Synthesis and modification method of upconversion nanometer material
A technology of nanomaterials and modification methods, which is applied in the fields of wave energy or particle radiation treatment materials, pharmaceutical formulations, drug combinations, etc., can solve the problems of lack of tumor tissue targeting, insignificant treatment effect, and difficulty in transmitting tumors, and achieves strong The luminous conversion efficiency, the effect is good, the effect of wide application prospect
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Embodiment 1
[0048] (1) Add 3 mL of oleic acid and 15 mL of 1-octadecene into a round bottom flask, and stir. The mixture was heated to 70°C under nitrogen atmosphere. Mix 397 μL YCl 3 , 300 μL YbCl 3, 30 μL ErCl 3 , 300 μL GdCl 3 Preparation of NaYF 4 : Yb / Er / Gd (30,0.3,30mol%) solution. The solution was added into the reaction liquid, and heated to 150° C., and kept warm for 30 minutes to obtain a clear and uniform solution.
[0049] (2) Cool the reaction solution in step (1) to 65°C, and add 10mL of 0.1g NaOH and 0.148gNH 4 F in methanol solution. The temperature of the reaction solution was raised to 110 ° C for 20 min. Connect the condenser tube and the piston, seal the three-necked bottle, and vacuumize it for 10 minutes. Repeat the cross evacuation and nitrogen filling three times, each lasting one minute.
[0050] (3) Fill the closed space with nitrogen, raise the temperature to 300°C at a rate of 10°C / min, and maintain this temperature for 1.5h. After the reaction, it w...
Embodiment 2
[0076] Step (1) to step (5) are the same as embodiment 1.
[0077] (6) Add 21mL cyclohexane, 1.5mL IGEPAL CO-520, and 2mL UCNPs solution into a 50ml single-necked bottle, add 211μL ammonia water with a mass fraction of 25% dropwise, stir for 30min, then add 100μL TEOS dropwise, and stir for 36 hours , The stirring speed was kept at 750r / min during the experimental reaction.
[0078] (7) Pack the reaction solution in step (6) into two centrifuge tubes respectively. Rinse the three-neck flask with 20mL of absolute ethanol, and transfer to two centrifuge tubes respectively. After vortexing and centrifuging for 1 min, add 10 mL of acetone each, and vortex for 30 s. Centrifuge at room temperature with a centrifugal force of 5200g for 20min, then remove the supernatant. Add 10 mL of ethanol to each centrifuge tube, vortex and sonicate for 10 min. Pour the solutions in the two centrifuge tubes into one centrifuge tube and add 15 mL of acetone. Centrifuge at 5200 g for 20 min at ...
Embodiment 3
[0082](1) Add 3 mL of oleic acid and 15 mL of 1-octadecene into a round bottom flask, and stir. The mixture was heated to 70°C under nitrogen atmosphere. Mix 390 μL YCl3, 250 μL YbCl3, 100 μL ErCl3, 350 μL GdCl3 to prepare NaYF4:Yb / Er / Gd (25, 1, 35 mol%) solution. The solution was added to the reaction solution, and the mixture was heated to 150° C., and after 30 min of heat preservation, a clear and uniform solution was obtained.
[0083] (2) Cool the reaction solution in step (1) to 65°C, and add 10mL of 0.1g NaOH and 0.148gNH 4 F in methanol solution. The temperature of the reaction solution was raised to 110 ° C for 20 min. Connect the condenser tube and the piston, seal the three-necked bottle, and vacuumize it for 10 minutes. Repeat the cross evacuation and nitrogen filling three times, each lasting one minute.
[0084] (3) Fill the closed space with nitrogen, raise the temperature to 300°C at a rate of 10°C / min, and maintain this temperature for 1.5h. After the re...
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