Hendrix Demers

Three-Dimensional Electron Microscopy Simulation with the CASINO Monte Carlo Software

Monte Carlo softwares are widely used to understand the capabilities of electron microscopes. To study more realistic applications with complex samples, 3D Monte Carlo softwares are needed. In this article, the development of the 3D version of CASINO is presented. The software feature a graphical user interface, an efficient (in relation to simulation time and memory use) 3D simulation model, accurate physic models for electron microscopy applications, and it is available freely to the scientific community at this website: www.gel.usherbrooke.ca/casino/index.html. It can be used to model backscattered, secondary, and transmitted electron signals as well as absorbed energy. The software features like scan points and shot noise allow the simulation and study of realistic experimental conditions. This software has an improved energy range for scanning electron microscopy and scanning transmission electron microscopy applications.

Nanometer-resolution electron microscopy through micrometers-thick water layers

Scanning transmission electron microscopy (STEM) was used to image gold nanoparticles on top of and below saline water layers of several micrometers thickness. The smallest gold nanoparticles studied had diameters of 1.4 nm and were visible for a liquid thickness of up to 3.3 microm. The imaging of gold nanoparticles below several micrometers of liquid was limited by broadening of the electron probe caused by scattering of the electron beam in the liquid. The experimental data corresponded to analytical models of the resolution and of the electron probe broadening as function of the liquid thickness. The results were also compared with Monte Carlo simulations of the STEM imaging on modeled specimens of similar geometry and composition as used for the experiments. Applications of STEM imaging in liquid can be found in cell biology, e.g., to study tagged proteins in whole eukaryotic cells in liquid and in materials science to study the interaction of solid:liquid interfaces at the nanoscale.

Simulating STEM imaging of nanoparticles in micrometers-thick substrates.

Scanning transmission electron microscope (STEM) images of three-dimensional (3D) samples were simulated. The samples consisted of a micrometer(s)-thick substrate and gold nanoparticles at various vertical positions. The atomic number (Z) contrast as obtained via the annular dark-field detector was generated. The simulations were carried out using the Monte Carlo method in the CASINO software (freeware). The software was adapted to include the STEM imaging modality, including the noise characteristics of the electron source, the conical shape of the beam, and 3D scanning. Simulated STEM images of nanoparticles on a carbon substrate revealed the influence of the electron dose on the visibility of the nanoparticles. The 3D datasets obtained by simulating focal series showed the effect of beam broadening on the spatial resolution and on the signal-to-noise ratio. Monte Carlo simulations of STEM imaging of nanoparticles on a thick water layer were compared with experimental data by programming the exact sample geometry. The simulated image corresponded to the experimental image, and the signal-to-noise levels were similar. The Monte Carlo simulation strategy described here can be used to calculate STEM images of objects of an arbitrary geometry and amorphous sample composition. This information can then be used, for example, to optimize the microscope settings for imaging sessions where a low electron dose is crucial for the design of equipment, or for the analysis of the composition of a certain specimen.

Atomic-resolution scanning transmission electron microscopy through 50-nm-thick silicon nitride membranes.

Silicon nitride membranes can be used for windows of environmental chambers for in situ electron microscopy. We report that aberration corrected scanning transmission electron microscopy (STEM) achieved atomic resolution on gold nanoparticles placed on both sides of a 50-nm-thick silicon nitride membrane at 200 keV electron beam energy. Spatial frequencies of 1∕1.2 Å were visible for a beam semi-angle of 26.5 mrad. Imaging though a 100-nm-thick membrane was also tested. The achieved imaging contrast was evaluated using Monte Carlo simulations of the STEM imaging of a sample of with a representative geometry and composition.

The probe profile and lateral resolution of scanning transmission electron microscopy of thick specimens.

Lateral profiles of the electron probe of scanning transmission electron microscopy (STEM) were simulated at different vertical positions in a micrometers-thick carbon sample. The simulations were carried out using the Monte Carlo method in CASINO software. A model was developed to fit the probe profiles. The model consisted of the sum of a Gaussian function describing the central peak of the profile and two exponential decay functions describing the tail of the profile. Calculations were performed to investigate the fraction of unscattered electrons as a function of the vertical position of the probe in the sample. Line scans were also simulated over gold nanoparticles at the bottom of a carbon film to calculate the achievable resolution as a function of the sample thickness and the number of electrons. The resolution was shown to be noise limited for film thicknesses less than 1 μm. Probe broadening limited the resolution for thicker films. The validity of the simulation method was verified by comparing simulated data with experimental data. The simulation method can be used as quantitative method to predict STEM performance or to interpret STEM images of thick specimens.

Dark-field imaging of thin specimens with a forescatter electron detector at low accelerating voltage.

A forescatter electron detector (FSED) was used to acquire dark-field micrographs (DF-FSED) on thin specimens with a scanning electron microscope. The collection angles were adjusted with the detector distance from the beam axis, which is similar to the camera length of the scanning transmission electron microscope annular DF detectors. The DF-FSED imaging resolution was calculated with SMART-J on an aluminum alloy and carbon nanotubes (CNTs) decorated with platinum nanoparticles. The resolution was three to six times worse than with bright-field imaging. Measurements of nanometer-size objects showed a similar feature size in DF-FSED imaging despite a signal-to-noise ratio 12 times smaller. Monte Carlo simulations were used to predict the variation of the contrast of a CNT/Fe/Pt system as a function of the collection angles. It was constant for very high collection angles (>450 mrad) and confirmed experimentally. The reverse contrast between carbon black particles and the smallest titanium dioxide (TiO2) nanoparticles was predicted by Monte Carlo simulations and observed in the DF-FSED micrograph of a battery electrode coating. However, segmentation of the micrograph was not able to isolate the TiO2 nanoparticle phase because of the close contrast of small TiO2 nanoparticles compared to the C black particles.

Three-dimensional electron energy deposition modeling of cathodoluminescence emission near threading dislocations in GaN and electron-beam lithography exposure parameters for a PMMA resist.

The Monte Carlo software CASINO has been expanded with new modules for the simulation of complex beam scanning patterns, for the simulation of cathodoluminescence (CL), and for the calculation of electron energy deposition in subregions of a three-dimensional (3D) volume. Two examples are presented of the application of these new capabilities of CASINO. First, the CL emission near threading dislocations in gallium nitride (GaN) was modeled. The CL emission simulation of threading dislocations in GaN demonstrated that a better signal-to-noise ratio was obtained with lower incident electron energy than with higher energy. Second, the capability to simulate the distribution of the deposited energy in 3D was used to determine exposure parameters for polymethylmethacrylate resist using electron-beam lithography (EBL). The energy deposition dose in the resist was compared for two different multibeam EBL schemes by changing the incident electron energy.

The influence of the sample thickness on the lateral and axial resolution of aberration-corrected scanning transmission electron microscopy.

The lateral and axial resolution of three-dimensional (3D) focal series aberration-corrected scanning transmission electron microscopy was studied for samples of different thicknesses. The samples consisted of gold nanoparticles placed on the top and at the bottom of silicon nitride membranes of thickness between 50 and 500 nm. Atomic resolution was obtained for nanoparticles on top of 50-, 100-, and 200-nm-thick membranes with respect to the electron beam traveling downward. Atomic resolution was also achieved for nanoparticles placed below 50-, 100-, and 200-nm-thick membranes but with a lower contrast at the larger thicknesses. Beam broadening led to a reduced resolution for a 500-nm-thick membrane. The influence of the beam broadening on the axial resolution was also studied using Monte Carlo simulations with a 3D sample geometry.

Imaging with a Commercial Electron Backscatter Diffraction (EBSD) Camera in a Scanning Electron Microscope: A Review

Scanning electron microscopy is widespread in field of material science and research, especially because of its high surface sensitivity due to the increased interactions of electrons with the target material’s atoms compared to X-ray-oriented methods. Among the available techniques in scanning electron microscopy (SEM), electron backscatter diffraction (EBSD) is used to gather information regarding the crystallinity and the chemistry of crystalline and amorphous regions of a specimen. When post-processing the diffraction patterns or the image captured by the EBSD detector screen which was obtained in this manner, specific imaging contrasts are generated and can be used to understand some of the mechanisms involved in several imaging modes. In this manuscript, we reviewed the benefits of this procedure regarding topographic, compositional, diffraction, and magnetic domain contrasts. This work shows preliminary and encouraging results regarding the non-conventional use of the EBSD detector. The method is becoming viable with the advent of new EBSD camera technologies, allowing acquisition speed close to imaging rates. This method, named dark-field electron backscatter diffraction imaging, is described in detail, and several application examples are given in reflection as well as in transmission modes.

High Spatial Resolution Spectroscopy in a FE-SEM: X-ray Microanalysis and Electron Energy-Loss Spectroscopy

For developing new technologies, it is important to characterize materials at the nanoscale. To achieve high resolution, field emission scanning electron microscopes (FE-SEM) with low voltage scanning transmitted electron microscope (STEM) were developed. Furthermore, some instrument has diffraction analysis, electron energy loss spectrometry (EELS), and energy dispersive spectrometry (EDS) systems, which allow crystallographic and chemical characterization at the nanoscale materials. However, the scanning electron microscope (SEM) was primary developed for imaging applications. With the introduction of the Si(Li) EDS, simultaneous imaging and x-ray microanalysis became possible. However, long working distance and high current were needed because the position and small solid angle of the EDS detector. SEM was initially and is still optimized for imaging applications, where the high spatial resolution is generally obtained at short working distance. This problem is still relevant today and unfortunately x-ray microanalysis is never performed in the best imaging conditions, i.e., not with the smallest probe size. With the introduction of improved geometry and design, modern silicon drift detector (SDD) systems (like the annular detector or low profile windowless detector) can be used for high spatial resolution x-ray microanalysis.