Two-mode nanometer fluorescence labelling material based on rare earth doped sodium gadolinium fluoride core-shell structure and preparation method thereof
A rare earth doping, sodium gadolinium fluoride technology, applied in luminescent materials, chemical instruments and methods, fluorescence/phosphorescence, etc., can solve the problem that the up-conversion and down-conversion luminescence cannot be integrated into the same nanoparticle, which limits the application and cannot be realized. The multifunctionalization of sodium fluoride gadolinium nanomaterials can achieve the effects of good water solubility and biocompatibility, uniform particles, and simple preparation process.
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example 1
[0016] Example 1: (1) NaGdF 4 : Preparation of 18%Yb, 2%Er nanocrystalline cores. Weigh 0.294g gadolinium chloride (GdCl 3 .6H 2 O), 0.0076g erbium chloride (ErCl 3 .6H 2 O) and 0.0697g ytterbium chloride (YbCl 3 .6H 2 O) join in the 100ml there-necked flask, add 5ml oleic acid and 16ml octadecene, stir to make it mix evenly. Under the protection of nitrogen flow, the above mixture was heated to 150° C. and kept at this temperature for 90 minutes to completely dissolve the rare earth chloride and obtain a transparent clear solution. After cooling to room temperature, 10 ml of methanol solution in which 0.14 g of ammonium fluoride and 0.14 g of sodium hydroxide were dissolved was added dropwise, stirred and allowed to react at room temperature for 30 minutes. Then the mixed solution was heated to 50° C. and kept for 30 minutes to remove methanol in the reaction system. After the methanol was removed, the reaction system was heated to 300° C. under the protection of nitr...
example 2
[0018] Example 2: (1) NaGdF 4 : 18% Yb, 1% Tm nanocrystalline core preparation. Weigh 0.3011g gadolinium chloride (GdCl 3 .6H 2 O), 0.0038g thulium chloride (TmCl 3 .6H 2 O) and 0.0697g ytterbium chloride (YbCl 3 .6H 2 O) join in the 100ml there-necked flask, add 4ml oleic acid and 16ml octadecene, stir to make it mix evenly. Under the protection of nitrogen flow, the above mixture was heated to 150°C, and kept at this temperature for 90 minutes to completely dissolve the rare earth chloride and obtain a transparent clear solution. After cooling to room temperature, add 0.14g of ammonium fluoride and 0.14 g of sodium hydroxide in methanol solution 10 ml, stirred and allowed to react at room temperature for 30 minutes, the mixed solution was heated to 50° C., and kept for 30 minutes to remove methanol in the reaction system. After the methanol was removed, the reaction system was heated to 300° C. under the protection of nitrogen flow, kept for 60 minutes, then stopped h...
example 3
[0020] Example 3: (1) NaGdF 4 : 18% Yb, 1% Tm, 0.5% Er nanocrystalline core preparation. Weigh 0.2992g gadolinium chloride (GdCl 3 .6H 2 O), 0.0038g thulium chloride (TmCl 3 .6H 2 O), 0.0697g ytterbium chloride (YbCl 3 .6H 2 O), 0.0019g erbium chloride (ErCl 3 .6H 2 O) join in the 100ml there-necked flask, add 4ml oleic acid and 16ml octadecene, stir to make it mix evenly. Under the protection of nitrogen flow, the above mixture was heated to 150°C, and kept at this temperature for 90 minutes to completely dissolve the rare earth chloride to obtain a transparent clear solution, which was then cooled to room temperature. Then, 10 ml of methanol solution in which 0.14 g of ammonium fluoride and 0.14 g of sodium hydroxide were dissolved was added dropwise, stirred and allowed to react at room temperature for 30 minutes. Then the mixed solution was heated to 50° C. and kept for 30 minutes to remove methanol in the reaction system. After the methanol was removed, the reac...
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