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Abstract Multiscale structural evolution of conjugated polymer (CP) solutions from disorder to aggregation via environmental perturbations is a universal phenomenon in condensed matter physics. Here, we take poly(3‐hexylthiophene‐2,5‐diyl) (P3HT) as a model material and use Ultraviolet–Visible (UV–Vis) spectroscopy to study the hierarchical structure evolution during prolonged aging at relatively low temperature. Using in‐situ UV–Vis spectroscopy and the Franck‐Condon (FC) method, the dynamics of multiscale structural transitions in P3HT were elucidated. Hierarchical structural details can be extracted from the UV–Vis spectra, including the overall percentage of aggregates, conjugation length, degree of H‐/J‐type molecular packing, and site energetic disorder. Through covariance analysis of conformational disorder to aggregation transitions of conjugated polymers obtained under multiple conditions, we find that the trends of the above four key parameters are not consistent, which informs the unique evolution of the degree of ordering at different length scales within the aggregates. This work facilitates the scrutiny of the hierarchical structural transition from multi‐length scale perspective.
Chu et al. (Sun,) studied this question.