Method for synthesizing monodisperse rare earth doped up-converted fluorescence nanocrystalline through microwave assistance, and product thereof and application
A rare earth doped, nanocrystalline material technology, applied in the field of materials, can solve the problems of harsh reaction conditions, low efficiency, and uneven product particle size.
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[0092] The present invention also provides a method for preparing the nanocrystalline material, comprising the steps of:
[0093] 1) providing a first mixed solution, said first mixed solution comprising a solvent and a salt of a sodium salt, an yttrium salt and a rare earth element dissolved therein;
[0094] 2) Circulating the first mixed solution to vacuumize and fill with protective gas to obtain the second mixed solution;
[0095] 3) sealing the second mixed solution, and heating it with microwave to obtain the third mixed solution;
[0096] 4) Optionally, the container loaded with the third mixed solution is rapidly cooled to room temperature by using high-speed flowing air;
[0097] 5) Adding an excessive amount of precipitating agent to the mixed solution obtained in the preceding steps, and the precipitated product is the nanocrystalline material.
[0098] In another preferred example, the solvent includes (but not limited to): oleic acid, olefin, or a combination t...
Embodiment 1
[0141] Synthetic NaY 0.8 f 4 :Yb 3+ 0.18 ,Er 3+ 0.02 The method is as follows:
[0142] a) Weigh 80mg sodium trifluoroacetate (Na-TFA) (powder), 180mg yttrium trifluoroacetate (Y-TFA) (powder), 42mg ytterbium trifluoroacetate (Yb-TFA) (powder), 4mg trifluoroacetic acid Add erbium (Er-TFA) (powder) into a reaction flask filled with 10 mL of 1:1 oleic acid:octadecene (OA:ODE), stir and heat to 110°C until all the added reactants are dissolved, Form a transparent and uniform solution (about 10ml);
[0143] b) The reaction solution was vacuumed and filled with nitrogen for several times to remove impurities such as water and oxygen (the resulting product was about 9ml);
[0144] c) Transfer the above reaction solution to the quartz reaction vessel of the microwave reactor, seal it, heat it with microwave to 280°C, and keep the reaction for 3 minutes;
[0145] d) After the reaction stops, use high-speed flowing air to cool the reaction vessel and solution to room temperatur...
Embodiment 2
[0156] Synthetic NaY 0.78 f 4 :Yb 3+ 0.2 ,Tm 3+ 0.02 The method is as follows:
[0157] a) Weigh 80mg sodium trifluoroacetate (Na-TFA) (powder), 180mg yttrium trifluoroacetate (Y-TFA) (powder), 42mg ytterbium trifluoroacetate (Yb-TFA) (powder), 4mg trifluoroacetic acid Add thulium (Tm-TFA) powder into a reaction bottle filled with 10mL 1:1 oleic acid:octadecene (OA:ODE), stir and heat to 110°C until all the added reactants dissolve and form a transparent homogeneous solution;
[0158] b) The reaction solution is vacuumed and filled with nitrogen several times to remove impurities such as water and oxygen;
[0159] c) Transfer the above reaction solution to the quartz reaction vessel of the microwave reactor, seal it, heat it with microwave to 280°C, and keep the reaction for 3 minutes;
[0160] d) After the reaction stops, use high-speed flowing air to cool the reaction vessel and solution to room temperature, take out the reaction vessel, add excess ethanol to promote...
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