The mechanical properties of poly(acrylic acid) (PAA) were investigated on the molecular scale by usingAFM. PAA was adsorbed onto a glass substrate and then picked up at one point of the chain with the AFMtip and stretched. The deformation of single PAA chains under tension was measured and modeled by amodified freely-joint-chain model. The length distribution of loops and tails of adsorbed PAA on the glasssubstrate was also studied by analyzing the extension of the filaments.