A new TCAD simulation method for direct CMOS electron detectors optimization.

A custom CMOS image sensor hardened by design is characterized in a transmission electron microscope, with the aim to extract basic parameters such as the quantum efficiency, the modulation transfer function and finally the detective quantum efficiency. In parallel, a new methodology based on the combination of Monte Carlo simulation of electron distributions and TCAD simulations is proposed and performed on the same detector, and for the first time the basic parameters of a direct CMOS electron detector are extracted thanks to the TCAD. The methodology is validated by means of the comparison between experimental and simulation results. This simulation method may be used for the development of future electron detectors.

Optimization of off-axis electron holography performed with femtosecond electron pulses.

We report on electron holography experiments performed with femtosecond electron pulses in an ultrafast coherent Transmission Electron Microscope based on a laser-driven cold field emission gun. We first discuss the experimental requirements related to the long acquisition times imposed by the low emission/probe current available in these instruments. The experimental parameters are first optimized and electron holograms are then acquired in vacuum and on a nano-object showing that useful physical properties can nevertheless be extracted from the hologram phase in pulsed condition. Finally, we show that the acquisition of short exposure time holograms assembled in a stack, combined with a computer-assisted shift compensation of usual instabilities encountered in holography, such as beam and biprism wire instabilities, can yield electron holograms acquired with a much better contrast paving the way to ultrafast time-resolved electron holography.

Development of a high brightness ultrafast Transmission Electron Microscope based on a laser-driven cold field emission source.

We report on the development of an ultrafast Transmission Electron Microscope based on a cold field emission source which can operate in either DC or ultrafast mode. Electron emission from a tungsten nanotip is triggered by femtosecond laser pulses which are tightly focused by optical components integrated inside a cold field emission source close to the cathode. The properties of the electron probe (brightness, angular current density, stability) are quantitatively determined. The measured brightness is the largest reported so far for UTEMs. Examples of imaging, diffraction and spectroscopy using ultrashort electron pulses are given. Finally, the potential of this instrument is illustrated by performing electron holography in the off-axis configuration using ultrashort electron pulses.

Optimising electron microscopy experiment through electron optics simulation.

We developed a new type of electron trajectories simulation inside a complete model of a modern transmission electron microscope (TEM). Our model incorporates the precise and real design of each element constituting a TEM, i.e. the field emission (FE) cathode, the extraction optic and acceleration stages of a 300kV cold field emission gun, the illumination lenses, the objective lens, the intermediate and projection lenses. Full trajectories can be computed using magnetically saturated or non-saturated round lenses, magnetic deflectors and even non-cylindrical symmetry elements like electrostatic biprism. This multi-scale model gathers nanometer size components (FE tip) with parts of meter length (illumination and projection systems). We demonstrate that non-trivial TEM experiments requiring specific and complex optical configurations can be simulated and optimized prior to any experiment using such model. We show that all the currents set in all optical elements of the simulated column can be implemented in the real column (I2TEM in CEMES) and used as starting alignment for the requested experiment. We argue that the combination of such complete electron trajectory simulations in the whole TEM column with automatic optimization of the microscope parameters for optimal experimental data (images, diffraction, spectra) allows drastically simplifying the implementation of complex experiments in TEM and will facilitate the development of advanced use of the electron microscope in the near future.

Quantitative 3D electromagnetic field determination of 1D nanostructures from single projection.

One-dimensional (1D) nanostructures have been regarded as the most promising building blocks for nanoelectronics and nanocomposite material systems as well as for alternative energy applications. Although they result in confinement of a material, their properties and interactions with other nanostructures are still very much three-dimensional (3D) in nature. In this work, we present a novel method for quantitative determination of the 3D electromagnetic fields in and around 1D nanostructures using a single electron wave phase image, thereby eliminating the cumbersome acquisition of tomographic data. Using symmetry arguments, we have reconstructed the 3D magnetic field of a nickel nanowire as well as the 3D electric field around a carbon nanotube field emitter, from one single projection. The accuracy of quantitative values determined here is shown to be a better fit to the physics at play than the value obtained by conventional analysis. Moreover the 3D reconstructions can then directly be visualized and used in the design of functional 3D architectures built using 1D nanostructures.

Development of TEM and SEM high brightness electron guns using cold-field emission from a carbon nanotip.

A newly developed carbon cone nanotip (CCnT) has been used as field emission cathode both in low voltage SEM (30 kV) electron source and high voltage TEM (200 kV) electron source. The results clearly show, for both technologies, an unprecedented stability of the emission and the probe current with almost no decay during 1h, as well as a very small noise (rms less than 0.5%) compared to standard sources which use tungsten tips as emitting cathode. In addition, quantitative electric field mapping around the FE tip have been performed using in situ electron holography experiments during the emission of the new tip. These results show the advantage of the very high aspect ratio of the new CCnT which induces a strong enhancement of the electric field at the apex of the tip, leading to very small extraction voltage (some hundred of volts) for which the field emission will start. The combination of these experiments with emission current measurements has also allowed to extract an exit work function value of 4.8 eV.

Dynamical effects in strain measurements by dark-field electron holography.

Here, we study the effect of dynamic scattering on the projected geometric phase and strain maps reconstructed using dark-field electron holography (DFEH) for non-uniformly strained crystals. The investigated structure consists of a {SiGe/Si} superlattice grown on a (001)-Si substrate. The three-dimensional strain field within the thin TEM lamella is modelled by the finite element method. The observed projected strain is simulated in two ways by multiplying the strain at each depth in the crystal by a weighting function determined from a recently developed analytical two-beam dynamical theory, and by simply taking the average value. We demonstrate that the experimental results need to be understood in terms of the dynamical theory and good agreement is found between the experimental and simulated results. Discrepancies do remain for certain cases and are likely to be from an imprecision in the actual two-beam diffraction conditions, notably the deviation parameter, and points to limitations in the 2-beam approximation. Finally, a route towards a 3D reconstruction of strain fields is proposed.

Dark-field electron holography for the measurement of geometric phase.

The genesis, theoretical basis and practical application of the new electron holographic dark-field technique for mapping strain in nanostructures are presented. The development places geometric phase within a unified theoretical framework for phase measurements by electron holography. The total phase of the transmitted and diffracted beams is described as a sum of four contributions: crystalline, electrostatic, magnetic and geometric. Each contribution is outlined briefly and leads to the proposal to measure geometric phase by dark-field electron holography (DFEH). The experimental conditions, phase reconstruction and analysis are detailed for off-axis electron holography using examples from the field of semiconductors. A method for correcting for thickness variations will be proposed and demonstrated using the phase from the corresponding bright-field electron hologram.

Optimal aperture sizes and positions for EMCD experiments.

The signal-to-noise ratio (SNR) in energy-loss magnetic chiral dichroism (EMCD)--the equivalent of X-ray magnetic circular dichroism (XMCD) in the electron microscope--is optimized with respect to the detector shape, size and position. We show that an important increase in SNR over previous experiments can be obtained when taking much larger detector sizes. We determine the ideal shape of the detector but also show that round apertures are a good compromise if placed in their optimal position. We develop the theory for a simple analytical description of the EMCD experiment and then apply it to dynamical multibeam Bloch wave calculations and to an experimental data set. In all cases it is shown that a significant and welcome improvement of the SNR is possible.

Mapping inelastic intensities in diffraction patterns of magnetic samples using the energy spectrum imaging technique.

We present the quantitative measurement of inelastic intensity distributions in diffraction patterns with the aim of studying magnetic materials. The relevant theory based on the mixed dynamic form factor (MDFF) is outlined. Experimentally, the challenge is to obtain sufficient signal for core losses of 3d magnetic materials (in the 700-900eV energy-loss range). We compare two experimental settings in diffraction mode, i.e. the parallel diffraction and the large-angle convergent-beam electron diffraction configurations, and demonstrate the interest of using a spherical aberration corrector. We show how the energy spectrum imaging (ESI) technique can be used to map the inelastic signal in a data cube of scattering angle and energy loss. The magnetic chiral dichroic signal is measured for a magnetite sample and compared with theory.

New approach for the dynamical simulation of CBED patterns in heavily strained specimens.

A new method for the dynamical simulation of convergent beam electron diffraction (CBED) patterns is proposed. In this method, the three-dimensional stationary Schrödinger equation is replaced by a two-dimensional time-dependent equation, in which the direction of propagation of the electron beam, variable z, stands as a time. We demonstrate that this approach is particularly well-suited for the calculation of the diffracted intensities in the case of a z-dependent crystal potential. The corresponding software has been developed and implemented for simulating CBED patterns of various specimens, from perfect crystals to heavily strained cross-sectional specimens. Evidence is given for the remarkable agreement between simulated and experimental patterns.

Effect of sample bending on diffracted intensities observed in CBED patterns of plan view strained samples.

Convergent beam electron diffraction is used to study the effect of the sample bending on diffracted intensities as observed in transmission electron microscopy (TEM). Studied samples are made of thin strained semiconductor Ga(1-)(x)In(x)As epitaxial layers grown on a GaAs substrate and observed in plan view. Strong variations of the diffracted intensities are observed depending on the thinning process used for TEM foil preparation. For chemically thinned samples, strong bending of the substrate occurs, inducing modifications of both kinematical and dynamical Bragg lines. For mechanically thinned samples, bending of the substrate is negligible. Kinematical lines are unaffected whereas dynamical lines have slightly asymmetric intensities. We analyse these effects using finite element modelling to calculate the sample strain coupled with dynamical multibeam simulations for calculating the diffracted intensities. Our results correctly reproduce the qualitative features of experimental patterns, clearly demonstrating that inhomogeneous displacement fields along the electron beam within the substrate are responsible for the observed intensity modifications.

Diffracted phase and amplitude measurements by energy-filtered convergent-beam holography (CHEF).

Interference between transmitted and diffracted disks in convergent-beam electron diffraction (CBED) patterns using the CBED+EBI method proposed by Herring et al. is explored using different optical configurations on a spherical aberration corrected transmission electron microscope equipped with a biprism and imaging energy filter: the SACTEM-Toulouse. We will relate the amplitude and phase of these interference patterns, which we call convergent-beam holography (CHEF), to microscope transfer theory and the complex amplitudes of the diffracted beams. Experimental CHEF patterns recorded in the absence of aberration correction will be compared with simulations to validate the theory concerning the effect of microscope aberrations and current instabilities. Then, using aberration correction, we propose a scheme for eliminating the effect of the microscope, so that the diffracted amplitudes and phase due to dynamical scattering within the specimen can be studied. Experimental results are compared with simulations performed using the full dynamical theory. The potential for studying diffracted amplitudes and phases using CHEF analysis is discussed.

LACDIF, a new electron diffraction technique obtained with the LACBED configuration and a C(s) corrector: comparison with electron precession.

By combining the large-angle convergent-beam electron diffraction (LACBED) configuration together with a microscope equipped with a C(s) corrector it is possible to obtain good quality spot patterns in image mode and not in diffraction mode as it is usually the case. These patterns have two main advantages with respect to the conventional selected-area electron diffraction (SAED) or microdiffraction patterns. They display a much larger number of reflections and the diffracted intensity is the integrated intensity. These patterns have strong similarities with the electron precession patterns and they can be used for various applications like the identification of the possible space groups of a crystal from observations of the Laue zones or the ab-initio structure identifications. Since this is a defocused method, another important application concerns the analysis of electron beam-sensitive materials. Successful applications to polymers are given in the present paper to prove the validity of this method with regards to these materials.

Quantitative analysis of HOLZ line splitting in CBED patterns of epitaxially strained layers.

A SiGe layer epitaxially grown on a silicon substrate is experimentally studied by convergent beam electron diffraction (CBED) experiments and used as a test sample to analyse the higher-order Laue zones (HOLZ) line splitting. The influence of surface strain relaxation on the broadening of HOLZ lines is confirmed. The quantitative fit of the observed HOLZ line profiles is successfully achieved using a formalism particularly well-adapted to the case of a z-dependent crystal potential (z being the zone axis). This formalism, based on a time-dependent perturbation theory approach, proves to be much more efficient than a classical Howie-Whelan approach, to reproduce the complex HOLZ lines profile in this heavily strained test sample.