Small-angle scattering (SAS) and ultra small-angle scattering techniques, employing x-rays and neutrons, were used to characterize six different aluminum nanopowders and nanopowders composed of molybdenum trioxide and tungsten trioxide nanoparticles. Each material has different primary particle morphology and aggregate and agglomerate geometry, and each is important to the development of nano-energetic materials. The combination of small-angle and ultra small-angle techniques allowed a wide range of length scales to be probed, providing a more complete characterization of the materials. For the aluminum-based materials, differences in the scattering of x-rays and neutrons from aluminum and aluminum oxide provided sensitivity to the metal core and metal oxide shell structure of the primary nanoparticles. Small-angle scattering was able to discriminate between particle size and shape and agglomerate and aggregate geometry, allowing analysis of both aspects of the structure. Using the results of these analyses and guided by scanning electron microscopy (SEM) images, physical models were developed, allowing for a quantitative determination of particle morphology, mean nanoparticle size, nanoparticle size distribution, surface layer thickness, and aggregate and agglomerate fractal dimension. Particle size distributions calculated using a maximum entropy algorithm or by assuming a log-normal particle size distribution function were comparable. Surface area and density determinations from the small-angle scattering measurements were comparable to those obtained from other, more commonly used analytical techniques: gas sorption using Brunauer–Emmett–Teller analysis, thermogravimetric analysis, and helium pycnometry. Particle size distribution functions derived from the SAS measurements agreed well with those obtained from SEM.
