1：Experimental Design and Method Selection:

The study employed an oil–water interface cation exchange method to fabricate Yb3+/Ln3+/Mn4+ tri-doped Na3ZrF7 phosphors, using solvothermal synthesis for precursors and cation exchange for Mn4+ incorporation. Theoretical models included Tanabe–Sugano energy-level diagrams for Mn4+ analysis.

2：Sample Selection and Data Sources:

Samples were synthesized with varying dopant concentrations (e.g., Yb3+ content from 5 to 60 mol%) using raw materials such as zirconium oxychloride, lanthanide nitrates, and K2MnF6. Data were collected from spectroscopic and structural characterizations.

3：Data were collected from spectroscopic and structural characterizations. List of Experimental Equipment and Materials:

3. List of Experimental Equipment and Materials: Instruments included a powder X-ray diffractometer (MiniFlex600, RIGAKU), SEM (FEI Quanta 400), TEM (JEOL JEM2010), EPR spectrometer (BRUKER A300-10-12), spectrofluorometer (Edinburgh Instruments FS5), and all-purpose fluorescence spectrometer (FLSP920). Materials included ZrOCl2·8H2O, Yb(NO3)3·5H2O, Er(NO3)3·5H2O, HoCl3·6H2O, TmCl3·6H2O, NaOA, NH4F, OA, OM, cyclohexane, HF, KHF2, KMnO4, H2O

4：0). Materials included ZrOCl2·8H2O, Yb(NO3)3·5H2O, Er(NO3)3·5H2O, HoCl3·6H2O, TmCl3·6H2O, NaOA, NH4F, OA, OM, cyclohexane, HF, KHF2, KMnO4, H2OExperimental Procedures and Operational Workflow:

2. 4. Experimental Procedures and Operational Workflow: Synthesis involved preparing K2MnF6, Yb3+/Ln3+:Na3ZrF7 via solvothermal reaction, and cation exchange with K2MnF6/HF solution. Characterizations included XRD, SEM, TEM, EPR, PL, PLE, UC emission spectra, decay curves, and temperature-dependent measurements.

5：Data Analysis Methods:

Data were analyzed using equations for decay lifetimes (t = ∫I(t)dt/I0), crystal-field parameters (Dq, B), and log–log plots for UC emission intensity versus pumping power. Software tools were not specified.