We give an account of X-ray diffuse scattering (XDS) as a non-destruct
ive technique to characterize the defect structure of organic multilay
ers. As well as the interface roughness we especially investigated the
lateral correlation length tau of scattering aggregates using the ang
le-dispersive as well as the energy-dispersive scattering from a Pb st
earate film. Although the present theoretical model is not satisfactor
y, it is possible to relate tau to the in-plane dimension of the micro
crystalline domains. The XDS and the X-ray specular reflectivity (XSR)
depend in a different manner on the interface roughness and the domai
n size. Therefore the ratio of XDS and XSR measured at special points
of reciprocal space can be used to observe the changes in these real s
tructure parameters. This is demonstrated in the case of thermally ind
uced melting of domains.