CN110016334A - The enhanced quantum dot fluorescence powder of forward scattering for pc-LEDs encapsulation - Google Patents
The enhanced quantum dot fluorescence powder of forward scattering for pc-LEDs encapsulation Download PDFInfo
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- CN110016334A CN110016334A CN201910350231.8A CN201910350231A CN110016334A CN 110016334 A CN110016334 A CN 110016334A CN 201910350231 A CN201910350231 A CN 201910350231A CN 110016334 A CN110016334 A CN 110016334A
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- quantum dot
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- dot fluorescence
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
- C09K11/562—Chalcogenides
- C09K11/565—Chalcogenides with zinc cadmium
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- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
- C09K11/592—Chalcogenides
- C09K11/595—Chalcogenides with zinc or cadmium
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- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/671—Chalcogenides
- C09K11/672—Chalcogenides with zinc or cadmium
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- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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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
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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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
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Abstract
The invention discloses the enhanced quantum dot fluorescence powder of the forward scattering encapsulated for pc-LEDs, grain diameter d meets d >=0.1 λ/π, and (λ is lambda1-wavelength, π is pi), it include quantum dot light emitting layer in particle using multi-layer core-shell structure.Front portion light intensity is greater than rearward portion light intensity when forward scattering enhancing characteristic scatters light, effectively avoid Multiple Scattering caused by back scattering/absorption bring light intensity loss, light extraction efficiency is promoted, the narrowband of incorporating quantum point shines, and realizes the improvement of spectrum efficiency.
Description
Technical field
The present invention relates to field of photoelectric technology, and in particular to is used for pc-LEDs (phosphor converted light-
Emitting diode, the light emitting diode based on fluorescent powder conversion) encapsulation forward scattering enhanced quantum dot fluorescence powder
Structure and its preparation.
Background technique
Quantum dot (Quantum Dots, QD), essence is a kind of nanoscale semiconductor material, and partial size usually exists
The range of 1nm to 10nm.Because of the effect of quantum confinement, band structure is not continuous, and its level structure is discrete
, optics behavior is similar with macromolecular to emit fluorescence, and volume size controls luminescent spectrum, that is, there is quantum size effect
It answers.Exactly because quantum size effect may be used as phosphor material powder, same material only needs to change its granular size can be real
The luminescent spectrum of existing different-waveband.Although it is prepared, simple and cost is relatively low, quantum yield with higher.
In pc-LEDs, for traditional micrometer fluorescent powder, quantum dot has very narrow half-wave peak width,
Excitation purity is higher, can substantially be more than NTSC color gamut range.So can be obtained based on the LED that color quantum point converts very high aobvious
The value of color performance, Ra and R9 can be more than 95, almost close to 100.Quantum dot coating is similar with conventional fluorescent powder coating, is all
The photon that the wave band of needs is launched in conversion is carried out by absorbing the photon that chip issues, pattern concentration equally influences chromaticity
Matter and light efficiency.Quantum dot is uniformly mixed by certain carrier material with silica gel usually, stable colloid is obtained and carries out coating system
Standby Colloidal Quantum Dots layer.Unlike, in traditional white light pc-LEDs encapsulation, the fluorescent powder of broad-band illumination spectrum (such as YAG:
Ce3+ etc.) since the visual sensitivity of the long feux rouges of its spectrum, far-red light ingredient is low additional luminous efficacy can be brought again
The loss of (LER, Luminous Efficacy of Radiation), i.e. white-light spectrum loss in efficiency；In order to improve luminous effect
Energy LER, peak value are located at high visual sensitivity wavelength region, the quantum dot fluorescence powder with relatively narrow transmitted bandwidth (FWHM=30nm)
(QDs) it is good selection, utilizes the narrow emission spectrum and Wavelength tunable control characteristic of quantum dot fluorescent powder, adjustment wavelength to human eye
The most sensitive green of vision, red band, can obtain high eye response；Spectral bandwidth is reduced simultaneously, radiation energy is concentrated
In the high range of visual sensitivity, the long feux rouges of conventional fluorescent powder is reduced, the low visual sensitivity of far-red light ingredient bring shines and imitates
The loss of energy.And plant illumination is encapsulated with pc-LEDs, corresponding spectrum can be adjusted, red, blue effective coverage is fallen in.
Therefore, quantum dot conversion, which shines, also will be the important trend of illumination and display, before wide application
Scape.
Summary of the invention
Problem to be solved by this invention is how to realize the light extraction efficiency coating for further improving quantum dot fluorescent powder.By
It is undersized in nano-quantum point itself, it generally can all be less than 12nm, Rayleigh scattering, back scattering are easily caused for visible light
It is relatively strong, Yi Yinqi light intensity loss.Experiment discovery, for common blue-light LED chip, the quantum dot less than 12nm can cause
Light intensity loss, Yao Shixian forward scattering enhances partial size will be in 15nm or more.Therefore the present invention proposes to increase based on forward scattering characteristic
Strong type core-shell quanta dots (Forward Mie Scattering--Quantum Dots, FMS-QDs) fluorescent powder, i.e., in quantum dot
Grown quantum luminescent layer on the layer surface that shines addition clad or seed crystal, improves the quantum dot fluorescence powder obtained after size, will have
There is the nano-phosphor to light forward scattering enhancing to evenly spread in medium, on the surface coated in LED chip light extraction direction,
It realizes forward scattering enhancing and narrowband shines, light extraction efficiency can be improved, but also spectrum is finely adjustable.
The present invention proposes the enhanced quantum dot fluorescence powder of forward scattering for pc-LED encapsulation.
The technical solution of the present invention is as follows:
For the enhanced quantum dot fluorescence powder of forward scattering of pc-LEDs encapsulation, quantum dot fluorescence powder particles are multilayer cores
Shell structure includes quantum dot light emitting layer, there is narrowband luminous spectrum after being stimulated；(λ is lambda1-wavelength to partial size d >=0.1 λ/π, and π is
Pi), it may occur that Mie scattering can cause the forward scattering of institute's transmission ray to enhance in grain diameter size；Described
Quantum dot fluorescence powder is used for the coating of pc-LED encapsulation, is coated on the surface of LED chip light extraction direction, forms quantum dot fluorescent powder
Coating.
The multi-layer core-shell structure is the partial size in order to improve particle, it is seen that light encounters the quantum dot fluorescence that package thickeies
Mie scattering occurs afterwards for powder particles (partial size d >=0.1 λ/π), it is seen that light encounters under stock size (12nm or less) quantum dot fluorescence
Occur Rayleigh scattering under powder particles, front portion light intensity is greater than rearward portion light intensity when light Mie scattering, and Rayleigh occurs and dissipates
Front and back is equal to light intensity when penetrating.
The multi-layer core-shell structure includes quantum dot light emitting layer/clad structure or seed crystal/quantum dot light emitting layer
Structure or seed crystal/quantum dot light emitting layer/clad structure；Quantum dot light emitting layer, clad are one or more layers.
The multi-layer core-shell quantum dot light emitting layer be CdSe, ZnS, CdTe, ZnO, ZnTe, CdS, MgO, CaO, MgS,
It is one or more in the II-VI group compound of CaS, MgSe, CaSe, MgTe, CaTe, or part other compounds MoSe2、
In2O3One kind or combination.
The multi-layer core-shell quantum dot can be two layers, three layers, four layers of even more multilayer.A kind of way is that internal layer core is made
Luminescent layer, for size in 2~10nm, the coating thickness range of last outside is 10nm or more；Another kind is that internal layer core is not sent out
Photosphere, size is in 2nm or more, and in 2~10nm, the coating thickness range of last outside is the light emitting layer thickness then coated
8nm or more；Its medium wavelength meets partial size d >=0.1 λ/π.
The covering material include CdSe, ZnS of II-VI group, CdTe, ZnO, ZnTe, CdS, MgO, CaO, MgS,
CaS, MgSe, CaSe, MgTe, CaTe are formed by clad, further include other oxide S iO2、TiO2、ZrO2、ITO、
In2O3、SnO2.Oxide is coated to quantum dot up in the way of hydrolysis, obtained quantum dot fluorescence powder particles need full
Sufficient partial size can cause the Mie scattering of light in nano-scale, enhance the forward scattering of institute's transmission ray.Such as to common blue light
Gallium nitride chip coating needs to meet whole partial size d >=15nm, needs to meet partial size d >=24.9nm to feux rouges.
To have and dispersing agent is cooperated to the quantum dot fluorescence powder of light forward scattering, evenly spread to in arogel, simple
The shape that photosphere is taken out in control can improve the distribution of light to a certain extent, in order to further promote uniformity, take out photosphere
Middle addition dispersing agent, light diffusing agent.There are commonly inorganic light diffusing agent earth silicon material, organic dispersing agent tetrahydrofuran；
QDs fluorescent powder is mixed with arogel with the ratio uniform of mass-adjustable score 1%~35%；QDs fluorescent powder can also be glimmering with other
Light powder is mixed with different proportions.
The arogel of matching is silica gel, epoxy resin, polymethyl methacrylate (PMMA), polycarbonate (PC) or photoresists
One or more of combination；The photoresists include following three classes negative-working photoresist: 1. SBQ photoresists (polyvinyl alcohol
Cyclic ketal styryl pyridinium resin photoresists), SBQ-PVA+ macromolecule emulsion, SBQ-PVA+ macromolecule emulsion+acrylic acid
The combination of one or more of ester or organic stibazole salt resin photoresists system；2. emulsion+film forming dosage form,
That is photosensitive compounds+high-molecular compound type, wherein emulsion is bichromate, chromate, diazonium compound or folds
The combination of one or more of nitrilo compound；Film forming agent be polyvinyl alcohol (PVA), gum arabic, polyimides or
The combination of one or more of polyvinyl acetate emulsion；3. the high-molecular compound type with photosensitive base, mainly there is poly- second
Enol cinnamate, polyvinyl alcohol cortex cinnamomi fork acetic acid esters, polyethylene oxygen ethyl-cinnamic acid ester, polyvinylpyrrolidone or polyethylene
The combination of one or more of the p- azidobenzoic acid ester (PVAB) of alcohol-.
The preparation method of the quantum dot fluorescence powder coating, can be dotting glue method, be also possible to electrophoresis, spray coating method,
The combination of one of infusion process, spin-coating method, the precipitation method, impact system or two kinds and two or more methods.
The quantum dot fluorescence powder is used for the encapsulation of pc-LEDs chip, and the LED is single LED chip, either
Plurality of LEDs chipset or whole wafer (Wafer) in same substrate.
The quantum dot fluorescence powder coating is coated in the fluorescent coating of LED light output surface, be direct contact LED
The mode on chip light emitting surface, or leave (hanging) painting of remote of the light output surface of LED chip light-emitting area a distance
Layer structure.
The quantum dot fluorescence powder coating is spontaneous curing according to the different curing methods with arogel, is heating and curing, or
It is photo-curing.
Detailed description of the invention
Fig. 1, the quantum dot fluorescent powder with core-shell structure of the invention based on forward scattering, this is 3 layers of core-shell structure, most intermediate
1 be seed crystal, next 2 are quantum dot light emitting layers, and outmost 3 be clad, and wavelength of light λ, whole particle size d are full
Sufficient d >=0.1 λ/π；
Fig. 2, light encounter particle scattering when light intensity with angular distribution, x be light transmission come direction, forward light it is powerful in
Backward light intensity (Mie scattering), partial size d >=0.1 λ/π；
Fig. 3, light encounter light intensity when particle scatters, and, with angular distribution, x is the direction that light transmission comes, forward direction light intensity
Greater than rear Xiang Guangqiang (Mie scattering), partial size d > > 0.1 λ/π；
For light intensity with angular distribution, z is the direction that light transmission comes when Fig. 4, light encounter particle scattering, and forward direction light intensity is equal to
Backward light intensity (Rayleigh scattering), partial size d < 0.1 λ/π；
Fig. 5, it being coated in chip surface for quantum dot fluorescence powder and the mixing of other micrometer fluorescent powders, 1 is chip in figure, 2
It is multi-layer quantum dot fluorescent powder, 3 be other micrometer fluorescent powders.
Specific embodiment
With reference to the accompanying drawing and embodiment the invention will be further described:
Embodiment 1
Take the zinc acetate of 0.05mol/L carries out hydro-thermal reaction, life at 75 DEG C with 0.05mol/L sodium sulfide solution 20ml
At ZnS nucleus, is controlled by the time of Ao Sidewaer maturing process, the ZnS seed crystal of 7 rans is obtained after 5 hours, then
LSS three-phase system solvent-thermal method is used again, takes 5mmol cadmium acetate, 5mmol selenium powder and the ethyl alcohol and 100mmol that are put into 100mmol
Enuatrol stir 30 minutes, be added in seed crystal solution, under agitation, kept for 1 hour under 85 degrees Celsius, growth 4nm
Left and right CdSe quantum luminescent layer and then take zinc acetate, vulcanized sodium, prepared again outside it one layer of 5nm or so ZnS cladding
Layer, forms ZnS/CdSe/ZnS multi-layer core-shell structure as shown in Figure 1, the product that reaction obtains is centrifuged, with third
Then sediment vacuum drying is obtained particle size in 16nm or so in 45 DEG C of conditions by ketone and deionized water washing sediment
QDs fluorescent powder, partial size and blue light wavelength have relationship d=0.107 λ/π (λ=470nm).Finally, according to arogel mass ratio 1:10
It takes the product of 0.1g to evenly spread in 1g silica gel, phosphor slurry is coated in by blue-light LED chip using dotting glue method and goes out light table
On face, (150 DEG C) are heated drying 2 hours with drying box, and experiment obtains light distribution such as Fig. 2 when fluorescent powder grain scatters light
It is shown.
Embodiment 2
Dosage is as described in Example 1, using in aqueous solution zinc acetate and vulcanized sodium hydro-thermal reaction, generate ZnS seed crystal,
It is controlled by the time of Ao Sidewaer maturing process, 7 nanometers of ZnS seed crystal is obtained after 5 hours, then uses LSS three-phase again
System solvent-thermal method, if embodiment 1 operates, originally on the basis of extend the reaction time about 1 hour, it is prepared by cadmium acetate and selenium powder
After the CdSe quantum luminescent layer of 5nm or so partial size, the ZnS clad of one layer of 5nm or so is prepared again outside it, form ZnS/
It is centrifuged after CdSe/ZnS multi-layer core-shell structure particle, filtration drying, obtains QDs fluorescent powder of the particle size in 17nm or so, grain
Diameter and blue light wavelength have relationship d=0.13 λ/π.Finally, taking arogel mass ratio is that 1:15 is uniformly mixed, deaeration machine vacuumizes removing
Bubble obtains phosphor slurry, coats on the chip surface phosphor slurry using dotting glue method, heats (150 DEG C) with drying box
It is 2 hours dry, obtain cured phosphor powder layer.
Embodiment 3
After preparing ZnS seed crystal according to embodiment 1, using LSS Three-phase solvent thermal method etc., prolong on the basis of embodiment 2
The long reaction time about one hour, change partial size.Cadmium acetate and selenium powder prepare 6nm or so partial size CdSe quantum luminescent layer it
Afterwards, it is centrifuged after preparing the ZnS clad of one layer of 5nm or so again outside it, filtration drying obtains ZnS/CdSe/ZnS particle size
In the QDs fluorescent powder of 18nm or so, partial size and blue light wavelength have relationship d=0.12 λ/π, and subsequent operation and embodiment 1 are consistent, apply
It is layed on chip.
Embodiment 4
After preparing ZnS seed crystal in the manner described above, LSS three-phase system solvent-thermal method is then used again, when control is reacted
Between, change partial size and prepares one layer of ZnS again outside it after cadmium acetate and selenium powder prepare the CdSe quantum luminescent layer of 7nm or so
Clad, centrifugation, filtration drying, obtaining particle size in the QDs fluorescent powder of 19nm or so, partial size and blue light wavelength has relationship d=
0.126λ/π.Respectively by a variety of different proportions weigh quantum dot fluorescence powder with arogel and the two being uniformly mixed, it is de- with vacuum
Bubble machine carries out vacuumize process to mixing slurry, obtains phosphor slurry after removing bubble；It is first uniform in glass surface with spray gun
Certain thickness silica gel is sprayed as pumping optical confinement layer, then the phosphor slurry of different quality arogel ratio is taken to be respectively coated on the layer
On, it is put into drying box and heats (150 DEG C) drying 2 hours, obtain cured phosphor powder layer.
Embodiment 5
After preparing ZnS seed crystal in the manner described above, LSS three-phase system solvent-thermal method, control reaction temperature are then used again
Degree or time change partial size.After cadmium acetate and selenium powder prepare the CdSe quantum luminescent layer of 8nm or so partial size, outside it again
One layer of ZnS clad is prepared, is centrifuged, filtration drying, obtains particle size in the QDs fluorescent powder of 20nm or so ZnS/CdSe/ZnS,
Partial size and blue light wavelength have relationship d=0.133 λ/π (λ=470nm).Subsequent operation and embodiment 1 are consistent.
Embodiment 6
After preparing ZnS seed crystal in the manner described above, LSS Three-phase solvent thermal method is then used again, unlike, control is anti-
It answers temperature or time, changes partial size.After the CdS quantum luminescent layer that cadmium acetate and vulcanized sodium reaction are prepared to 7nm or so, package
The ZnS shell of 7nm, obtains ZnS/CdS/ZnS multi-layer core-shell structure, and centrifugal drying obtains particle size in the QDs fluorescence of 21nm
Powder, partial size and blue light wavelength have relationship d=0.14 λ/π.Subsequent operation and embodiment 1 are consistent.
Embodiment 7
The predecessor of the cadmium of 5mmol, selenium, zinc, sulphur is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, such as embodiment 1
Meet water-soluble CdSe/ZnS core shell type quantum point of emission wavelength requirement with the preparation of LSS Three-phase solvent thermal method, size is in 12nm
Hereinafter, the backward ingredient of Rayleigh scattering is larger, conventional fluorescent powder (such as YAG:Ce3+) SiO is further used2Film coats molten
Glue method realizes the SiO to CdSe/ZnS quantum dot surface by hydrolysis with ethyl orthosilicate (TE0S) for silicon source2Film packet
It is centrifuged after covering, filtration drying, the CdSe/ZnS/SiO of 22nm side-to-side dimensions can be obtained2Quantum dot nucleocapsid fluorescent powder, partial size with
Blue light wavelength has relationship d=0.146 λ/π (λ=470nm).Remaining operation is same as Example 1.
Embodiment 8
It is consistent with operation order before above-described embodiment, the difference is that changing clad, with butyl titanate Ti (OC4H9)4For
Titanium source realizes the TiO to CdSe/ZnS quantum dot surface by hydrolysis2Centrifugal drying after film cladding, can obtain 23nm
The CdSe/ZnS/TiO of size2Quantum dot nucleocapsid, d=0.15 λ/π (λ=470nm).Finally, take 0.1g quantum dot fluorescence powder (or
Upper conversion ultraviolet fluorescence powder is mixed with rouge and powder), 0.4ml photoresists (with PVA solution and the mixing of ADC solution with) and the two is mixed
It closes uniform；It will be coated on LED chip surface with the mixed phosphor slurry of photoresists using dotting glue method again, and expose 0.75ms
And it completes to develop.
Embodiment 9
Predecessor and embodiment 1 are consistent, after preparing ZnS seed crystal, are met using preparations such as LSS Three-phase solvent thermal methods and are shone
The water-soluble CdSe quantum dot light emitting layer of wavelength requirement, size in 12nm hereinafter, Rayleigh scattering it is rear larger to ingredient, further
Using conventional fluorescent powder (such as YAG:Ce3+) SiO2The sol method of film cladding passes through with ethyl orthosilicate (TE0S) for silicon source
Hydrolysis realizes the SiO to ZnS/CdSe quantum dot surface2It is centrifuged after film control thickness cladding, filtration drying can obtain
The ZnS/CdSe/SiO of 24nm side-to-side dimensions2Quantum dot nucleocapsid, partial size and blue light wavelength have relationship d=0.16 λ/π (λ=
470nm).Remaining operation is same as Example 1.
Embodiment 10
By the SiO in embodiment 102It is changed to TiO2, with butyl titanate Ti (OC4H9)4For titanium source, CdTe/ZnS/ is obtained
TiO2Quantum dot nucleocapsid.Remaining operation is same as Example 1.
Embodiment 11
The predecessor of the cadmium of 5mmol, tellurium, zinc, sulphur is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS tri-
Phase solvent thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare partial size 8nm CdTe seed crystal, and package 7nm is left
The quantum dot ZnS of right thickness, then the SiO of one layer of 10nm is coated by modes such as hydrolysis2, thickness is obtained in the CdTe/ZnS/ of 25nm
SiO2Quantum dot nucleocapsid, partial size and blue light wavelength have relationship d=0.167 λ/π (λ=470nm).Remaining operation and 1 phase of embodiment
Together.
Embodiment 12
By the SiO in upper embodiment2It is changed to TiO2, with butyl titanate Ti (OC4H9)4For titanium source, 25 nanometers are obtained
CdTe/ZnS/TiO2Quantum dot nucleocapsid.Remaining operation is same as Example 1.
Embodiment 13
The predecessor of 5mmol cadmium, tellurium, zinc, sulphur is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS three-phase
Solvent method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the CdTe seed crystal of 8nm, the amount of package 7nm or so
Son point layer ZnS, then the SiO by one layer of 11nm of hydrolysis method cladding2, thickness is obtained in the CdTe/ZnS/SiO of 26nm2Quantum dot
Nucleocapsid, d=0.173 λ/π (λ=470nm).Remaining operation is same as Example 1.
Embodiment 14
By the SiO in upper embodiment2It is changed to TiO2, obtain CdTe/ZnS/TiO2Quantum dot nucleocapsid.Remaining operation and implementation
Example 1 is identical.
Embodiment 15
The predecessor of the cadmium of 5mmol, tellurium, zinc, oxygen is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS tri-
Phase solvent thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the CdTe seed crystal of 7nm, package 7nm or so
Quantum dot layer ZnO, then the SiO by one layer of 13nm of hydrolysis method cladding2, thickness is obtained in the CdTe/ZnO/SiO of 27nm2Quantum
Point nucleocapsid, d=0.18 λ/π (λ=470nm).Remaining operation is same as Example 1.
Embodiment 16
By the SiO in upper embodiment2It is changed to TiO2, obtain CdTe/ZnO/TiO2Quantum dot nucleocapsid.Remaining operation and implementation
Example 1 is identical.
Embodiment 17
The predecessor of the cadmium of 5mmol, tellurium, zinc, oxygen is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS tri-
Phase solvent thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the ZnO seed crystal of 8nm, wrap up 8nm quantum dot
Luminescent layer CdTe, then the SiO by one layer of 12nm of hydrolysis method cladding2, thickness is obtained in the ZnO/CdTe/SiO of 28nm2Quantum
Point nucleocapsid, d=0.187 λ/π (λ=470nm).Remaining operation is same as Example 1.
Embodiment 18
By the SiO in upper embodiment2It is changed to TiO2, obtain ZnO/CdTe/TiO2Quantum dot nucleocapsid.Remaining operation and implementation
Example 1 is identical.
Embodiment 19
The predecessor of 5mmol cadmium, sulphur, zinc, oxygen is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS three-phase
Solvent-thermal method, synthesis reaction temperature control the reaction time, first prepare the CdS seed crystal of 6nm, wrap up the quantum dot of 8nm at 85 DEG C
Layer ZnO, then the SiO by one layer of 10nm of hydrolysis cladding2, thickness is obtained in the CdS/ZnO/SiO of 24nm2Quantum dot nucleocapsid.Remaining
It operates same as Example 1.
Embodiment 20
By the SiO in upper embodiment2It is changed to TiO2, obtain CdS/ZnO/TiO2Quantum dot nucleocapsid.Remaining operation and embodiment
1 is identical.
Embodiment 21
The predecessor of 5mmol cadmium, zinc, oxygen is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS Three-phase solvent
Thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the CdO seed crystal of 8nm diameter, the amount of package 7nm or so
Son point layer ZnO, then one layer of SiO2 is coated by hydrolysis method, thickness is obtained in the CdO/ZnO/SiO of 25nm2Quantum dot nucleocapsid.
Remaining operation is same as Example 1.
Embodiment 22
By the SiO in upper embodiment2It is changed to TiO2, obtain CdO/ZnO/TiO2Quantum dot nucleocapsid.Remaining operation and embodiment
1 is identical.
Embodiment 23
The predecessor of 5mmol cadmium, zinc, oxygen is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS Three-phase solvent
Thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the ZnO seed crystal of 6nm or more, package 3nm quantum dot hair
Photosphere CdO, then the SiO by one layer of 17nm of hydrolysis method cladding2, thickness is obtained in the ZnO/CdO/SiO of 26nm2Quantum dot core
Shell.Remaining operation is same as Example 1.
Embodiment 24
By the SiO in upper embodiment2It is changed to TiO2, obtain ZnO/CdO/TiO2Quantum dot nucleocapsid.Remaining operation and embodiment
1 is identical.
Embodiment 25
The predecessor of 5mmol cadmium, zinc, sulphur is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS Three-phase solvent
Thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the ZnS seed crystal of 7nm, wrap up 4nm quantum dot light emitting layer
CdS, then by the SiO2 of one layer of 16nm of hydrolysis method cladding, thickness is obtained in the ZnS/CdS/SiO of 27nm2Quantum dot nucleocapsid,
Partial size and blue light wavelength (λ=470nm) have relationship d=0.121 λ/π.Remaining operation is same as Example 1.
Embodiment 26
By the SiO in embodiment 252It is substituted for TiO2, and the thickness of clad is improved, obtain ZnS/CdS/TiO2Quantum dot
Fluorescent powder, total partial size arrive 30nm, take red LED chip, and partial size and red light wavelength (λ=775nm) have relationship d=0.121
λ/π.And it is coated on red LED chip surface according to the operation of embodiment 1.
Embodiment 27
Using different predecessors, by the middle luminescent layer in embodiment 25 be substituted for CdSe, CdTe, ZnO, ZnTe,
One of CdS, MgO, CaO, MgS, CaS, MgSe, CaSe, MgTe, CaTe, and the thickness of clad is controlled, obtain ZnS/ hair
Photosphere/SiO2Quantum dot fluorescence powder, total partial size arrives 30nm, taking red LED chip, partial size and red light wavelength (λ=
775nm) there is relationship d=0.121 λ/π.And it is coated on red LED chip surface according to the operation of embodiment 1.
Embodiment 28
The predecessor of 5mmol cadmium, zinc, sulphur is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS Three-phase solvent
Thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the ZnS seed crystal of 8nm, wrap up 4nm quantum dot light emitting layer
CdS, then the SiO by hydrolysis method one layer of 17nm thickness of cladding2, thickness is obtained in the ZnS/CdS/SiO of 31nm2Quantum dot nucleocapsid,
Partial size and blue light wavelength (λ=775nm) have relationship d=0.125 λ/π.Red LED chip is taken, remaining operation and 1 phase of embodiment
Together.
Embodiment 29
By the SiO in upper embodiment2It is changed to TiO2, shorten growth time, ZnS layers of 8nm, CdS layer 4nm coat one layer of 8nm
Thick TiO2, obtain the ZnS/CdS/TiO that thickness reaches 20nm2Quantum dot nucleocapsid takes purple LED chip, partial size and violet wavelength
λ=400nm has relationship d=0.157 λ/π, and is coated on purple LED chip surface according to the operation of embodiment 1.
Embodiment 30
The predecessor of 5mmol cadmium, zinc, sulphur is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS Three-phase solvent
Thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the ZnS seed crystal of 7nm, wrap up 6nm quantum dot light emitting layer
CdS, then coat by way of hydrolysis the SiO of one layer of 8nm2, thickness is obtained in the ZnS/CdS/SiO of 21nm2, partial size and purple light
Wavelength X=400nm has relationship d=0.164 λ/π.Remaining operation is same as Example 1.
Embodiment 31
By the SiO in upper embodiment2It is changed to TiO2, obtain the ZnS/CdS/TiO of size 21nm2After quantum dot fluorescence powder, take
Purple LED chip gets on according to the operation coating of embodiment 1.
Embodiment 32
The predecessor of 5mmol selenium, molybdenum, sulphur, zinc is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS three-phase
Solvent-thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the ZnS seed crystal of 7nm, package 6nm quantum dot hair
Photosphere MoSe2, then coat by way of hydrolysis the SiO of one layer of 8nm2, thickness is obtained in the ZnS/MoSe of 21nm2/SiO2, grain
Diameter and violet wavelength λ=400nm have relationship d=0.164 λ/π.Remaining operation is same as Example 1.
Embodiment 33
The predecessor of 5mmol indium, zinc, sulphur, selenium is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS three-phase
Solvent-thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the ZnS seed crystal of 7nm, package 6nm quantum dot hair
Photosphere In2Se3, then coat by way of hydrolysis the SiO of one layer of 8nm2, thickness is obtained in the ZnS/In of 21nm2Se3/SiO2, grain
Diameter and violet wavelength λ=400nm have relationship d=0.164 λ/π.Remaining operation is same as Example 1.
Embodiment 34
The predecessor of 5mmol cadmium, zinc, sulphur is taken respectively, is dissolved by heating at 40 DEG C, after obtaining solution, using LSS Three-phase solvent
Thermal method, synthesis reaction temperature control the reaction time at 85 DEG C, first prepare the CdS seed crystal of 8nm, wrap up 6nm quantum dot layer ZnS,
The SiO2 for coating one layer of 8nm by hydrolysis method again, obtains thickness in the CdS/ZnS/SiO of 22nm2Quantum dot nucleocapsid, partial size with
Violet wavelength λ=400nm has relationship d=0.173 λ/π.Remaining operation is same as Example 1.
Embodiment 35
By the SiO in embodiment 312It is changed to TiO2, obtain the CdS/ZnS/TiO of size 22nm2After quantum dot fluorescence powder, take
Purple LED chip, remaining operation are same as Example 1.
Embodiment 36
Based on the embodiment of above-mentioned hydrolysis cladding, using 4 layers of core-shell structure, in the TiO of third layer2(SiO2) pass through again outside
One layer of SiO of hydrolysis package2(TiO2) or other oxides, further increase nucleocapsid thickness.By obtained fluorescent powder by embodiment 1
Mode be coated to LED chip.
Embodiment 37
The quantum dot fluorescence powder of above-described embodiment and micrometer fluorescent powder are mixed with mass ratio 1:1, according to reality
The mode for applying example 1 is made into slurry and is coated to chip, forms coat as shown in Figure 5.
Claims (10)
1. the enhanced quantum dot fluorescence powder of forward scattering for pc-LEDs encapsulation, it is characterised in that: the quantum dot fluorescence
Powder particles are multi-layer core-shell structures, include quantum dot light emitting layer, there is narrowband luminous spectrum；(λ is incident light wave to partial size d >=0.1 λ/π
Long, π is pi), cause Mie scattering, the light intensity of front portion is more than the light intensity of rearward portion when scattering, makes transmitted light
The forward scattering of line enhances；The quantum dot fluorescence powder is used for the coating of pc-LED encapsulation, is coated in LED chip light extraction direction table
On face.
2. the forward scattering enhanced quantum dot fluorescence powder according to claim 1 for pc-LEDs encapsulation, feature exist
In: the multi-layer core-shell structure or quantum dot light emitting layer/clad structure or seed crystal/quantum dot light emitting layer knot
Structure or seed crystal/quantum dot light emitting layer/clad structure；Quantum dot light emitting layer, clad are one or more layers；The quantum
Point light emitting layer thickness is in 2~10nm.
3. the forward scattering enhanced quantum dot fluorescence powder according to claim 1 for pc-LEDs encapsulation, feature exist
In: the quantum dot light emitting layer be II-VI group compound be CdSe, ZnS, CdTe, ZnO, ZnTe, CdS, MgO, CaO, MgS,
One or more combination of CaS, MgSe, CaSe, MgTe, CaTe or other elements compound MoSe2、In2Se3One kind
Or combination.
4. the forward scattering enhanced quantum dot fluorescence powder according to claim 1 for pc-LEDs encapsulation, feature exist
In: the clad of the multi-layer core-shell structure is II-VI group compound or other oxide S iO2、TiO2、ZrO2、ITO、In2O3、
SnO2One or more combinations；Grain diameter d >=0.1 λ/π after cladding.
5. the forward scattering enhanced quantum dot fluorescence powder according to claim 1 for pc-LEDs encapsulation, feature exist
It is that quantum dot fluorescence powder is distributed to the mixture obtained with arogel or quantum dot fluorescence powder and its in: the coating composition
He is distributed to the mixture obtained with arogel at fluorescent powder mixing.
6. the forward scattering enhanced quantum dot fluorescence powder according to claim 1 for pc-LEDs encapsulation, feature exist
In: the coating method is traditional dispensing, electrophoresis, spraying, dipping, spin coating, precipitating, printing.
7. the forward scattering enhanced quantum dot fluorescence powder according to claim 1 for pc-LEDs encapsulation, feature exist
In: the LED chip light extraction direction surface is the surface of chip, or leaves the either table along beam projecting direction of chip
Face.
8. the forward scattering enhanced quantum dot fluorescence powder according to claim 1 for pc-LEDs encapsulation, feature exist
In: the LED chip is organic or inorganic light-emitting diode；It is single light-emitting diode chip for backlight unit or same substrate
On more LED chips or whole wafer.
9. according to claim 5 match arogel, it is characterised in that: described is the one of hot-setting adhesive and photoresists with arogel
Kind；The thermosetting cement is the thermosetting cements such as silica gel, epoxy resin, polymethyl methacrylate (PMMA), polycarbonate (PC)
One or more combinations；The photosensitive colloid includes three classes negative-working photoresist: 1. emulsion+film forming dosage form, i.e. photonasty
Compound+high-molecular compound type, wherein emulsion is bichromate, chromate, diazonium compound either azido chemical combination
The combination of one or more of object, film forming agent are polyvinyl alcohol (PVA), gum arabic, polyimides or poly- acetic acid second
The combination of one or more of enester emulsion；2. the high-molecular compound type with photosensitive base, mainly there is polyvinyl alcohol cortex cinnamomi
Acid esters, polyvinyl alcohol cortex cinnamomi fork acetic acid esters, polyethylene oxygen ethyl-cinnamic acid ester, polyvinylpyrrolidone or polyvinyl alcohol-are p- folded
The combination of one or more of pyridine formic acid esters (PVAB)；3. SBQ photoresists (polyvinyl alcohol cyclic ketal stibazole
Salt resin photoresists), SBQ-PVA+ macromolecule emulsion, SBQ-PVA+ macromolecule emulsion+acrylate or organic benzene, organic vinylpyridine
The combination of one or more of pyridine salt resin photoresists system；The photoresists are above-mentioned one or more combinations.
10. according to claim 5 match arogel, it is characterised in that: described solidifies with arogel according to different its of its type
Mode is to be heating and curing or spontaneous curing or be photo-curing.
Priority Applications (1)
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