IP Library Granted Patent US 9,899,575
Granted Patent B2
US 9,899,575 · App. 15/140,501 · Granted Feb 20, 2018

Method of continuous flow synthesis and method of correcting emission spectrum of light emitting device

Inventors: Chenmin Liu (Hong Kong, HK); Chi Ho Kwok (Hong Kong, HK)
Assignee: Nano and Advanced Materials Institute Limited
H01L33/502C09K11/02C09K11/883H01L33/508H01L2933/0041
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Quick Facts
Patent No.
US 9,899,575
App. No.
15/140,501
Granted
Feb 20, 2018
Kind
B2
Abstract

The present application provides a method of continuous flow synthesis of core/shell quantum dots doped polymer mats (QD-MAT), including mixing a first core precursor with a second core precursor and feeding the reaction mixture into a first furnace to obtain quantum dot cores; feeding a first shell precursor and a second shell precursor into a second furnace and simultaneously injecting the quantum dot cores to obtain core/shell quantum dots; mixing the core/shell quantum dots with a polymer solution to obtain a QD-polymer composite; and introducing the QD-polymer composite to an electrospinning system to fabricate the core/shell quantum dots doped polymer mats. The present application also provides a method of correcting emission spectrum of light emitting devices with the core/shell quantum dots doped polymer mats with light diffusing properties which can be used to replace the diffuser layer of light emitting devices.

Claims (28)

1. A method of continuous flow synthesis of core/shell quantum dots doped polymer mats (QD-MAT), comprising:

mixing a first core precursor with a second core precursor and feeding the reaction mixture into a first furnace to obtain quantum dot cores;

feeding a first shell precursor and a second shell precursor into a second furnace and simultaneously injecting the quantum dot cores to obtain core/shell quantum dots;

mixing the core/shell quantum dots with a polymer solution to obtain a QD-polymer composite; and

introducing the QD-polymer composite to an electrospinning system comprising a high voltage power supply, a metallic needle and a collector to obtain quantum dot nanofibers (QD-nanofibers) and thereby fabricating the core/shell quantum dots doped polymer mats, wherein the QD-nanofibers with desired diameter and optical properties and the QD-MAT with controlled thickness are obtained by varying multiple parameters, and wherein the parameters comprise a voltage of about 10-50 kV between the needle tip and the collector, a tip-to-collector distance (TCD) of about 10-50 mm, a concentration of the QD-polymer solution of about 10-25 weight %, a feed rate of the QD-polymer solution of about 1-10 ml/hour, the QD-nanofibers with a diameter ranging from about 0.1 μm to 5 μm and a thickness of the QD-MATs ranging from about 10-100 μm.

2. The method of claim 1 , wherein the temperature of the first furnace is maintained with a temperature deviation no more than about 3° C.

3. The method of claim 1 , wherein the core/shell quantum dots have a double layer or triple layer core/shell structure.

4. The method of claim 1 , wherein the first and second core precursors and the first and second shell precursors comprise at least one element selected from the group consisting of In, P, Zn, S, Se, N, Ga, Si, Ti, Ce, La, V, O and Cd.

5. The method of claim 4 , wherein the core/shell quantum dots have a core/shell structure selected from the group consisting of InP/ZnS, InP/ZnSe, InN/GaN, InP/ZnS/SiO 2 , InP/ZnS/InZnS, GaP/ZnS/SiO 2 , GaP/ZnS/GaZnS, InN/GaN/SiO 2 and CdSe/ZnS.

6. The method of claim 1 , wherein the size distribution of the core/shell quantum dots has a standard deviation of about 10% or less.

7. The method of claim 1 , further comprising forming an additional coating around the core/shell QDs.

8. The method of claim 7 , wherein the additional coating comprises a compound having an affinity for the polymer solution.

9. The method of claim 7 , wherein the additional coating comprises at least one selected from the group consisting of silicon dioxide, zirconium oxide, titanium dioxide and other inorganic oxides having an affinity for the polymer solution, wherein a precursor of the additional coating is at least one of tetraethyl orthosilicate (TEOS) and/or tetramethoxylsilane (TMOS).

10. The method of claim 7 , wherein the additional coating is formed by micro emulsion synthesis.

11. The method of claim 1 , wherein the polymer solution comprises at least one polymer selected from the group consisting of nylon 6.6, polyurethanes (PU), polybenzimidazole (PBI), polycarbonate (PC), polyacrylonitrile (PAN), poly(methyl methacrylate) (PMMA), polyaniline (PANI), polystyrene (PS), polyethylene terephthalate (PET), poly(vinylidene fluoride) (PVDF), polyvinyl fluoride (PVF), polyvinylchloride (PVC), poly(9-vinylcarbazole) (PVK) and polyvinylacetate (PVAc).

12. The method of claim 1 , wherein the core/shell QDs are dispersed in a polymer solution at about 25-50° C. to obtain a QD-polymer composite with a concentration of about 0.1-5 wt % of QD.

13. The method of claim 12 , wherein the QD-polymer composite contains at least one solvent selected from the group consisting of toluene, N,N-dimethylforamide, acetone, chloroform and dichloromethane.

14. The method of claim 1 , wherein the method is carried out in a flow reactor with a flow rate in the range of 2.9 ml/min to 15 ml/min.

15. A method of correcting emission spectrum of a light emitting device, comprising:

mixing a first core precursor with a second core precursor and feeding the reaction mixture into a first furnace to obtain quantum dot cores;

feeding a first shell precursor and a second shell precursor into a second furnace and simultaneously injecting the quantum dot cores to obtain core/shell quantum dots;

mixing the core/shell quantum dots with a polymer solution to obtain a QD-polymer composite;

introducing the QD-polymer composite to an electrospinning system comprising a high voltage power supply, a metallic needle and a collector to obtain quantum dot nanofibers (QD-nanofibers) and thereby fabricating the core/shell quantum dots doped polymer mats, wherein the QD-nanofibers with desired diameter and optical properties and the QD-MAT with controlled thickness are obtained by varying multiple parameters, and wherein the parameters comprise a voltage of about 10-50 kV between the needle tip and the collector, a tip-to-collector distance (TCD) of about 10-50 mm, a concentration of the QD-polymer solution of about 10-25 weight %, a feed rate of the QD-polymer solution of about 1-10 ml/hour, the QD-nanofibers with a diameter ranging from about 0.1 μm to 5 μm and a thickness of the QD-MATs ranging from about 10-100 μm; and

laminating at least one layer of the QD-MATs prepared on the light emitting device.

16. The method of claim 15 , wherein the at least one layer of QD-MATs comprises QDs with same or different sizes.

17. The method of claim 15 , wherein the at least one layer of QD-MATs is directly laminated on either of a diffuser or a brightness enhancement film of an LED display of the light emitting device.

18. The method of claim 15 , wherein the at least one layer of QD-MATs is laminated on the surface of the encapsulant of an LED lighting of the light emitting device as a remote phosphor.

19. The method of claim 15 , wherein the at least one layer of QD-MATs is doped with InP/ZnS/SiO 2 or InP/ZnS/TiO 2 core/shell QDs and Cu (Mn) doped ZnSe/SiO 2 core/shell QDs of different sizes.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 17, 2026
From: NANO AND ADVANCED MATERIALS INSTITUTE LIMITED
To: HONG KONG APPLIED SCIENCE AND TECHNOLOGY RESEARCH INSTITUTE COMPANY LIMITED
Reel/Frame 075402/0553 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 29, 2016
From: LIU, CHENMIN; KWOK, CHI HO
To: NANO AND ADVANCED MATERIALS INSTITUTE LIMITED
Reel/Frame 038415/0794 →
Continuity (2)
Provisional Application 62179186 · Apr 30, 2015
Related Publication 20160322541A1 · Nov 3, 2016