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A facile colloidal solution method has been developed for the fast, scalable synthesis of orthorhombic@cubic core–shell nonstoichiometric Cu5FeS4 icosahedral nanoparticles. Such nanoparticles contain high‐density twin boundaries in the form of fivefold twins. Spark plasma sintering consolidates the nanoparticles into nanostructured pellets, which retain high‐density twin boundaries and a tuned fraction...
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