Probe size study of apatite irradiation in stem

Abstract

The effect of electron beam irradiation of stoichiometric hydroxyapatite (Ca10(PO4)6(OH)2, HAP) is investigated using electron energy loss spectroscopy (EELS) in the scanning transmission electron microscope (STEM) mode equipped with a LaB6 gun. Initial irradiation at 160 A cm −2 dose rate shows no modification of the low loss spectra. No difference of mass loss for Ca, O and P is observed for two different probe diameters: 4 nm (dose rate = 160 A cm −2) and 24 nm (dose rate = 70 A cm −2). Furthermore no formation of CaO is observed for both experimental conditions. It is proposed that the low values of both electron dose rates and doses (from 350 to 2400 C cm −2) avoid mass loss. At the higher dose rate obtained with a field emission gun (FEG), transformations are observed for the lowloss signal as well as for the Ca, P and O signals. These results might be very useful for the future studies of apatite particles at the nanoscale.