Reduction of Specimen Contamination in Electron-Beam Instruments

Author(s):  
G. Lehmpfuhl ◽  
P. J. Smith

Specimens being observed with electron-beam instruments are subject to contamination, which is due to polymerization of hydrocarbon molecules by the beam. This effect becomes more important as the size of the beam is reduced. In convergent-beam studies with a beam diameter of 100 Å, contamination was observed to grow on samples at very high rates. Within a few seconds needles began forming under the beam on both the top and the underside of the sample, at growth rates of 400-500 Å/s, severely limiting the time available for observation. Such contamination could cause serious difficulty in examining a sample with the new scanning transmission electron microscopes, in which the beam is focused to a few angstroms.We have been able to reduce the rate of contamination buildup by a combination of methods: placing an anticontamination cold trap in the sample region, preheating the sample before observation, and irradiating the sample with a large beam before observing it with a small beam.

2014 ◽  
Vol 20 (2) ◽  
pp. 484-492 ◽  
Author(s):  
B. Layla Mehdi ◽  
Meng Gu ◽  
Lucas R. Parent ◽  
Wu Xu ◽  
Eduard N. Nasybulin ◽  
...  

AbstractThe recent development of in-situ liquid stages for (scanning) transmission electron microscopes now makes it possible for us to study the details of electrochemical processes under operando conditions. As electrochemical processes are complex, care must be taken to calibrate the system before any in-situ/operando observations. In addition, as the electron beam can cause effects that look similar to electrochemical processes at the electrolyte/electrode interface, an understanding of the role of the electron beam in modifying the operando observations must also be understood. In this paper we describe the design, assembly, and operation of an in-situ electrochemical cell, paying particular attention to the method for controlling and quantifying the experimental parameters. The use of this system is then demonstrated for the lithiation/delithiation of silicon nanowires.


Author(s):  
M.E. Mochel ◽  
C. J. Humphreys ◽  
J. M. Mochel ◽  
J. A. Eades

Holes 20 Å in diameter and fine lines 20 Å wide can be cut in the metal-β-aluminas using the 10 Å electron beam of the Vacuum Generators, HB5 scanning transmission electron microscope. The minimum current density required for cutting was 103 amp/cm2. Electron energies of 40,60,80,100 keV were used.This technique has higher resolution than current lithography methods and is direct, requiring no chemical development. The width of isolated lines made on solid substrates is currently about .1μm (Ahmed and McMahon, 1981) and .03μm (Jackel et al., 1980). M. Isaacson and A. Murry have carried out electron beam writing on NaCl crystals supported on a carbon film on the scale we report here.In our case uniform 20Å holes and lines can be cut through self-supporting 1000A thick slabs of sodium-β-alumina to provide very high electron contrast. Once cut, the β-aluminas are stable and will tolerate exposure to air without degradation of the electron cut patterns. They may be used directly as masks (eg. for ion implantation). We believe they could be cut on the substrate with no damage to the underlying material.


Author(s):  
T. Tomita ◽  
Y. Harada ◽  
H. Watanabe ◽  
T. Etoh

For conventional transmission electron microscopy, specimen contamination is not so important as to take it into account, because recent electron microscopes are designed so as to provide the specimen chamber with a vacuum of the order of 10-7 Torr. However, in analytical electron microscopy, contamination still presents serious problems requiring solution, because a very fine electron probe (less than 200Å) remains stationary on the specimen for a few minutes. In this case, a contamination spot is formed by the reaction of the electron probe with hydrocarbon molecules adsorbed on the specimen surface. The present paper describes detailed observations of contamination spots caused by very fine electron probe and the reduction of contamination spots by means of a specially designed liquid nitrogen cold trap assembly.This cold trap assembly shown in Fig. 1 consists of two traps; an inner trap and outer trap. The inner trap, which is a conventional type, is designed to enclose the specimen.


Author(s):  
E. Zeitler ◽  
M. G. R. Thomson

In the formation of an image each small volume element of the object is correlated to an areal element in the image. The structure or detail of the object is represented by changes in intensity from element to element, and this variation of intensity (contrast) is determined by the interaction of the electrons with the specimen, and by the optical processing of the information-carrying electrons. Both conventional and scanning transmission electron microscopes form images which may be considered in this way, but the mechanism of image construction is very different in the two cases. Although the electron-object interaction is the same, the optical treatment differs.


Author(s):  
H. M. Thieringer

It has repeatedly been show that with conventional electron microscopes very fine electron probes can be produced, therefore allowing various micro-techniques such as micro recording, X-ray microanalysis and convergent beam diffraction. In this paper the function and performance of an SIEMENS ELMISKOP 101 used as a scanning transmission microscope (STEM) is described. This mode of operation has some advantages over the conventional transmission microscopy (CTEM) especially for the observation of thick specimen, in spite of somewhat longer image recording times.Fig.1 shows schematically the ray path and the additional electronics of an ELMISKOP 101 working as a STEM. With a point-cathode, and using condensor I and the objective lens as a demagnifying system, an electron probe with a half-width ob about 25 Å and a typical current of 5.10-11 amp at 100 kV can be obtained in the back focal plane of the objective lens.


Author(s):  
J.T. Fourie

Contamination in electron microscopes can be a serious problem in STEM or in situations where a number of high resolution micrographs are required of the same area in TEM. In modern instruments the environment around the specimen can be made free of the hydrocarbon molecules, which are responsible for contamination, by means of either ultra-high vacuum or cryo-pumping techniques. However, these techniques are not effective against hydrocarbon molecules adsorbed on the specimen surface before or during its introduction into the microscope. The present paper is concerned with a theory of how certain physical parameters can influence the surface diffusion of these adsorbed molecules into the electron beam where they are deposited in the form of long chain carbon compounds by interaction with the primary electrons.


Author(s):  
J W Steeds

That the techniques of convergent beam electron diffraction (CBED) are now widely practised is evident, both from the way in which they feature in the sale of new transmission electron microscopes (TEMs) and from the frequency with which the results appear in the literature: new phases of high temperature superconductors is a case in point. The arrival of a new generation of TEMs operating with coherent sources at 200-300kV opens up a number of new possibilities.First, there is the possibility of quantitative work of very high accuracy. The small probe will essentially eliminate thickness or orientation averaging and this, together with efficient energy filtering by a doubly-dispersive electron energy loss spectrometer, will yield results of unsurpassed quality. The Bloch wave formulation of electron diffraction has proved itself an effective and efficient method of interpreting the data. The treatment of absorption in these calculations has recently been improved with the result that <100> HOLZ polarity determinations can now be performed on III-V and II-VI semiconductors.


Author(s):  
B. L. Armbruster ◽  
B. Kraus ◽  
M. Pan

One goal in electron microscopy of biological specimens is to improve the quality of data to equal the resolution capabilities of modem transmission electron microscopes. Radiation damage and beam- induced movement caused by charging of the sample, low image contrast at high resolution, and sensitivity to external vibration and drift in side entry specimen holders limit the effective resolution one can achieve. Several methods have been developed to address these limitations: cryomethods are widely employed to preserve and stabilize specimens against some of the adverse effects of the vacuum and electron beam irradiation, spot-scan imaging reduces charging and associated beam-induced movement, and energy-filtered imaging removes the “fog” caused by inelastic scattering of electrons which is particularly pronounced in thick specimens.Although most cryoholders can easily achieve a 3.4Å resolution specification, information perpendicular to the goniometer axis may be degraded due to vibration. Absolute drift after mechanical and thermal equilibration as well as drift after movement of a holder may cause loss of resolution in any direction.


Author(s):  
W. T. Pike

With the advent of crystal growth techniques which enable device structure control at the atomic level has arrived a need to determine the crystal structure at a commensurate scale. In particular, in epitaxial lattice mismatched multilayers, it is of prime importance to know the lattice parameter, and hence strain, in individual layers in order to explain the novel electronic behavior of such structures. In this work higher order Laue zone (holz) lines in the convergent beam microdiffraction patterns from a thermal emission transmission electron microscope (TEM) have been used to measure lattice parameters to an accuracy of a few parts in a thousand from nanometer areas of material.Although the use of CBM to measure strain using a dedicated field emission scanning transmission electron microscope has already been demonstrated, the recording of the diffraction pattern at the required resolution involves specialized instrumentation. In this work, a Topcon 002B TEM with a thermal emission source with condenser-objective (CO) electron optics is used.


Sign in / Sign up

Export Citation Format

Share Document