Model-based quantification of EELS spectra: Including the fine structure

An extension to model-based electron energy loss spectroscopy (EELS) quantification is reported to improve the possibility of modelling fine structure changes in electron energy loss spectra. An equalisation function is used in the energy loss near edge structure (ELNES) region to model the differences between a single atom differential cross section and the cross section for an atom in a crystal. The equalisation function can be shown to approximate the relative density of unoccupied states for the given excitation edge. On a set of 200 experimental h-BN spectra, this technique leads to statistically acceptable models resulting into unbiased estimates of relative concentrations and making the estimated precisions come very close to the Cramér-Rao lower bound (CRLB). The method greatly expands the useability of model-based EELS quantification to spectra with pronounced fine structure. Another benefit of this model is that one also gets an estimate of the unoccupied density of states for a given excitation edge, without having to do background removal and deconvolution, making the outcome intrinsically more reliable and less noisy.     

Advances in EELS spectroscopy by using new detector and new specimen preparation technologies

First results obtained with a Gatan UHV Enfina system, which was attached to a VG HB 501 UX dedicated STEM, are reported. The Enfina system is based on a CCD detector and offers, compared to the previously used photodiode array, a narrower point‐spread function, higher sensitivity, and faster read‐out capabilities. These improvements are demonstrated with electron energy‐loss measurements on various oxides, such as Al₂O₃, TiO₂ and SrTiO₃. It is shown that a better energy resolution is achieved and that acquisition of high‐energy absorption edges with a reasonable signal‐to‐noise ratio becomes possible. Furthermore, we report on the influence of the TEM specimen quality on the energy‐loss spectra. Thin amorphous layers at the specimen surfaces, which are induced by ion‐milling processes, can modify specific electron energy‐loss near‐edge structure features. We found that for the investigated ceramics the use of low‐energy ion‐milling systems is highly recommended, since the loss of energy‐loss near‐edge structure details by the presence of the amorphous layers is considerably reduced. This is especially true for very thin specimens.     

Electron energy-loss spectroscopy study of thin film hafnium aluminates for novel gate dielectrics

We have used conventional high‐resolution transmission electron microscopy and electron energy‐loss spectroscopy (EELS) in scanning transmission electron microscopy to investigate the microstructure and electronic structure of hafnia‐based thin films doped with small amounts (6.8 at.%) of Al grown on (001) Si. The as‐deposited film is amorphous with a very thin (～0.5 nm) interfacial SiO_x layer. The film partially crystallizes after annealing at 700 °C and the interfacial SiO₂‐like layer increases in thickness by oxygen diffusion through the Hf‐aluminate layer and oxidation of the silicon substrate. Oxygen K‐edge EELS fine‐structures are analysed for both films and interpreted in the context of the films’ microstructure. We also discuss valence electron energy‐loss spectra of these ultrathin films.     

Surface effects in the energy loss near edge structure of different cobalt oxides

The energy loss near edge structure (ELNES) of the O-K and Co-L edges of both Co(3)O(4) and CoO particles were studied. Significant changes between the edge and nearby thicker regions are found for the O-K edge, the Co-L edge, the O/Co atomic ratio, the separation between the prepeaks in the O-K edge, as well as the L(3)/L(2) intensity ratios in the Co-L edge. These reflect the changes in the average oxidation state of the specimen from the edge to nearby thicker regions. These variations originate from a surface layer which dominates the results near the edge of the particles. These variations allow us to infer the surface structure, which indicates that both particles are encapsulated by different non-stoichiometric oxides.     

抗流量饱和系统控制阀节流损失降低研究

负载敏感系统具有良好的多执行器并行控制特性和高能量效率,被广泛应用于中小型工程装备和工业设备中,主要有阀前补偿系统和抗流量饱和阀后补偿系统两种。目前市场上应用的阀多在补偿阀之后仍设置有换向段,存在大的节流。针对此问题,设计了新型阀后补偿多路阀,降低阀口压力损失。建立了仿真模型,进行仿真研究,并与原多路阀进行仿真对比。新设计的多路阀阀口压力损失比原多路阀可减少0.8 MPa,能量损失降低7.5%。     

Electron energy-loss near edge structure (ELNES) of InGaN quantum wells

Lasers and light‐emitting diodes (LEDs) that emit in the blue to green region are often based on In_xGa_1–xN quantum well structures. Ionization edges in the electron energy‐loss spectrum contain fine structures (called the energy‐loss near edge structure (ELNES)) and provide information about the electronic structure. In this paper we compare the experimental and calculated ELNES for the N‐K ionization edge of In_xGa_1–xN quantum wells. When the effects of the core‐hole are included in the calculations, agreement between experimental and calculated spectra is very good. Strain has been shown to accentuate the effects of In on the ELNES and moves the ionization edge onset down in energy, relative to the other features. These results suggest that ELNES may provide an alternative method to lattice imaging to determine the presence of strain in this system.     

Electron inelastic scattering and anisotropy: The two-dimensional point of view

The measurement of the electronic structure of anisotropic materials using energy loss near edge structure (ELNES) spectroscopy is an important field of microanalysis in transmission electron microscopy. We present a novel method to study the angular dependence of electron inelastic scattering in anisotropic materials. This method has been applied to the study of 1s-->pi* and sigma* transitions on the carbon K edge in pyrolitic graphite. An excellent agreement between experimental and theoretical two-dimensional scattering patterns has been found. In particular, the need of a fully relativistic calculation of the inelastic scattering cross-section to explain the experimental results is demonstrated.     

TEM-EELS study of low-friction superlattice TiAlN/VN coating: the wear mechanisms

A 20–50 nm thick tribofilm was generated on the worn surface of a multilayer coating TiAlN/VN after dry sliding test against an alumina counterpart. The tribofilm was characterized by applying analytical transmission electron microscopy techniques with emphasis on detailed electron energy loss spectrometry and energy loss near edge structure analysis. Pronounced oxygen in the tribofilm indicated a predominant tribo-oxidation wear. Structural changes in the inner-shell ionization edges of N, Ti and V suggested decomposition of nitride fragments.     

Spectroscopic imaging of electron energy loss spectra using ab initio data and function field visualization

We have devised a technique for spectral imaging using accurate ab initio electron energy loss near edge structure (ELNES) data and function field visualization. The technique is initially applied to a planar defect model in Si with different ring structures and no broken bonds where experimental probes are severely limited. The same model with B doping is also considered. It is shown that specific deviations in different energy ranges of the ELNES spectra are correlated with different structural components of the models.     

A proposal for dichroic experiments in the electron microscope

Building upon the similarities between inelastic electron scattering and X-ray absorption we show that dichroism can be observed in electron energy loss spectrometry (EELS) in the transmission electron microscope (TEM). Natural or magnetic linear dichroism can be studied in electron scattering experiment with definite wave vector transfer in the interaction.The detection of circular dichroism in the TEM relies on interferometric EELS in a particular scattering geometry that allows extraction of the mixed dynamic form factor from energy loss spectra. Similarities between dichroic signals in energy loss near edge structures and X-ray absorption near edge structures are discussed, and a new experimental setup for dichroic measurements in the TEM is proposed.     

Momentum-resolved energy loss near edge structure in SrCu2(BO3)2

In this paper, we present a detailed study of the electronic structure of the strontium copper borate SrCu(2)(BO(3))(2) using momentum-resolved energy loss near edge structure (ELNES) and ab initio band structure calculations. Information on the energy position, the character and the spatial orientation of the unoccupied states of this compound can be efficiently retrieved taking advantage of the nearly parallel illumination available in a conventional transmission electron microscope (CTEM). These results shed light on the bonding mechanisms taking place in complex oxides such as SrCu(2)(BO(3))(2).     

Combining FIB milling and conventional Argon ion milling techniques to prepare high‐quality site‐specific TEM samples for quantitative EELS analysis of oxygen in molten iron

This paper reports a procedure to combine the focused ion beam micro‐sampling method with conventional Ar‐milling to prepare high‐quality site‐specific transmission electron microscopy cross‐section samples. The advantage is to enable chemical and structural evaluations of oxygen dissolved in a molten iron sample to be made after quenching and recovery from high‐pressure experiments in a laser‐heated diamond anvil cell. The evaluations were performed by using electron energy‐loss spectroscopy and high‐resolution transmission electron microscopy. The high signal to noise ratios of electron energy‐loss spectroscopy core‐loss spectra from the transmission electron microscopy thin foil, re‐thinned down to 40 nm in thickness by conventional Argon ion milling, provided us with oxygen quantitative analyses of the quenched molten iron phase. In addition, we could obtain lattice‐fringe images using high‐resolution transmission electron microscopy. The electron energy‐loss spectroscopy analysis of oxygen in Fe_0.94O has been carried out with a relative accuracy of 2%, using an analytical procedure proposed for foils thinner than 80 nm. Oxygen K‐edge energy‐loss near‐edge structure also allows us to identify the specific phase that results from quenching and its electronic structure by the technique of fingerprinting of the spectrum with reference spectra in the Fe‐O system.     

Numerical evaluation of flow and performance of turbo pump inducers

Steady state flow calculations are executed for turbo-pump inducers of modern design to validate the performance of Tascflow code. Hydrodynamic performance of inducers is evaluated and structure of the passage flow and leading edge recirculation are also investigated. Calculated results show good coincidence with experimental data of static pressure performance and velocity profiles over the leading edge. Upstream recirculation, tip leakage and vortex flow at the blade tip and near leading edge are main sources of pressure loss. Amount of pressure loss from the upstream to the leading edge corresponds to that of whole pressure loss through the blade passage. The viscous loss is considerably large due to the strong secondary flow. There appears more stronger leading edge recirculation for the backswept inducer. and this increases the pressure loss. However, blade loading near the leading edge is considerably reduced and cavitation inception delayed.     

Electron energy-loss near-edge structure studies at the atomic level: reliability of the spatial difference technique

The spatial difference technique was applied to determine the interface‐specific components of electron energy‐loss near‐edge structures and the results are in good agreement to those obtained by atomic column resolved measurements averaged over one atomic layer. In previous studies an experimental set‐up had been chosen where the scanning areas, which are used to measure electron energy‐loss spectra, were symmetrical in respect to the location of the investigated interfaces. In the present study, an asymmetric setting of the scanning areas was applied, which allows the interfacial signals to be determined directly. Comparing the results of the different measurements shows that the spatial difference technique is valid and can be used to obtain information about the electronic structure of interfaces where single atomic column resolved measurements are not yet possible.     

Stoichiometry and valence measurements of niobium oxides using electron energy-loss spectroscopy

Qualitative and quantitative electron energy‐loss spectroscopy analyses have been performed on niobium and stable niobium oxides (NbO, NbO₂ and Nb₂O₅). At integration windows (Δ) greater than 75 eV, k‐factor analysis can be used to distinguish between the stoichiometry of the three oxides within 5.7% error. As seen in other metal oxides, with increasing oxidation state the metal ionization edges shift to higher energies relative to the O‐K edge. Normalized M_2,3 white‐line intensities show a strong correlation with 4d occupancy for each compound. The data are in correspondence with that observed in the literature for 4d transition metals using normalized L_2,3 white lines. Lastly, a distinctive energy‐loss near‐edge, structure of the O‐K edge was observed for each oxide, which could be used as a fingerprint for analysis of unknowns.     

Structure influence on the operating limit range and mixing performance of non-axisymmetric jet pump

Although cavitation chocked jet pumps guarantee a steady and accurate liquid mixture, the existing pumps have the shortcomings of big energy loss and small cavitation working range. In the current study, aiming at enhancing the performance of the cavitation mixing devices, an innovative non-axisymmetric jet pump design is proposed. The cavitation characteristics and the mixing performance of the new design have been investigated by both computational simulation and experimental testing. Based on the results of computational fluid dynamics (CFD), it is found that the cavitation on the suction tube side is strengthened due to the turbulence caused by the abrupt change in the local flow channel structure, while the cavitation on the opposite side is weakened due to the gradual flow channel structure. Our experimental testing results prove that our new design can provide a steady mixing ratio as long as the non-axisymmetric vapor cloud steadily covers the suction tube outlet. Furthermore, geometric parameters (convergent angle, divergent angle, throat length and area ratio) of the device have been optimized through the orthogonal analysis. The critical pressure ratio of the optimized device ranges from 0.76 to 0.63 when the critical flow ratio is in the range of 0–10%, which indicates that the optimized device has much less energy loss and a wider working range than the current axisymmetric cavitating jet pumps. Through quantitative energy loss analysis, we have found that the cavitation maintenance corresponds to the greatest energy loss in the jet pumps, yet our non-axisymmetric structure design could effectively reduces energy loss. The current research reveals the physical mechanism on how a non-axisymmetric structure affects the cavitation characteristics as well as the performance of jet pumps.     

HREM image contrast from supported small metal particles

HREM, image calculations and small probe diffraction/AEM have been used to characterize structure and contrast of supported small metal particles of ≤5 nm diameter. Such small particles are thought to be active species in industrial applications such as in heterogeneous catalysis where, in general, the particles employed as catalysts are supported. Image calculations (HREM and diffraction contrast) carried out at both 200 keV and 400 keV at various defoci and support thicknesses have shown that in HREM, particle images are obscured by the support contrast with the loss of edge definition and particles appear to be smaller than they actually are. The particle visibility is better at 400 keV. The calculations have also indicated that particle shape varies as a function of support thickness and defocus. The results have clear implications for identification and interpretation of surface structure of the supported small particles accurately by HREM if not performed under controlled conditions and for determining their size and shape.     

破拆机器人负载敏感系统多臂复合动作能量回收研究

 破拆机器人臂系负载敏感系统具有功率自适应节能降耗、结构紧凑等特点,应用十分广泛。然而负载敏感系统中负载敏感泵流量压力仅与系统最大负载相适应,导致多臂复合动作时小负载回路上压力补偿阀能量损失较大。为进一步降低能耗,利用液压马达回收小负载回路压力补偿阀的能量损失,并带动液压泵将回收能量储存在蓄能器中,蓄能器回收能量通过扭矩耦合的方式回馈至主泵实现能量回收。通过AMESim建模仿真结果表明,增加能量回收系统可使复合动作能量回收利用率提升20%以上,系统阶跃响应与未安装能量回收的系统响应基本一致,且速度振荡减小改善了瞬态响应。     

Simulation of electron energy loss near-edge structure at the Al and N K edges and Al L(23) edge in cubic aluminium nitride

Calculations of electron energy near edge structures (ELNES) are compared with experimental data obtained in a high-resolution transmission electron microscope. This study concerns small precipitates of aluminium nitride in low carbon steel. The ELNES technique allows to clearly establish that these precipitates crystallize in a cubic rather than in a hexagonal crystallographic cell. The influence on simulated spectra of different parameters are investigated: the size of the atomic shell and its relation with the electron inelastic mean free path. We also examine the influence of the core hole and the sensitivity to cell parameters. We particularly examine the Al L(23) near edge structure and features relating to the different transition channels (A(1g), E(g) and T(2g)). Results of a multiple scattering and band structure calculations using ICXANES and WIEN97 codes, respectively, are compared in the region from 0 to 30 eV above the edge onsets. Both calculations are in a rather good agreement.     

基于区块链和边缘代理的电力资源动态监测调度系统

以电力系统内分布式电源的渗透率为出发点,提出了基于区块链和边缘计算的电力系统调度资源动态监测系统。分析了区块链中的区块结构以及边缘代理的基本模型,提出了基于区块链的能源互联网系统。针对电力调度资源监测进行建模,分析了包括风电、光伏、储能和需求响应等形式在内的调度资源模型,说明了可调度资源监视的基本内容。提出了基于区块链和边缘代理的调度资源监视系统架构,分析了系统的硬件结构,说明了数据对比分析流程,利用边缘代理进行数据资源监视。仿真结果表明,该系统在调度管理以及数据监视方面是有效性的。