Thermochromism and solvatochromism of solutions of poly(3‐alkylthienylenes) are reported. The experimental results indicate the presence of two coexisting phases: polymer in solution and polymer in microcrystalline aggregates. From the concentration independence of the thermochromism, it is concluded that the transition is fundamentally driven by a single chain mechanism, and that the aggregation (microcrystallization) of the poly(3‐alkylthienylene) macromolecules can occur only after the single chain conformational change has occurred.

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