Rare earth-doped upconversion nanometer crystal-based fluorescent coding microspheres and preparation method thereof
A technology of nanocrystals and fluorescent coding, which is applied in the field of fluorescent coding microspheres and its preparation, can solve the problems of large deviation of the design value of the fluorescent coding value, interference with test results, and decreased accuracy, so as to improve sensitivity and detection quantity, and broaden Application prospects, phototoxicity reduction effect
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Embodiment 1
[0022] Example 1: NaYF 4 : Preparation of 0.2 mol % Yb / 0.2 mol % Ho / 0.2 mol % Tm up-conversion nanocrystals. Specific steps are as follows:
[0023] (1) Take a 50 mL three-neck round bottom flask as the reaction vessel, first add 1 mmol CF 3 COONa, 0.4mmol Y(CF 3 COO) 3 , 0.14mmol Yb (CF 3 COO) 3 , 0.011mmol Ho(CF 3 COO) 3 and 0.011mmol Tm(CF 3 COO) 3 ; followed by the addition of 10 g of tri-n-octylphosphine oxide (TOPO).
[0024] (2) Stir and heat the reactants in step (1) to 120 o C. Vacuum dehydration and deoxygenation for 30 minutes, and finally obtain a transparent mixed solution.
[0025] (3) Under the protection of high-purity argon, the reactants were heated at 10 oC / min speed up to 340 oC After incubation, the reaction was carried out for 1 hour.
[0026] (4) Cool the reactants to 50 oC Afterwards, ethanol is added to precipitate the product from the solution, followed by centrifugation, and repeated washing with absolute ethanol for 3-5 times to o...
Embodiment 2
[0028] Example 2: NaYF 4 : Preparation of 0.2 mol % Yb / 0.2 mol % Er / 0.2 mol % Tm upconversion nanocrystals. Specific steps are as follows:
[0029] (1) Take a 50 mL three-neck round bottom flask as the reaction vessel, first add 0.4 mmol YCl 3 , 0.14mmol YbCl 3 , 0.011mmol ErCl 3 and 0.011 mmol TmCl 3 ; followed by the addition of 10g oleic acid (OA), 10g octadecene (ODE).
[0030] (2) Stir and heat the reactants in step (1) to 120 o C. Vacuum dehydration and deoxygenation for 30 minutes, and finally obtain a transparent mixed solution.
[0031] (3) Add 2.25 mmol NH 4 F was dissolved in 5 mL of methanol solution, mixed and injected into the above reaction solution for reaction. After continuous stirring for 20 minutes, the reactant was heated under the protection of high-purity argon for 10 oC / min speed up to 340 oC After incubation, the reaction was carried out for 1 hour.
[0032] (4) Cool the reactants to 50 oC Afterwards, ethanol is added to precipitate the...
Embodiment 3
[0034] Example 3: Y 2 o 3 : Preparation of 0.2 mol % Yb / 0.2 mol % Er / 0.2 mol % Tm up-conversion nanocrystals. Specific steps are as follows:
[0035] (1) Take a 50 mL three-neck round bottom flask as the reaction vessel, first add 0.4 mmol Y(Ac) 3 , 0.14mmol Yb(Ac) 3 , 0.011mmol Er(Ac) 3 and 0.011mmol Tm(Ac) 3 ; followed by the addition of 10g oleic acid (OA), 10g octadecene (ODE).
[0036] (2) Stir and heat the reactants in step (1) to 120 o C. Vacuum dehydration and deoxygenation for 30 minutes, and finally obtain a transparent mixed solution.
[0037] (3) Under the protection of high-purity argon, the reactants were heated at 10 oC / min speed up to 340 oC After incubation, the reaction was carried out for 1 hour.
[0038] (4) Cool the reactants to 50 oC Afterwards, ethanol is added to precipitate the product from the solution, followed by centrifugation, and repeated washing with absolute ethanol for 3-5 times to obtain the product.
[0039] In addition, the ...
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