In Situ X-Ray Reciprocal Space Mapping for Characterization of Nanomaterials
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Definition of Topic
In this chapter, we will focus on the small-angle X-ray scattering (SAXS) technique performed on planar samples in the grazing-incidence small-angle X-ray scattering (GISAXS) geometry. This particular method of SAXS allows a fast, nondestructive analysis of the near-surface electron density variations on the lateral length scale ranging from several angstroms up to several hundreds of nanometers with adjustable in-depth sensitivity down to several nanometers. Special emphasis will be given to GISAXS experiments with laboratory X-ray sources as these are much more easily accessible as compared to synchrotron facilities.
The steadily growing research field of applied nanomaterials calls for development of advanced analytical methods for rapid and nondestructive structural characterization. A relatively simple grazing-incidence small-angle X-ray scattering (GISAXS) technique is an efficient analytical tool for structural studies of layered nanomaterials and self-assembled nanostructures. The feasibility to obtain statistically relevant parameters that characterize position correlations and size distributions in the surface or embedded nanoparticle assemblies or interface correlations in the layered nanostructures render the GISAXS technique a valuable complementary tool to the standard real-space investigation methods like transmission electron microscopy (TEM), scanning tunneling microscopy (STM), scanning electron microscopy (SEM), atomic force microscopy (AFM), etc. While a sophisticated sample preparation is often required for the real-space imaging techniques, the GISAXS has no special requirements. This technique is especially valuable for a real-time tracking of the nucleation and growth phases of nanomaterials preparation due to the long X-ray attenuation length in air and absence of special requirements for the experimental setup.
In this chapter, we will review applications of GISAXS for in situ studies of nanomaterial formation including the nucleation, agglomeration, self-assembly, and reassembly phenomena. Majority if not all in situ GISAXS experiments of nanomaterial formation have been performed at synchrotron facilities, taking the advantage of their high X-ray photon flux and low beam divergence. Only the advent of new micro-focusing X-ray sources coupled with high-performance reflective X-ray optics has allowed such GISAXS in situ experiments in a laboratory as will be demonstrated on several examples in this chapter.
KeywordsReciprocal Space Nanoparticle Layer High Photon Flux Nanoparticle Monolayer Lateral Correlation Length
The work was supported by the Slovak Research and Development Agency, project no. APVV-0308-11; Grant Agency VEGA Bratislava, project no. 2/0004/15; and Centre of Excellence SAS FUNMAT. The support of the M-ERA-Net project XOPTICS and COST Actions MP1203 and MP1207 is also acknowledged.
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