Bombardments of iron (commercially pure) with self-ions having energies of 50 and 100 keV were performed in–situ in a High–Voltage Electron Microscope at temperatures of 40 and 300 K. The resulting damage microstructures were examined at the irradiation temperature in the HVEM using 200, 300, 500 and 1000 keV electrons (damage threshold in Fe is ∼330 keV). Dislocation loop densities were measured as functions of ion dose, ion energy, irradiation temperature, electron dose (500 keV), and step annealing to room temperature. Loop geometries, size distributions, and nature (interstitial or vacancy) were also determined.
Vapor-deposited Zr-Fe multilayered thin films with various wavelengths and of overall composition either 50% Fe or Fe-rich up to 57 % Fe were either irradiated with 300 keV Kr ions at temperatures from 25K to 623 K to fluences up to 2 × 1016 cm−2, or simply annealed at 773Kin-situ in the Intermediate Voltage Electron Microscope at Argonne National Laboratory. Under irradiation, the final reaction product is the amorphous phase in all cases studied, but the dose to amorphization depends on the temperature and on the wavelength. In the purely thermal case (annealing at 773 K), the 50-50 composition produces the amorphous phase but for the Fe-rich multilayers the reaction products depend on the multilayer wavelength. For small wavelength, the amorphous phase is still formed, but at large wavelength the Zr-Fe crystalline intermetallic compounds appear. These results are discussed in terms of existing models of irradiation kinetics and phase selection during solid state reaction.
A detailed study has been conducted of the effect of Kr ion irradiation on phase formation in Zr-Fe metallic multilayers, using the Intermediate Voltage Electron Microscopy (IVEM) at Argonne National Laboratory. Metallic multilayers were prepared with different overall compositions (near 50-50 and Fe-rich), and with different wavelengths (repetition thicknesses). These samples were irradiated with 300 keV Kr ions at various temperatures to investigate the final products, as well as the kinetics of phase formation. For the shorter wavelength samples, the final product was in all cases an amorphous Zr-Fe phase, in combination with Fe, while specially for the larger wavelength samples, in the Fe-rich samples the intermetallic compounds ZrFe2 and Zr3Fe were formed in addition to the amorphous phase. The dose to full reaction decreases with temperature, and with wavelength in a manner consistent with a diffusion-controlled reaction.