Spring 2011 MAT 571 Introduction to Electron Microscopy Homework 2 Please provide clear and organized answers to the

questions below. Avoid copy-pastes and taking sentences directly from reference sources Compile the texts with your own words and understanding. 1. Explain absorption edge and its effect on the EDX analysis. Absorption value is a characteristic value for each element. In the inelastic scattering, when the incident beam's energy is just sufficient enough to energy corresponds to energy which is necessary to excite an electron from its orbit, x rays or other waves are not formed and emitted. This happens through this equation;

Eincident=Ebinding + Ekinetic

Fig.1. Shows the absorption increasing in a Pt atom. This increasing at absorption causes drastic decreasing in x-ray EDS peak. [1] Absorption density has highest value when the energy of x rays are just enough to to excite sample electrons from their orbitals. Excited electrons are being scattered and leaves their positions empty. The electron from upper shell fills this space. It also excites waves which has the energy comes from energy difference between two orbitals. Here, emitted waves are called as flourescent radiaton. Since the flourescent radiation is one of the strong reasons of background during the analysis, we need to get them as much as lower amounts.

In the x ray peaks, sharp discontinuances are called as Absorption Edge. Each element has characteristic Absorption Edge which is decreasing with increasing atomic number. [2] 2. Why is there more than one type of diffracting crystal in a WDX detector? Explain. In WDX, it's not possible to cover entire angular range with a detector stage. Even if it is possible, wouldn't be time efficient. To make detection at shorter period and compensate the time disadvantage, instead we're using 4 (or less/ more) detectors at certain angle ranges. They're working simultaneously and making process faster. Each detectors has different crystals with different d-spacing. [3] 3. Why do we choose to work at low accelerating voltages to get a good resolution image in SEM while X-ray analysis requires higher acceleration voltages? In SEM, there are several reasons for working with low accelerating voltages. Most important one is overlapping of electron interaction volumes at the scanning sequence. Bombarding the specimens with higher kV causes that overlapping of interaction volumes. Possibility of having overlapping is very high when we are working with heavy elements. This causes that images are being fuzzy. Also, at higher kV's, background and noise are increasing and effecting the image quality.[4] In X-ray analysis, Since it is more about statistics, accelerating voltage is increasing the number of detected x rays and makes the statistical calculations more precise.
N = hf / E N implies electron-hole pairs generated by incident beam, it equals to incident beam's energy over required average energy to overcome electron binding. If we have higher hf value, we have more ruptured x-rays.[5]

4.

Discuss the formation of satellite peaks and peak shifts in characteristic X-ray analysis in detail. Would WDX or EDX be a good option to observe them? In some cases, especially the moment that working with high overvoltages, incident beam may trigger the ejection of more than one electron from an atom. At that case, overall shell structure of the atom may be changed. This may cause more than one type x-ray formations. This second type x rays can be detected by the detector if their energy is sufficient to be detected. This low energetic secondary waves are named as satellite peaks. Also auger electrons can attribute and form satellite peaks. [6]

Peak shifts are like the deviation on the x ray analysis, which may come from several reasons. Protective Be window, Single crystal Si atoms or any contamination around the stage can cause peak shifts. WDX can be an option to observe these peaks since process produces numerically stronger waves. But EDS detector is most likely not enough to detect these very low energetic waves.

Sources [1] http://www.chem.ucalgary.ca/research/groups/faridehj/xas.pdf [2] Bob H. He, Two Dimensional X Ray Diffraction, 56. [3] Ray F. Egerton, Physical Principles of Electron Microscopy, Page:169 [4] http://www.ccmr.cornell.edu/igert/modular/docs/3_Scanning_Electron_ Microscopy.pdf [5] Ray F. Egerton,Physical Principles of Electron Microscopy, Page:161 [6] http://www4.nau.edu/microanalysis/microprobe/Xray-SatellitePeaks.html