Method for preparing semiconductor nanocrystals
View Patent ↗A method for making semiconductor nanocrystals is disclosed, the method comprising adding a secondary phosphine chalcogenide to a solution including a metal source and a liquid medium at a reaction temperature to form a reaction product comprising a semiconductor comprising a metal and a chalcogen, and quenching the reaction mixture to form quantum dots. Methods for overcoating are also disclosed. Semiconductor nanocrystals are also disclosed.
1. A method for making semiconductor nanocrystals, the method comprising:
providing a solution including a metal source and a liquid medium at a reaction temperature greater than 200° C.,
adding a secondary phosphine chalcogenide to the solution to form a reaction product comprising a semiconductor comprising a metal and a chalcogen, and
quenching the reaction mixture immediately upon completion of addition of the secondary phosphine chalcogenide resulting in quantum dots comprising the semiconductor.
2. A method in accordance with claim 1 wherein the solution further includes a phosphonate species.
3. A method in accordance with claim 2 wherein the solution further includes phosphonite species.
4. A method in accordance with claim 1 wherein the solution further includes a phosphonite species.
5. A method in accordance with claim 1 wherein the solution further includes carboxylate species.
6. A method in accordance with claim 1 wherein the step of quenching includes rapidly cooling the reaction mixture immediately upon completion of addition of the secondary phosphine chalcogenide.
7. A method in accordance with claim 6 wherein the reaction mixture is cooled to a temperature that is about 200° C. or below.
8. A method in accordance with claim 6 wherein the reaction mixture is cooled to a temperature that is about 100° C. or below and further comprising isolating the semiconductor nanocrystals after cooling.
9. A method in accordance with claim 8 wherein the method further comprises overcoating at least a portion of the isolated semiconductor nanocrystals with a coating.
10. A method in accordance with claim 9 wherein the method further comprises overcoating at least a portion of the isolated semiconductor nanocrystals with a coating in the absence of an amine.
11. A method in accordance with claim 6 wherein the reaction mixture is cooled to a temperature at which the quantum dot growing process is terminated.
12. A method in accordance with claim 1 wherein the step of quenching includes rapidly cooling the reaction mixture immediately upon completion of addition of the secondary phosphine chalcogenide to stop growth of the semiconductor nanocrystals formed in reaction mixture.
13. A method in accordance with claim 1 wherein the ratio of moles of secondary phosphine chalcogenide to moles of metal included in the solution is greater than or equal to 1.
14. A method in accordance with claim 1 wherein the semiconductor nanocrystals are made in the absence of an amine.
15. A method in accordance with claim 1 wherein the semiconductor nanocrystals formed in the reaction mixture are overcoated without being isolated from the reaction mixture.
16. A method in accordance with claim 1 wherein the secondary phosphine chalcogenide is formed by adding a chalcogen to an oxygen-treated liquid tertiary phosphine.
17. A population of semiconductor nanocrystals prepared in accordance with claim 1 .
18. A method for preparing semiconductor nanocrystals, the method comprising mixing one or more chalcogen sources with an oxygen-treated tertiary phosphine to form a chalcogen precursor, forming a reaction mixture including the chalcogen precursor and one or more metal precursors, and heating the reaction mixture to form semiconductor nanocrystals comprising one or more metals and one or more chalcogens.
19. A method in accordance with claim 18 wherein the reaction temperature is greater than 200° C.
20. A method in accordance with claim 18 wherein the reaction is quenched to control the particle size of the nanocrystals formed.