Compounds of Formula (I): R1-O-(CF2-O)n-R1, wherein: n is an integer from 2 to 100; and R1 is perfluorinated alkyl or substituted perfluorinated alkyl are described. Also described are methods of preparing the compounds of Formula (I). For example, compounds of Formula (I) can be prepared by providing a poly(oxymethylene) compound and fluohnating the poly(oxymethylene) compound, for instance, via direct aerosol fluorination.