It has become very important to study and find optimal conditions for imaging electron-beam (e-beam) sensitive materials in scanning transmission electron microscopy under low electron-dose with high signal-to-noise ratio (SNR). Convergence and collection angles and electron-probe current are essential parameters. However, these parameters have rarely been discussed in a systematic way. In this paper, the illumination and collection conditions are optimized according to the resolution requirement of different materials by adjusting the condenser and intermediate lenses in a commercial transmission electron microscope. To demonstrate the significance of optimizing these parameters, two examples, zeolite MFI and metal–organic framework (MOF) MIL-101, are taken among the sensitive materials, with the most important electron incidences along the [010] and <110> directions, respectively. High SNR atomic resolution images of MFI are obtained with e-beam current as low as 0.50 pA, reaching information transfer for reflection up to 18 0 2 corresponding to d-spacing of 0.11 nm, close to the resolution limit of 0.098 nm from resolvable diffraction limit. MOF MIL-101 is characterized under an even lower e-beam 0.2 pA to avoid severe beam damage. High-quality annular dark and bright field images are obtained, which proves the wide applicability of this method on more e-beam sensitive materials. 相似文献
Designs, Codes and Cryptography - According to a magnific method due to I. Tamo and A. Barg, a class of polynomials over finite fields, called good polynomials, was introduced and used to construct... 相似文献
A novel single-atom Ni(II) catalyst ( Ni-OH ) is covalently immobilized onto the nano-channels of mesoporous Santa Barbara Amorphous (SBA)-15 particles and isotropic Anodized Aluminum Oxide (AAO) membrane for confined-space ethylene extrusion polymerization. The presence of surface-tethered Ni complexes ( Ni@SBA-15 and Ni@AAO ) is confirmed by the inductively coupled plasma-optical emission spectrometry (ICP-OES) and X-ray photoelectron spectroscopy (XPS). In the catalytic spinning process, the produced PE materials exhibit very homogeneous fibrous morphology at nanoscale (diameter: ~50 nm). The synthesized PE nanofibers extrude in a highly oriented manner from the nano-reactors at ambient temperature. Remarkably high Mw (1.62×106 g mol−1), melting point (124 °C), and crystallinity (41.8 %) are observed among PE samples thanks to the confined-space polymerization. The chain-walking behavior of surface tethered Ni catalysts is greatly limited by the confinement inside the nano-channels, leading to the formation of very low-branched PE materials (13.6/1000 C). Due to fixed supported catalytic topology and room temperature, the filaments are expected to be free of entanglement. This work signifies an important step towards the realization of a continuous mild catalytic-spinning (CATSPIN) process, where the polymer is directly synthesized into fiber shape at negligible chain branching and elegantly avoiding common limitations like thermal degradation or molecular entanglement. 相似文献
In this work, ultrafine Cu1.5Mn1.5O4 spinel nanoparticles were successfully synthesized by a sol–gel method combined with two complexing agents, which was firstly employed in the reductive transformation from p-nitrophenol into p-aminophenol. The effect of calcination temperature on the crystal phase and microstructure of Cu1.5Mn1.5O4 nanoparticles was investigated in this article. It was found that Cu1.5Mn1.5O4 nanoparticles with pure spinel phase can be obtained at 500 °C with the help of EDTA acid–citric acid complexing agents. Below 500 °C, there exists some Mn2O3 impure phase. SEM characterization indicated that the particle size of the spinel Cu1.5Mn1.5O4 rapidly increases above 600 °C. The catalytic experimental results show that the Cu1.5Mn1.5O4 nanoparticles prepared at 500 °C exhibit the highest catalytic activity which is even superior to some precious metal catalysts. With the calcination temperature increasing, the catalytic activity of Cu1.5Mn1.5O4 spinel nanoparticles gradually degrades which can be ascribed to the particle size growth of Cu1.5Mn1.5O4. It can also be observed that all the oxide samples, namely CuO, Mn2O3 and Cu1.5Mn1.5O4, possess certain catalytic ability for the transformation from p-nitrophenol into p-aminophenol. However, the catalytic activity of Cu1.5Mn1.5O4 spinel nanoparticles is obviously higher than CuO and Mn2O3. Especially, Mn2O3 alone has very poor catalytic activity in the reduction of p-nitrophenol.