A convenient and effective technique for polymerization to produce the poly(acrylic acidco-acrylamide)/montmorillonite superabsorbent composite in aqueous solution was developed, in which the reaction was initiated by the glow discharge electrolysis (GDE) plasma rather than chemical initiators. The resulted superabsorbent has higher water absorbency, for example, 1024 g g(-1) for distilled water and 56 g g(-1) for 0.9% NaCl solution. To optimize the synthesis conditions, the following parameters were examined in detail: the discharge voltage, discharge time, ratio of acrylic acid to acrylamide, neutralization of acrylic acid, amount of crosslinking agent and montmorillonite added. The superabsorbent composite was characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). Results indicated that montmorillonite was effectively bonded with polymer. Moreover, the water absorbency, water retention and thermal stability of the superabsorbent composite prepared by GDE were higher than those of the superabsorbent composite by conventional chemical method under the same polymerization conditions. (C) 2008 Elsevier Ltd. All rights reserved.