Nanoparticle characterization by continuous contrast variation in small-angle X-ray scattering with a solvent density gradient

Many low-density nanoparticles show a radial inner structure. This work proposes a novel approach to contrast variation with small-angle X-ray scattering based on the constitution of a solvent density gradient in a glass capillary in order to resolve this internal morphology. Scattering curves of a polymeric core-shell colloid were recorded at different suspending medium contrasts at the four-crystal monochromator beamline of PTB at the synchrotron radiation facility BESSY II. The mean size and size distribution of the particles as well as an insight into the colloid electron density composition were determined using the position of the isoscattering points in the Fourier region of the scattering curves and by examining the Guinier region in detail. These results were corroborated with a model fit to the experimental data, which provided complementary information about the inner electron density distribution of the suspended nanoparticles.