Molybdenum dioxide (MoO 2) a kind of semi-metal material shows many unique properties, such as high melting point, good thermal stability, large surface area-to-volume ratio, high-density surface unsaturated atoms, and excellent conductivity. There is a strong connection between structural type and optoelectronic properties of 2D nanosheet. Herein, the rectangular and hexagonal types of thin and thick MoO 2 2D nanosheets were successfully prepared from MoO 3 powder using two-zone chemical vapor deposition (CVD) with changing the experimental parameters, and these fabricated nanosheets displayed different colors under bright-field microscope, possess margins and smooth surface. The thickness of the blue hexagonal and rectangular MoO 2 nanosheets are~25 nm and~30 nm, respectively, while typical thickness of orange-colored nanosheet is around~100 nm. Comparative analysis and investigations were carried out, and mix-crystal phases were indentified in thick MoO 2 as main matrix through Raman spectroscopy. For the first time, the emission bands obtained in thick MoO 2 nanosheets via a Cathodoluminescence (CL) system exhibiting special properties of semi-metallic and semiconductors ; however, no CL emission detected in case of thin nanosheets. The electrical properties of thin MoO 2 nanosheets with different morphologies were compared, and both of them demonstrated varying metallic properties. The resistance of thin rectangular nanosheet was~25 Ω at ± 0.05 V while 64 Ω at ± 0.05 V was reported for hexagonal nanosheet, and observed lesser resistance by rectangular nanosheet than hexagonal nanosheet.