Two fluorinated polyphenylquinoxalines (FPPQs) have been prepared from the newly developed trifluoromethyl-containing aromatic bis(alpha-diketone) monomers (FTKs) and aromatic bis(o-diamine). The thermal, electrical, and hydrolytic properties of the FPPQs were investigated. The results reveal that the developed FPPQ films exhibit low dielectric constants of 2.78-2.85, which are closely related to their excellent hydrophobic nature. The FPPQ films also manifest excellent hydrolytic stability in the aqueous environment. Meanwhile, the intrinsically high thermal stability and electrical resistivity are maintained for the FPPQs.