In-focus electron microscopy of frozen-hydrated biological samples with a Boersch phase plate

We report the implementation of an electrostatic Einzel lens (Boersch) phase plate in a prototype transmission electron microscope dedicated to aberration-corrected cryo-EM. The combination of phase plate, C_s corrector and Diffraction Magnification Unit (DMU) as a new electron-optical element ensures minimal information loss due to obstruction by the phase plate and enables in-focus phase contrast imaging of large macromolecular assemblies. As no defocussing is necessary and the spherical aberration is corrected, maximal, non-oscillating phase contrast transfer can be achieved up to the information limit of the instrument. A microchip produced by a scalable micro-fabrication process has 10 phase plates, which are positioned in a conjugate, magnified diffraction plane generated by the DMU. Phase plates remained fully functional for weeks or months. The large distance between phase plate and the cryo sample permits the use of an effective anti-contaminator, resulting in ice contamination rates of <0.6 nm/h at the specimen. Maximal in-focus phase contrast was obtained by applying voltages between 80 and 700 mV to the phase plate electrode. The phase plate allows for in-focus imaging of biological objects with a signal-to-noise of 5-10 at a resolution of 2-3 nm, as demonstrated for frozen-hydrated virus particles and purple membrane at liquid-nitrogen temperature.     

A method to determine the local surface profile from reconstructed exit waves

Reconstructed exit waves are useful to quantify unknown structure parameters such as the position and composition of the atom columns at atomic scale. Existing techniques provide a complex wave in a flat plane which is close to the plane where the electrons leave the atom columns. However, due to local deviation in the flatness of the exit surface, there will be an offset between the plane of reconstruction and the actual exit of a specific atom column. Using the channelling theory, it has been shown that this defocus offset can in principle be determined atom column-by-atom column. As such, the surface roughness could be quantified at atomic scale. However, the outcome strongly depends on the initial plane of reconstruction especially in a crystalline structure. If this plane is further away from the true exit, the waves of the atom columns become delocalized and interfere mutually which strongly complicates the interpretation of the exit wave in terms of the local structure. In this paper, we will study the delocalization with defocus using the channelling theory in a more systematic way.     

Efficient parallel implementation of iterative reconstruction algorithms for electron tomography

Electron tomography (ET) combines electron microscopy and the principles of tomographic imaging in order to reconstruct the three-dimensional structure of complex biological specimens at molecular resolution. Weighted back-projection (WBP) has long been the method of choice since the reconstructions are very fast. It is well known that iterative methods produce better images, but at a very costly time penalty. In this work, it is shown that efficient parallel implementations of iterative methods, based primarily on data decomposition, can speed up such methods to an extent that they become viable alternatives to WBP. Precomputation of the coefficient matrix has also turned out to be important to substantially improve the performance regardless of the number of processors used. Matrix precomputation has made it possible to speed up the block-iterative component averaging (BICAV) algorithm, which has been studied before in the context of computerized tomography (CT) and ET, by a factor of more than 3.7. Component-averaged row projections (CARP) is a recently introduced block-parallel algorithm, which was shown to be a robust method for solving sparse systems arising from partial differential equations. It is shown that this algorithm is also suitable for single-axis ET, and is advantageous over BICAV both in terms of runtime and image quality. The experiments were carried out on several datasets of ET of various sizes, using the blob model for representing the reconstructed object.     

Electron beam lithography-assisted fabrication of Au nano-dot array as a substrate of a correlated AFM and confocal Raman spectroscopy

This paper documents a study of an Au nano-dot array that was fabricated by electron beam lithography on a glass wafer. The patterns that had features of 100nm dots in diameter with a 2-mum pitch comprised a total area of 200x200mum(2). The dot-shaped Cr underlayer was open to the air after developing Poly(methyl methacrylate) (PMMA). When dipped into the Cr etchant, the exposed Cr layer was eliminated from the glass wafer in a short period of time. In order to ultimately fabricate the Ti/Au dot arrays, Ti and Au were deposited onto the arrays with a thickness of 2 and 40nm, respectively. The lift-off procedure was carried out in the Cr etchant using sonication in order to completely remove the residual Cr/PMMA layer. The fabricated Au nano-dot array was then immersed in an Ag enhancing solution and then into an ethanol solution containing (N-(6-(Biotinamido)hexyl)-3'-(2'-pyridyldithio)-propionamide (Biotin-HPDP). The substrate was analyzed using a correlated atomic force microscopy (AFM) and confocal Raman spectroscopy. Through this procedure, position-dependent surface-enhanced Raman spectroscopy (SERS) signals could be obtained.     

Planar diffracted-beam interferometry/holography

A method to interfere planar electron diffracted beams that have been created by a primary electron beam passing through a crystal specimen has been invented and referred to as planar diffracted-beam interferometry/holography (planar DBI/H). Planar DBI/H is able to measure the intensity and coherence properties of the diffracted electron beams. When the diffracted electron beams are energy filtered, planar DBI/H is also able to measure the intensity and coherence properties of the zero-loss electrons, phonon-loss electrons and plasmon-loss electrons. These coherence properties are useful to help our understanding of the Stobbs factor and the properties of advanced materials, necessary for our understanding of nanoscience and the development of nanotechnology.     

锰红柱石中Mn~（3＋）谱的分析

本文利用锰红柱石的吸收光谱,考虑到锰红柱石中Ｍｎ３＋处于一种Ｃ２ｖ（Ｃ２＇＇）的低对称晶位,采用一简化的强场方案,把单电子晶场矩阵元用自旋允许吸收带代替,克服了多参数的困难．计算出了锰红柱石中处于八面体配位的Ｍｎ３＋的电子能谱,对锰红柱石的分析首次获得了较为理想的理论计算结果,并对Ｍｎ３＋和Ｆｅ３＋谱带的识别提出了新的看法．     

插拔式单晶LaB6阴极制备与应用

插拔式单晶LaB₆阴极是我国电子束类高端仪器及设备必需的关键元件和发展的主要瓶颈。本文围绕插拔式单晶LaB₆,开展了单晶精密加工、高效加热、机械夹持等制备工艺研究,并对阴极的发射性能、静态寿命等进行了测试,还开展了阴极在多个领域的应用研究。研究结果表明,所制备的阴极在电子发射性能及工作寿命方面均达到与进口阴极相当的水平,可应用于增材制造、扫描电镜、高分辨率CT等领域。     

Effects of microstructural heterogeneity on very high cycle fatigue properties of 7050-T7451 aluminum alloy friction stir butt welds

In this study, the very high cycle fatigue (VHCF) properties of 7050-T7451 aluminum alloy and its friction stir welding (FSW) butt welds have been investigated. The results show that the failure of FSW joints still occurs at 7.0 × 10⁸ cycles. The fatigue properties of the FSW joints are superior to those of the base material, especially in the super long life regime. Most fatigue cracks initiate at the thermo-mechanically affected zone and heat affected zone on the advancing side of the FSW joints, and the susceptibility of these zones to fatigue is attributed to the metallurgical heterogeneity.     

Low temperature annealing of metals with electrical wind force effects

Conventional annealing is a slow, high temperature process that involves heating atoms uniformly, i.e., in both defective and crystalline regions. This study explores an electrical alternative for energy efficiency,where moderate current density is used to generate electron wind force that produces the same outcome as the thermal annealing process. We demonstrate this on a zirconium alloy using in-situ electron back scattered diffraction(EBSD) inside a scanning electron microscope(SEM) and juxtaposing the results with that from thermal annealing. Contrary to common belief that resistive heating is the dominant factor, we show that 5 × 10~4 A/cm~2 current density can anneal the material in less than 15 min at only135?C. The resulting microstructure is essentially the same as that obtained with 600?C processing for360 min. We propose that unlike temperature, the electron wind force specifically targets the defective regions, which leads to unprecedented time and energy efficiency. This hypothesis was investigated with molecular dynamics simulation that implements mechanical equivalent of electron wind force to provide the atomistic insights on defect annihilation and grain growth.     

Temperature-gradient induced microstructure evolution in heat-affected zone of electron beam welded Ti-6Al-4V titanium alloy

The heat-affected zone (HAZ) of electron beam welded (EBW) joint normally undergoes a unique heat-treating process consisting of rapid temperature rising and dropping stages, resulting in temperature-gradient in HAZ as a function of the distance to fusion zone (FZ). In the current work, microstructure, elements distribution and crystallographic orientation of three parts (near base material (BM) zone, mid-HAZ and near-FZ) in the HAZ of Ti-6Al-4V alloy were systematically investigated. The microstructure observation revealed that the microstructural variation from near-BM to near-FZ included the reduction of primary α (α_p) grains, the increase of transformed β structure (β_t) and the formation of various α structures. The rim-α, dendritic α and abnormal secondary α (α_s) colonies formed in the mid-HAZ, while the “ghost” structures grew in the near-FZ respectively. The electron probe microanalyzer (EPMA) and electron back-scattered diffraction (EBSD) technologies were employed to evaluate the elements diffusion and texture evolution during the unique thermal process of welding. The formation of the various α structures in the HAZ were discussed based on the EPMA and EBSD results. Finally, the nanoindentation hardness of “ghost” structures was presented and compared with nearby β_t regions.