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The cation exchange method has been demonstrated to be efficient in doping Mn4+ ions into various fluorides to synthesize the red‐emitting LED phosphors. This paper, however, reports the challenge in using this method to dope Mn4+ into the Na2SiF6 single crystals, to prepare the fluoride phosphor in single‐crystal form, a state‐of‐the‐art study in the white LED lighting field. The millimeter‐sized...
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