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Although considerable progress has been made to optimize the optoelectronic properties of conjugated polymers (CPs), the rational design of CPs with tailored physical properties for end-use applications remains a significant challenge. Specifically, experimental characterization of conjugated polymer backbone conformations remains underexplored due to limited techniques that are capable of distinguishing the backbone and side-chain structures at nanoscopic resolution. Thus, relating the electronically functional backbone conformation to the material’s macroscopic optoelectronic property is an ongoing challenge. Here, small-angle neutron scattering techniques (SANS) with contrast-variation (CV) experiments are employed on poly(3-alkylthiophenes) (P3ATs) with both deuterated and protonated side chains in a mixture of protonated and deuterated solvents to decouple the backbone and side-chain …