CN111009604A - Preparation method of white light emitting diode based on Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots - Google Patents
Preparation method of white light emitting diode based on Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910000796 S alloy Inorganic materials 0.000 title claims abstract description 11
- 229910002059 quaternary alloy Inorganic materials 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims abstract 8
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical compound CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011572 manganese Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000011550 stock solution Substances 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- BSAIOBTVVJQIBU-UHFFFAOYSA-N chloroform;2-methylprop-2-enoic acid Chemical compound ClC(Cl)Cl.CC(=C)C(O)=O BSAIOBTVVJQIBU-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 5
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002474 experimental method Methods 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- ZVYYAYJIGYODSD-LNTINUHCSA-K (z)-4-bis[[(z)-4-oxopent-2-en-2-yl]oxy]gallanyloxypent-3-en-2-one Chemical compound [Ga+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O ZVYYAYJIGYODSD-LNTINUHCSA-K 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229940071125 manganese acetate Drugs 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- RZJRJXONCZWCBN-UHFFFAOYSA-N alpha-octadecene Natural products CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 claims description 2
- 238000011534 incubation Methods 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims 1
- 239000000956 alloy Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 238000001308 synthesis method Methods 0.000 abstract 1
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
- C09K11/621—Chalcogenides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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Abstract
The invention discloses a preparation method of a white light emitting diode based on Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots, which comprises the step of preparing green and environment-friendly quantum dots AgInGaS2The method comprises the steps of preparing Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dots, and obtaining the white light emitting diode of the quantum dots on a blue light emitting diode chip by using the Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dots. The invention adopts a step-by-step synthesis method, a coating technology and an ultraviolet curing technology to realize the preparation of the white light emitting diode of the Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot. The preparation method is simple, the yield of the prepared quantum dots is high, the display index of the prepared luminescent chip is high, and the effect of emitting double peaks can be achieved by only one quantum dot.
Description
Technical Field
The invention relates to the technical field of white light emitting diodes, In particular to a preparation method of a white light emitting diode based on Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots.
Background
White Light Emitting Diodes (WLEDs) have high luminous efficiency and long lifetime and are therefore considered to be a green illumination source. Conventional WLEDs consist of a blue-emitting GaN-based chip and yellow YAG: ce fluorescent powder. The phosphor converts a portion of the blue light from the chip into yellow light and mixes the yellow light with the remaining blue light to emit bichromatic white light. As a new generation of luminescent materials, quantum dots have been successfully applied in the field of WLED to enhance the color performance of the device. Mn-doped I-III-VI quantum dots have large Stokes shift, so optical self-absorption can be avoided, and WLED can be obtained by integrating the same with a blue LED chip.
Recently, Pradhan et al synthesized manganese-doped CuInS2(CIS) quantum dots, and an effective Mn emission peak is obtained near 600nm, so that the emission of a CIS internal trap state is completely eliminated. In our experiments, an AgInGaS based for dual color emission2Quantum dots, we synthesized Mn doped dual-emission Ag-In-Ga-S quaternary alloy quantum dots, In which Mn2+Adsorbed on AgInGaS2Surface, hence Mn2+Ions and AgInGaS2May be transmitted simultaneously. The obtained Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot has a wide spectral range and has two emission peaks at 528nm and 610nm respectively.
The Mn-doped dual-emission Ag-In-Ga-S is a non-toxic, green and environment-friendly quaternary alloy quantum dot, and can be excited by a commercial GaN-based blue chip (440 nm-460 nm) to realize the preparation of a WLED (white light emitting diode) with high color rendering index based on a quantum dot luminescent material.
Disclosure of Invention
The invention aims to solve the problems that: the preparation method of the white light emitting diode based on the Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots is simple, the yield of the prepared quantum dots is high, the display index of the prepared light emitting chip is high, and the dual-emission effect can be achieved by only one quantum dot.
The technical scheme provided by the invention for solving the problems is as follows: a preparation method of a white light emitting diode based on Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots comprises the following steps,
(1) preparing to obtain the green environment-friendly quantum dot AgInGaS2；
(2) AgInGaS in step (1)2Mn is injected on the basis of quantum dot reaction2+Obtaining Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dots by using the stock solution;
(3) and coating the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dots on a blue light emitting diode chip to obtain the white light emitting diode.
Preferably, the green environment-friendly quantum dot AgInGaS is prepared in the step (1)2Putting silver nitrate, indium acetate and gallium acetylacetonate into a container according to the molar ratio of 1:6:1, and adding 2ml of n-dodecyl mercaptan, 2ml of oleylamine and 5ml of 1-octadecene into a 50ml three-neck round-bottom flask by using a dropper to perform main reaction; mixing the mixture in a three-mouth bottle in N2Heating to 80 ℃ under the condition of gas, starting vacuumizing, and vacuumizing for 15 minutes; after the vacuumizing is finished, starting ventilation, introducing argon for 2 minutes, vacuumizing for 10 minutes, and circulating ventilation for 3 times; introducing argon after the ventilation is finished until the experiment is finished and heating to 90 ℃, and quickly injecting a mixed solution of 1mmol of sulfur prepared in advance and 2.5ml of 1-octadecane, wherein the solution is changed from clear and transparent to reddish brown; the incubation was continued at 90 ℃ for about 30 min.
Preferably, Mn is injected in the step (2)2+The reaction temperature of the stock solution is raised to 150 ℃, 0.2mmol of manganese acetate and 2mL of oleylamine are dropwise added and mixed, and the reaction temperature is kept at 150 ℃; and after about 60min, cooling the reaction temperature to room temperature to obtain the Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot.
Preferably, the step (3) is to mix Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot stock solution, acetone and n-hexane In a volume ratio of 1: 1: 3, mixing to precipitate the quantum dots; then centrifuging the mixture at 8000rpm for 5min at high speed, removing supernatant, and repeating the step for three times; then, drying the precipitate for two hours at 40-50 ℃ in a vacuum drying oven to obtain quantum dot powder; in order to prepare a white light emitting diode, the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot powder is dissolved In chloroform, and the concentration is 0.12 g/mL; and preparing polymethyl methacrylate-chloroform solution with the concentration of 0.2g/mL for standby; and uniformly mixing the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot-chloroform solution and polymethyl methacrylate-chloroform solution In equal volume, dripping the mixture on a blue GaN LED chip, and evaporating the solvent under an ultraviolet lamp to solidify PMMA containing the quantum dots to obtain the quantum dot white light-emitting diode.
Compared with the prior art, the invention has the advantages that: the preparation method is simple, the prepared quantum dots are high in yield, the prepared luminescent chip is high in display index, and the effect of emitting double peaks can be achieved by only one quantum dot.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, so that how to implement the technical means for solving the technical problems and achieving the technical effects of the present invention can be fully understood and implemented.
A preparation method of a white light emitting diode based on Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots comprises the following steps,
(1) adding silver nitrate (AgNO) under inert gas atmosphere3) Indium acetate (in (Ac))3) 0.2mmol of silver nitrate (AgNO) is weighed according to the molar ratio of 1:6:1 to the gallium acetylacetonate3) 1.2mmol of indium acetate (in (Ac)3) 0.2mmol of gallium acetylacetonate (Ga (Ac)3) Into a 50ml three-necked round-bottomed flask, 2ml of n-dodecyl mercaptan (DDT), 2ml of oleylamine (OAm) and 5ml of 1-octadecene (1-ODE) were added by a dropper to the 50ml three-necked round-bottomed flask for main reaction. Mixing the mixture in a three-mouth bottle in N2Heating to 80 ℃ under the condition of gas, starting vacuumizing, and vacuumizing for 15 minutes. After the vacuumizing is finished, air exchange is started, argon is introduced for 2 minutes, and then the vacuumizing is carried out for 10 minutes, so thatCirculating ventilation for 3 times. Argon was introduced until the end of the experiment and heated to 90 ℃ after purging, and a mixed solution of 1mmol of sulfur (S) prepared in advance and 2.5ml of 1-octadecene (1-ODE) was rapidly injected, at which time the solution changed from clear to reddish brown. Keeping the temperature at 90 ℃ for about 30min, sampling and measuring the quantum dot AgInGaS2The light-emitting band of (A) is about 610 nm.
(2) AgInGaS in step (1)2Mn is injected on the basis of quantum dot reaction2+The reaction solution was heated to 150 ℃ and 0.2mmol of manganese acetate (Mn (OAc))2) Mixed with 2mL oleylamine (OAm). The reaction temperature is kept at 150 ℃, which is favorable for Mn2+Better adsorption on quantum dots AgInGaS2Of (2) is provided. After about 60min the reaction temperature was lowered to room temperature. And obtaining the Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot. The dual emission wavelengths are 610nm and 528 nm.
(3) The volume ratio of Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot stock solution to acetone to n-hexane is 1: 1: 3, mixing to precipitate the quantum dots; then centrifuging the mixture at 8000rpm for 5min at high speed, removing supernatant, and repeating the step for three times; then, drying the precipitate for two hours at 40-50 ℃ in a vacuum drying oven to obtain quantum dot powder; in order to prepare a white light emitting diode, the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot powder is dissolved In chloroform, and the concentration is 0.12 g/mL; and preparing polymethyl methacrylate-chloroform solution with the concentration of 0.2g/mL for standby; and uniformly mixing the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot-chloroform solution and polymethyl methacrylate-chloroform solution In equal volume, dripping the mixture on a blue GaN LED chip, and evaporating the solvent under an ultraviolet lamp to solidify PMMA containing the quantum dots to obtain the quantum dot white light-emitting diode.
The foregoing is merely illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary. All changes which come within the scope of the invention as defined by the independent claims are intended to be embraced therein.
Claims (4)
1. A preparation method of a white light emitting diode based on Mn-doped dual-emission Ag-In-Ga-S alloy quantum dots is characterized by comprising the following steps: the method comprises the following steps of,
(1) preparing to obtain the green environment-friendly quantum dot AgInGaS2；
(2) AgInGaS in step (1)2Mn is injected on the basis of quantum dot reaction2+Obtaining Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dots by using the stock solution;
(3) and coating the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dots on a blue light emitting diode chip to obtain the white light emitting diode.
2. The method for preparing the white light-emitting diode based on the Mn-doped dual-emission Ag-In-Ga-S alloy quantum dot according to claim 1, wherein the method comprises the following steps: the green environment-friendly quantum dot AgInGaS is prepared in the step (1)2Putting silver nitrate, indium acetate and gallium acetylacetonate into a container according to the molar ratio of 1:6:1, and adding 2ml of n-dodecyl mercaptan, 2ml of oleylamine and 5ml of 1-octadecene into a 50ml three-neck round-bottom flask by using a dropper to perform main reaction; mixing the mixture in a three-mouth bottle in N2Heating to 80 ℃ under the condition of gas, starting vacuumizing, and vacuumizing for 15 minutes; after the vacuumizing is finished, starting ventilation, introducing argon for 2 minutes, vacuumizing for 10 minutes, and circulating ventilation for 3 times; introducing argon after the ventilation is finished until the experiment is finished and heating to 90 ℃, and quickly injecting a mixed solution of 1mmol of sulfur prepared in advance and 2.5ml of 1-octadecane, wherein the solution is changed from clear and transparent to reddish brown; the incubation was continued at 90 ℃ for about 30 min.
3. The method for preparing the white light-emitting diode based on the Mn-doped dual-emission Ag-In-Ga-S alloy quantum dot according to claim 1, wherein the method comprises the following steps: mn is injected in the step (2)2+The reaction temperature of the stock solution is raised to 150 ℃, 0.2mmol of manganese acetate and 2mL of oleylamine are dropwise added and mixed, and the reaction temperature is kept at 150 ℃; after about 60min, the reaction temperature is reduced to room temperature to obtain Mn-doped dual-emission Ag-In-Ga-S IVAnd (3) a meta-alloy quantum dot.
4. The method for preparing the white light-emitting diode based on the Mn-doped dual-emission Ag-In-Ga-S alloy quantum dot according to claim 1, wherein the method comprises the following steps: the step (3) is to mix Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot stock solution, acetone and normal hexane In a volume ratio of 1: 1: 3, mixing to precipitate the quantum dots; then centrifuging the mixture at 8000rpm for 5min at high speed, removing supernatant, and repeating the step for three times; then, drying the precipitate for two hours at 40-50 ℃ in a vacuum drying oven to obtain quantum dot powder; in order to prepare a white light emitting diode, the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot powder is dissolved In chloroform, and the concentration is 0.12 g/mL; and preparing polymethyl methacrylate-chloroform solution with the concentration of 0.2g/mL for standby; and uniformly mixing the prepared Mn-doped dual-emission Ag-In-Ga-S quaternary alloy quantum dot-chloroform solution and polymethyl methacrylate-chloroform solution In equal volume, dripping the mixture on a blue GaN LED chip, and evaporating the solvent under an ultraviolet lamp to solidify PMMA containing the quantum dots to obtain the quantum dot white light-emitting diode.
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| CN110729389A (en) * | 2019-10-24 | 2020-01-24 | 南昌航空大学 | Preparation method of white light emitting diode based on I-III-VI group quantum dots |
| CN113214834A (en) * | 2021-04-28 | 2021-08-06 | 武汉工程大学 | Ag/Mn double-doped Zn-In-Se core-shell structure quantum dot and preparation method and application thereof |
| CN114015436A (en) * | 2021-11-13 | 2022-02-08 | 复旦大学 | White light LED based on single-phase multi-emission multi-element alloy quantum dots and preparation method thereof |
| CN114045168A (en) * | 2021-11-19 | 2022-02-15 | 复旦大学 | Water-soluble alloy quantum dot nanoenzyme and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110729389A (en) * | 2019-10-24 | 2020-01-24 | 南昌航空大学 | Preparation method of white light emitting diode based on I-III-VI group quantum dots |
| CN113214834A (en) * | 2021-04-28 | 2021-08-06 | 武汉工程大学 | Ag/Mn double-doped Zn-In-Se core-shell structure quantum dot and preparation method and application thereof |
| CN113214834B (en) * | 2021-04-28 | 2023-03-07 | 武汉工程大学 | Ag/Mn double-doped Zn-In-Se core-shell structure quantum dot and preparation method and application thereof |
| CN114015436A (en) * | 2021-11-13 | 2022-02-08 | 复旦大学 | White light LED based on single-phase multi-emission multi-element alloy quantum dots and preparation method thereof |
| CN114045168A (en) * | 2021-11-19 | 2022-02-15 | 复旦大学 | Water-soluble alloy quantum dot nanoenzyme and preparation method and application thereof |
| CN114045168B (en) * | 2021-11-19 | 2023-09-05 | 复旦大学 | Water-soluble alloy quantum dot nano enzyme and preparation method and application thereof |
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