Morphological evolution of nanopores and cracks as fundamental components of ultrashort pulse laser-induced nanogratings

Within recent years the phenomena of so-called nanogratings induced by tightly focussed femtosecond laser pulses has gained significant interest. These self-organized structures appearing after several laser pulses show strong formbirefringence which allows, when combining with the three-dimensional freedom of the direct laser writing technique, to fabricate versatile functionalities. However, the underlying structure has been the subject of intensive debate since the discovery of the nanogratings ten years ago. In order to uncover the primary constituents of nanogratings typical visualisation techniques (e.g. SEM) rely on cleaving and subsequent etching of laser treated samples. Fine details are effectively erased by such invasive preparation methods. Recent investigations based on exclusively cleaved samples report on hollow cracks embedded within the bulk material. However, these time-consuming imaging methods only provide two-dimensional cross sections and can hardly address the evolution of cracks (size, shape) depending on various laser parameters. To overcome these limitations we performed a comprehensive study of nanopores and cracks using small-angle x-ray scattering (SAXS) in combination with focussed ion beam milling (FIB) and scanning electron microscopy (SEM). By probing nanogratings inscribed in the bulk of fused silica we found nanopores with dimensions of (30x25x75)nm3 and (280x25x380)nm3. While the dimensions remain constant with ongoing laser exposure and different pulse energies the nanopore shape changes from cuboidal cracks to ellipsoidal