CN107353889B - A method of improving aqueous phase quantum point stability - Google Patents
A method of improving aqueous phase quantum point stability Download PDFInfo
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- CN107353889B CN107353889B CN201710479931.8A CN201710479931A CN107353889B CN 107353889 B CN107353889 B CN 107353889B CN 201710479931 A CN201710479931 A CN 201710479931A CN 107353889 B CN107353889 B CN 107353889B
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Abstract
The invention discloses a kind of methods for improving aqueous phase quantum point stability, ligand exchange is carried out with ionic liquid and aqueous phase quantum point, quantum dot ionic liquid boiling point is very high after being modified, general above 200 DEG C, stability is higher than conventional aqueous phase quantum point preparation smaller ligand used, such as thioacetic acid, mercaptopropionic acid, glutathione, ligand exchange is carried out using ionic liquid and aqueous phase quantum point, it realizes the quantum dot that ionic liquid is wrapped up as ligand, improves the stability of single quantum dot；Ionic liquid is ionic crystals, inorganic salt crystal is similarly ionic crystals, quantum dot after Ionic Liquid Modified can preferably match inorganic salts crystal growing process, after being mixed with inorganic salts, reunion between quantum dot is not susceptible to reunite, available quantum dot is evenly dispersed, high stability solid state quantum point, by the partial size of the controllable solid state quantum points of techniques such as grinding, then obtains the different solid state quantum points for going out light characteristic.
Description
Technical field
The present invention relates to lighting technical fields, and in particular to a method of improve aqueous phase quantum point stability.
Background technique
Semiconductor illumination technique is a kind of based on efficient white light light emitting diode (White Light Emitting
Diode, WLED) novel illumination technology, be acknowledged as 21 century one of high-tech sector most with prospects.Domestic LED
In terms of industry, China's semiconductor lighting industry entirety output value breaks through 500,000,000,000 yuan for the first time within 2016, and industry size reaches 521,600,000,000
Member, but it is largely focused on downstream packaging technology, production capacity is lower in terms of new and high technology, and main competing technology still rests in state
Outer patent.Nine powers emphasis research and development plan in 2016 proposes nanometer, quantal concept again, urgent need quantum dot nano technology
Development is shown and Lighting Industry core competitiveness with grasping LED.
Existing White light LED technology is mainly GaN base blue-light LED chip excitation YAG:Ce3+Yellow rare-earth fluorescent powder is compound
Form white light.Although its light efficiency is higher, emission peak half-peak breadth is wider (FWHM > 80nm), smaller (the NTSC standard of gamut range
70% or so), very big (> 50%) especially for colored filter absorption loss.High photosynthetic efficiency, wide colour gamut, high aobvious finger white light
LED technology is that LED shows the Key Common Technologies faced with lighting area, colloidal semiconductor quantum dot (Colloidal
Quant μm of Dots, QDs) its half-peak breadth is relatively narrow (25-50nm), and excitation purity is high, can greatly improve gamut range (> 110%
NTSC), high aobvious finger (Ra > 90, R9 > 90) is easily realized, and quantum yield is high (> 90%).It is predicted according to IHS, quantum dot shows city
From 2014 to the year two thousand twenty, its average growth rate per annum is expected to up to 110% for field.Therefore, novel quantum spot white light LED (QD-WLED) will
It is important trend and current research hotspot of the generation semiconductor illumination with display, wide market.
Since the Brus in nineteen eighty-three Bell laboratory report for the first time CdS it is nanocrystalline with dimensional effect, in quantum dot
Preparation aspect people have carried out a large amount of research work.Organic phase system prepares high performance Colloidal Quantum Dots material
Prepare existing in-depth study, such as thickness shell emitting red light CdSe/CdS core-shell quanta dots, thick shell green emitting alloy quantum
Point etc..
Urgent need for current WLED display field to wide colour gamut, high stability etc., the preparation of high stability quantum dot
It is extremely urgent.The quantum dot for carrying out industrial application at present mostly uses oil to be combined to, but oil is mutually prepared on a large scale at high cost, need
Carry out a kind of quantum dot preparation method of low-cost and high-quality.German Weller seminar reports on JPCB within 2002
Synthesis in water CdTe quantum realizes the inexpensive water phase preparation of quantum dot for the first time.And water phase quantum conventional at present
Point, especially red quantum dot, luminescent properties are poor, and half-peak is roomy, quantum yield is lower；Preparation time length, stability simultaneously
Difference cannot be used directly for efficient LED, especially display backlight field.
But the obtained quantum dot crystal quality of aqueous phase system, luminous intensity, stability etc. are poor, while it is more difficult can
Control prepares core-shell structure, and to improving, stability is relatively difficult.The application of existing aqueous phase quantum point mainly also focuses on biology
Fluorescence probe field, while the aqueous phase quantum point crystal quality that conventional preparation techniques obtain is poor, the research work applied to WLED
Make relatively fewer, especially with regard to wide colour gamut (> 110%NTSC), high aobvious refers to that (Ra > 90, R9 > 90) show that lighting area is still
Blank.
A kind of method that can be improved aqueous phase quantum point stability, which is provided, so that aqueous phase quantum point can be used in WLED is
Important and urgent.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of methods for improving aqueous phase quantum point stability.
The technical solution used in the present invention is:
A method of improving aqueous phase quantum point stability, comprising the following steps: with ionic liquid and aqueous phase quantum point into
Row ligand exchange, quantum dot after being modified.
In some preferred embodiments, ionic liquid is quaternary amines, season phosphine, pyridines, pyrrolidines, piperidines
Or glyoxaline ion liquid.
In some preferred embodiments, the ionic liquid have sulfydryl, amino, carboxyl, alkene, ether, ester group,
At least one of itrile group, phosphoric acid functionalized, benzyl functionalization, guanidine functional group.
In some preferred embodiments, the method also includes following steps: by quantum dot and nothing after the modification
The mixing of machine salt saturated solution, obtains quantum dot-inorganic salts mixed crystal, i.e. solid state quantum point.
In some further preferred embodiments, the inorganic salts be sodium chloride, sodium bromide, potassium chloride, potassium bromide,
One of lithium chloride, lithium bromide, sodium tetraborate are a variety of.
In some preferred embodiments, the aqueous phase quantum point be CdTe, CdSe, CdS, ZnSe, InP, CuInS,
Any quantum dot in CuInSe, PbS.
In some preferred embodiments, the specific step that ligand exchange is carried out with ionic liquid and aqueous phase quantum point
Suddenly are as follows: take ionic liquid to mix with aqueous phase quantum point, be stirred to react.
It is described to be stirred to react time >=30min in some further preferred embodiments.
In some further preferred embodiments, the mass ratio of the ionic liquid and the aqueous phase quantum point is
10-10000:1.
The beneficial effects of the present invention are:
The present invention provides a kind of methods for improving aqueous phase quantum point stability, and ionic liquid boiling point is very high, generally all super
Cross 200 DEG C, stability is higher than conventional aqueous phase quantum point preparation smaller ligand used, as thioacetic acid, mercaptopropionic acid,
Glutathione etc. carries out ligand exchange using ionic liquid and aqueous phase quantum point, realizes the amount that ionic liquid is wrapped up as ligand
It is sub-, improve the stability of single quantum dot；Ionic liquid is ionic crystals, and inorganic salt crystal is similarly ionic crystals, ion
Quantum dot after liquid modification can preferably match inorganic salts crystal growing process, after mixing with inorganic salts, between quantum dot
Reunion be not susceptible to reunite, available quantum dot is evenly dispersed, high stability quantum dot-inorganic salts mixed crystal, i.e. solid-state
Quantum dot, quantum dot is stable, evenly dispersed in quantum dot-inorganic salts mixed crystal, can prevent from directly acting between quantum dot, mention
High quantum dot luminescent properties reduce quantum dot itself under long-term light conditions and reunite to luminous influence；Grinding etc. can be passed through
The partial size of the controllable solid state quantum point of technique then obtains the different solid state quantum points for going out light characteristic, and quantum dot-nothing
Machine salt mixed crystal can make optical path repeatedly reflect the light excitation number for improving quantum dot, further increase luminescent properties.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of green CdTe quantum dot-NaCl mixed crystal.
Fig. 2 is the structural schematic diagram of red CdTe quantum-NaCl mixed crystal.
Fig. 3 is the preparation flow schematic diagram of the quantum dot laminated film of multilayered structure.
Fig. 4 is the preparation process schematic diagram of quantum dots-polymer microballoon.
Specific embodiment
Since aqueous phase quantum point preparation temperature is lower, crystalline quality is poor, stability is poor；Quantum point grain diameter simultaneously
It is small, serious fluorescence resonance energy transfer (FRET) is generated because reuniting between quantum dot, substantially reduces luminous efficiency, it is not easy-to-use
In the LED of long-life.
Embodiment 1:
(1) the red CdTe quantum 2mg being prepared in water intaking phase system, with 2g 1- amine propyl -3- methylimidazole bromine
Ionic liquid mixing, is stirred to react 30min-12h, and, passes through a large amount of ionic liquid by amino and quantum dot surface key
The thiol ligand for exchanging quantum dot surface, realizes the quantum dot of Ionic Liquid Modified.
After being exchanged by ionic liquid, quantum dot surface key and the ionic liquid protective layer of 10-20nm thickness, quantum dot
Between spacing > 10nm, can effectively reduce the fluorescence resonance energy transfer (FRET) between quantum dot, reduce between quantum dot
Reunion.
(2) water-soluble quantum dot itself is dispersed in the colloid in aqueous solution, and existing forms are liquid.LED wrapper
It is solid state powder or the light conversion layer of film required by part, can not be needed directly using the quantum dot in liquid solution
To the solid states of quantum dot.It takes the quantum dot of Ionic Liquid Modified to mix with inorganic salt saturated solution, realizes quantum dot by liquid
State is converted into solid-state.The inorganic salts be sodium chloride, sodium bromide, potassium chloride, potassium bromide, lithium chloride, lithium bromide, sodium tetraborate,
One of sucrose is a variety of.The quantum dot of Ionic Liquid Modified can be evenly dispersed in inorganic salt saturated solution, uniformly ties
Crystalline substance is formed.Such as the water phase CdTe quantum and the inorganic salt saturated solution of NaCl for modifying 1- amine propyl -3- methylimidazole bromide
Mixing realizes quantum dot stabilization, evenly dispersed CdTe-NaCl mixed crystal, i.e. solid-state amount by inorganic salts crystal growth technique
It is sub-, it is mixed using green CdTe quantum dot with NaCl saturated solution, available green CdTe-NaCl mixed crystal, structure is shown
It is intended to as shown in Figure 1, being mixed using red CdTe quantum with NaCl saturated solution, available red CdTe-NaCl is mixed
Crystalline substance, structural schematic diagram are as shown in Figure 2.Quantum dot is dispersed in the inorganic salt crystal of NaCl, forms the amount of polyhedral structure
Sub- point-inorganic salts mixed crystal realizes quantum dot liquid to solid conversion, and the mixed crystal has quantum dot monomer dispersibility,
It can prevent from directly acting between quantum dot, improve quantum dot light emitting performance, reduce quantum dot itself under long-term light conditions and roll into a ball
Gather to luminous influence.Resulting mixed crystal is ground using equipment such as agate mortar or ball mills, obtains micron, submicron order
Quantum dot-inorganic salts mixed crystal particle, 100nm-10 μm of partial size adjustable；By selecting the solid state quantum point particle of different-grain diameter, i.e.,
Controllable to realize different light characteristics out, such as: micron level (> 1 μm) realizes Mie scattering, except stable dispersion quantum dot acts on
Outside, light diffusing agent can also be played the role of, further promote luminescent properties.
Because the refractive index of CdTe-NaCl mixed crystal is different from polymer, optical path can be made repeatedly to reflect and improve the excitation time of QDs light
Number, further increases luminous efficiency.
(3) prepared by high stability quantum dot laminated film, and structural schematic diagram is as shown in Figure 3.
Referring to the preparation flow schematic diagram of the quantum dot laminated film of multilayered structure shown in Fig. 3, multilayered structure is prepared
Quantum dot laminated film.It disperses quantum dot-inorganic salts mixed crystal in polymer solution (such as PMMA, PS, PC, silicone resin),
It is coated by gravity flow coating, shape-preserving coating and far from three kinds of coating processes of coating, solidification, available quantum dot composite material is thin
Quantum dot laminated film is made in film, can prevent quantum dot from reuniting, so that quantum dot has high stability.Using different amounts
Different quantum dot laminated films can be obtained in sub- point-inorganic salts mixed crystal.Different quantum dot laminated films is compound, in outer layer
The quantum dot laminated film of multilayered structure can be obtained in coated polymer film.
Embodiment 2:
The green CdSe quantum dot 10mg being prepared in water intaking phase system, with 1g 1- carboxyethyl -3- methylimidazole bromide
Ionic liquid mixing, is stirred to react 30min-12h, carries out ligand exchange by a large amount of carboxyl and quantum dot surface sulfydryl, obtains
Quantum dot after to modification.Quantum dot is mixed with potassium bromide saturated solution after modifying, and obtains quantum dot-potassium bromide mixed crystal.Reference
The preparation process schematic diagram of quantum dots-polymer microballoon shown in Fig. 4, (such as with polymer by quantum dot-potassium bromide mixed crystal
PMMA, PS etc.) solution mixing, realize that micron, the quantum dot-of sub-micron (100nm-10 μm) are poly- by microfluid spining technology
Object microballoon is closed, which is used directly for the On-Chip encapsulation of LED.
Embodiment 3:
The CdS quantum dot 10mg that is prepared in water intaking phase system, with 0.1g 1- carboxyethyl -3- methylimidazole villaumite from
Sub- liquid mixing, is stirred to react 30min-12h, carries out ligand exchange by a large amount of carboxyl and quantum dot surface sulfydryl, obtains
Quantum dot after modification.Quantum dot is mixed with sodium tetraborate saturated solution after modifying, and obtains quantum dot-sodium tetraborate mixed crystal.
Embodiment 4:
The ZnSe quantum dot 10mg that is prepared in water intaking phase system, with 10g 1- carboxymethyl -3- methylimidazole bromide from
Sub- liquid mixing, is stirred to react 30min-12h, carries out ligand exchange by a large amount of carboxyl and quantum dot surface sulfydryl, obtains
Quantum dot after modification.Quantum dot is mixed with saturated potassium chloride solution after modifying, and obtains quantum dot-potassium chloride mixed crystal.
Embodiment 5:
The InP quantum dot 10mg that is prepared in water intaking phase system, with 100g 1- carboxymethyl -3- methylimidazole villaumite from
Sub- liquid mixing, is stirred to react 30min-12h, carries out ligand exchange by a large amount of carboxyl and quantum dot surface sulfydryl, obtains
Quantum dot after modification.Quantum dot is mixed with lithium chloride saturated solution after modifying, and obtains quantum dot-lithium chloride mixed crystal.
Embodiment 6:
The CuInS quantum dot 20mg10mg being prepared in water intaking phase system, with 0.5g1-10- sulfydryl decyl -3- methyl
The mixing of imidazoles bromide ionic liquid, is stirred to react 10min-4h, is matched by sulfhydryl ion liquid and quantum dot surface ligand
Body exchange, obtains the quantum dot of Ionic Liquid Modified.Quantum dot is mixed with sodium bromide saturated solution after modifying, and obtains quantum
Point-sodium bromide mixed crystal.
Claims (8)
1. a kind of method for improving aqueous phase quantum point stability, which comprises the following steps: use ionic liquid and water phase
Quantum dot carries out ligand exchange, quantum dot after being modified；
It is further comprising the steps of: quantum dot after the modification being mixed with inorganic salt saturated solution, it is mixed to obtain quantum dot-inorganic salts
Crystalline substance, i.e. solid state quantum point.
2. the method according to claim 1 for improving aqueous phase quantum point stability, which is characterized in that ionic liquid is quaternary ammonium
Class, season phosphine, pyridines, pyrrolidines, piperidines or glyoxaline ion liquid.
3. the method according to claim 2 for improving aqueous phase quantum point stability, which is characterized in that the ionic liquid tool
There is at least one of sulfydryl, amino, carboxyl, phosphate, guanidine radicals functional group.
4. the method according to claim 1 for improving aqueous phase quantum point stability, which is characterized in that the inorganic salts are chlorine
Change one of sodium, sodium bromide, potassium chloride, potassium bromide, lithium chloride, lithium bromide, sodium tetraborate or a variety of.
5. the method according to claim 1-4 for improving aqueous phase quantum point stability, which is characterized in that the water
Phase quantum dot is any quantum dot in CdTe, CdSe, CdS, ZnSe, InP, CuInS, CuInSe, PbS.
6. the method according to claim 1-4 for improving aqueous phase quantum point stability, which is characterized in that the use
Ionic liquid and aqueous phase quantum point carry out the specific steps of ligand exchange are as follows: take ionic liquid to mix with aqueous phase quantum point, stir
Reaction.
7. the method according to claim 6 for improving aqueous phase quantum point stability, which is characterized in that described when being stirred to react
Between >=30min.
8. it is according to claim 6 improve aqueous phase quantum point stability method, which is characterized in that the ionic liquid with
The mass ratio of the aqueous phase quantum point is 10-10000:1.
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| US11702590B2 (en) | 2018-04-25 | 2023-07-18 | Nichia Corporation | Light-emitting material and light-emitting device |
| CN110962427A (en) * | 2019-11-25 | 2020-04-07 | Tcl华星光电技术有限公司 | Quantum dot film |
| CN111500289A (en) * | 2020-04-21 | 2020-08-07 | 陕西科技大学 | 1-allyl-3-methyl-halogenated imidazole/gelatin synergistically stabilized tin halide perovskite quantum dot and preparation method thereof |
| CN113583678B (en) * | 2021-08-13 | 2022-11-11 | 南开大学 | Preparation method of water-dispersible silver telluride quantum dots modified by different mercapto compounds |
| CN114195552B (en) * | 2021-12-27 | 2022-09-23 | 杭州电子科技大学 | Film forming method for grafting nitrogen-doped carbon quantum dots on surface of silicon nitride ceramic ball |
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