“…Most synthesis methods are multi-step, take long time, low yield, contain solvents, and are not suitable for scaled production. [27][28][29][30][31][32][33][34] On the other hand, many materials contain surfacants and the size of them is relatively large (>50 nm), [33][34][35][36][37][38] which mask a large number of active sites so that catalysts cannot be utilized fully. Therefore, it is particularly important to synthesize surfactant-free ultra-small (<5 nm) nanocatalysts with excellent performance and largescale production.In this work, a series of noble metal doped ultra-small size (4 nm) M-Ni/NiO nanoparticals supported on CNT (M = Ir, Ru, Pd, CNT is carboxylated multi-walled carbon nanotube) were prepared by solvent-free microwave method that is simple, fast, high yield (82.7%), large-scale (>1 g), and no surfactants for the first time.…”