Exfoliation of layered materials into ultrathin nanosheets introduces a new cost-effective and 10 environmentally safe fabrication method for novel nanostructured devices. In the present study, we have 11 developed for the first time inorganic oxide nanosheets with near-infrared (NIR) luminescent properties. 12 KLa 1-x Nd x Nb 2 O 7 (x = 0.025, 0.05, 0.1, 0.2, or 0.3) powders obtained by a solid state reaction were exfoliated 13 into single-layer metal oxide nanosheets with approximately 1.7 nm thickness by osmotic swelling with 14 tetrabutylammonium cations, followed by the pronation of KLa 1-x Nd x Nb 2 O 7. We observed strong coupling of 15 high-energy OH vibration with the Nd 3+ energy levels upon protonation and exfoliation steps because of the 16 extremely thin nature of oxide nanosheet-layers. Colloidal oxide nanosheets with an optimized Nd-doping 17 concentration yielded detectable NIR luminescence due to 4 F 3/2-4 I 11/2 (Nd 3+) radiative transitions, which opens 18
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