The high entropy alloy (HEA) nanoparticles have been prepared using cast cum cryo-milling process. In which, the Au, Ag, Pd, Pt and Cu (99.9 at. % pure, Alfa Aesar, USA) melted under argon environment to synthesize cast HEAs and afterwardcast HEA have been milled in cryomill for 6 hours. The detailed synthesis process can be found elsewhere. 1 The cryomilled powder (HEA nanoparticles) has been characterizedin order tothe crystalline phase, size, chemical homogeneity, composition, and catalyst activity. The X-ray diffraction recorded using Panalytical empyrean ( max =1.54056 A),and size of nanoparticles have been estimated using Transmission electron microscope (FEI, Technai G 2 , UT 20 operated at 200

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The advancement of nanotechnology demands large scale preparation of nanocrystalline powder of innovative materials. High entropy alloys (HEAs) exhibit unique properties; mechanical, thermal, magnetic etc., making them potentials candidates for applications in energy, environment and biomaterials etc. Thus, there is a need to develop novel synthesis methods to prepare nanocrystalline high purity HEAs in large quantity. Conventional mechanical alloying (MA) of the multi component metallic powder mixture requires larger milling time and it is prone to contaminations and phase transformation. The present investigation reports a unique approach, involving casting followed by cryomilling, leading to formation of nanocrystalline HEAs powder, which are relatively contaminations free with narrow size distribution. Using examples of two FCC and one BCC single phase HEAs, it has been shown that large scale nanocrystalline HEAs powder can be prepared after few hours of cryomilling at 123 K. The formation of nanocrystalline HEAs during cryomilling has been discussed using theoretically available approaches.

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