Analyses, spatial resolution

A summary and comparison of the performance of electron microscopes is found in Table 7.7. This lists typical specimen thickness, viewing mode, accelerating voltage, image resolution and x-ray analysis spatial resolution by either energy... 

The systems of such type have been developed of all last 10 years. We shall bring some characteristics of one of the last development within the framework of European BRITE project, carried out in LETT This 3D cone-beam tomograph is referred to as EVA Bench or Equipment for Voludensimetry Analysis. It is oriented on NDT of industrial products from ceramics and other composites. One of the main task of this tomograph is achievement of high resolution at study of whole internal volume of researched object. For test sample of the size 10mm spatial resolution in 50mm was obtained [14]. 

The echo phase does not depend on the initial position of the nuclei, only on their displacement, vA, occurring in the interval between the gradient pulses. Analysis of the phase of the echo yields a measure of flow velocity in a bulk sample. Spatial resolution is easily obtained by the incorporation of additional imaging gradients. 

This analysis was perfonned witii spatial resolution of better than 1 nin. (Taken from [20], figure 2 and figure... 

The STEM instrument itself can produce highly focused high-intensity beams down to 2 A if a field-emission source is used. Such an instrument provides a higher spatial resolution compositional analysis than any other widely used technique, but to capitalize on this requires very thin samples, as stated above. EELS and EDS are the two composition techniques usually found on a STEM, but CL, and even AES are sometimes incorporated. In addition simultaneous crystallographic information can be provided by diffraction, as in the TEM, but with 100 times better spatial resolution. The combination of diffraction techniques and analysis techniques in a TEM or STEM is termed Analytical Electron Microscopy, AEM. A well-equipped analytical TEM or STEM costs well over 1,000,000. 

Electron Probe Microanalysis, EPMA, as performed in an electron microprobe combines EDS and WDX to give quantitative compositional analysis in the reflection mode from solid surfaces together with the morphological imaging of SEM. The spatial resolution is restricted by the interaction volume below the surface, varying from about 0.2 pm to 5 pm. Flat samples are needed for the best quantitative accuracy. Compositional mapping over a 100 x 100 micron area can be done in 15 minutes for major components Z> 11), several hours for minor components, and about 10 hours for trace elements. 

Overall a customer needs to know under what circumstances it is best to use either the electron-beam techniques of EDS and WDS or the X-ray technique of XRF for an analysis problem. If both are equally available, the choice usually resides in whether high spatial resolution is needed, as would be obtained only with electron-beam techniques. If liquids are to be analyzed, the only viable choice is XRF. If one s choice is to use electron-beam methods, the further decision between EDS and WDS is usually one of operator preference. That is, to commence study on a totally new sample most electron-beam operators will run an EDS spectrum first. If there are no serious peak overlap problems, then EDS may be sufficient. If there is peak overlap or if maximum sensitivity is desired, then WDS is usually preferred. Factored into all of this must be the beam sensitivity of the sample, since for WDS analysis the beam current required is lO-lOOx greater than for EDS. This is of special concern in the analysis of polymer materials. 

The uniqueness and desirability of EELS is realized when it is combined with the power of a TEM or STEM to form an Analytical Electron Microscope (AEM). This combination allows the analyst to perform spatially resolved nondestructive analysis with high-resolution imaging (< 3 A). Thus, not oiJy can the analyst observe the microstructure of interest (see the TEM article) but, by virtue of the focusing ability of the incident beam in the electron microscope, he or she can simultaneously analyze a specific region of interest. Lateral spatial resolutions of regions as small as 10 A in diameter are achievable with appropriate specimens and probe-forming optics in the electron microscope. 

Cathodoluminescence (CL), i.e., the emission of light as the result of electron-beam bombardment, was first reported in the middle of the nineteenth century in experiments in evacuated glass tubes. The tubes were found to emit light when an electron beam (cathode ray) struck the glass, and subsequendy this phenomenon led to the discovery of the electron. Currendy, cathodoluminescence is widely used in cathode-ray tube-based (CRT) instruments (e.g., oscilloscopes, television and computer terminals) and in electron microscope fluorescent screens. With the developments of electron microscopy techniques (see the articles on SEM, STEM and TEM) in the last several decades, CL microscopy and spectroscopy have emerged as powerfirl tools for the microcharacterization of the electronic propenies of luminescent materials, attaining spatial resolutions on the order of 1 pm and less. Major applications of CL analysis techniques include ... 

Optical CL microscopes are instruments that couple electron gun attachments to optical microscopes. Although such systems have a limited spatial resolution, they are used widely in the analysis of minerals. ... 

As mentioned earlier, CL is a powerful tool for the characterization of optical properties of wide band-gap materials, such as diamond, for which optical excitation sources are not readily available. In addition, electron-beam excitation of solids may produce much greater carrier generation rates than typical optical excitation. In such cases, CL microscopy and spectroscopy are valuable methods in identifying various impurities, defects, and their complexes, and in providing a powerful means for the analysis of their distribution, with spatial resolution on the order of 1 pm and less. ... 

In summary, CL can provide contactless and nondestructive analysis of a wide range of electronic properties of a variety of luminescent materials. Spatial resolution of less than 1 pm in the CL-SEM mode and detection limits of impurity concentrations down to 10 at/cm can be attained. CL depth profiling can be performed by varying the range of electron penetration that depends on the electron-beam energy the excitation depth can be varied from about 10 nm to several pm for electron-beam energies ranging between about 1 keV and 40 keV. 

STEM can provide image resolution of thin specimens rivaling TEM, but in addition can provide simultaneous crystallographic and compositional analysis at a higher spatial resolution than any other widely-used technique. Any solid material may be examined, provided that a specimen can be prepared that is less than about 100 nm in thickness. 

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