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When using bifunctional core@shell catalysts, the stability of both the shell and core–shell interface is crucial for catalytic applications. In the present study, we elucidate the stability of a CuO/ZnO/Al2O3@ZSM-5 core@shell material, used for one-stage synthesis of dimethyl ether from synthesis gas. The catalyst stability was studied in a hierarchical manner by complementary environmental transmission electron microscopy (ETEM), scanning electron microscopy (SEM) and in situ hard X-ray ptychography with a specially designed in situ cell. Both reductive activation and reoxidation were applied. The core–shell interface was found to be stable during reducing and oxidizing treatment at 250°C as observed by ETEM and in situ X-ray ptychography, although strong changes occurred in the core on a 10 nm scale due to the reduction of copper oxide to metallic copper particles. At 350°C, in situ X-ray ptychography indicated the occurrence of structural changes also on the µm scale, i.e. the core material and parts of the shell undergo restructuring. Nevertheless, the crucial core–shell interface required for full bifunctionality appeared to remain stable. This study demonstrates the potential of these correlative in situ microscopy techniques for hierarchically designed catalysts.
A tomographic heating holder for transmission electron microscopy that can be used to study supported catalysts at temperatures of up to ~1,500°C is described. The specimen is placed in direct thermal contact with a tungsten filament that is oriented perpendicular to the axis of the holder without using a support film, allowing tomographic image acquisition at high specimen tilt angles with minimum optical shadowing. We use the holder to illustrate the evolution of the active phases of Pt nanoparticles on carbon black and PtPd nanoparticles on γ-alumina with temperature. Particle size distributions and changes in active surface area are quantified from tilt series of images acquired after subjecting the specimens to increasing temperatures. The porosity of the alumina support and the sintering mechanisms of the catalysts are shown to depend on distance from the heating filament.
We use off-axis electron holography in the transmission electron microscope (TEM) to study magnetic flux closure (FC) states in self-assembled nanoparticle rings that each contain between five and eleven 25-nm-diameter Co crystals. Electron holograms are acquired at room temperature in zero-field conditions after applying chosen magnetic fields to the samples in situ in the TEM by partially exciting the conventional microscope objective lens. Mean inner potential contributions to the phase shift are determined by turning the samples over, and subsequently subtracted from each recorded phase image to obtain magnetic induction maps. Our results show that most nanoparticle rings form FC remanent magnetic states, and occasionally onion-like states. Although the chiralities (the directions of magnetization) of the FC states are determined by the shapes, sizes and positions of the constituent nanoparticles, reproducible magnetization reversal of each ring can be achieved by using an out-of-plane magnetic field of between 1600 and 2500 Oe.
Closely-spaced ferromagnetic nanoparticles are of interest for applications that include data storage, magnetic imaging and drug delivery. Here, we use off-axis electron holography and micromagnetic simulations to study the magnetic properties of iron nanoparticles encapsulated in three-dimensional arrays of carbon nanotubes. The nanotubes constrain the shapes, sizes and separations of the nanoparticles, as well protecting them from oxidation. We record magnetic induction maps from individual particles that each contain a single magnetic domain. We also discuss the use of electron holography to assess magnetostatic interactions between adjacent particles.
The mean inner potentials of wurtzite GaN nanowires are measured using off-axis electron holography in the transmission electron microscope (TEM). The nanowires have a circular cross-section and are suspended across holes in a holey carbon film, resulting in an accurate knowledge of their thickness profiles and orientations. They are also free of the implantation and damage that is present in mechanically-polished ion-milled TEM specimens. The effect of a thin amorphous coating, which is present on the surfaces of the nanowires, on measurements of their mean inner potential is assessed. A value for the mean inner potential of GaN of (16.7 ± 0.3) V is obtained from these samples.
One of the most widely studied types of magnetic nanostructure is that used in devices based on the giant magnetoresistance (GMR) or tunnel magnetoresistance (TMR) phenomena. In order to understand the behaviour of these materials it is important to be able to follow their magnetisation reversal mechanism, and one of the techniques enabling micromagnetic studies at the sub-micron scale is transmission electron microscopy. Two techniques can be used: Lorentz transmission electron microscopy and off-axis electron holography, both of which allow the magnetic domain structure of a ferromagnetic material to be investigated dynamically in real-time with a resolution of a few nanometres. These techniques have been used in combination with in situ magnetizing experiments, to carry out qualitative and quantitative studies of magnetization reversal in a range of materials including spin-tunnel junctions, patterned thin film elements and magnetic antidot arrays. Quantitative analysis of the Lorentz TEM data has been carried out using the transport of intensity equation (TIE) approach.
Two recent developments related to the application of off-axis electron holography to the characterization of magnetic and electrostatic fields in nanoscale materials and devices are described. The first is based on the design and implementation of a three-contact electrical biasing specimen holder that allows electron holograms to be recorded from samples as they are tilted to angles of up to ±70° with voltages applied to them in situ in the electron microscope. The second relates to the prospect of characterizing magnetic vector fields in materials in three dimensions using electron holography.
The lichen Trapelia involuta from uraniferous spoil heaps in Cornwall, England, growing directly on the secondary uranium minerals, metazeunerite and metatorbernite, was examined by field-emission scanning electron microscopy and transmission electron microscopy to assess the effect of Trapelia on uranium migration. We observed metazeunerite, sericite and scorodite as well as unidentified Fe-, Pb/As-, Fe/As-, Al/P-, Pb-bearing minerals concentrated in the lichen exciple and medulla. In addition, metazeunerite also occurred in the epithecium. The chemistries, sizes, and occurrences of the above minerals in the lichen suggest that fixation of U as well as Pb, As, Fe, and Al is dependent on lichen physiological processes. We suggest Trapelia accumulates these elements from groundwater and precipitates the above minerals within specific tissues. Our results indicate that some lichens retard uranium migration by accumulating uranium from groundwater and forming uranium-bearing minerals within their tissues.
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