The structure of nanospheres with a crystalline core and an amorphous diffuse shell was investigated by small-angle neutron scattering (SANS), small-, medium-, and wide-angle X-ray scattering (SAXS, MAXS and WAXS), and differential scanning calorimetry (DSC). Nanospheres, 28 to 35 nm in diameter, were prepared from a triblock copolymer with poly(ethylene glycol) (PEG) hydrophilic end-blocks and oligomers of alternating desaminotyrosyl-tyrosine octyl ester (DTO) and suberic acid (SA) as the central hydrophobic block. In the lyophilized nanospheres, the diffraction patterns show that the PEG shell is ∼10 nm in thickness and crystalline, and the hydrophobic core is ∼10 nm in diameter with a smectic liquid crystalline texture.
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