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In this Letter, sodium dodecyl sulfate (SDS) was applied not only as surfactant, but also as sulfur source to produce lead sulfate (PbSO4) micro/nanostructures via a microwave-assisted route. All experiments were carried out in propylene glycol as a solvent. The effect of preparation parameters, such as microwave power and irradiation time, on the morphology of products was studied. Scanning electron microscopy images indicated that after microwave irradiation for 12 min at 750 and 900 W, star-like microstructures of PbSO4 composed of cubic-like nanostructures were obtained. Pure orthorhombic PbSO4 was obtained after annealing at 450°C for 3°h. Photoluminescence properties of PbSO4 micro/nanostructures at room temperature were investigated.