Polycrystalline powders of ZrSiS were first synthesized by mixing high-purity zirconium (99.99%), silicon (99.999%), and sulfur (99.99%) and sintering at 1000°C for 5 days. From the polycrystalline precursor, the single crystals were grown by chemical vapor transport method with iodine as agent. The polycrystalline powders and iodine in a mass ratio of 1:0.07 were sealed in silica tubes under vacuum. Then, the silica tubes were put in a gradient tube furnace with the source powders at 1050°C and the cold end at around 950°C for 7 days. Rectangular plane-like crystals were obtained from the cold end of the silica tubes.

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