An evaporation-induced method for aggregation of polystyrene-block-poly(acrylic acid) (PS-b-PAA) micelles to unusual polymeric microcubic particles is reported. PS-b-PAA self-assembles into spherical nanomicelles in the block-selective solvent water. After addition of butanone, 1-propanol, acetic acid, N,N-dimethyl-formamide (DMF), or n-butylamine, evaporation of the solvent mixture induces aggregation of the nanomicelles into microcubic particles on the substrate a glass slide. The concentration of the additive, temperature, and substrate affect the morphology of the aggregation of the nanomicelles. Vaporizing the additive/water mixture at 120 degreesC results in the formation of highly symmetrical microcubic particles on a glass slide. The size of microcubic particles is in range from 200 x 200 x 200 nm(3) to 600 x 600 x 600 nm(3). Microcubic particles can also form on a silicon and gold wafer with a size similar to that of those formed on a glass slide. The morphology of the microcubic particles almost remains unchanged at temperatures lower than 150 degreesC, while it is destroyed above 200 degreesC.