X-ray emission analysis in the electron microscope

The technique by which sample-emitted X-rays are recorded in the electron microscope is assessed. Although the method is relatively insensitive for elements of low atomic number, its applicability in the field of s imultaneous structural and compositional investigations is discussed, together with a critical examination of the analytical precision possible. Various examples of its use are described, including some where structure and stoichiometry can be determined in crystals containing fewer than 10 10 atoms.

Author(s):  
D. F. Parsons ◽  
V. A. Phillips ◽  
J. S. Lally

This investigation was initiated to provide the first assessment, from the users viewpoint, of the health hazards of X-ray leakages from conventional (40-200 Kv acceleration voltage) electron microscopes. Scanning microscopes were not considered at this point.X-rays are produced in the electron microscope when the beam strikes metal parts of the instrument. The degree of X-ray leakage depends on two factors--the intensity of the X-ray source and the amount of metal shielding surrounding it. The efficiency of total (continuous and characteristic) X-ray production is approximately proportional to the atomic number of the metal and to the acceleration voltage (platinum apertures are three times as efficient as the iron of pole pieces). However, the fraction of beam striking the metal has to be taken into account and the efficiency of the shielding. The thickness (number of Half Value Layers), the effect of absorption edges on X-ray transmission, and the cracks or openings in the shielding all have to be taken into account.


Author(s):  
M.D. Ball ◽  
H. Lagace ◽  
M.C. Thornton

The backscattered electron coefficient η for transmission electron microscope specimens depends on both the atomic number Z and the thickness t. Hence for specimens of known atomic number, the thickness can be determined from backscattered electron coefficient measurements. This work describes a simple and convenient method of estimating the thickness and the corrected composition of areas of uncertain atomic number by combining x-ray microanalysis and backscattered electron intensity measurements.The method is best described in terms of the flow chart shown In Figure 1. Having selected a feature of interest, x-ray microanalysis data is recorded and used to estimate the composition. At this stage thickness corrections for absorption and fluorescence are not performed.


Author(s):  
W. Brünger

Reconstructive tomography is a new technique in diagnostic radiology for imaging cross-sectional planes of the human body /1/. A collimated beam of X-rays is scanned through a thin slice of the body and the transmitted intensity is recorded by a detector giving a linear shadow graph or projection (see fig. 1). Many of these projections at different angles are used to reconstruct the body-layer, usually with the aid of a computer. The picture element size of present tomographic scanners is approximately 1.1 mm2.Micro tomography can be realized using the very fine X-ray source generated by the focused electron beam of a scanning electron microscope (see fig. 2). The translation of the X-ray source is done by a line scan of the electron beam on a polished target surface /2/. Projections at different angles are produced by rotating the object.During the registration of a single scan the electron beam is deflected in one direction only, while both deflections are operating in the display tube.


Author(s):  
Werner P. Rehbach ◽  
Peter Karduck

In the EPMA of soft x rays anomalies in the background are found for several elements. In the literature extremely high backgrounds in the region of the OKα line are reported for C, Al, Si, Mo, and Zr. We found the same effect also for Boron (Fig. 1). For small glancing angles θ, the background measured using a LdSte crystal is significantly higher for B compared with BN and C, although the latter are of higher atomic number. It would be expected, that , characteristic radiation missing, the background IB (bremsstrahlung) is proportional Zn by variation of the atomic number of the target material. According to Kramers n has the value of unity, whereas Rao-Sahib and Wittry proposed values between 1.12 and 1.38 , depending on Z, E and Eo. In all cases IB should increase with increasing atomic number Z. The measured values are in discrepancy with the expected ones.


Author(s):  
Marc H. Peeters ◽  
Max T. Otten

Over the past decades, the combination of energy-dispersive analysis of X-rays and scanning electron microscopy has proved to be a powerful tool for fast and reliable elemental characterization of a large variety of specimens. The technique has evolved rapidly from a purely qualitative characterization method to a reliable quantitative way of analysis. In the last 5 years, an increasing need for automation is observed, whereby energy-dispersive analysers control the beam and stage movement of the scanning electron microscope in order to collect digital X-ray images and perform unattended point analysis over multiple locations.The Philips High-speed Analysis of X-rays system (PHAX-Scan) makes use of the high performance dual-processor structure of the EDAX PV9900 analyser and the databus structure of the Philips series 500 scanning electron microscope to provide a highly automated, user-friendly and extremely fast microanalysis system. The software that runs on the hardware described above was specifically designed to provide the ultimate attainable speed on the system.


Author(s):  
C. Newton ◽  
W. T. W. Potts

Magnesium/chlorine and sulphur/chlorine ratios have been measured in the body fluids of some planktonic organisms by x-ray emission analysis of frozen hydrated specimens in a scanning electron microscope. Homarus vulgaris (Anthropoda: Decapoda) larvae excluded Mg2+ and SO42-ions from the haemolymph, but to a lesser extent than does the adult lobster. Bipinnaria larvae of Asterias (Echinodermata) excluded Mg2+ and SO42-ions from the coelomic fluid. Obelia medusae excluded Mg2+ and SO42-ions from the mesogloea but concentrate them in the gastrovascular system. The high concentration of sulphate in the gastrovascular fluid of medusae has been confirmed by rhodizonate titration in Cyanea and Rhizostoma jellyfish. Some implications of magnesium and sulphate regulation are discussed.


In a previous paper it was shown that 0·0007 per cent, of 29 Cu and 0·0003 per cent, of 26 Fe could be detected in 30 Zn by atomic analysis by X-ray spectroscopy. This sensitivity is greater than that which was claimed by Noddack, Tacke, and Berg, who set the limit at about 0·1 per cent, for non-metals, and by Hevesy, who stated it to be about 0·01 per cent, for an element present in an alloy. It was later suggested by Hevesy that the high value of the sensitivity which we found might result from the fact that some of the alloys we had used were composed of elements of almost equal atomic number, and that the sensitivity would be smaller for a constituent of low atomic number mixed with a major constituent of high atomic number. To elucidate these disagreements we have made further observations of the sensitivity with elements of different atomic number and have investigated the conditions which can influence the sensitivity. The Factors Determining Sensitivity . The detection of one element in a mixture of elements depends upon the identification of its K or L lines in the general spectrum emitted by the mixture under examination. The intensity with which these lines are excited in the target (“excited intensity”) is proportional to the number of atoms of the constituent element excited, i. e ., to its concentration and to the volume of the target in which the cathode ray energy is absorbed. The depth of penetration of the cathode rays is determined by the density of the target material and by their velocity ( i. e ., by the voltage applied to the X-ray tube). Schonland has shown that the range of homogeneous cathode rays in different elements, expressed as a mass per unit area, is approximately constant and is independent of the atomic number of the absorbing element. When their velocity is increased, the cathode rays will penetrate to a greater depth, and therefore a greater number of atoms of all constituents will be ionised. This will increase the “excited intensity” of the lines due to the particular constituent sought equally with those lines of the other elements present. The intensity of a line further depends upon the difference between the voltage applied to the X-ray tube and that necessary to excite the series. For these reasons, a high applied voltage is required for a high sensitivity.


1969 ◽  
Vol 13 ◽  
pp. 26-48
Author(s):  
A. K. Baird

Qualitative and quantitative analyses of elements below atomic number 20, and extending to atomic number 4, have been made practical and reasonably routine only in the past five to ten years by advances in: 1) excitation sources; 2) dispersive spectrometers; 3) detection devices; and 4) reductions of optic path absorption. At present agreement is lacking on the best combination of parameters for light element analysis. The principal contrasts in opinion concern excitation.Direct electron excitation, particularly as employed in microprobe analysis (but not limited to such instruments), provides relatively high emission intensities of all soft X-rays, but also generates a high continuum, requires the sample to be at essentially electron gun vacuum, and introduces practical calibration problems (“matrix effects“). X-ray excitation of soft X-rays overcomes some of the latter three disadvantages, and has its own limitations. Sealed X-ray sources of conventional or semi-conventional design can provide useful (if not optimum) light element emission intensities down to atomic number 9, hut with serious loss of efficiency in many applications below atomic number 15 largely because of window-thinness limitations under electron bombardment.


1963 ◽  
Vol 7 ◽  
pp. 555-565
Author(s):  
Frank Bernstein

AbstractMineralogical effects, which relate to the occurrence of an element in different forms of chemical combination, often are a problem to the X-ray analyst since these forms usually differ in X-ray sensitivity. An example of this is cited in connection with the analysis of sylvite concentrates for potassium. An evaluation is made of mineralogical effects and a quantitative relationship between X-ray intensity and mineral form and particle size is derived. If the particle size of a minor constituent is reduced sufficiently the mineralogical effect disappears. Target materials for X-ray sources are found to have only minor effects on relative intensities of different compounds of an element. Finally, it is concluded that the advantages of higher intensities gained through the use of target materials close in atomic number to the material being analyzed far outweigh particle size effects which are shown to be relatively small.


2004 ◽  
Vol 03 (03) ◽  
pp. 281-292 ◽  
Author(s):  
J. NAYAK ◽  
S. VARMA ◽  
D. PARAMANIK ◽  
S. N. SAHU

The synthesis of the GaAs nanoparticles, having sizes 7 nm to 15 nm, by a low cost electrochemical technique has been reported. The absence of any foreign impurity has been confirmed by the Proton-Induced X-rays Emission analysis. Rutherford Backscattering measurement has been performed in order to estimate the thickness of the nanoparticle-generated thin film as a function of the electrolysis current density. The X-ray Photoelectron Spectroscopic study confirms the formation of GaAs and exhibits the binding energy shift of the core shell electrons as an implication of the nanostructure effect. Very weak infrared luminescence due to the radiative recombination of the impurity bound exciton has been detected from yttrium-doped GaAs nanocrystals, even at room temperature.


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