In order to validate the SAXS results we use a freeze-drying method to directly image the structure of aggregates in solution, which are then imaged using AFM and SEM. For the freezedrying process 2 μL of polymer solution were sandwiched between a bare Si substrate and a glass coverslip. The sandwiched sample is first submerged in liquid mixture of 63% propane, 37% ethane and then stored in liquid nitrogen. Since this mixture has a larger heat capacity than liquid nitrogen, it can quickly freeze the sample without boiling off and therefore prevent aggregation during the cooling process . In samples frozen with liquid nitrogen alone, solvent crystallization is observed whereas samples frozen in the liquid propane/ethane mixture exhibit amorphous frozen solvent (as observed under cross-polarized optical microscopy). The top coverslip is separated while submerged in liquid nitrogen and the sample is then quickly transferred to a sealed Linkam stage chamber (LTS420) which is held at -100 °C in a nitrogen atmosphere. The temperature is raised to -80 °C (0.5 °C/min) for chlorobenzene (mp = -45 °C ) solutions and to -60 °C for decane (mp = -30 °C ) while vacuum is applied for ~6 hours in order to fully sublimate the solvent while preventing melting. The sample is imaged using tapping mode AFM (Asylum Research Cypher) and SEM (JEOL JSM-7000F) at 25 kV accelerating voltage.