In both EG/GOPS-PEDOT:PSS and pg2T-TT, the differences in GISAXS patterns across conditions indicate small morphological changes relative to the meso-scale changes that occur in related conjugated polymer systems during co-deposition, in response to changes in humidity, and operation in a thermoelectric 25 or photovoltaic devices. In contrast to the subtle changes in small angle scattering in EG/GOPS-PEDOT:PSS and pg2T-TT, crys-PEDOT:PSS showed much larger differences in small angle scattering between ex situ conditions (Figure , Figure ). In this case, the conditions were neat (as prepared, Figure ), electrolyte exposed (Figure ), dedoped (-0.6 V vs Ag/AgCl, Figure ), and redoped to a high oxidation state (+0.6 V vs Ag/AgCl, Figure ). As discussed above, sulfuric acid treatment of PEDOT:PSS removed excess PSS and drove the formation of a crystallized nanofibrillar structure. Thus, the anticipated possible effects of ex situ electrolyte exposure and electrochemical (de)doping are differential accumulation of ions within the crystalline nanofibers and voids, and swelling of the crystalline nanofibers. Neat film GISAXS line-cuts displayed a pronounced shoulder around 0.02 Å -1 (Figure ). This feature was enhanced and shifted to higher q-vector upon electrolyte exposure, diminished upon dedoping, and enhanced once again when redoped to a high oxidation state, all in keeping with previously reported low q-vector in situ GIWAXS scattering behavior. The normalized intensity contrast is significantly enhanced when crys-PEDOT:PSS is in the doped state (both electrolyte exposed and redoped states, Figure ), implying a non-uniform ion distribution.