X. Guo, A. Gutsche, M. Wagner, M. Seipenbusch, H. Nirschl

Journal of Nanoparticle Research, 2013, 15, 1559

A small- and wide-angle X-ray scattering (SWAXS) technique using a laboratory X-ray source is reported in this article. This non-destructive SWAXS technique allows simultaneous measurements of the primary particle or pore size, surface and mass-fractal dimensions, as well as quantitative determination of the crystallite properties, like phase identification, the co-existence of crystallite components, and their fractions. Some selected experimental results of the SWAXS study of the metallic and oxide nanostructured particles (such as pure Silver nanoparticles, commercial AEROXIDE® TiO₂ P25, Nickel and Nickel oxide nanoparticles as well as Titanium nanoparticles generated by a laboratory electric discharge generator) are presented and discussed in detail, covering a size range of 1-50 nm. The results obtained by SWAXS are compared to those observed with the transmission electron microscope and scanning electron microscope, as well as the XRD reference patterns from the RRUFF database, showing good agreement. In addition, a comparison between powder and dispersion measurements was carried out for estimating the existence and accessibility of microporous structures inside the synthesized nanoparticles, as well as the fraction of open pores. Because of many advantages, such as the high intensity of the primary beam while using a conventional laboratory X-ray source equipped with unique X-ray focusing optics, a short measurement time can be realized. By noninvasive simultaneous measurement of SAXS and WAXS spectra using a single detector; this unique technique allows for fast and extensive in-situ characterizations of metal and metal oxide nanoparticles, respectively, as well as nanostructured materials in many other potential application fields.