Solvent‐free synthesis of bismuth‐based photocatalysts with hierarchical architectures has been rarely reported yet. Herein, BiOCl hierarchical microflowers (MFs) were prepared via a solvent‐free route for the first time, using chlorobutanol as the chlorine source. The reaction temperature (T) plays a key role for formation of MFs. The MFs were formed at T >120 °C and some MFs merged into large nanosheets (LNs). MF/LN homojunctions were constructed because considerable differences in sizes and exposed facets between the MFs and the LNs cause differences in their energy band levels. The sample prepared at 120 °C possesses the highest contents of MFs and homojunctions, specific surface area (SBET, 13 m2 g−1), and photoactivity, indicating the high photoactivity of the sample arises from fabrication of homojunctions as well as the high SBET. This work provides a solvent‐free way to simultaneously synthesize BiOCl MFs and homojunctions, which paves an avenue for solvent‐free synthesis of other photocatalysts.
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