Thin films of oriented Fe and Cr intercalated (NbSe2)(x)(TiSe2)(y) superlat
tices have been synthesized by controlled annealing of elementally modulate
d reactants. Analytic techniques have been developed to extract the average
c-axis structure of the unit cell, the distribution of c-axis crystal size
s, and the distribution of structural defects from X-ray diffraction data.
High-resolution synchrotron source X-ray diffraction data were collected fr
om a [(Fe0.33NbSe2)(8)(Fe0.33TiSe2)(8)](12) Sample (i.e., 12 superlattice u
nit cells in the film, each cell containing 8 layers of Fe0.33NbSe2 followe
d by 8 layers of Fe0.33TiSe2) at three anomalously scattering wavelengths.
Analysis determined structural parameters within 2% of published values fur
the parent compounds, typical crystal sizes of 200-500 Angstrom, and typic
al coherence losses over a unit cell of +/-1%. Theoretical diffraction prof
iles calculated directly from the model structure are shown to agree satisf
actorily with experiment. The flexibility offered by our growth technique s
uggests that synthesis of many such superlattices with a variety of differe
nt materials properties should be possible.