Alloyed bimetallic Pd-Ru nanocatalysts prepared by in situ reduction of a mixture of a Ru(iii) source and a Pd(ii)@alkyne-PVA aerogel and characterized by TEM and XPS exhibit very highly catalytic activity towards hydrogen release from ammonia borane hydrolysis with a TOF value of 578.2 molH2 molcat-1 min-1.