AbstractIt is shown that amine‐terminated poly(aryl ether ketone)s based on the reaction of 4,4'‐difluorobenzophenone, and a substituted hydroquinone [either methylhydroquinone (MePK),t‐butylhydroquinone (tBPK), or phenylhydroquinone (PhPK)] of controlled molecular weight and high amine‐termination efficiency can be synthesized by a two‐step reaction technique. Attempts to synthesize analogous materials by a one‐step method were shown to be unsuccessful. The side groups are shown to have a large influence on the aromatic proton chemical shifts and this effect is characterized. The side groups and molecular weight are also shown to influence the thermal transitions of the respective polymers. The tBPK polymer possessed the highest glass transition temperature, while the MePK polymer was found to be the only semi‐crystalline polymer; a unit cell is proposed. The side groups and molecular weight effects are also characterized as a function of thermal stability and mechanical properties. © 1994 John W