EXELFS (Extended Electron Energy Loss Fine Structure) spectroscopy con
tains the same local atomic structure information as XAFS in addition
to having good low Z element sensitivity, much higher spatial resoluti
on (nanoscale), and the capacity of combining other high spatial resol
ution TEM measurements. Due to poor quality of the EELS data, however,
the EXELFS technique has not been developed to its full advantage. In
this work, various new methods have been introduced to improve data a
cquisition technique and obtain now high quality EXELFS spectra. Also,
the XAFS data analysis software has been interfaced to perform EXELFS
data analysis at the same level of sophistication; this is a signific
ant improvement over the previous cases. To develop EXELFS as a standa
rd tool for structure determination, several additional problems must
also be taken into consideration. Some of these are monitoring thickne
ss variation, energy resolution variation, radiation damage during mea
surements, and better dark-current correction, as well as chi data ren
ormalization. In this investigation, Al and SiC samples were used as c
alibration materials. Al K-edge, Si K-edge, and C K-edge EXELFS spectr
a were measured and analyzed using theoretical calculations and r-spac
e non-linear least-squares fits to determine the structural parameters
. Good agreement with the known structures was obtained.