The interaction of the electron beam with materials during TEM/STEM imaging often leads to radiation damage. While a variety of low-dose techniques can help mitigate beam damage, true dose management starts with knowing the precise total accumulated dose and dose rate that a sample has seen throughout an experiment. AXON Dose allows users to calibrate their instruments, track electron dose/dose rate across a sample as a function of time and location, and quantify the impact of dose on individual samples.

The development of microfabricated liquid cells has enabled dynamic studies of nanostructures within a liquid environment with electron microscopy. While such setups are most commonly found in transmission electron microscope (TEM) holders, their implementation in a scanning electron microscope (SEM) offers intriguing potential for multi-modal studies where the large chamber volume allows for the integration of multiple detectors. Here, we describe an electrochemical liquid cell SEM platform that employs the same cells enclosed by silicon nitride membrane windows found in liquid cell TEM holders and demonstrate the imaging of copper oxide nanoparticles in solution using both backscattered and transmitted electrons. In particular, the transmitted electron images collected at high scattering angles show contrast inversion at liquid layer thicknesses of several hundred nanometers, which can be used to determine the presence of liquid in the cell, while maintaining enough resolution to image nanoparticles that are tens of nanometers in size. Using Monte Carlo simulations, we show that both imaging modes have their advantages for liquid phase imaging and rationalize the contrast inversion observed in the transmitted electron image.

In microstructural corrosion studies, knowledge on the initiation of corrosion on an nm-scale is lacking. In situ transmission electron microscope (TEM) studies can elucidate where/how the corrosion starts, provided that the proper corrosive conditions are present during the investigation. In wet corrosion studies with liquid cell nanoreactors (NRs), the liquid along the electron beam direction leads to strong scattering and therefore image blurring. Thus, a quick liquid removal or thickness control of the liquid layer is preferred. This can be done by the use of a Peltier element embedded in an NR. As a prelude to such in situ work, we demonstrate the local wetting of a TEM sample, by creating a temperature decrease of 10 ± 2°C on the membrane of an NR with planar Sb/BiSb thermoelectric materials for the Peltier element. TEM samples were prepared and loaded in an NR using a dual-beam focused ion beam scanning electron microscope. A mixture of water vapor and carrier gas was passed through a chamber, which holds the micro-electromechanical system Peltier device and resulted in quick formation of a water layer/droplets on the sample. The TEM analysis after repeated corrosion of the same sample (ex situ studies) shows the onset and progression of O2 and H2S corrosion of the AA2024-T3 alloy and cold-rolled HCT980X steel lamellae.

Significant developments in micro-electrical-mechanical systems (MEMS)-based devices have led to the commercialization of windowed gas cells that now enable atomic-resolution scanning transmission electron microscopy (STEM) observation of phenomena occurring during gas-solid interactions at atmospheric pressure. An in situ atmospheric STEM study provides information that is beneficial to correlating the structure-properties relationship of catalytic nanomaterials, particularly under realistic gaseous reaction conditions. In this article, we illustrate the advantages of this tool as applied to our study of two important systems: (1) the CO-induced Pt nanoparticle surface reconstruction at saturation coverage and (2) the ordering and Pt surface enrichment in supported Pt3Co nanoparticles.

One of the fundamental challenges in understanding the early stages of corrosion pitting in metals protected with an oxide film is that there are relatively few techniques that can probe microstructure with sufficient resolution while maintaining a wet environment. Here, we demonstrate that microstructural changes in Al thin films caused by aqueous NaCl solutions of varying chloride concentrations can be directly observed using a liquid flow cell enclosed within a transmission electron microscope (TEM) holder. In the absence of chloride, Al thin films did not exhibit significant corrosion when immersed in de-ionized water for 2 days. However, introducing 0.01 M NaCl solutions led to extensive random formation of blisters over the sample surface, while 0.1 M NaCl solutions formed anomalous structures that were larger than the typical grain size. Immersion in 1.0 M NaCl solutions led to fractal corrosion consistent with previously reported studies of Al thin films using optical microscopy. These results show the potential of in situ liquid cell electron microscopy for probing the processes that take place before the onset of pitting and for correlating pit locations with the underlying microstructure of the material.

We report the evolution of titanium dioxide nanostructures when Au nanoparticles, supported on single crystal TiO2 substrates, were heated under ∼260 Pa of flowing O2 in an environmental transmission electron microscope. Nanostructures with different morphologies were first observed around 500°C. Our measurements show that temperature, oxygen pressure, and the electron beam control the nanostructure growth. We propose a reaction-controlled growth mechanism where mobile Ti atoms generated by the electron- beam-induced reduction of TiO2 are preferentially reoxidized at the Au-TiO2 interface.

Extrapolating from a brief survey of the literature, we outline a vision for the future development of time-resolved electron probe instruments that could offer levels of performance and flexibility that push the limits of physical possibility. This includes a discussion of the electron beam parameters (brightness and emittance) that limit performance, the identification of a dimensionless invariant figure of merit for pulsed electron guns (the number of electrons per lateral coherence area, per pulse), and calculations of how this figure of merit determines the trade-off of spatial against temporal resolution for different imaging modes. Modern photonics' ability to control its fundamental particles at the quantum level, while enjoying extreme flexibility and a very large variety of operating modes, is held up as an example and a goal. We argue that this goal may be approached by combining ideas already in the literature, suggesting the need for large-scale collaborative development of next-generation time-resolved instruments.

We have used the technique of in situ electron microscopy to study the oxidation and reduction of the palladium (Pd) catalysts. In this study, we have subjected a Pd catalyst to oxidation and reduction cycles and studied the changes in particle structure and morphology with in situ electron diffraction and imaging. The PdO particles can be reduced to Pd metal in situ at temperatures as low as 200°C in an atmosphere of a few Torr of both H2 and O2. We also found that essentially the same reduction occurred in the vacuums of 10−6 to 10−7 Torr in two different electron microscopes. Our in situ reduction studies show that many of the oxide particles form voids when reduced to Pd metal. The decrease in volume that occurs during reduction is often accommodated by a combination of particle shrinkage and void formation. The production of voids does not seem to depend on either the reducing atmosphere or the rate of reduction, although the voids appear to be unstable above 500°C.