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High-performance PtNi alloy nanoparticle-supported multiwalled carbon nanotube composite (PtNi/MWCNT) electrocatalysts can be prepared via one-pot preparation for oxygen reduction reaction. This route of preparation utilizes the pyrolytic decomposition of metal precursors, such as Pt(acac) 2 with Ni precursors, nickel bis(trifluoromethanesulfonyl)amide (Ni[Tf 2 N] 2 ) or nickel acetylacetonate (Ni(acac) 2 ), in an ionic liquid (IL), N , N , N -trimethyl- N -propylammonium bis(trifluoromethanesulfonyl)amide ([N 1,1,1,3 ][Tf 2 N]). Currently, there is insufficient information concerning the effect of difference in preparation conditions on the formation mechanism and catalytic activity of PtNi/MWCNT. In this article, a staircase heating process was used to investigate the PtNi alloy nanoparticle formation mechanism and catalytic activity of the resulting PtNi/MWCNT. We found that the alloy formation process, composition, and crystal structure, which directly affect the electrocatalytic activity, strongly depended on the Ni precursor species and heating process. The catalytic performance of certain PtNi/MWCNTs collected during the staircase heating process was better than that of PtNi/MWCNTs produced via the conventional heating process.

One-Pot Synthesis of PtNi Alloy Nanoparticle-Supported Multiwalled Carbon Nanotubes in an Ionic Liquid Using a Staircase Heating Process