Towards 1-Ångstrom-resolution STEM

Author(s):  
H.S. von Harrach ◽  
D.E. Jesson ◽  
S.J. Pennycook

Phase contrast TEM has been the leading technique for high resolution imaging of materials for many years, whilst STEM has been the principal method for high-resolution microanalysis. However, it was demonstrated many years ago that low angle dark-field STEM imaging is a priori capable of almost 50% higher point resolution than coherent bright-field imaging (i.e. phase contrast TEM or STEM). This advantage was not exploited until Pennycook developed the high-angle annular dark-field (ADF) technique which can provide an incoherent image showing both high image resolution and atomic number contrast.This paper describes the design and first results of a 300kV field-emission STEM (VG Microscopes HB603U) which has improved ADF STEM image resolution towards the 1 angstrom target. The instrument uses a cold field-emission gun, generating a 300 kV beam of up to 1 μA from an 11-stage accelerator. The beam is focussed on to the specimen by two condensers and a condenser-objective lens with a spherical aberration coefficient of 1.0 mm.

Author(s):  
Earl J. Kirkland ◽  
Robert J. Keyse

An ultra-high resolution pole piece with a coefficient of spherical aberration Cs=0.7mm. was previously designed for a Vacuum Generators HB-501A Scanning Transmission Electron Microscope (STEM). This lens was used to produce bright field (BF) and annular dark field (ADF) images of (111) silicon with a lattice spacing of 1.92 Å. In this microscope the specimen must be loaded into the lens through the top bore (or exit bore, electrons traveling from the bottom to the top). Thus the top bore must be rather large to accommodate the specimen holder. Unfortunately, a large bore is not ideal for producing low aberrations. The old lens was thus highly asymmetrical, with an upper bore of 8.0mm. Even with this large upper bore it has not been possible to produce a tilting stage, which hampers high resolution microscopy.


Author(s):  
Mehmet Sarikaya ◽  
James M. Howe

The image resolution in bright-field (BF) and dark-field (DF) conventional transmission electron microscopy (TEM) is given by: r = 0.66 CS¼¾¾, where Cs and ¾ are the spherical aberration coefficient of the objective lens and electron wavelength, respectively. Based on this formula, it should be possible to resolve single atoms or clusters of atoms by phase contrast imaging with a highly coherent electron beam and a properly defocused objective lens; this has been demonstrated for both BF and DF imaging. However, for most situations encountered in conventional TEM, the type of information that can be obtained about the specimen is the most important, rather than the instrumental resolution. Atomicresolution microscopy of crystalline specimens relies on phase contrast produced when two or more beams interfere to form an image and this is discussed elsewhere in this symposium. This paper discusses the contrast and resolution when either a single beam or diffuse scattering is used to form an image.


Author(s):  
R.D. Leapman ◽  
S.B. Andrews

The recent availability of a cryotransfer stage, efficient electron energy loss spectrometers (EELS), and ultrathin window energy-dispersive x-ray spectrometers (EDXS) for the VG Microscopes HB501 field-emission STEM now provides this instrument with the potential for high resolution (<20 nm) biological microanalysis. In practice, limits are normally imposed by the sample itself, due to damage in the electron beam and to changes in structure and composition during freezing, sectioning, transfering and freeze-drying. We have therefore investigated what types of useful high-resolution analytical information can be obtained from rapidly frozen samples, including thin tissue cryosections and frozen isolated macromolecules and macromolecular assemblies.Frozen-hydrated samples were cryotransfered at ~-175C into the VG STEM after which a vacuum of ~3x10-9 mbar was maintained. Samples were freeze-dried by warming to ~-90C over 30 min and were then recooled to below ~-160C to minimize radiation damage and contamination during analysis. Digital annular dark-field images were obtained at low dose (~10 e/Å2) with single electron sensitivity, using a probe current of 2 to10 pA and a beam energy of 100 keV.


Author(s):  
T. Tomita ◽  
T. Honda ◽  
M. Kersker

Interpretation of the high resolution transmission image typically requires simulation since the contrast changes in a complicated way due to changes in focus and specimen thickness. The contrast in images formed by collecting high angle forward scattered electrons in STEM does not change with changes in thickness or defocus.Until recently, high angle annular dark field (HADF) images were obtained only from instruments using cold field emission guns. Recently we have attempted to obtain HADF images using Schottky (ZrO/W(100)) thermal field emission and using a 200kV instrument designed as a comprehensive TEM/STEM. Advantages of the ZrO/W emitter are easy operation, very good short and long term stability, high brightness, and narrow energy spread. This microscope, The JEM2010F with thermal field emission, allows subnanometer analysis with EDS(spot, line, and mapping), EELS, holograms, etc, and has a standard TEM imaging system for high resolution imaging and for various diffraction modes, viz., CBED, selected area, Tanaka, etc.


2001 ◽  
Vol 7 (S2) ◽  
pp. 904-905
Author(s):  
M. Lentzen ◽  
B. Jahnen ◽  
C.L. Jia ◽  
K. Urban

In electron microscopy high-resolution imaging of finest object structures is generally hampered by the influence of aberrations of the lens system, especially the high spherical aberration of the objective lens. The delocalization of contrast details induced by aberrations is especially strong for microscopes equipped with a field emission gun providing a high spatial coherence. in recent years a prototype of an aberration correction system has been constructed by Haider et al., following a suggestion by Rose, consisting of two hexapole elements and four additional round lenses. The correction system was adapted to a Philips CM 200 FEG ST microscope with an information limit of 0.13 nm. The alignment is carried out using aberration measurements deduced from Zemlin tableaus. By appropriately exciting the hexapole elements it is possible to reduce or even fully compensate the spherical aberration of the objective lens.With the freedom of a variable spherical aberration Cs new operation modes can be accessed that are not available in standard microscopes. with Cs = 0 and defocus Z = 0 pure amplitude contrast occurs, together with a vanishing contrast delocalization; phase contrast with a single, narrow pass-band up to the information limit can still be achieved by Z = ±7 nm, which introduces a delocalization of R = 0.13 nm. with Cs = 97 μm and Z = −18 nm the broad Scherzer pass-band for phase contrast can be extended to the information limit, with R = 0.35 nm. For the CM 200 Cs = 43 fim and Z = −12 nm still produces a high level of phase contrast, comparable with the extended Scherzer pass-band, but with R = 0.08 nm only. in the latter mode Scherzer’s defocus equals Lichte's defocus of least confusion.


Author(s):  
Peirong Xu

Atomic structure imaging using bright field phase contrast at less than 2Å resolution has become routinely possible in medium and high voltage microscopes (>200 keV). Radiation damage at these elevated voltages can be serious and this limits the length of useful observation time. For example, the knock-on threshold energy for silicon is 120-190keV. Recently, a VG HB501A STEM equipped with a newly developed ultra-high resolution pole piece (Cs=0.7mm) has demonstrated the capability of achieving sub-2Å resolution in imaging the (111) silicon latticer using both bright field (BF) and annular dark field (ADF) modes at an operating voltage of l00keV (Fig.1).A thin silicon specimen was prepared through successive steps of chemical etching, anodic etching and reactive ion etching. Large flat thin areas about 100Å thick were produced in the specimen. Since there is no tilting mechanism for the stage used with this ultra-high resolution pole piece, the specimen was not oriented exactly along the (111) zone axis as indicated by CBED but was less than 1-2° off.


Author(s):  
R. Reichelt ◽  
U. Aebi ◽  
A. Engel

Various high resolution scanning electron microscopes (HRSEM) are now commercially available providing probe sizes in the range of 0.5 to 1.5 nm at 30 keV due to their field emission gun 1.2. Equipped with efficient detector systems (which collect different signals and applied to specifically prepared samples) HRSEM challenge the conventional transmission electron microscope (TEM) with high resolution surface images of biological specimens collecting secondary (SE) or backscattered (BSE) electrons. However, the yield of (SE) carrying high resolution information is rather small, i.e. the SE-I yield at 20 keV primary electron energy amounts to < 1% for the major elements (H; C; N; O; P) constituting biological matter. The yield of BSE is greater than the corresponding total SE yield (electron energy >15 keV), but BSE emerge due to high angle elastic scattering from a surface area with a diameter of typically 30% of the deepest electron penetration R (e.g. R≈10 μm for elements mentioned above at 30 keV).


Author(s):  
M. Kelly ◽  
D.M. Bird

It is well known that strain fields can have a strong influence on the details of HREM images. This, for example, can cause problems in the analysis of edge-on interfaces between lattice mismatched materials. An interesting alternative to conventional HREM imaging has recently been advanced by Pennycook and co-workers where the intensity variation in the annular dark field (ADF) detector is monitored as a STEM probe is scanned across the specimen. It is believed that the observed atomic-resolution contrast is correlated with the intensity of the STEM probe at the atomic sites and the way in which this varies as the probe moves from cell to cell. As well as providing a directly interpretable high-resolution image, there are reasons for believing that ADF-STEM images may be less suseptible to strain than conventional HREM. This is because HREM images arise from the interference of several diffracted beams, each of which is governed by all the excited Bloch waves in the crystal.


Author(s):  
Michael Beer ◽  
J. W. Wiggins ◽  
David Woodruff ◽  
Jon Zubin

A high resolution scanning transmission electron microscope of the type developed by A. V. Crewe is under construction in this laboratory. The basic design is completed and construction is under way with completion expected by the end of this year.The optical column of the microscope will consist of a field emission electron source, an accelerating lens, condenser lens, objective lens, diffraction lens, an energy dispersive spectrometer, and three electron detectors. For any accelerating voltage the condenser lens function to provide a parallel beam at the entrance of the objective lens. The diffraction lens is weak and its current will be controlled by the objective lens current to give an electron diffraction pattern size which is independent of small changes in the objective lens current made to achieve focus at the specimen. The objective lens demagnifies the image of the field emission source so that its Gaussian size is small compared to the aberration limit.


Author(s):  
M. G. R. Thomson

The variation of contrast and signal to noise ratio with change in detector solid angle in the high resolution scanning transmission electron microscope was discussed in an earlier paper. In that paper the conclusions were that the most favourable conditions for the imaging of isolated single heavy atoms were, using the notation in figure 1, either bright field phase contrast with β0⋍0.5 α0, or dark field with an annular detector subtending an angle between ao and effectively π/2.The microscope is represented simply by the model illustrated in figure 1, and the objective lens is characterised by its coefficient of spherical aberration Cs. All the results for the Scanning Transmission Electron Microscope (STEM) may with care be applied to the Conventional Electron Microscope (CEM). The object atom is represented as detailed in reference 2, except that ϕ(θ) is taken to be the constant ϕ(0) to simplify the integration. This is reasonable for θ ≤ 0.1 θ0, where 60 is the screening angle.


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