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Elastically strained supermultiperiod (100–1000 periods) AlGaAs/GaAs superlattices with different doping levels and slightly differing period thicknesses have been investigated. The proposed technique of characterization consisting of combined application of deep X-ray reflectometry based on a rigorous calculation method, as well as the well-known method of high-resolution X-ray reflectometry, has made it possible to investigate 100-period structures with 2-nm-wide Al0.3Ga0.7As barriers and 10-nm-wide GaAs wells and determine with a high accuracy the layer thicknesses and spread of interfaces. This achievement can be considered as a first step in further analysis of thick structures using bright synchrotron radiation source. The difference between the expected and obtained by the proposed method layer thicknesses is several percent, including that for samples with a high doping level (up to 1018 cm–3). All supermultiperiod structures are characterized by sharp interfaces with a standard deviation of about 0.1 nm. Based on the obtained data on the thicknesses, one can accurately determine the layer compositions using high-resolution X-ray diffraction. [ABSTRACT FROM AUTHOR]