Sulfonated poly(arylene ether sulfone)s (S-PESs) were synthesized from sulfonated 4,4'-dichlorodiphenylsulfone (S-DCDPS), 4,4'-dichlorodiphenylsulfone (DCDPS), and 4,4'-biphenol through variations in the molar ratio of S-DCDPS to DCDPS from 10/90 to 40/60. The S-PES sodium form was characterized with Fourier transform infrared, H-1-NMR, thermogravimetric analysis, differential scanning calorimetry, and dynamic mechanical analysis, and the intrinsic viscosity and solubility were also evaluated. The sodium form was then subjected to acidification by immersion in 1.5M HCl for 24 h at room temperature, which was followed by washing with deionized water. The S-PES adhesive properties were measured with single laboratory shear samples with aluminum alloys, and the failure mode was investigated. The synthesized S-PESs exhibited increased glass-transition temperatures with increased S-DCDPS/DCDPS ratios; their acid forms provided much lower glass-transition temperatures than their sodium forms. In addition, the S-PES sodium form exhibited a high intrinsic viscosity, which indicated a high molecular weight. The S-PES acid form exhibited an adhesion strength similar to that of the sodium form, and the single-lap-shear strength increased with 10% S-PES and then decreased with 20, 30, and 40% S-PES. (C) 2004 Wiley Periodicals, Inc.