Complementary techniques for the characterization of thin film Ti/Nb multilayers

An aberration corrector on the probe-forming lens of a scanning TEM (STEM) equipped with an electron energy-loss spectrometer (EELS) and X-ray energy-dispersive spectrometer (XEDS) has been employed to investigate the compositional variations as a function of length scale in nanoscale Ti/Nb metallic multilayers. The composition profiles of EELS and XEDS were compared with the profiles obtained from the complementary technique of 3D atom probe tomography. At large layer widths (h≥7 nm, where h is the layer width) of Ti and Nb, XEDS composition profiles of Ti/Nb metallic multilayers are in good agreement with the EELS results. However, at reduced layer widths (h≈2 nm), profiles of EELS and atom probe exhibited similar compositional variations, whereas XEDS results have shown a marked difference. This difference in the composition profiling of the layers has been addressed with reference to the effects of beam broadening and the origin of the signals collected in these techniques. The advantage of using EELS over XEDS for these nanoscaled multilayered materials is demonstrated.     

The measurement of atomic number and composition in an SEM using backscattered detectors

The atomic number dependence of electron backscattering can be used as the basis of a microanalysis technique. The operating procedures and condition for quantitative measurements of specimen atomic number are outlined and an expression relating the accuracy of composition to the atomic number sensitivity has been derived. Some measurements of the spatial resolution of backscattered electron microanalysis are also presented and compared with the resolution of X-ray microanalysis. Although the range of application of this technique is limited, where it can be applied it has the following advantages: (i) higher spatial resolution than X-ray microanalysis for bulk specimens; (ii) very rapid measurement; (iii) can be applied to compounds of low atomic number elements, (e.g. borides, carbides, nitrides, etc.); (iv) specimen preparation is often relatively straightforward.     

A new aberration-corrected,energy-filtered LEEM/PEEM instrument. I. Principles and design

We describe a new design for an aberration-corrected low energy electron microscope (LEEM) and photo electron emission microscope (PEEM), equipped with an in-line electron energy filter. The chromatic and spherical aberrations of the objective lens are corrected with an electrostatic electron mirror that provides independent control over the chromatic and spherical aberration coefficients C_c and C₃, as well as the mirror focal length, to match and correct the aberrations of the objective lens. For LEEM (PEEM) the theoretical resolution is calculated to be ∼1.5 nm (∼4 nm). Unlike previous designs, this instrument makes use of two magnetic prism arrays to guide the electron beam from the sample to the electron mirror, removing chromatic dispersion in front of the mirror by symmetry. The aberration correction optics was retrofitted to an uncorrected instrument with a base resolution of 4.1 nm in LEEM. Initial results in LEEM show an improvement in resolution to ∼2 nm.     

The measurement and calculation of the X-ray spatial resolution obtained in the analytical electron microscope

The X-ray microanalytical spatial resolution is determined experimentally in various analytical electron microscopes by measuring the degradation of an atomically discrete composition profile across an interphase interface in a thin-foil of Ni-Cr-Fe. The experimental spatial resolutions are then compared with calculated values. The calculated spatial resolutions are obtained by the mathematical convolution of the electron probe size with an assumed beam-broadening distribution and the single-scattering model of beam broadening. The probe size is measured directly from an image of the probe in a TEM/STEM and indirectly from dark-field signal changes resulting from scanning the probe across the edge of an MgO crystal in a dedicated STEM. This study demonstrates the applicability of the convolution technique to the calculation of the microanalytical spatial resolution obtained in the analytical electron microscope. It is demonstrated that, contrary to popular opinion, the electron probe size has a major impact on the measured spatial resolution in foils < 150 nm thick.     

Modification of an EM6G electron microscope for X-ray microanalysis

A dual purpose stage has been constructed for an EM6G 100 kV transmission electron microscope. With this stage the composition of thin films and bulk specimens can be determined by X-ray microanalysis. With thin films a change of specimen cartridge then enables a full analysis of crystal defects in the film to be made using tilt controls incorporated in the stage. Modifications to the stage to reduce background effects in X-ray microanalysis spectra are also described. The alternative use of this system in the bulk analysis of specimens by an X-ray fluorescence technique is also discussed.     

Design of an aberration corrected low-voltage SEM

The low-voltage foil corrector is a novel type of foil aberration corrector that can correct for both the spherical and chromatic aberration simultaneously. In order to give a realistic example of the capabilities of this corrector, a design for a low-voltage scanning electron microscope with the low-voltage foil corrector is presented. A fully electrostatic column has been designed and characterised by using aberration integrals and ray tracing calculations. The amount of aberration correction can be adjusted relatively easy. The third order spherical and the first order chromatic aberration can be completely cancelled. In the zero current limit, a FW50 probe size of 1.0 nm at 1 kV can be obtained. This probe size is mainly limited by diffraction and by the fifth order spherical aberration.     

Electron probe x-ray microanalysis of frozen-hydrated biological specimens.

A technique is described for preparing frozen-hydrated bulk samples of biological specimens for electron probe X-ray microanalysis. The method allows reproducible quantitative analyses to be made. Specimens are rapidly frozen, transferred to a vacuum evaporator, fractured under high vacuum at - 180 degrees C and coated with 20 nm of chromium. Transferal to the cryostage of a scanning electron microscope is accomplished without exposure to the atmosphere and without the specimen temperature rising above -120 degrees C. Analyses are made at a temperature of -145 degrees C. Contamination by frost does not occur. Etching and charging of the specimen are eliminated. Specimen charging is shown to be related to temperature. It can be eliminated at low temperature by coating with carbon, aluminium or chromium but consistent elimination could only be achieved with chromium. The chromium coat does not appear to have an absorption effect on quantitative analysis.     

The tuning of a Zernike phase plate with defocus and variable spherical aberration and its use in HRTEM imaging

With the advent of the double-hexapole aberration corrector in transmission electron microscopy the spherical aberration of the imaging system has become a tunable imaging parameter like the objective lens defocus. Now Zernike phase plates, altering the phase of the diffracted electron wave, can be approximated more perfectly than with the lens defocus alone, and the amount of phase change can be adjusted within wide limits. The tuning of the phase change allows an optimum contrast transfer in high-resolution imaging even for thick crystalline objects, thus surpassing the limits of the well-known Scherzer lamda/4 phase plate to the imaging of thin objects. The optimum values for the spherical aberration and the lens defocus are derived, and the limits and imperfections of the approximation explored. A mathematical link to the channelling approximation of high-energy electron diffraction shows how the image contrast of atomic columns can be improved systematically within wide thickness limits. Depending on the specimen thickness different combinations of spherical aberration and defocus are favourable: positive spherical aberration with an underfocus, zero spherical aberration with zero defocus, as well as negative spherical aberration with an overfocus.     

Mass determination of thin biological specimens using backscattered electrons. Application in quantitative X-ray microanalysis on an automated STEM system

The capabilities of modern computerized X-ray analysis systems can be expanded to the acquisition of various signals available in the electron probe microanalyzer, in parallel with the X-rays. These facilities allow the use of backscattered electrons for the measurement of the total specimen mass thickness, which can be used in mass fraction calculations, up to a (biological) specimen thickness of 10 micron. A mass measurement procedure based on the use of backscattered electrons may become an alternative for the X-ray continuum normalization method, often used in electron probe X-ray microanalysis. A mass measurement procedure using backscattered electrons is described, and preliminary results are given.     

Effect of electron beam parameters on simulated CBED patterns from edge-on grain boundaries

Convergent beam electron diffraction (CBED) at vertical grain boundaries (parallel to the electron beam) can be applied to determine the symmetry of bicrystals. It can also be used to investigate the structure of the boundary region itself when subnanometre probe sizes are employed. In this paper it is shown that (sub)nanometre-probe CBED patterns are largely influenced by the electron-beam geometry. In particular, simulations of coherent CBED patterns based on the multislice algorithm show that the CBED pattern of an edge-on interface depends on the defocus distance between the probe position and the specimen midplane, the probe size and the beam-convergence angle. The pattern symmetry may be lower than the theoretically predicted symmetry in case of large spherical aberration. This effect increases with smaller accelerating voltages. An increase in the beam-convergence angle also increases the possibility of a non-optimum symmetry due to spherical aberration of a coherent probe. Thus, for the determination of an interface structure using subnanometre (coherent) probes, the imaging conditions play an important role.     

On the optimum probe in aberration corrected ADF-STEM

New aberration correctors present new challenges in optimizing (minimizing) the probe size in the STEM (Scanning Transmission Electron Microscope). A small probe is important for high resolution imaging and analytical microscopy. Some effects of aperture size, corrector accuracy, and higher order aberrations on probe size and image artifacts are calculated. Accumulated small errors in the aberration corrector can produce a significant decrease in image contrast, which may be important in quantitative image comparisons of theory and experiment. It is important to match the objective aperture to the accuracy of the corrector instead of just the (third order) spherical aberration of the objective as in the commonly used Scherzer conditions.     

Aberration characteristics of immersion lenses for LVSEM

This paper investigates the on-axis aberration characteristics of various immersion objective lenses for low voltage scanning electron microscopy (LVSEM). A simple aperture lens model is used to generate smooth axial field distributions. The simulation results show that mixed field electric-magnetic immersion lenses are predicted to have between 1.5 and 2 times smaller aberration limited probe diameters than their pure-field counterparts. At a landing energy of 1 keV, mixed field immersion lenses operating at the vacuum electrical field breakdown limit are predicted to have on-axis aberration coefficients between 50 and 60 microm, yielding an ultimate image resolution of below 1 nm. These aberrations lie in the same range as those for LVSEM systems that employ aberration correctors.     

5.4 nm spatial resolution in biological photoemission electron microscopy

We report a spatial resolution of 5.4 nm in images of sarcoplasmic reticulum from rabbit muscle. The images were obtained in an aberration-corrected photoemission electron microscope with a hyperbolic mirror as the correcting element for spherical and chromatic aberration. In-situ measurements and numerical simulations confirm the low residual aberration in the instrument and indicate the ultimate resolution in this type of microscopy to be below 2 nm.     

Breaking the spherical and chromatic aberration barrier in transmission electron microscopy

Since the invention of transmission electron microscopy (TEM) in 1932 (Z. Physik 78 (1932) 318) engineering improvements have advanced system resolutions to levels that are now limited only by the two fundamental aberrations of electron lenses; spherical and chromatic aberration (Z. Phys. 101 (1936) 593). Since both aberrations scale with the dimensions of the lens, research resolution requirements are pushing the designs to lenses with only a few mm space in the pole-piece gap for the specimen. This is in conflict with the demand for more and more space at the specimen, necessary in order to enable novel techniques in TEM, such as He-cooled cryo electron microscopy, 3D-reconstruction through tomography (Science 302 (2003) 1396) TEM in gaseous environments, or in situ experiments (Nature 427 (2004) 426). All these techniques will only be able to achieve Angstrom resolution when the aberration barriers have been overcome. The spherical aberration barrier has recently been broken by introducing spherical aberration correctors (Nature 392 (1998) 392, 418 (2002) 617), but the correction of the remaining chromatic aberrations have proved to be too difficult for the present state of technology (Optik 57 (1980) 73). Here we present an alternative and successful method to eliminate the chromatic blur, which consists of monochromating the TEM beam (Inst. Phys. Conf. Ser. 161 (1999) 191). We show directly interpretable resolutions well below 1A for the first time, which is significantly better than any TEM operating at 200 KV has reached before.     

Limits to the spatial, energy and momentum resolution of electron energy-loss spectroscopy

We discuss various factors that determine the performance of electron energy-loss spectroscopy (EELS) and energy-filtered (EFTEM) imaging in a transmission electron microscope. Some of these factors are instrumental and have undergone substantial improvement in recent years, including the development of electron monochromators and aberration correctors. Others, such as radiation damage, delocalization of inelastic scattering and beam broadening in the specimen, derive from basic physics and are likely to remain as limitations. To aid the experimentalist, analytical expressions are given for beam broadening, delocalization length, energy broadening due to core-hole and excited-electron lifetimes, and for the momentum resolution in angle-resolved EELS.     

The assessment of microscopic charging effects induced by focused electron and ion beam irradiation of dielectrics

Energetic beams of electrons and ions are widely used to probe the microscopic properties of materials. Irradiation with charged beams in scanning electron microscopes (SEM) and focused ion beam (FIB) systems may result in the trapping of charge at irradiation induced or pre-existing defects within the implanted microvolume of the dielectric material. The significant perturbing influence on dielectric materials of both electron and (Ga(+)) ion beam irradiation is assessed using scanning probe microscopy (SPM) techniques. Kelvin Probe Microscopy (KPM) is an advanced SPM technique in which long-range Coulomb forces between a conductive atomic force probe and the silicon dioxide specimen enable the potential at the specimen surface to be characterized with high spatial resolution. KPM reveals characteristic significant localized potentials in both electron and ion implanted dielectrics. The potentials are observed despite charge mitigation strategies including prior coating of the dielectric specimen with a layer of thin grounded conductive material. Both electron- and ion-induced charging effects are influenced by a delicate balance of a number of different dynamic processes including charge-trapping and secondary electron emission. In the case of ion beam induced charging, the additional influence of ion implantation and nonstoichiometric sputtering from compounds is also important. The presence of a localized potential will result in the electromigration of mobile charged defect species within the irradiated volume of the dielectric specimen. This electromigration may result in local modification of the chemical composition of the irradiated dielectric. The implications of charging induced effects must be considered during the microanalysis and processing of dielectric materials using electron and ion beam techniques.     

Aberration correction for confocal imaging in refractive-index-mismatched media

A major limitation to the use of confocal microscopes to image thick biological tissue lies in the dramatic reduction in both signal level and resolution when focusing deep into a refractive-index-mismatched specimen. This limitation may be overcome by measuring the wavefront aberration and pre-shaping the input beam so as to cancel the effects of aberration. We consider the images of planar and point objects in brightfield, single-photon fluorescence and two-photon fluorescence imaging. In all cases, the specimens are imaged using an oil-immersion objective through various thicknesses of water. The question of finite-sized pinhole is addressed and it is found, in general, that it is sufficient to correct only the first two or three orders of spherical aberration to restore adequate image signal level and optical resolution, at imaging depths of up to 50-100 wavelengths.     

Emission microscopy and related techniques: resolution in photoelectron microscopy, low energy electron microscopy and mirror electron microscopy.

A unified treatment of the resolution of three closely related techniques is presented: emission electron microscopy (particularly photoelectron microscopy, PEM), low energy electron microscopy (LEEM), and mirror electron microscopy (MEM). The resolution calculation is based on the intensity distribution in the image plane for an object of finite size rather than for a point source. The calculations take into account the spherical and chromatic aberrations of the accelerating field and of the objective lens. Intensity distributions for a range of energies in the electron beam are obtained by adding the single-energy distributions weighted according to the energy distribution function. The diffraction error is taken into account separately. A working resolution is calculated that includes the practical requirement for a finite exposure time, and hence a finite non-zero current in the image. The expressions for the aberration coefficients are the same in PEM and LEEM. The calculated aberrations in MEM are somewhat smaller than for PEM and LEEM. The resolution of PEM is calculated to be about 50 A, assuming conventional UV excitation sources, which provide current densities at the specimen of 5 x 10(-5) A/cm2 and emission energies ranging up to 0.5 eV. A resolution of about 70 A has been demonstrated experimentally. The emission current density at the specimen is higher in LEEM and MEM because an electron gun is used in place of a UV source. For a current density of 5 x 10(-4) A/cm2 and the same electron optical parameters as for PEM, the resolution is calculated to be 27 A for LEEM and 21 A for MEM.     

High resolution imaging properties of the stem

The effect of the finite size of the atom on the resolution of the STEM is investigated. When the probe size becomes comparable to the size of the atom, the quality of the image depends on the scattering properties of the atom as well as the distribution of electrons in the probe. A technique for calculating the image of a single atom is developed by expanding the scattering amplitude. This allows the image of an atom or its spatial frequency to be expanded into various components. The specific case of dark field contrast formed with elastically scattered electrons is considered. The coefficients of the components are evaluated for carbon and thorium using complex scattering amplitudes derived from relativistic Hartree-Fock-Slater wavefunctions. The coefficients are evaluated for a 100 keV microscope using an immersion type objective lens whose aperture is limited to 12 mrad by primary spherical aberration and a 100 keV microscope using the same objective lens in conjunction with a corrector lens for spherical aberration. Secondary spherical aberration limits the objective aperture of the corrected microscope to 30 mrad.