Article ID: ISIJINT-2019-387
To investigate the performance of the size measurement by asymmetric flow field-flow fractionation (AF4), the measurement results of gold nanoparticles were compared among AF4, transmission electron microscopy (TEM), and small-angle X-ray scattering (SAXS) in terms of the average size and full width at half maximum (FWHM) of the size distribution. Although the average size was almost the same for the three methods, the FWHM measured using AF4 was larger than those measured using TEM and SAXS. This is attributed to the diffusion of the gold nanoparticles inside the AF4 instruments. The broadening coefficient of AF4 analysis was determined as 2.08 by the average of FWHM ratio of AF4 to TEM measured using the several sphere-like gold nanoparticles. In addition, the effect of particle shape on the above broadening coefficient was investigated using the sphere-like and plate-like silver nanoparticles. The broadening coefficient for plate-like particles apparently became smaller than that for sphere-like particles, possibly because the Brownian motion of plate-like particles was suppressed.
Furthermore, the AF4 analysis with the FWHM correction method using the broadening coefficient was applied to niobium carbide (NbC) precipitates in steels. The average size measured by AF4 was mostly consistent with the results obtained in regions observed by TEM. Moreover, an increase in the number density of nanometer-sized NbC by heat treatment was successfully detected. The effect of particle shape on FWHM should be further investigated and improved; however, AF4 with the broadening coefficient can semi-quantitatively analyze the size distribution of nanoprecipitates in steels.