In this study, particle loading, polyfluorinated alkyl silanes (PFAS or FAS) content, superhydrophobicity, and crack formation for nanocomposite coatings created by the spray coating process were investigated. The formulations comprised hydrophobic silica, epoxy resin, and fluorine-free or FAS constituents. The effect of FAS content and FAS-free compositions on the silica and epoxy coatings’ chemistry, topography, and wetting properties was also studied. All higher particle loadings (~30 wt.%) showed superhydrophobicity, while lower particle loading formulations did not show superhydrophobic behavior until 13% wt. FAS content. The improved water repellency of coatings with increased FAS (low particle loadings) was attributed to a combination of chemistry and topography as described by the Cassie state. X-ray photoelectron spectroscopy (XPS) spectra showed fluorine enrichment on the coating surface, which increases the intrinsic contact angle. However, increasing the wt.% of FAS in the final coating resulted in severe crack formation for higher particle loadings (~30 wt.%). The results show that fluorine-free and crack-free coatings exhibiting superhydrophobicity can be created.