Backscattering spectrometry with channeling and x‐ray rocking curves have been employed to analyze metalorganic chemical‐vapor‐deposition‐grown AlxGa1−xAs/GaAs strained superlattice structures in significant detail. Both techniques complement each other in the precise determination of composition, thickness, and strain in the individual layers of the superlattices. In addition, the sensitivity of the two techniques allows quantitative measurements of transition regions at the interfaces of various layers. Such fine probing into thin layered superlattice structures provides essential feedback in controlling their growth.