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Nickel‐ and cobalt‐substituted yttrium aluminum garnets (YAGs) were synthesized varying their stoichiometries and the details of the thermal treatment procedures at elevated temperatures. Ni and/or Co substitution into the framework of Y3Al5O12 was found to be feasible up to molar metal contents of 6 mol %. The synthesis conditions were optimized towards a compromise of high phase purity of the high‐temperature...