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We report a simple one-pot route to fabricate PbSe hollow single-crystalline nanoboxes with the presence of trioctylphosphine as the structure-directing agent and stabilizer. Various controlling parameters were examined, such as trioctylphosphine amounts, reaction temperature, reaction time, and lead(II) precursors. On the basis of the experimental results, the gas bubbles assisted Ostwald ripening process was proposed to explain the formation of hollow PbSe nanoboxes. The morphology and composition of the products were characterized by X-ray diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and transmission electron microscopy.

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