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A 0.5-T pure-in-plane-field magnetizing holder for in-situ Lorentz microscopy
摘要： A side-entry specimen holder capable of applying a 0.5-tesla in-plane magnetic-induction field for in-situ transmission electron microscopy was developed. Three miniaturized electromagnets with 300 × 300-μm pole area and 180-μm pole gap are stacked along the electron-beam path in the holder. The middle magnet is used for magnetizing the specimen, which is inserted into the pole gap by using a 40-μm-width cantilever for atomic-force microscopy. The upper and lower magnets are used to keep the electron beam parallel to the optical axis. Magnetic-field magnitude was determined on the basis of experimentally measured electron-deflection angles and induction-field profiles along the electron-beam path calculated by finite element electromagnetic simulation. Magnetization reversal in 300-nm-thick Nd-Fe-B magnets from the saturated state was in-situ observed by using the holder and a 1-MeV cold-field-emission transmission electron microscope. The observation revealed that domain-wall pinning occurred in different manners at the c-plane and non-c-plane grain boundaries. The holder was thereby shown to be useful for analysis of magnetization-reversal behaviors of hard magnetic materials.
关键词： In situ transmission electron microscopy,Specimen holder,Magnetic domains,Finite element method,Lorentz microscopy,Hard magnetic material
更新于2025-09-23 15:21:01
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Phase transformation at controlled locations in nanowires by in situ electron irradiation
摘要： Solid state phase transformations have drawn great attention because they can be effectively exploited to control the microstructure and property of materials. Understanding the physics of such phase transformation processes is critical to designing materials with controlled structure and with desired properties. However, in traditional ex situ experiments, it is hard to achieve position controlled phase transformations or obtain desirable crystal phase on nanometer scale. Meanwhile the underlying mechanisms of the reaction processes are not fully understood due to the lack of direct and real-time observation. In this paper, we observe phase transformation from body-centered tetragonal PX-PbTiO3 to monoclinic TiO2(B) on the atomic scale by in situ electron irradiation during heat treatment in transmission electron microscope, at pre-defined locations on the sample. We demonstrate that by controlling the location of the incident electron beam, a porous TiO2(B) crystal structure can be formed at the desired area on the nanowire, which is difficult to achieve by traditional synthesis methods. Upon in situ heating, the Pb atoms in the crystal migrate out of the pristine nanowire through inelastic scattering under incident electrons while high temperature(> 400 °C) provides energy for the crystallization of TiO2(B) and the volatilization of a substantial number of Pb atoms, which makes the resultingTiO2(B) nanowires to be porous. In contrast, at temperatures < 400 °C, the segregated Pb atoms form Pb particles and the TiOx nanowires remain in the amorphous state. This work not only provides in situ visualization of the phase transition from the PX-PbTiO3 to monoclinic TiO2(B), but also suggests a crystallography engineering strategy to obtain the desired crystal phase at controlled locations on the nanometer scale.
关键词： controlled locations,phase transformation,in situ,transmission electron microscopy
更新于2025-09-16 10:30:52
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Nanoscale temperature measurement during temperature controlled in situ TEM using Al plasmon nanothermometry
摘要： Over recent years, the advent of microelectromechanical system (MEMS)-type microheaters has pushed the limits of temperature controlled in situ transmission electron microscopy (TEM). In particular, by enabling the observation of the structure of materials in their application environments, temperature controlled TEM provides unprecedented insights into the link between the properties of materials and their structure in real-world problems, a clear knowledge of which is necessary for rational development of functional materials with new or improved properties. While temperature is the key parameter in such experiments, accessing the precise temperature of the sample at the nanoscale during observations still remains challenging. In the present work, we have applied aluminium plasmon nanothermometry technique that monitors the temperature dependence of the volume plasmon of Al nanospheres using electron energy loss spectroscopy for in situ local temperature determination over a MEMS microheater. With access to local temperatures between room temperature to 550°C, we have assessed the spatial and temporal stabilities of the microheater when it operates at different setpoint temperatures both under vacuum and in the presence of a static H2 gas environment. Temperature comparisons performed under the two environments show discrepancies between local and setpoint temperatures.
关键词： in situ transmission electron microscopy,electron energy loss spectroscopy,volume expansion of metal,local temperature determination,volume plasmons shift
更新于2025-09-12 10:27:22
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Real-Time Electron Nanoscopy of Photovoltaic Absorber Formation from Kesterite Nanoparticles
摘要： Cu2ZnSnS4 nanocrystals are annealed in a Se-rich atmosphere inside a transmission electron microscope. During the heating phase, a complete S-Se exchange reaction occurs while the cation sublattice and morphology of the nanocrystals are preserved. At the annealing temperature, growth of large Cu2ZnSnSe4 grains with increased cation ordering is observed in real-time. This yields an annealing protocol which is transferred to an industrially-similar solar cell fabrication process resulting in a 33% increase in the device open circuit voltage. The approach can be applied to improve the performance of any photovoltaic technology that requires annealing because of the criticality of the process step.
关键词： cation ordering,Kesterite,photovoltaics,in situ transmission electron microscopy (TEM),annealing
更新于2025-09-12 10:27:22