A straightforward and facile procedure for the fabrication of superhydrophobic luminescent 3D nanomaterials was developed. Chemical modification of ultra-lightweight highly porous nanostructured aluminum oxyhydroxide (NOA) monoliths in 8-hydroxyquinoline vapors resulted in the formation of tris(8-hydroxyquinoline)aluminum on the surface of NOA nanofibrils. The original shape and size of the initial NOA monolith and its internal 3D nanostructure were completely preserved during the modification. Surface modified NOA samples demonstrated intense green luminescence as well as superhydrophobicity, the water contact angle being ~153°.