The work presented in this book is totally based on experimental aspects. Here author describes growth as well as some characterizations of ZrSe3 and ZrS3 single crystals. The ribon like single crystals of ZrSe3 and ZrS3 are grown by chemical vapor transport method using iodine as a transporting agent. The stoichiometric proportion of constitute elements are confirmed by EDAX. Structure was confirmed by Powder X-ray diffraction technique. Micro topography, High temperature resistivity, High pressure resistivity, Hall Effect measurements, Thermoelectric Power measurements, Optical properties are discussed in this book.