If you are interested in intermixing between the layers you can try specular and non-specular low angle x-ray scattering techniques, as well as high angle x-ray diffraction. See for example N. Zotov et al. J. Appl. Phys. 100 (2006), 073517.
If one film is somewhat transparent and you want a quick method you can try ellipsometry or spectrophotometry. Provided you have a decent optical model (i.e. you know n&k and thickness) of the films themselves, you can get an idea of the abruptness of the interface from optical data.
As pointed above, you can also use x-ray reflectivity (XRR). You can also have a look at some related discussions on similar topics on RG, making possible use of XRR (or other techniques)
https://www.researchgate.net/post/Is_it_possible_to_find_the_interface_diffusion_in_multilayer_thin_films_by_XRR?_tpcectx=home_feed
or
https://www.researchgate.net/post/How_can_measure_thin_film_thickness_by_XRD2?_tpcectx=home_feed
Regards
cristian
In addition to the good comments you already got, SIMS can be useful to track diffusion. You'll need to design a careful, comparative experiment because SIMS suffers from many artifacts and quantification is a serious challenge; however, when you do it right, SIMS can offer some of the best depth resolutions and elemental sensitivities out there.
Depth profile by Rutherford Backscattering (RBS) could be very useful.
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