A fast low-pressure transport route to large black phosphorus single crystals

Black phosphorus, a promising candidate for lithium battery electrodes, can be prepared by a low-pressure transport reaction route representing the first effective and scalable access to this element modification. Crystal sizes larger than 1 cm were obtained at low-pressure conditions in silica ampoules. X-ray phase analyses, EDX, ICP-MS and optical microscopy were applied to characterize the resulting black phosphorus. The present method drastically improves the traditional preparation ways like mercury catalysis, bismuth-flux or high-pressure techniques and represents an easy, non-toxic, fast and highly efficient method to achieve black phosphorus. In contrast to a previously reported low-pressure route the present transport reaction allows an up-scaling to higher masses of starting materials, a larger black phosphorus yield and faster reaction time under retention of the high product crystallinity.