纯锆上离子注入钇和镧后的表面分析

用金属蒸汽真空弧源，以40kV加速电压对纯锆样品分别进行了10¹⁶—10¹⁷/cm²的钇、镧离子注入，注入温度约为130℃.然后对注入样品进行表面分析.x射线光电子能谱分析表明，注入的钇以Y₂O₃形式存在，镧以La₂O₃形式存在.俄歇电子能谱表明，纯锆基体表面的氧化膜厚度随着离子注入剂量的增加而增加，当离子注入剂量达到10¹⁷/cm²时，氧化膜的厚度达到了最大值.卢瑟福背散射显示镧层的厚度约为30nm，同时直接观察到当离子注入剂量为(La+Y)10¹⁷/cm²时，纯锆样品表面发生了严重的溅射. 关键词： 纯锆 钇和镧离子共注入 卢瑟福背散射 x射线光电子能谱     

强流脉冲电子束作用下金属锆的微观结构与应力状态

利用强流脉冲电子束 (HCPEB) 技术对金属纯锆进行表面处理, 采用X射线衍射, 扫描电子显微镜及透射电子显微镜详细分析了辐照诱发的表层微观结构和缺陷. X射线分析结果表明, HCPEB辐照后在材料表层诱发幅值为GPa量级的压应力, 并形成{0002}, {1012}, {1120}及{1013}织构. 表层微观结构观察表明, 与其他金属材料不同, HCPEB辐照在材料表层诱发的熔坑数量极少, 多次轰击甚至几乎没有表面熔坑的形成. 此外, 在快速的加热和冷却状态下, 在表面熔化层形成大量的超细晶粒结构, 同时诱发马氏体相变和强烈的塑性变形. 1次HCPEB辐照后表层内形成的变形微结构以位错为主, 孪晶数量较少; 5 次辐照样品的位错密度迅速增高, 孪晶数量也显著增加; 10次辐照后样品中的变形微结构以变形孪晶为主, 且出现二次孪晶现象. 表层晶粒内部变形的晶体学特征不仅决定了表层的织构演化行为, 而且还起到细化晶粒的作用, 为纯锆及锆合金表面强化提供了一条有效的途径. 关键词： 强流脉冲电子束 纯锆 微观结构 应力状态     

Mechanism of defect evolution in H+ and He+ implanted InP

The defect evolution in InP with the 75 keV H⁺ and 115 keV He⁺ implantation at room temperature after subsequent annealing has been investigated in detail. With the same ion implantation fluence, the He⁺ implantation caused much broader damage distribution accompanied by much higher out-of-plane strain with respect to the H⁺ implanted InP. After annealing, the H⁺ implanted InP did not show any blistering or exfoliation on the surface even at the high fluence and the H₂ molecules were stored in the heterogeneously oriented platelet defects. However, the He molecules were stored into the large bubbles which relaxed toward the free surface, creating blisters at the high fluence.     

横向限制下凝固微观组织演化的相场法模拟

凝固过程中横向限制挡板的存在对晶体微观结构的演化存在重要的影响, 不同性质的横向挡板将产生不同的限制效应, 对最终凝固微观组织形成起着决定性作用. 本文利用非等温相场模型, 定性地模拟了纯金属Ni凝固过程中横向限制的存在对其枝晶微观形貌演化的影响, 研究了不同尺寸及性质的横向挡板对枝晶微观结构形成的影响, 讨论了横向限制对不同初始枝晶间距枝晶形貌发展的作用. 计算结果表明, 横向限制挡板的存在将直接影响凝固过程中微观组织的形貌演化过程并最终改变微观结构. 随着横向挡板间距的减小, 微观组织变化更加明显; 挡板初始温度越低, 枝晶形貌改变越明显; 初始枝晶间距越大, 形貌变化越明显; 不同挡板高度对微观结构具有基本相同的影响. 关键词： 相场模拟 微观组织演化 横向限制     

快速凝固Ti-Cu-Fe合金的相组成与组织演变规律

采用落管无容器处理技术实现了Ti_61.2Cu_32.5Fe_6.3三元包共晶合金在自由落体条件下的快速凝固,获得了直径为80—1120μm液滴的凝固组织.实验中获得的过冷度范围为34—293 K,最大过冷度达0.23T_L.研究发现,在自由落体条件下,由于受到无容器、微重力、超高真空等因素的影响,合金熔体的凝固组织中包含Cu_0.8Fe_0.2Ti相、CuTi₂相和CuT₃相,显著偏离了平衡状态.Cu_0.8Fe_0.2Ti为初生相,同时又与CuTi₂相形成两相共晶;CuTi₃相则呈现枝晶形貌,并发生了明显的溶质截留效应.随着过冷度的增大,共晶组织由层片共晶向不规则共晶转变,形貌由长条状共晶团变为椭球状共晶团,最终变为球状共晶胞;Cu_0.8Fe_0.2Ti相枝晶形貌由粗大枝晶变为碎断枝晶,进一步变成不规则的粒状晶粒;CuTi₃相枝晶则由碎块状转变为完整枝晶.     

Structural and size evolution of indium nanoparticles embedded in aluminum synthesized by ion implantation

The structural and the size evolution of embedded In nanoparticles in Al synthesized by ion implantation and subsequent annealing are experimentally investigated. The average radius r of In nanoparticles is determined as a function of annealing time in a temperature range between 423 K and 453 K. The structural transition of In nanoparticles with the crystallographic orientation In(200)[002] Al(200)[002] is observed to change into In(111)[110] Al(002)[110] with a critical particle radius between 2.3 nm and 2.6 nm. In addition, the growth of In nanoparticles in the annealing process is evidently governed by the diffusion limited Ostwald ripening. By further analyzing the experimental data, values of diffusion coefficient and activation energy are obtained.     

Effects on the evolution of microstructure and properties of low-silicon cast aluminum alloys in service

ABSTRACT

The microstructure evolution and property change of four kinds of low silicon cast aluminum alloy exposed to heat for 0–50?h at 200°C were studied by means of Brinell hardness test, tensile property test, friction and wear property test and XRD analysis. The results show that with increasing thermal exposure time, the tensile strength of each group of samples decreased and the amount of wear increased. The tensile strength of samples with more Si content decreased slowly. When the time increased to 50?h, the increase of wear loss was the largest. The hardness of samples after thermal exposure increases compared with that before thermal exposure. The residual stress of (311) diffraction crystal surface of AlSi3.5Mg0.66 under different thermal exposure time was measured. The type of residual stress changed from residual tensile stress to residual compressive stress after thermal exposure. There is an abnormal phenomenon that the hardness of the sample increased and the amount of wear increased, and it is evident that the distribution of residual stress was inhomogeneous after thermal exposure. It is found that with increasing thermal exposure time to 50?h, the average lattice distortion ε of the low-index crystal plane and the high-index crystal plane in the aluminum alloys gradually increased.     

Surface chemical disorder and lattice strain of GaN implanted by 3-MeV Fe10+ ions

Chemical disorder on the surface and lattice strain in GaN implanted by Fe¹⁰⁺ ions are investigated. In this study, 3-MeV Fe¹⁰⁺ ions fluence ranges from 1×10¹³ ions/cm² to 5×10¹⁵ ions/cm² at room temperature. X-ray photoelectron spectroscopy, high-resolution x-ray diffraction, and high-resolution transmission electron microscopy were used to characterize lattice disorder. The transition of Ga-N bonds to oxynitride bonding is caused by ion sputtering. The change of tensile strain out-of-plane with fluence was measured. Lattice disorder due to the formation of stacking faults prefers to occur on the basal plane.     

In situ investigation on rapid microstructure evolution in extreme complex environment by developing a new AFBP-TVM sparse tomography algorithm from original CS-XPCMT

A new sparse tomography method for observing the rapid internal microstructure evolution of material, called the Algebraic Filtered-Back-Projection and Total Variation Minimization (AFBP-TVM) iteration sparse reconstruction algorithm, was proposed in this paper. The new algorithm was developed by combining the two techniques of the Algebraic Reconstruction Technique (ART) and the Filtered-Back-Projection (FBP) on the basis of analysis in linear space. A series of numerical reconstruction experiments were conducted to validate the new algorithm. The results indicated the new algorithm can obtain satisfactory reconstruction images from 1/6 of the projections that were used in traditional algorithms. So the time spent on projection acquisition process can be reduced to 1/6 of that in traditional tomography method. The quality of images reconstructed by new algorithm was better than other algorithms, which was evaluated by three quantitative parameters. The normalized average absolute distance criterion and the normalized mean square criterion, which were used to evaluate the relative error of the reconstruction results (smaller value means better quality of reconstruction), decreased from 0.3758 to 0.1272 and from 0.1832 to 0.0894 respectively. The standardized covariance criterion, which was used to evaluate the similarity level (greater value means higher accuracy of reconstruction), increased from 92.72% to 99.30%. Finally, the new algorithm was validated under actual experimental conditions. The results indicated that the AFBP-TVM algorithm obtained better reconstruction quality than other algorithms. It meant that the AFBP-TVM algorithm may be a suitable method for in situ investigation on material's rapid internal microstructure evolution in extreme complex environment.     

Orientation sensitivity of focused ion beam damage in pure zirconium: direct experimental observations and molecular dynamics simulations

A high-purity predominantly single crystalline zirconium was subjected to controlled focused ion beam (FIB) damage. Damage estimates were obtained from electron backscattered diffraction (EBSD) and nano-indentation measurements on exactly the same area/orientation. The damage kinetics, between different crystallographic orientations, differed by one order of magnitude and a clear hierarchy of orientation sensitive ion damage emerged. Use of a simple geometric approach, linear density of atoms and corresponding scattering cross-sections to impinging gallium ions, could differentiate between extreme damage kinetics; but failed when such differences were relatively minor. Numerically intensive molecular dynamics (MD) simulations, on the other hand, were more effective. However, MD simulations or direct EBSD observations failed to justify anisotropic irradiation hardening (AIH): 3–8 times more hardening for near basal. Though explanation for AIH is indirect, evidence and rationalization for orientation-sensitive radiation damage appears clear and statistically reproducible.     

Oxygen vacancies and V co-doped Co_3O_4 prepared by ion implantation boosts oxygen evolution catalysis

Introducing heteroatoms and defects is a significant strategy to improve oxygen evolution reaction(OER) performance of electrocatalysts. However, the synergistic interaction of the heteroatom and defect still needs further investigations. Herein, we demonstrated an oxygen vacancy-rich vanadium-doped Co_3O_4(V–O_v–Co_3O_4), fabricated by V-ion implantation, could be used for high-efficient OER catalysis. X-ray photoelectron spectra(XPS) and density functional theory(DFT) calculations show that the charge density of Co atom increased, and the reaction barrier of reaction pathway from O*to HOO*decreased. V–O_v–Co_3O_4 catalyst shows a low overpotential of 329 mV to maintain current density of 10 m A·cm~(-2), and a small Tafel slope of 74.5 m V·dec~(-1). This modification provides us with valuable perception for future design of heteroatom-doped and defect-based electrocatalysts.     

The study of damage and optical properties in LiNbO3 implanted by MeV Er and He ions

Abstract

Two LiNbO₃ (X and Y cut) crystals from different companies were implanted by 3.0 MeV Er ions to a dose of 7.5 × 10¹⁴ ions/cm² and 3.5 × 10¹⁴ ions/cm² with different beam current densities, respectively. After annealing at 1060°C in air for 2 hours, one LiNbO₃ sample was implanted by 1.5 MeV He ions to a dose of 1.5 × 10¹⁶ ions/cm². The Rutherford backscattering/channeling and prism coupling method have been used to study the damage and optical properties in implanted LiNbO₃. The results show: (1) the damage in LiNbO₃ created by 3.0 MeV Er ions depends strongly on the beam current density; (2) after annealing at 1060°C in air for 2 hours, a good Er doped LiNbO₃ crystal was obtained; (3) there is waveguide formation possible in this Er-doped annealed LiNbO₃ after 1.5 MeV He ion implantation. It is suggested that annealing is needed to remove the damage created by MeV Er ions before the MeV He ion implantation takes place, to realize the waveguide laser for Er doped LiNbO₃.     

Thermal evolution of vacancy defects induced in sintered UO2 disks by helium implantation

A slow positron beam coupled with Doppler broadening (DB) spectrometer was used to measure the low- and high-momentum annihilation fractions, S and W, respectively, as a function of positron energy in UO₂ disks implanted with different 1 MeV ³He fluences and annealed in ArH₂ or in vacuum. The S(E) and W(E) behaviors indicate that for fluences in the range from 2 × 10¹⁴ to 2 × 10¹⁶³He cm⁻², the vacancy defects distribution evolves with the annealing temperature in the range from 264 to 700 °C under ArH₂. This evolution is found to be dependent on the ³He fluence implanted in the sintered UO₂ disks. For the lowest fluence of 2 × 10¹⁴³He cm⁻², the S(W) plot with positron energy as the running parameter suggests that only the concentration of vacancy defects decreases when annealing temperature increases. For the highest implantation fluences (from 5 × 10¹⁵ to 2 × 10¹⁶³He cm⁻²) the S(W) plot suggests that the nature of the vacancy defects changes in the annealing temperature range from 260 to 400 °C. Measurements performed in implanted UO₂ disks annealed in vacuum have revealed a partial recovery of the vacancy defects possibly due to their recombination with mobile oxygen interstitials. The role of the hydrogen infusion into the disk is also discussed.     

湿度环境下钙钛矿太阳能电池薄膜微结构演化的同步辐射原位实时研究

环境湿度对有机-无机杂化钙钛矿薄膜太阳能电池稳定性有着相当重要的影响,在湿度环境下原位实时观测钙钛矿薄膜微结构的演化有助于揭示湿度导致的器件性能衰减的微观机理.本文基于上海光源X射线衍射线站,建立了一套湿度可调可控的原位X射线衍射实验装置用以实时观测湿度环境下钙钛矿薄膜的微结构演化.在相对湿度为60%±2%的环境中,采用原位同步辐射掠入射X射线衍射发现在钙钛矿薄膜暴露在湿度环境的最初阶段,其(110)衍射峰附近逐渐出现了中间相结构,应该是来源于部分钙钛矿晶体结构的逐渐分解所形成的钙钛矿多相结构;同时,紫外可见吸收光谱实验表明,经环境湿度处理后的薄膜吸收有所降低,尤其是在约770 nm处吸收台阶发生蓝移,在一定程度上反映出钙钛矿晶体结构的减少或结晶性变弱;扫描电子显微镜结果进一步显示,湿度实验后薄膜形貌的均匀性明显变差,覆盖率降低、孔洞变大及晶界变明显;采用环境湿度实验前后的钙钛矿薄膜上制备的太阳能电池J-V性能测试结果显示,器件的填充因子和光电转换效率均由于环境湿度处理降低了30%以上.因此,同步辐射原位实验观测清晰地揭示了器件性能与钙钛矿薄膜形貌以及微结构演化的密切关联,为理解有机-无机杂化的钙钛矿薄膜的降解微观机理提供了实验依据和指导.     

Fission of Pb nuclei induced by 0.5, 1.0, 1.5, 3.7 and 7.4 GeV protons in the volume of massive U/Pb and Pb targets

Experiments with relativistic protons accelerated at the Synchrophasotron LHE, Dubna, with energies of 0.5, 1.0, 1.5, 3.7 and 7.5 GeV hitting massive targets of (nat. U)/Pb and Pb were carried out using SSNTD during the years 1996–1999. The beam profiles and intensities of both primary particles and fast secondary neutrons were measured inside the massive cylinder blocks of Pb and U by counting fission fragment tracks due to the induced fission of Pb nuclei. The beam diameter typically increases by 20–30% at the depth 10 and 20 cm. With increasing the energy of protons the number of secondary neutrons increases with the depth of the target.

Further studies on beam profile measurements inside the massive heavy metal targets are discussed.     

Study of defect evolution by TEM with in situ ion irradiation and coordinated modeling

The paper describes a novel transmission electron microscopy (TEM) experiment with in situ ion irradiation designed to improve and validate a computer model. TEM thin foils of molybdenum were irradiated in situ by 1?MeV Kr ions up to ～0.045 displacements per atom (dpa) at 80°C at three dose rates ?5?×?10^?6, 5?×?10^?5, and 5?×?10^?4?dpa/s – at the Argonne IVEM-Tandem Facility. The low-dose experiments produced visible defect structure in dislocation loops, allowing accurate, quantitative measurements of defect number density and size distribution. Weak beam dark-field plane-view images were used to obtain defect density and size distribution as functions of foil thickness, dose, and dose rate. Diffraction contrast electron tomography was performed to image defect clusters through the foil thickness and measure their depth distribution. A spatially dependent cluster dynamic model was developed explicitly to model the damage by 1?MeV Kr ion irradiation in an Mo thin foil with temporal and spatial dependence of defect distribution. The set of quantitative data of visible defects was used to improve and validate the computer model. It was shown that the thin foil thickness is an important variable in determining the defect distribution. This additional spatial dimension allowed direct comparison between the model and experiments of defect structures. The defect loss to the surfaces in an irradiated thin foil was modeled successfully. TEM with in situ ion irradiation of Mo thin foils was also explicitly designed to compare with neutron irradiation data of the identical material that will be used to validate the model developed for thin foils.     

Fabrication and evolution of Cu nanoparticles in Al2O3 crystal by ion implantation and annealing at different atmospheres

Single crystal Al₂O₃ samples were implanted with 45 keV Cu ion implantation at a dose of 1 × 10¹⁷ ions/cm², and then subjected to furnace annealing in vacuum or with a flow of oxygen gas. Various techniques, such as ultraviolet-visible spectroscopy, X-ray diffraction spectroscopy and atomic force microscopy, have been used to investigate formation of Cu NPs and their evolution. Our results clearly show that the evolution of Cu NPs depends strongly on annealing atmosphere in the temperature range up to 600 °C. Annealing in vacuum only gives rise to a slight change in the size of Cu NPs. No evidence for oxidization of Cu NPs has been revealed. Remarkable modifications in Cu NPs, including the size increase and the effective transformation into CuO NPs, have been observed for the samples annealed at oxygen atmosphere. The results have been tentatively discussed in combination with the role of oxygen from atmosphere in diffusion of Cu atoms towards the surface and its interactions with Cu NPs during annealing.