Analysis of Gibbsian Segregation at Heterophase Cu-MnO Interfaces

An alternative methodology to analyze Gibbsian segregation at heterophase interfaces with transmission electron microscopy (TEM) is presented and discussed. In this approach the actual concentration of the segregating element in a monolayer at the interface is obtained. This is in contrast to line scans or maps where the concentrations determined are a convolution of the concentration profiles with the electron probe and where for general interfaces the deconvolution problem can not be solved accurately. This is possible because the present approach uses explicitly the information offered by hetero-interfaces. The method is tested on the possible segregation of indium and gallium dissolved in a Cu matrix to interfaces between MnO precipitates and the Cu matrix. The occurrence of indium segregation is clearly demonstrated and the In concentration in the terminating Cu monolayer at the parallel {111} Cu/MnO interface is determined to be 15 ± 3 at.%, whereas the average In concentration in the Cu matrix is 3.8 ± 0.4 at.%. Further it was found that indium effectively blocks gallium segregation towards the oxide side of the interface. On the other hand, the presence of gallium does not influence the segregation of indium. Explanation for the gallium segregation at the oxide side relies on a thin spinel type Ga _x Mn _y O₄, which reduces the misfit at the metal-oxide interface.     

高分辨扫描透射电子显微镜原理及其应用

扫描透射电子显微术是目前应用最广泛的电子显微表征手段之一,具有分辨率高、对化学成分敏感和图像直观易解释等特点。其中高分辨扫描电子显微镜可以直接获得原子分辨率的Z 衬度像,结合X射线能谱(EDS)和电子能量损失谱(EELS),可在亚埃尺度上对材料的原子和电子结构进行分析。文章简述了扫描透射电子显微镜的基本原理及其应用现状,重点论述了高角环形暗场(HAADF)和环形明场(ABF)像的成像原理、特征和应用。此外,文中还对原子尺度分辨率的X射线能谱及电子能量损失谱元素分析方法进行了简述。     

Investigations on Thermal Conductivity of Carbon Nanotubes Reinforced Composites

Natural rubber, as well as natural reinforced rubber, with different carbon nanotubes concentrations, 10 and 20 mm, thick, have been structurally, chemically, and thermally investigated. Scanning electron microscopy techniques, as well as X-ray energy dispersive analysis, Raman, and thermal conductivity analysis, were used in characterizing materials in order to establish a connection among the CNT concentration, homogeneity of reinforcing elements within the natural rubber, and their thermal conductivity characteristics. The theoretical approach reveals the dependence between the thermal conductivity and reinforcing elements. The final result confirms the increase of the effective thermal conductivity with the concentration of CNT.     

The study of Al3(Mn,Pd) crystal and Al–Mn–Pd decagonal quasicrystal by spherical aberration-corrected scanning transmission microscopy and atomic-resolution energy dispersive X-ray spectroscopy

An Al₃Mn-type Al₃(Mn, Pd) crystal and an Al–Mn–Pd decagonal quasicrystal (DQC) in an Al₇₀Mn₂₀Pd₁₀ alloy are studied using a spherical aberration (Cs)-corrected scanning transmission electron microscope (STEM) with high-angle annular dark-field (HAADF) and annular bright-field (ABF) techniques, together with atomic-resolution energy dispersive X-ray spectroscopy (EDS). Mn and Pd atomic positions in the Al₃(Mn, Pd) structure projected along the b-axis (pseudo-tenfold rotational axis) are represented by separate bright dots in observed HAADF-STEM images. Besides, Al as well as Mn and Pd atomic positions are represented as dark dots in ABF-STEM images. Most Mn and Pd atomic positions in the Al₃(Mn, Pd) structure can be observed on atomic-resolution EDS maps. On the basis of the good correlation between the STEM images and the EDS maps, and also considering the structure of the Al₃(Mn, Pd) crystal, which was determined by X-ray diffraction using a single crystal, observed HAADF and ABF-STEM images of the Al–Mn–Pd DQC have been interpreted. Pd and Mn atomic positions in the Al–Mn–Pd DQC can be detected on the observed EDS maps. It can be seen that Pd is enriched around the centre of the columnar clusters, having a decagonal section with 2 nm in diameter. It can therefore be concluded that Pd plays an important role in the stabilization of the decagonal clusters, which form the Al–Mn–Pd DQC structure.     

A TEM study of the stability of intermetallic precipitates in Zircaloy nuclear reactor components

Transmission electron microscopy (TEM) has been used to characterise the radiation-induced changes in Zr(Cr,Fe)₂ intermetallic precipitates present in Zircaloy-2 and -4 nuclear reactor components. The results show that the precipitates become completely amorphous at low fluences (<1 × 10²⁴ n·m⁻²) during low temperature neutron irradiation (about 330 K) with no associated chemical composition change. At higher temperatures (about 573 K), a duplex amorphous-crystalline structure is produced. The precipitates retain a crystalline core surrounded by a peripheral amorphous layer that advances inwards with increasing fluence. The amorphous outer layer is coincident with a depletion of Fe that is dispersed into the surrounding hcp -phase matrix. Subsequent post-irradiation heat-treatment below the amorphous phase recrystallisation temperature results in the back-diffusion of Fe into the precipitates.     

Analytical electron microscopy of a reaction-bonded Si3N4-based ceramic containing oxide additions

The microstructure of a silicon nitride (Si₃N₄)-based ceramic, prepared by a process combining direct nitridation and reactive liquid phase sintering of silicon/ceramic oxide powder compacts, has been characterised using analytical transmission electron microscopy. The presence of the reactive liquid phase, promoted by the addition of oxides from the CaO-Al₂O₃-SiO₂ ternary system, resulted in an as-fired microstructure containing a mixture of crystalline phases based on -Si₃N₄, β-Si₃N₄ and Si₂ N₂O, and distinct amorphous regions rich in Si, Al and Ca. X-ray microanalysis revealed the calcium to be wholly partitioned to the glassy phase, while significant concentrations of aluminium were detected in both β-Si₃N₄ and Si₂N₂O. The observed compositions of these phases, together with measured lattice parameters systematically in excess of those of the pure compounds, imply that they are in fact β- and O-sialons respectively. Semi-quantitative energy dispersive X-ray spectroscopy, using an ultra-thin window detector, is demonstrated to be capable of distinguishing clearly between these phases according to their oxygen content and of determining the aluminium content of both phases to within ± 1 equ.%, even at concentration levels of <5 equ.%.     

掺Mo对NiSi薄膜热稳定性的改善

报导了在镍薄膜中掺入少量Mo提高了镍硅化物的热稳定性.结果表明,经650— 800℃快速热 退火形成的Ni(Mo)Si硅化物薄膜电阻值较低,约为2．4(Ω／□).XRD分析表明薄膜中只存在 NiSi相,而没有NiSi₂生成.由吉布斯自由能理论分析表明在Ni薄膜中掺人5．9 ％Mo对改善 Ni硅化物热稳定性起到至关重要的作用.经650—800℃快速热退火后的 Ni(Mo)Si／Si肖特基 二极管电学特性良好,势垒高度Φ_B为0．64—0．66eV,理想因子接近于1,更 进一步证明掺少量的Mo能够改善NiSi薄膜的热稳定性.关键词：镍硅化物快速热退火x射线衍射分析卢瑟福背散射     

Interdiffusion in two-layer Pd/Ag films III. TEM investigation of diffusion-induced grain boundary migration

Diffusion-induced grain boundary migration (DIGM) is studied by the transmission electron microscopy method in polycrystalline two-layer Pd/Ag thin films with a grain size (100–2000 nm). In addition to the typical features of DIGM known for coarse-grained bulk objects and foils, new features are found which are caused by a quite dense network of triple junctions and by misfit dislocations: fast increase of grain boundary curvature and inclination; back motion of grain boundaries owing to recrystallization forces and termination of DIGM. Homogenization resulted from diffusion-induced migration of misfit dislocations is observed in addition to DIGM.     

室温下金属中电子格林艾森常数的测量

在室温条件下用自己研制的超快电子衍射实验设备精确测量了金属铝的电子格林艾森常数(γ_e).当飞秒脉冲激光瞬间加热铝膜时,电子和晶格对固体热膨胀的作用在时间域上是不同步的,借助于超快电子衍射实验设备的高时间分辨能力,可以摆脱以往测量非磁性金属材料时低温的限制,在室温条件下,实验通过直接观测瞬间加热的铝膜中电子和晶格对热膨胀的不同贡献得到电子的格林艾森常数.关键词：格林艾森常数超快电子衍射晶格热运动电子热运动     

Effects of magnesium film thickness and annealing temperature on formation of Mg2Si films on silicon (1 1 1) substrate deposited by magnetron sputtering

Magnesium films of various thicknesses were first deposited on silicon (1 1 1) substrates by magnetron sputtering method and then annealed in annealing furnace filled with argon gas. The effects of the magnesium film thickness and the annealing temperature on the formation of Mg₂Si films were investigated by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The Mg₂Si thin films thus obtained were found to be polycrystalline and the Mg₂Si (2 2 0) orientation is preferred regardless of the magnesium film thickness and annealing temperature. XRD results indicate that high quality magnesium silicide films are produced if the magnesium/silicon samples are annealed at 400 °C for 5 h. Otherwise, the synthesized films annealed at annealing temperatures lower than 350 °C or higher than 450 °C contain magnesium crystallites or magnesium oxide. SEM images have revealed that microstructure grains in the polycrystalline films are about 1-5 μm in dimensions, and the texture of the Mg₂Si films becomes denser and more homogeneous as the thickness of the magnesium film increases.     

Transmission electron microscopy and X-ray diffraction study of microstructural evolution in magnetoresistive Cu–Fe–Ni ribbons

The evolution of the microstructure of a granular Cu₈₀Fe₁₀Ni₁₀ (at%) melt-spun ribbon is studied by transmission electron microscopy (TEM), energy-filtered transmission electron microscopy (EFTEM) and X-ray diffraction. This system is interesting as large giant magnetoresistance (GMR) values have been measured for this composition. We have shown the presence of two face-centred cubic phases, an (Fe,Ni)-rich phase and a Cu-rich phase. The lattice parameters of these two phases are close and no diffraction or elastic contrast is involved in displaying the two phases in TEM bright-field mode. With EFTEM imaging, we have shown the presence of a fine-scale (Fe,Ni)-rich precipitation inside the Cu-rich fcc matrix. The precipitates are 2–4 nm in the as-spun state and 4–6 nm after annealing for 2 h at 400°C. The lattice parameter of the Cu-rich phase in the as-spun sample is 0.3608 nm and 0.3610 nm for the (Fe,Ni)-rich phase. After a 24-h annealing treatment at 600°C, the mean diameter of the particle is 20 nm and the lattice parameter of the (Fe,Ni)-rich phase has decreased to 0.3600 nm, while that of the Cu-rich phase has increased to 0.3613 nm, which is consistent with a segregation of Fe and Ni in the precipitates. The composition and volume fraction of the two phases measured for this annealed sample are in good agreement with the Thermocalc® predictions.     

LPCVD Si基转换生长3C-SiC薄膜的光学性质初探

本文采用LPCVD技术在高温条件下, 利用甲烷和氢气混合气体作为碳源, 在n-Si(111)衬底上制备3C-SiC薄膜。通过XRD、XPS、SEM、FT-IR和PL研究发现: 温度对3C-SiC薄膜的形貌和晶体质量有较大的影响, 并且生长温度对3C-SiC薄膜的780 cm-1左右的FT-IR反射峰强度影响非常大; 在室温测试条件下, 3C-SiC薄膜有较强的蓝光波段的荧光峰。     

Three-dimensional size and orientation of the precipitates in AZ91 magnesium alloys measured by TEM techniques

Knowledge of the microscopic structure, including three-dimensional (3-D) size and orientation of the precipitates, is essential to fully understand the mechanical properties of the magnesium alloys and designing the alloys with better performance. Analytical TEM with high spatial resolution offers the simultaneous measurements of 3-D size, structure, orientation, composition of the precipitates from one typical sample along an established crystallographic axis. Besides popular Burgers orientation relationship (OR), other ORs such as Pitsch--Schrader OR, Crawley OR, Potter OR and a new OR with the form of [0001]_α 1.0° from [311]_γ and (11\bar 20)_α 2.0° from (03\bar 3)_γ between the magnesium matrix and the precipitate γ -Mg₁₇Al₁₂ are identified by TEM imaging and diffraction techniques. As a case study, the thicknesses of the individual precipitates with Burgers OR are further measured to be 100--200~nm through both electron energy-loss spectroscopy and x-ray energy dispersive spectroscopy combining differential x-ray absorption and extrapolation, which are in agreement with the overall 3-D size statistic distribution results obtained through analysing various samples along various directions. Furthermore, the fabricated wedge-shape structure provides a platform on which to study the dependence of the interfacial strain on the variation of the thickness.     

Martensitic transformation in Ni-Mn-Ga alloys

Single crystals of different compositions in shape memory alloys Ni-Mn-Ga have been studied by electron and low temperature X-ray diffraction as well as by differential scanning calorimetry. It is shown that the cooling-induced martensitic phases are long-periodic ones modulated along the (110) directions by a transverse wave of atomic shifts with 5 and 7 atomic layers periodicity for the alloys studied exhibiting a martensitic transformation at 180 K and 446 K, respectively. The transformation heats appeared to be about 10 times different for both alloys.     

多壁碳纳米管的爆轰改性

为研究爆轰反应对多壁碳纳米管(MWCNTs)形貌与物相的影响,将按一定质量配比制备的MWCNTs混合炸药在密闭的反应釜内引爆,并利用透射电镜和X射线衍射仪对爆轰前、后MWCNTs的形貌与物相分别进行了表征。结果发现：MWCNTs的质量分数在30%~40%时,混合炸药能够顺利起爆,并可收集到大量的样品;爆轰反应后,MWCNTs的形貌与物相发生了巨大变化,由管状结构变成以碳片、碳棒、碳球为主的结构,并有明显的团聚现象;有少量MWCNTs依附于碳片等结构边缘;样品以不定型碳为主,其石墨化程度远低于初始MWCNTs,并随着MWCNTs质量比的增大,样品的石墨化程度增大。

     

软X射线条纹相机光阴极能谱响应灵敏度

通过对条纹相机光阴极在光电转换过程中光电子产生过程的分析,推导了光阴极在软X射线波段的能谱响应灵敏度计算公式,并运用该公式探讨了阴极厚度、掠入射角度等参数对能谱响应灵敏度的影响,计算并分析了Au,CsI在0.1~10keV范围内的能谱响应曲线和特性,并利用标定试验数据对共识和模型的可靠性进行了验证。结果表明,CsI阴极的最佳厚度在60nm左右,Au阴极的最佳厚度在10nm左右;CsI阴极的能谱响应灵敏度比Au阴极高1~2量级。