TECHNOLOGY FOCUS - INORGANIC CHEMISTRY - Preparation: No preparation method is given. Preferred Components: The noble metal-based electrocatalyst further comprises bimetallic particles, and a support underlying the bimetallic particles, where the bimetallic particles are dispersed on the support. The bimetallic particles are agglomerated or non-agglomerated. The bimetallic particle has a size of at least 10 nm. The polyhedral shape is cube, truncated octahedron, octahedron, truncated tetrahedron, tetrahedron, or icosahedron shape. The noble metal is platinum (preferred), palladium, gold, silver, ruthenium, rhodium, osmium or iridium. The non-noble metal is titanium, vanadium, chromium, manganese, molybdenum, zirconium, niobium, tantalum, zinc, indium, tin, antimony, lead, tungsten, cobalt, copper, nickel (preferred) or iron. The atomic ratio of the noble metal to the non-noble metal is 0.5-4, preferably 0.2-3. The core region has a size of 40-60% of a size of the bimetallic particle. The surface region has a thickness of 10-30% of the size of the bimetallic particle. The sub-surface region has a thickness of 10-50% of the size of the bimetallic particle. The polyhedral shape comprises facets. Preferred Method: The annealing step is carried out in a vacuum environment of 10-3 Pa or lower. The method further comprises exposing the bimetallic particle to an electrochemical treatment. The electrochemical treatment comprises a multi-cycle oxygen reduction reaction measurement. The bimetallic particle exhibits an oxygen reduction reaction activity of at least 0.5 mA/ mu g of the noble metal, after the annealing. EXAMPLE - Carbon black particles were dispersed in hexane and sonicated for 1 hour. A designed amount of platinum nickel nanoparticles were added to the dispersion at the nanoparticle-to-carbon-black mass ratio of 20:80. The mixture was further sonicated for 30 minutes and stirred overnight. The resultant solids were precipitated out by centrifugation and dried under an argon stream. The solid product was then re-dispersed in n-butylamine at a concentration of 0.5 mg-catalyst/ml. The mixture was kept under stirring for 3 days and then collected using a centrifuge at a rate of 5000 rpm for 5 minutes. The precipitate was re-dispersed in 10 ml methanol and then separated by centrifugation. The carbon-supported platinum-based catalysts were dried before transferring them into the vacuum tube furnace.