In Situ Observation of Structural and Optical Changes of Phase-Separated Ag-Cu Nanoparticles during a Dewetting Process via Transmission Electron Microscopy.

Metallic nanoparticles with localized surface plasmon resonance have suitable optical properties for various applications such as optical filters, efficient photocatalysts, and high-sensitivity sensors. Phase-separated plasmonic nanoparticles with heterogeneous metastructures exhibit unique resonance features with separate optical field enhancements in each phase and hot electron transfer across the interface. Hence, interface engineering is crucial, particularly for catalyst applications. In this study, we investigated the evolution of the interface at high temperatures during nanoparticle formation using the dewetting method. We selected a Ag-Cu binary alloy system as a representative case and observed the nanoparticles via in situ transmission electron microscopy using a dedicated specimen heating holder. In situ elemental mapping revealed that the initial as-deposited film, which was composed of core-shell structures with Ag cores and Cu shells, converted into phase-separated Janus nanoparticles through marbled structures. A major structural change was observed at approximately 200 °C, which was in agreement with optical measurements. These results confirmed that the optical properties and metastructures of the phase-separated nanoparticles could be tuned by selecting the appropriate temperature and duration of the heat treatment.

Methods for Calibration of Specimen Temperature During In Situ Transmission Electron Microscopy Experiments.

One of the biggest challenges for in situ heating transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) is the ability to measure the local temperature of the specimen accurately. Despite technological improvements in the construction of TEM/STEM heating holders, the problem of being able to measure the real sample temperature is still the subject of considerable discussion. In this study, we review the present literature on methodologies for temperature calibration. We analyze calibration methods that require the use of a thermometric material in addition to the specimen under study, as well as methods that can be performed directly on the specimen of interest without the need for a previous calibration. Finally, an overview of the most important characteristics of all the treated techniques, including temperature ranges and uncertainties, is provided in order to provide an accessory database to consult before an in situ TEM/STEM temperature calibration experiment.

Development of 2000 K Class High Temperature In Situ Transmission Electron Microscopy of Nanostructured Materials via Resistive Heating.

We report the development of a new type of a 2000 K class high temperature stage for transmission electron microscopy (TEM) of various shaped nanostructured materials, i.e., nanometer-sized isolated nanostructures, such as particles, fibers, and thin films, and nanocrystalline bulk materials. The maximum temperature of the heating stage was 300­700 K higher than that of prevailing heating stages. In addition, we found that since the structure of the developed heating stage is simple, the stage can be applied to most of transmission electron microscopes without any additional modification. The stability of the heating stage was confirmed by In Situ high-resolution observation of the lattice fringes of the zirconium dioxide nanoparticles heated at 1183 K. We observed In Situ the nanoscale structural variation of titanium plate surfaces around 900 K and the melting of nanocrystalline iron thin films around 1808 K by this method. It was demonstrated that the heating stage is useful for the analysis of high temperature structural dynamics of various shaped nanostructured materials.

Current status and future directions for in situ transmission electron microscopy.

This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs and private sector entities (predominantly commercial vendors) during a workshop, held at the Center for Nanoscale Science and Technology- National Institute of Science and Technology (CNST-NIST), are discussed. We provide a comprehensive review of the scientific needs and future instrument and technique developments required to meet them.

Design of a 300-kV gas environmental transmission electron microscope equipped with a cold field emission gun.

A new in situ environmental transmission electron microscope (ETEM) was developed based on a 300 kV TEM with a cold field emission gun (CFEG). Particular caution was taken in the ETEM design to assure uncompromised imaging and analytical performance of the TEM. Because of the improved pumping system between the gun and column, the vacuum of CFEG was largely improved and the probe current was sufficiently stabilized to operate without tip flashing for 2-3 h or longer. A high brightness of 2.5 × 10(9) A/cm(2) sr was measured at 300 kV, verifying the high quality of the CFEG electron beam. A specially designed gas injection-heating holder was used in the in situ TEM study at elevated temperatures with or without gas around the TEM specimen. Using this holder in a 10 Pa gas atmosphere and specimen temperatures up to 1000°C, high-resolution ETEM performance and analysis were achieved.