Carbyne is a new carbon allotropes based on sp hybridization that contains alternating triple and single bonds(linear carbon allotropes).Carbyne was synthesized with homogeneous dehydro-chlorination of PVDC.Thermal stability of carbyne was studied by self-manufacture instantaneous-measure device.The result shows that carbyne is stabile at room temperature and carbyniod structure is disappeared when the temperature is higher than 220℃.