光谱仪对注He尖晶石样品随退火温变化而引起光吸收性能的变化进行了研究。发现尖晶石样品在626.4cm^-1附近的吸收峰随注入剂量的增加向小波数方向移动,而在随后退火过程该吸收峰随退火温度的增加而向大波数方向回复。该吸收峰的回复行为依赖于注入剂量和退火温度。认为在626.4cm^-1附近吸收峰随注入剂量和退火温度的这种变化与尖晶石中He的俘获以及释放有关。     

Hardening of an ODS Ferritic Steel after Helium Implantation and Thermal Annealing

Specimens of an oxide dispersion strengthened(ODS) ferritic steel(15 Cr-4 Al-0.6 Zr-0.1 Ti) are implanted with multiple-energy He ions at room temperature to create a damage plateau of 0.4 dpa for the average(corresponding to an He concentration of about 7000 appm) from the near surface to a depth about 1 um. The specimen is subsequently thermally annealed at 800°C for 1 h in a vacuum so that simple defects can be formed in the as-implanted state that has undergone significant recombination, meanwhile helium bubbles at nano-scale are formed. Hardness of the specimens are tested with the nano-indentation technique. A hardening by 25% is observed. Microstructures of the specimen after irradiation/annealing are investigated with transmission electron microscopy. Helium bubbles are generally located at dislocations and grain boundaries. Using the dispersed barrier strength model, the strength factor of helium bubbles in the ODS ferritic steel is estimated to be between0.1 and 0.26, which is close to that of helium bubbles in austenitic steels.     

Charge-sensitive deep level transient spectroscopy of helium-ion-irradiated silicon, as-irradiated and after thermal annealing

Electrically active defects in the phosphor-doped single-crystal silicon, induced by helium-ion irradiation under thermal annealing, have been investigated. Isothermal charge-sensitive deep-level transient spectroscopy was employed to study the activation energy and capture cross-section of helium-induced defects in silicon samples. It was shown that the activation energy levels produced by helium-ion irradiation first increased with increasing annealing temperature, with the maximum value of the activation energy occurring at 873K, and reduced with further increase of the annealing temperature. The energy levels of defects in the samples annealed at 873 and 1073K are found to be located near the mid-forbidden energy gap level so that they can act as thermally stable carrier recombination centres.     

Surface Erosion of GaN Bombarded by Highly Charged 208Pbq+-Ions

Surface change of gallium nitride specimens after bombardment by highly charged Pbq^＋-ions （q = 25, 35） at room temperature is studied by means of atomic force microscopy. The experimental results reveal that the surface of GaN specimens is significantly etched and erased. An unambiguous step-up is observed. The erosion depth not only strongly depends on the charge state of ions, but also is related to the incident angle of Pbq^＋-ions and the ion dose. The erosion depth of the specimens in 60° incidence （tilted incidence） is significantly deeper than that of the normal incidence. The erosion behaviour of specimens has little dependence on the kinetic energy of ion （Ek = 360, 700 keV）. On the other hand, surface roughness of the irradiated area is obviously decreased due to erosion compared with the un-irradiated area. A fiat terrace is formed.     

注入Ar+的蓝宝石晶体退火前后光致发光谱的分析

对注入Ar 后不同晶面取向的蓝宝石晶体在不同退火条件下的光致发光谱进行了分析.分析结果表明:三种晶面取向的蓝宝石样品经Ar 注入后,其光致发光谱中均出现了新的位于506 nm处的发光峰;真空和空气气氛下的退火均对样品在506 nm处的发光有增强作用,不同晶面取向的样品发光增强程度不同,且发光增强至最大时的退火温度也不同,空气气氛下的退火使样品发光增强程度更为显著.由此可以看出,退火气氛、退火温度和晶面取向均对样品发光峰强度有影响.     

离子注入/辐照引起Al2O3单晶的改性研究

600K温度下用110keV的He^＋,Ne^＋,Ar^＋离子注入及320K温度下用230MeV的^208Pb^27＋辐照Al2O3单晶样品,研究了离子注入和辐照对Al2O3单晶样品结构和光学特性的影响。从测得的光致发光谱可以清楚地看到,所有样品在波长为375,413和450nm处出现了强的发光峰。且所有5×10^16ion／cm^2注入样品的发光峰均最强。经过高能Pb辐照后的样品,在390nm处出现了新的发光峰。透射电镜分析发现在注入氖样品100nm入射深度以内形成了高浓度的小空洞（1-2nm）,在Ne沉积区域有少量大空洞形成。傅立叶变换红外光谱分析发现,波数在460-510cm^-1间的振动吸收带经过离子辐照后展宽,随着辐照量的增大,该振动吸收强度显著减弱。1000—1300cm^-1对应Al-O-Al桥氧伸缩振动模式的吸收带,辐照后向高波数方向移动。对离子注入和辐照对Al2O3单晶样品结构损伤机理进行了初步探讨。Single crystal sapphire （Al2O3 ） samples were implanted at 600 K by He, Ne and Ar ions with energy of 110 keV to doses ranging from 5 × 10^16 to 2× 10^17 ion/cm^2 or irradiated at 320 K by ^208Pb^27＋ ion with energy of 1.1 MeV/u to the fluences ranging from 1 × 10^12 to 5 × 10^14 ion/cm^2. The modification of structure and optical properties induced by ion implantation or irradiation were analyzed by using photoluminescence（PL） and Fourier transformation infrared spectrum（FIR） spectra and transmission electron microscopy（ TEM ） measurements. The PL measurements showed that absorption peaks located at 375,413 and 450 nm appeared in all the implanted or irradiated samples, the PL intensities reached up to the maximum for the 5 × 10^16 ion/cm^2 implanted samples. After Pb-ion irradiation, a new peak located at 390 nm formed. TEM analyses showed that small size voids,（ 1--2 nm） with high density were formed in the region from the surface till to about 100 nm in depth and also large size Nebubble formed in the Ne-doped region. From the obtained FTIR spectra, it was found that Pb-ion irradiation induced broadening of the absorption band in 460-510 cm^-1 and position shift of the absorption band in 1 000- 1 300 cm^- 1 towards to high wavenumber. The possible damage mechanism in single crystal sapphire induced by energetic ion implantation or irradiation was briefly discussed.     

高能238U离子辐照AlN 晶体薄膜的光学特性研究

通过傅里叶变换红外光谱、拉曼光谱和光致发光谱测试手段分析了由HIRFL 提供的高能238U离子辐照AlN 晶体薄膜的光学特性变化。辐照后出现了A1(To),A1(Lo),E1(To) 和E2 等声子振动吸收模式,并且辐照使其在样品近表面Al—N 等振动模式遭到破坏后悬空的Al— 键很快与空气中的O离子发生结合,形成了Al—O 键。综合分析得出了蓝光发射带是与O 离子相关的VAl-ON-3N 和VAl-2ON-2N两种类型缺陷以及F-型缺陷聚合所致;绿光发射带是由基底中Al 原子产生的价带之间的跃迁所致。AlN thin film irradiated with 100 MeV 238U ions delivered from HIRFL (Heavy Ion Research Facility in Lanzhou) were investigated by Fourier Transform Infrared spectra, Raman spectra and Photoluminescence spectra. Phonon vibration absorption modes including A1(To), A1(Lo), E1(To) and E2 appeared in the irradiated samples. The irradiation made the Al—N bonds broken and the formation of Al—dangling bonds, which combined soon with oxygen atoms existing in air to form Al—O bonds. Blue light emission band are related to the two types of defects of VAl-ON-3N and VAl-2ON-2N and F-type defects aggregation. Green light emission band is due to energy transition among valence band of Al atoms in sapphire substrate.