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Recently, a laser‐scanning technique for patterning layer disordering has been reported in which silicon impurities are incorporated by laser irradiation into GaAs‐AlGaAs heterostructures. The sample is subsequently annealed to diffuse the Si deep into the heterostructure. The GaAs‐AlGaAs layers are locally intermixed by diffusion of the silicon impurities. In this report, this two‐step process of laser‐assisted disordering is studied in detail with several material characterization techniques. Scanning electron microscopy and secondary ion mass spectrometry are used to correlate the extent of the layer‐disordered region with the presence of laser‐incorporated Si and oxygen. Transmission electron microscopy (TEM) is used to obtain high resolution images of the disordered/as‐grown interface and to evaluate the crystallinity of the laser‐affected material. TEM images allow the determination of the distribution of the Al and Ga constituents at the interface between the impurity‐disordered alloy and the as‐grown crystal. The data indicate a more rapid Si diffusion in the GaAs layers relative to the Al‐rich layers. The data are discussed in the context of device fabrication.