Hard X-ray microprobes from synchrotron radiation ( SR ) sources should be powerful tools for various fields of research. A Fresnel zone plate ( FZP ) is a promising focusing element for X-ray. In order to develop high performance multilayer FZP for use in hard X-ray region, Ag/C and Cu/Al concentric multilayers were prepared by some deposition parameters. A dependence of the zone boundary structures on the Ar gas pressure was observed: the multilayer prepared at lower Ar gas pressure had smoother zones. Substrate cooling did not improve the zone boundary structures. From the focusing test of the Cu/Al FZP by the SR, a microbeam of 1.3 μ m ø has been obtained for 8 KeV X-ray (λ =0.154nm).