Imaging using electron spectrometers

The irradiating X-ray beam cannot be focussed upon and scanned across the specimen surface as is possible with an electron beam. Practical methods of small-spot XPS imaging rely on restriction of the source size or the analysed area. By using a focussing crystal monochromator for the X-rays, beam sizes of less than 10 pm may be achieved. This must in turn correspond with the acceptance area and alignment on the sample of the electron spectrometer, which involves the use of an electron lens of low aberration. The practically achievable spatial resolution is rarely better than 100 pm. A spatial resolution value of 200 pm might be regarded as typical, and it must also be remembered that areas of up to several millimetres in diameter can readily be analysed. 

Characterization methods. The 100 kV Vacuum Generator HB-5 STEM was used to mlcroanalyze samples. The HB-5 has a KEVEX SI(LI) energy dispersive X-ray spectrometer (EDS) and micro area electron diffraction (MAED) capabilities In conjunction with simultaneous bright and dark field Imaging capabilities. A more detailed explanation of the Instrumental operation can be obtained In a publication by C. Lyman(12). 

Characterization. IR spectra of the samples were recorded on Nicolit AVATAR360 spectrometer. The TEM images were obtained on Hitachi H-8100IV electron microscope. TGA and DTA analyses were carried out in Du pont 9900 Thermal Analysis System. X-ray diffraction (XRD) measurement was conducted on a Siemens D5005 diffractometer using Cu Ka radiation (X = 1.54 °A). 

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