Optimum HRTEM image contrast at 20 kV and 80 kV--exemplified by graphene

The dependence of high-resolution transmission electron microscopy (HRTEM) image contrast of graphene on the adjustable parameters of an aberration-corrected microscope operated at 80 and 20 kV has been calculated and, for 80 kV, compared with measurements. We used density functional theory to determine the projected atom potential and obtained the image intensity by averaging over the energy distribution of the imaging electrons, as derived from the electron energy loss spectroscopy measurements. Optimum image contrast has been determined as a function of energy spread of the imaging electrons and chromatic aberration coefficient, showing that significant improvement of contrast can be achieved at 80 kV with the help of a monochromator, however at 20 kV only with chromatic aberration correction and bright atom contrast conditions.     

Bright-field TEM imaging of single molecules: Dream or near future?

We examine the suitability of spherical aberration (C(S))-corrected (CS) and uncorrected (UC) transmission electron microscopes (TEM) for conventional bright-field imaging of radiation-sensitive materials. We have chosen an individual molecule suspended in vacuum as a hypothetical example of a well-defined radiation-sensitive sample. We find that for this particular sample, CS instruments provide about 30% improvement over an UC instrument in terms of signal/noise ratio per unit electron dose at 300kV. The lowest imaging doses can be achieved in CS instruments equipped with high-brightness electron source operated at low incident electron energies. Our calculations suggest that it may be possible to image individual, iodine- or bromine-substituted organic molecules in bright-field mode, at doses lower than the accepted values for radiation damage of aromatic molecules.     

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.     

Contrast in the electron spectroscopic imaging mode of a TEM. I. Influence of zero-loss filtering on scattering contrast

Measured values of the transmission of amorphous films as a function of the objective aperture and film thickness can be described by a single-scattering theory for unfiltered and zero-loss filtered images in the electron spectroscopic imaging mode of a transmission electron microscope. The theory can be applied to estimate the gain of contrast by zero-loss filtering for specimen structures larger and smaller than the chromatic aberration disc.     

Adaptive aberration correction using a triode hyperbolic electron mirror

A converging electron mirror can be used to compensate spherical and chromatic aberrations in an electron microscope. This paper presents an analytical solution to a novel triode (three electrode) hyperbolic mirror as an improvement to the well-known diode (two electrode) hyperbolic mirror for aberration correction. A weakness of the diode mirror is a lack of flexibility in changing the chromatic and spherical aberration coefficients independently without changes in the mirror geometry. In order to remove this limitation, a third electrode can be added. We calculate the optical properties of the resulting triode mirror analytically on the basis of a simple model field distribution. We present the optical properties-the object/image distance, z(0), and the coefficients of spherical and chromatic aberration, C(s) and C(c), of both mirror types from an analysis of electron trajectories in the mirror field. From this analysis, we demonstrate that while the properties of both designs are similar, the additional parameters in the triode mirror improve the range of aberration that can be corrected. The triode mirror is also able to provide a dynamic adjustment range of chromatic aberration for fixed spherical aberration and focal length, or any permutation of these three parameters. While the dynamic range depends on the values of aberration correction needed, a nominal 10% tuning range is possible for most configurations accompanied by less than 1% change in the other two properties.     

Low-voltage electron microscopy of polymer and organic molecular thin films

We have demonstrated the capabilities of a novel low-voltage electron microscope (LVEM) for imaging polymer and organic molecular thin films. The LVEM can operate in transmission electron microscopy, scanning transmission electron microscopy, scanning electron microscopy, and electron diffraction modes. The microscope operates at a nominal accelerating voltage of 5 kV and fits on a tabletop. A detailed discussion of the electron-sample interaction processes is presented, and the mean free path for total electron scattering was calculated to be 15 nm for organic samples at 5 kV. The total end point dose for the destruction of crystallinity at 5 kV was estimated at 5 x 10(-4) and 3.5 x 10(-2) C/cm2 for polyethylene and pentacene, respectively. These values are significantly lower than those measured at voltages greater than 100 kV. A defocus series of colloidal gold particles allowed us to estimate the experimental contrast transfer function of the microscope. Images taken of several organic materials have shown high contrast for low atomic number elements and a resolution of 2.5 nm. The materials studied here include thin films of the organic semiconductor pentacene, triblock copolymer films, single-molecule dendrimers, electrospun polymer fibers and gold nanoparticles.     

Prerequisites for a Cc/Cs-corrected ultrahigh-resolution TEM

After the introduction of a corrector to compensate for the spherical aberration of a TEM and the acceptance of this new instrumentation for high-resolution CTEM (conventional transmission electron microscope) and STEM (scanning transmission electron microscope) by the electron microscopy community, a demand for even higher resolution far below 1A has emerged. As a consequence several projects around the world have been launched to make these new instruments available and to further push the resolution limits down toward fractions of 1A. For this purpose the so-called TEAM (transmission electron aberration-corrected microscope) has been initiated and is currently under development. With the present paper we give a detailed assessment of the stability required for the base instrument and the electric stability, the manufacturing precision, and feasible semi-automatic alignment procedures for a novel C(c)/C(s)-corrector in order to achieve aberration-free imaging with an information limit of 0.5A at an acceleration voltage of 200 kV according to the goals for the first TEAM instrument. This new aberration corrector, a so-called Achroplanat, in combination with a very stable high-resolution TEM leads to an imaging device with unprecedented resolving power and imaging properties.     

The influence of lens chromatic aberration on electron energy-loss spectroscopy quantitative measurements.

An investigation has been made into the effect of chromatic aberrations of a pre-spectrometer lens system on quantitative elemental analysis by electron energy loss spectroscopy (EELS). In transmission electron microscopy (TEM) diffraction mode, the measured effects are typically 150-330 times larger than if only objective-lens chromatic aberration were important. We discuss several methods of avoiding errors arising from chromatic aberration, including selection of a suitable optical mode (dependent on the desired spatial resolution), adjustment of the TEM imaging system so as to focus the system for a chosen energy loss, and analysis of a large area of a uniform specimen.     

Measurement method of aberration from Ronchigram by autocorrelation function

Aberrations up to the fifth-order were successfully measured using an autocorrelation function of the segmental areas of a Ronchigram. The method applied to aberration measurement in a newly developed 300kV microscope that is equipped with a spherical aberration corrector for probe-forming systems. The experimental Ronchigram agreed well with the simulated Ronchigram that was calculated by using the measured aberrations. The Ronchigram had an infinite magnification area with a half-angle of 50mrad, corresponding to the convergence angle of a uniform phase.     

Low-energy foil aberration corrector

A spherical and chromatic aberration corrector for electron microscopes is proposed, consisting of a thin foil sandwiched between two apertures. The electrons are retarded at the foil to almost zero energy, so that they can travel ballistically through the foil. It is shown that such a low-voltage corrector has a negative spherical aberration for not too large distances between aperture and foil, as well as a negative chromatic aberration. For various distances the third- and fifth-order spherical aberration coefficients and the first- and second-order chromatic aberration coefficients are calculated using ray tracing. Provided that the foils have sufficient electron transmission the corrector is able to correct the third-order spherical aberration and the first-order chromatic aberration of a typical low-voltage scanning electron microscope. Preliminary results show that the fifth-order spherical aberration and the second-order chromatic aberration can be kept sufficiently low.     

Seeing atoms with aberration-corrected sub-Angström electron microscopy

High-resolution electron microscopy is able to provide atomic-level characterization of many materials in low-index orientations. To achieve the same level of characterization in more complex orientations requires that instrumental resolution be improved to values corresponding to the sub-Ångström separations of atom positions projected into these orientations. Sub-Ångström resolution in the high-resolution transmission electron microscope has been achieved in the last few years by software aberration correction, electron holography, and hardware aberration correction; the so-called “one-Ångström barrier” has been left behind. Aberration correction of the objective lens currently allows atomic-resolution imaging at the sub-0.8 Å level and is advancing towards resolutions in the deep sub-Ångström range (near 0.5 Å). At current resolution levels, images with sub-Rayleigh resolution require calibration in order to pinpoint atom positions correctly. As resolution levels approach the “sizes” of atoms, the atoms themselves will produce a limit to resolution, no matter how much the instrumental resolution is improved. By arranging imaging conditions suitably, each atom peak in the image can be narrower, so atoms are imaged smaller and may be resolved at finer separations.     

Low voltage scanning electron microscopy

The scanning electron microscope (SEM) is usually operated with a beam voltage, V₀, in the range of 10–30 kV, even though many early workers had suggested the use of lower voltages to increase topographic contrast and to reduce specimen charging and beam damage. The chief reason for this contradiction is poor instrumental performance when V₀=1–3 kV, The problems include low source brightness, greater defocusing due to chromatic aberration greater sensitivity to stray fields, and difficulty in collecting the secondary electron signal. Responding to the needs of the semiconductor industry, which uses low V₀ to reduce beam damage, considerable efforts have been made to overcome these problems. The resulting equipment has greatly improved performance at low kV and substantially removes the practical deterrents to operation in this mode. This paper reviews the advantages of low voltage operation, recent progress in instrumentation and describes a prototype instrument designed and built for optimum performance at 1 kV. Other limitations to high resolution topographic imaging such as surface contamination, the de-localized nature of the inelastic scattering event and radiation damage are also discussed.     

Low-dose performance of parallel-beam nanodiffraction

We evaluate the low-dose performance of parallel nano-beam diffraction (NBD) in the transmission electron microscope as a method for characterizing radiation sensitive materials at low electron irradiation dose. A criterion, analogous to Rose's, is established for detecting a diffraction spot with desired signal-to-noise ratio. Our experimental data show that a dose substantially lower than in high-resolution bright-field imaging is sufficient to determine structure and orientation of individual nanoscale objects embedded in amorphous matrix. In an instrument equipped with a cold field-emission gun it is possible to form a probe with sub-3 nm diameter and sub-0.3 mrad convergence angle with sufficient beam current to record a diffraction pattern with less than 0.2 s acquisition time. The interpretation of NBD patterns is identical to that of selected area diffraction patterns. We illustrate the physical principles underlying good low-dose performance of NBD by means of a phase grating. The electron irradiation dose needed to detect a diffraction peak in NBD is found proportional to 1/N2, where N is the number of lattice planes contributing to the peak.     

Imaging columns of the light elements carbon, nitrogen and oxygen with sub Angstrom resolution.

It is reported that lattice imaging with a 300 kV field emission microscope in combination with numerical reconstruction procedures can be used to reach an interpretable resolution of about 80 pm for the first time. A retrieval of the electron exit wave from focal series allows for the resolution of single atomic columns of the light elements carbon, nitrogen, and oxygen at a projected nearest neighbor spacing down to 85 pm. Lens aberrations are corrected on-line during the experiment and by hardware such that resulting image distortions are below 80 pm. Consequently, the imaging can be aberration-free to this extent. The resolution enhancement results from increased electrical and mechanical stability of the instrument coupled with a low spherical aberration coefficient of 0.595 + 0.005 mm.     

Low-dose aberration corrected cryo-electron microscopy of organic specimens

Spherical aberration (C(s)) correction in the transmission electron microscope has enabled sub-angstrom resolution imaging of inorganic materials. To achieve similar resolution for radiation-sensitive organic materials requires the microscope to be operated under hybrid conditions: low electron dose illumination of the specimen at liquid nitrogen temperature and low defocus values. Initial images from standard inorganic and organic test specimens have indicated that under these conditions C(s)-correction can provide a significant improvement in resolution (to less than 0.16nm) for direct imaging of organic samples.     

Chromatic aberration effects in small electron probes

The tolerance for chromatic aberration in low voltage probe-forming systems is much larger than we had believed previously. In this article, we calculate the effect of chromatic aberration on small probes on the basis of wave optics. An upper limit for chromatic aberration is established as a practical guide.     

The GIF Quantum,a next generation post-column imaging energy filter

We describe a new post-column imaging energy filter for (scanning) transmission electron microscopy from 60 to 300 kV operating voltage. The completely redesigned GIF quantum has a gradient magnetic prism, dodecapole optics, a 10-times faster 40 Mpixel/sec CCD camera, a 1 μs electrostatic shutter, and new user interface, control, and auto-alignment software. An 8 dodecapole lens system, performs full 2nd and 3rd, and partial 4th and 5th order aberration correction. The improved aberration correction has allowed the size of the entrance aperture to be nearly doubled to 9.0 mm compared to current generation post-column designs. The electrostatic shutter provides exposure control down to 1 μs, extending the exposure time range to over 7 orders of magnitude. Spectroscopy operation has been improved with a larger 2 keV field of view at 200 kV, and a maximum acquisition rate of 1000 spectra per second. A high-speed DualEELS mode simultaneously acquires core- and low-loss spectra up to 2 keV apart. A more intuitive user interface includes new capabilities such as automated exposure control and optimized full spectrum acquisition. The auto-alignment software has been significantly enhanced to use the full flexibility of the dodecapole lens system.     

Higher-order aberration corrector for an image-forming system in a transmission electron microscope

We developed a new electron optical system with three dodecapoles to compensate for spherical aberration and six-fold astigmatism, which generally remains in a two-hexapole type corrector. In this study, we applied the corrector for image-forming system in transmission electron microscope. Compensation for higher-order aberration was demonstrated through a diffractogram tableau using a triple three-fold astigmatism field system, which was then compared with a double hexapole field system. Using this electron optical system, six-fold astigmatism was measured to be less than 0.1 mm at an acceleration voltage of 60 kV, showing that the system successfully compensated for six-fold astigmatism.     

消像差光栅的理论及实验研究

对消像差光栅进行了理论和实验研究。用光程函数和费马原理研究光栅的成像,用刻槽分布函数表示光栅的刻槽曲率及间距变化。对成像的理论分析表明光栅刻槽分布函数比刻槽间距更容易表达像差,给出了消像差光栅的表达形式。比较了SD、WFA、LPF等光栅的参数优化方法。探讨了消像差光栅密度的干涉测量法,设计了光路,对光栅密度进行了测量。     

Optical modifications enabling simultaneous confocal imaging with dyes excited by ultraviolet- and visible-wavelength light

Optical modifications to a confocal scanning laser microscope are described which allow simultaneous fluorescence imaging of living specimens excited by ultraviolet (UV)- and visible-wavelength light. Modifications to a Bio-Rad MRC 600 Lasersharp confocal microscope include the introduction of UV-path-specific lenses and a specially designed UV transmitting eyepiece and tube lens. Upon UV excitation these modifications provide similar resolution and field flatness when compared with visible confocal microscopy. The UV-path-specific optics could be adjusted to correct for varying amounts of longitudinal chromatic aberration in commercially available objectives. Eyepiece and tube lenses were chromatically corrected for UV through visible wavelengths to minimize lateral chromatic error. With these modifications, UV-wavelength light may be used to excite ratioing dyes to quantify intracellular ion concentrations, or as an energy source to release caged compounds in a spatially restricted volume, while simultaneously imaging with dyes excited by visible-wavelength light.