Doped semiconductor nanocrystalline quantum dots having core-shell structure and preparation method thereof
A technology of nanocrystals and quantum dots, which is applied in the field of doped semiconductor nanocrystal quantum dots and its preparation, to achieve the effects of good air stability, high fluorescence efficiency and quantum efficiency
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[0033] According to a preferred embodiment of the present invention, the doped semiconductor nanocrystal quantum dot has a spherical shape and a zinc blende structure, and the particle size distribution of the doped semiconductor nanocrystal quantum dot is 4-15 nm. Preferably, the particle size distribution is 5.05 nm to 9.5 nm, more preferably, the particle size distribution is 5.95 nm to 7.75 nm. Due to the spherical shape and zinc blende structure, the high-quality nanocrystalline quantum dots have good air stability, temperature stability and optical stability. That is to say, at a high temperature of 130°C, the quantum yield of the nanocrystal only decreased by 5%, and the initial yield could be restored when the temperature dropped to 30°C. During three consecutive cycles of heating and cooling, the quantum The yield can basically return to the initial value, and the loss of quantum yield at high temperature is also very small, which shows that the nanocrystal has good t...
Embodiment 1
[0044] 1) Preparation of Mn-doped nanocrystalline nuclei:
[0045] 0.2 mmol of manganese-containing metal salt precursor MnSt 2 and 0.1mol non-complexing solvent ODE were added to a 250mL three-necked round-bottomed flask, exhausted, heated to 280°C to dissolve and form a solution containing Mn ions; inject 1ml of Se into the solution containing Mn ions obtained above at 300°C / TBP (2.4mol / L) and 3mmol oleylamine (the first ligand) mixed solution, reacted for 10 minutes to form solution A, that is, the nanocrystal nucleus solution of MnSe.
[0046] Inject 10ml of bimolecular zinc-containing precursor zinc stearate (ZnSt 2 ) solution (0.1mol / L) and 1ml of a mixed solution of oleylamine and ODE (2mol / L), reacted for 15 minutes to form a Mn-doped ZnSe nanocrystal nucleus solution.
[0047] 2) Using the epitaxial growth method to coat the shell on the surface of the nanocrystalline core:
[0048] Adjust the temperature of the nanocrystal nucleus solution obtained in step 1) to ...
Embodiment 2
[0053] 1) Preparation of Mn-doped nanocrystalline nuclei:
[0054] Add 0.2 mmol of manganese-containing metal salt precursor manganese acetylacetonate and 0.1 mol non-complexing solvent octadecane into a 250 mL three-neck round bottom flask, exhaust, and heat to 150 ° C to dissolve manganese acetylacetonate to obtain a solution containing Mn ions ; Inject 1.0ml of Se-octadecene solution (2.4mol / L) and 3.0mmol of the first ligand oleylamine mixture at 270°C for 1 minute to form a MnSe nanocrystal nucleus solution, namely solution A.
[0055] Inject 10ml of a bimolecular zinc-containing precursor zinc stearate solution (0.1mol / L) and 1ml of a mixed solution of the second ligand octadecylamine (2mol / L) into the above solution A at 350°C, and react for 1 minute , forming a Mn-doped ZnSe nanocrystal nucleus solution.
[0056] 2) Using the epitaxial growth method to coat the shell on the surface of the nanocrystalline core:
[0057] Adjust the temperature of the above-mentioned na...
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