CN107482104B - Quantum dot AAO curved surface film, quantum dot film lens, preparation method and quantum dot conversion of white light LED, packaging method - Google Patents
Quantum dot AAO curved surface film, quantum dot film lens, preparation method and quantum dot conversion of white light LED, packaging method Download PDFInfo
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- CN107482104B CN107482104B CN201710776173.6A CN201710776173A CN107482104B CN 107482104 B CN107482104 B CN 107482104B CN 201710776173 A CN201710776173 A CN 201710776173A CN 107482104 B CN107482104 B CN 107482104B
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 165
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims description 58
- 230000003647 oxidation Effects 0.000 claims description 36
- 238000007254 oxidation reaction Methods 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000741 silica gel Substances 0.000 claims description 16
- 229910002027 silica gel Inorganic materials 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000004411 aluminium Substances 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000004528 spin coating Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- 210000003934 vacuole Anatomy 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 230000004888 barrier function Effects 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000000137 annealing Methods 0.000 claims 1
- 239000010408 film Substances 0.000 description 120
- 239000000243 solution Substances 0.000 description 15
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 238000011010 flushing procedure Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- H01L33/505—Wavelength conversion elements characterised by the shape, e.g. plate or foil
-
- 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
- H01L33/58—Optical field-shaping elements
-
- 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
- H01L33/64—Heat extraction or cooling elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
A kind of quantum dot AAO curved surface film, quantum dot film lens, preparation method and quantum dot conversion of white light LED, packaging method are related to white light LEDs and show and lighting area.Quantum dot AAO curved surface film includes in curved surface or plane porous array anodic aluminum oxide film, the radius of curvature of porous array anodic aluminum oxide film is equal to the radius of curvature of inner surface of the lens, the duct of porous array anodic aluminum oxide film is embedded with quantum dot nano crystalline substance, quantum dot AAO curved surface film can encapsulate quantum dot wherein, while the radiating efficiency of quantum dot can be improved;The simple process of the preparation method of quantum dot AAO curved surface film, can be made quantum dot encapsulating curved surface film therein.Quantum dot film lens include the lens and above-mentioned quantum dot AAO curved surface film in hat, and the film adhered inner surface in lens of quantum dot AAO curved surface, which, which is used to encapsulate, forms quantum dot conversion of white light LED.
Description
Technical field
It is shown the present invention relates to white light LEDs and lighting area, and in particular to a kind of quantum dot AAO curved surface film, quantum
Point thin film lens, preparation method and quantum dot conversion of white light LED, packaging method.
Background technique
In recent years, quanta point material is gradually taken seriously, and especially quantum dot has spectrum with size adjustable, shine half-peak
A series of unique optical properties such as width, Stokes shift are big, launching efficiency is high, by the wide of LED and LCD backlight industry
General concern.Current commercialized display white light for illumination LED carries out light mixing using blue chip excitation yellow fluorescent powder and obtains, though
It can so be obtained by the doping of high color fluorescent powder compared with high color rendering index (CRI) Ra, but be limited by material level structure itself, emitted
Spectrum is too wide, and monochromaticjty is poor, and especially special colour rendering index R9 value is difficult to significantly be promoted, and colour gamut area coverage is not wide.For this purpose,
The color developing that quantum dot adjusts LED is introduced, is the future thrust of such device.
The relieved package of quanta point material becomes in need of consideration during encapsulation quantum dot conversion of white light LED and important asks
Topic.Quantum dot conversion of white light LED based on on-chip mode is not only encapsulated simply, and can directly utilize existing big function
Rate LED packaging technology, fast implements commercialization, is the mainstream of the current area research.However due to the temperature of quanta point material
Stability is poor, and photothermal is more serious in quanta point material progress light conversion process, and the self-absorption of quantum dot makes it
Constantly raised trend is presented in body temperature, on the one hand excessively high temperature causes quantum dot that thermal quenching occurs, on the other hand makes light
Decrease in efficiency forms vicious circle, seriously affects the optical property of device.
Therefore, it is necessary to a kind of optical and thermal stability that can improve quanta point material, enhance the packaged type of device reliability.
Summary of the invention
The purpose of the present invention is to provide a kind of quantum dot AAO curved surface films, can encapsulate quantum dot wherein, simultaneously
The radiating efficiency of quantum dot can be improved.
Another object of the present invention is to provide a kind of preparation methods of quantum dot AAO curved surface film, and simple process can
It is made and quantum dot is encapsulated into curved surface film therein.
Another object of the present invention is to provide a kind of quantum dot film lens, it is used to encapsulate that form quantum dot conversion white
Light LED.
Another object of the present invention is to provide a kind of preparation method of quantum dot film lens, simple processes.
It is highly reliable another object of the present invention is to provide a kind of quantum dot conversion of white light LED.
Another object of the present invention is to provide the packaging methods of quantum dot conversion of white light LED a kind of, and this method is simple, can
It is strong by property.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of quantum dot AAO curved surface film comprising in curved surface or plane porous array anodic oxidation
Aluminium film, the radius of curvature of porous array anodic aluminum oxide film are equal to the radius of curvature of inner surface of the lens, porous array anode
The duct of aluminum oxide film is embedded with quantum dot nano crystalline substance.
A kind of preparation method of quantum dot AAO curved surface film comprising following steps:
In outer surface, Al grown on substrates in curved surface forms porous array anodic aluminum oxide film, Al outer surface of substrate
Radius of curvature is equal to the radius of curvature of inner surface of the lens;
Quantum dot nano crystalline substance is uniformly embedded into the duct of porous array anodic aluminum oxide film.
Further, in a preferred embodiment of the present invention, the growing method of porous array anodic aluminum oxide film are as follows:
The Al substrate for taking purity >=99.999% deoils, oxide layer, polishing, obtains pretreated Al substrate;
Pretreated Al substrate is subjected to anodic oxidation twice, obtains the Al substrate that growth has aluminum oxide film;
There is the Al substrate of aluminum oxide film to handle growth, removes Al substrate.
Further, in a preferred embodiment of the present invention, pretreated mode is: by Al substrate, using mass fraction first
For acetone soln ultrasound 15~25 minutes of 92%~97%, next used distilled water flushing;Be placed in again concentration be 0.8~
8~13 minutes in the NaOH solution of 1.2mol/L, cleaned with distilled water;It anneals 3~4 hours in 450~520 DEG C later, it is cooling;
Then at 0 DEG C, it is placed in volume ratio [V (C2H5OH): V (HClO4)=3~4:1] mixed solution in constant pressure electrochemical polish,
8~12V of voltage is polished 4~6 minutes.
Further, in a preferred embodiment of the present invention, the method for anodic oxidation twice is: using 0 DEG C, concentration 0.2
The H of~0.4mol/L2C2O solution does electrolyte, and stereotype does cathode, and it is small to carry out oxidation 3.5~4.5 for the first time by 35~45V of voltage
When;At 56~62 DEG C, H is first used3PO4And H2CrO4Mixing vacuole 1.5~2.5 hours, then carry out under the same conditions
Secondary oxidation 2.5~3.5 hours.
Further, in a preferred embodiment of the present invention, the method for removing Al substrate is:
At 0 DEG C, the corrosive liquid that copper sulphate and hydrochloric acid form is poured into glass container, plastic filter screen is fixed on glass and is held
In device, there is the Al substrate of aluminum oxide film to be placed on plastic filter screen growth, Al substrate is located in corrosive liquid, until Al substrate disappears
It loses, obtains porous oxidation aluminium sheet;
At 30 DEG C or at room temperature, the barrier layer on phosphoric acid solution removal porous oxidation aluminium sheet is used.
A kind of quantum dot film lens comprising in the lens and above-mentioned quantum dot AAO curved surface film of hat, amount
The film adhered inner surface in lens of sub- point AAO curved surface.
A kind of preparation method of quantum dot film lens comprising following steps:
In the inner surface spin coating a thin layer silica gel of lens;Again by the film adhered inner surface in lens of quantum dot AAO curved surface,
Solidification.
A kind of quantum dot conversion of white light LED comprising lead frame, the LED blue chip in lead frame, and
Above-mentioned quantum dot film lens, quantum dot film lens cover is in the opening of lead frame, and quantum dot AAO curved surface film court
Into the opening of lead frame, encapsulating has silica gel between lead frame and quantum dot film lens.
A kind of packaging method of quantum dot conversion of white light LED comprising following steps:
Quantum dot film lens are placed in the opening of lead frame, quantum dot AAO curved surface film is towards lead frame
In opening, make to form closed space between quantum dot film lens and lead frame, the encapsulating silica gel in space, solidify.
Quantum dot AAO curved surface film, quantum dot film lens, preparation method and the quantum dot of the embodiment of the present invention are converted white
Light LED, packaging method beneficial effect be: the quantum dot AAO curved surface film of the embodiment of the present invention includes porous battle array in curved surface
Column anodic aluminum oxide film, the radius of curvature of porous array anodic aluminum oxide film is equal to the radius of curvature of inner surface of the lens, more
The duct of hole array anodic aluminum oxide film is embedded with quantum dot nano crystalline substance, and quantum dot AAO curved surface film can be by quantum dot
Wherein, while the radiating efficiency of quantum dot can be improved in encapsulation;The simple process of the preparation method of quantum dot AAO curved surface film, can
It is made and quantum dot is encapsulated into curved surface film therein.The quantum dot film lens of the embodiment of the present invention include the lens in hat,
And above-mentioned quantum dot AAO curved surface film, the film adhered inner surface in lens of quantum dot AAO curved surface, the quantum dot film
Lens form quantum dot conversion of white light LED for encapsulating;The simple process of the preparation method of quantum dot film lens.The present invention is real
The quantum dot conversion of white light LED for applying example includes lead frame, the LED blue chip in lead frame and above-mentioned amount
Son point thin film lens, quantum dot film lens cover is in the opening of lead frame, and quantum dot AAO curved surface film is towards lead frame
In the opening of frame, encapsulating has silica gel between lead frame and quantum dot film lens, the reliability of quantum dot conversion of white light LED
By force;The packaging method of quantum dot conversion of white light LED is simple, highly reliable.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
FIG. 1 to FIG. 3 is the structural representation of quantum dot AAO curved surface film provided in an embodiment of the present invention during the preparation process
Figure;
Fig. 4 is the structural schematic diagram of quantum dot AAO curved surface film provided in an embodiment of the present invention;
Fig. 5~Fig. 6 is the structural schematic diagram of quantum dot film lens provided in an embodiment of the present invention during the preparation process;
Fig. 7 is the structural schematic diagram of quantum dot film lens provided in an embodiment of the present invention;
Fig. 8~Fig. 9 is structural representation of the quantum dot conversion of white light LED provided in an embodiment of the present invention in encapsulation process
Figure;
Figure 10 is the structural schematic diagram of quantum dot conversion of white light LED provided in an embodiment of the present invention.
Icon: 100- quantum dot AAO curved surface film;110- porous array anodic aluminum oxide film;120- quantum dot nano
It is brilliant;130-Al substrate;200- quantum dot film lens;210- lens;220- layer of silica gel;300- quantum dot conversion of white light LED;
310- lead frame;320-LED blue chip;330- fluorescent powder glue-line;340- silica gel.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being usually described and illustrated herein in the accompanying drawings is implemented
The component of example can be arranged and be designed with a variety of different configurations.
Therefore, the detailed description of the embodiment of the present invention provided in the accompanying drawings is not intended to limit below claimed
The scope of the present invention, but be merely representative of selected embodiment of the invention.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
It should also be noted that similar label and letter indicate similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined in a attached drawing, does not then need that it is further defined and explained in subsequent attached drawing.
In the description of the present invention, it should be noted that the orientation or position of the instructions such as term " on ", "lower", "inner", "outside"
Set relationship be based on the orientation or positional relationship shown in the drawings or the invention product using when the orientation or position usually put
Relationship is set, is merely for convenience of description of the present invention and simplification of the description, rather than the device or element of indication or suggestion meaning are necessary
It with specific orientation, is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.
In the description of the present invention, it is also necessary to which explanation is unless specifically defined or limited otherwise, term " setting ",
" installation ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally connect
It connects;It can be mechanical connection, be also possible to be electrically connected;It can be directly connected, can also indirectly connected through an intermediary, it can
To be the connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood with concrete condition
Concrete meaning in the present invention.
First embodiment
Shown in Figure 4, the present embodiment provides a kind of quantum dot AAO curved surface films 100 comprising in curved surface or plane
Porous array anodic aluminum oxide film 110, porous array anodic aluminum oxide film 110 are that surface curvature is infinitely great in plane
Special case, the radius of curvature of porous array anodic aluminum oxide film 110 is equal to the radius of curvature of 210 inner surface of lens, porous battle array
The duct of column anodic aluminum oxide film 110 is embedded with quantum dot nano crystalline substance 120 (quanta point material).Porous battle array in the present embodiment
Column anodic aluminum oxide film 110 is in curved surface.
Referring to FIG. 1 to FIG. 4, the present embodiment also provides the preparation method of above-mentioned quantum dot AAO curved surface film 100,
The following steps are included:
S101, as depicted in figs. 1 and 2, on the Al substrate 130 in curved surface of outer surface growth form porous array anodic oxygen
Change aluminium (AAO) film, the radius of curvature of 130 outer surface of Al substrate is equal to the radius of curvature of 210 inner surface of lens.
S102, as shown in Figure 3 and Figure 4, using spin coating proceeding, in the duct of porous array anodic aluminum oxide film 110
It is uniformly embedded into quantum dot nano crystalline substance 120, forms quantum dot AAO curved surface film 100.
Wherein, the growing method of porous array anodic aluminum oxide film 110 are as follows:
A. it pre-processes: taking the Al substrate 130 of purity >=99.999%, deoil, oxide layer, polishing, after obtaining pretreatment
Al substrate 130.Transparency of the purity of Al substrate 130 to quantum dot AAO curved surface film 100 obtained, fenestra (i.e. duct)
The consistency of size influences very big: the purity of Al substrate 130 is higher, and the transparency of film and the consistency of fenestra size are better.
Pretreated concrete mode is: by Al substrate 130, the acetone soln for being first 92%~97% with mass fraction
Ultrasonic oil removing 15~25 minutes, next uses distilled water flushing;Be placed in again concentration be 0.8~1.2mol/L NaOH solution in 8~
13 minutes, oxide layer is removed, is cleaned with distilled water;It anneals 3~4 hours in 450~520 DEG C later, it is cooling;Then at 0 DEG C,
It is placed in volume ratio [V (C2H5OH): V (HClO4)=3~4:1] mixed solution in constant pressure electrochemical polish, 8~12V of voltage, throw
Light 4~6 minutes, in order that improving surface smoothness.
The present embodiment is by the Al substrate 130 of purity 99.999%, and the acetone soln for being first 95% with mass fraction is super
Sound 20 minutes, next used distilled water flushing;It is placed in the NaOH solution that concentration is 1mol/L 10 minutes, is cleaned with distilled water again;
It anneals 4 hours in 500 DEG C later, it is cooling;Then at 0 DEG C, it is placed in volume ratio [V (C2H5OH): V (HClO4)=4:1]
Constant pressure electrochemical polish in mixed solution, voltage 10V are polished 5 minutes.
B. anodic oxidation: carrying out anodic oxidation twice for pretreated Al substrate 130, and obtaining growth has aluminum oxide film
Al substrate 130.The flowing of 100 duct electrolyte inside of quantum dot AAO curved surface film is conducive to maintain the constant of temperature, improves mould
The degree of order of plate;The aperture of different electrolytes extreme influence quantum dot AAO curved surface film 100;Voltage minimal effect quantum dot AAO
The aperture of curved surface film 100, larger impact hole density.
The specific method of anodic oxidation twice is: using 0 DEG C, concentration is the oxalic acid (H of 0.2~0.4mol/L2C2O) solution
Electrolyte is done, stereotype does cathode, and 35~45V of voltage carries out oxidation 3.5~4.5 hours for the first time;At 56~62 DEG C, first use
H3PO4(mass fraction 5%~7%) and H2CrO4The mixing vacuole of (mass fraction 1.5%~2%) 1.5~2.5 hours, goes
Except the oxidation film that first time oxidation is formed, then second of oxidation 2.5~3.5 hours is carried out under the same conditions.
The present embodiment is using 0 DEG C, and concentration is the oxalic acid (H of 0.3mol/L2C2O) solution does electrolyte, and stereotype does cathode,
Voltage 40V carries out oxidation 4 hours for the first time;At 60 DEG C, H is first used3PO4(mass fraction 6%) and H2CrO4(mass fraction
1.8%) mixing vacuole 2 hours, then second of oxidation 3 hours is carried out under the same conditions.
C. it removes Al substrate 130: thering is the Al substrate 130 of aluminum oxide film to handle growth, remove Al substrate 130.
The specific method of removal Al substrate 130 is:
It (is 75% copper/saturated copper sulphate and quality by mass percent by the corrosive liquid that copper sulphate and hydrochloric acid form at 0 DEG C
The mixed liquor that the hydrochloric acid that percentage is 25% forms) glass container is poured into, by plastic filter screen (aperture 2um, hole period 3um, thickness
It 1um) is fixed in glass container, there is the Al substrate of aluminum oxide film to be placed on plastic filter screen growth and carry out demoulding, Al substrate
In corrosive liquid, bottom is visually observed without aluminium, sample bleach indicates that Al substrate disappears, obtains porous oxidation aluminium sheet;
At 30 DEG C or at room temperature, the barrier layer on porous oxidation aluminium sheet is removed using the phosphoric acid solution that mass fraction is 5%,
The porous oxidation aluminium sheet with barrier layer is specifically transferred to the surface of phosphoric acid solution, barrier layer downward, porous oxidation aluminium sheet
Hole upward, place 45 minutes after the porous array anodic aluminum oxide film with through-hole can be obtained.
Second embodiment
Shown in Figure 7, the present embodiment provides a kind of quantum dot film lens 200 comprising in 210 He of lens of hat
Quantum dot AAO curved surface film 100.Quantum dot AAO curved surface film 100 includes porous array anodic aluminum oxide film in curved surface
110, the radius of curvature of porous array anodic aluminum oxide film 110 is equal to the radius of curvature of 210 inner surface of lens, porous array sun
The duct of pole aluminum oxide film 110 is embedded with quantum dot nano crystalline substance 120;Quantum dot AAO curved surface film 100 passes through layer of silica gel 220
Fit in the inner surface of lens 210.
Referring to shown in Fig. 1 to Fig. 7, the present embodiment also provides the preparation method of above-mentioned quantum dot film lens 200,
The following steps are included:
S201, referring to figure 1 and figure 2, growth forms porous array anode on the Al substrate 130 in curved surface of outer surface
Aluminum oxide film 110, the radius of curvature of 130 outer surface of Al substrate are equal to the radius of curvature of 210 inner surface of lens.
S202, join as shown in figure 3 and figure 4, using spin coating proceeding, in the duct of porous array anodic aluminum oxide film 110
It is inside uniformly embedded into quantum dot nano crystalline substance 120, forms quantum dot AAO curved surface film 100.
S203, referring to shown in Fig. 5 to Fig. 7, in the inner surface spin coating a thin layer silica gel of lens 210, form layer of silica gel 220;
Quantum dot AAO curved surface film 100 is fitted in the inner surface of lens 210 again, is solidified, quantum dot thin film lens 200 is formed.
Wherein, the growing method of porous array anodic aluminum oxide film 110 are as follows:
A. it pre-processes: taking the Al substrate 130 of purity 99.999%, it is super with the acetone soln that mass fraction is 92% first
Sound oil removing 25 minutes, next used distilled water flushing;It is placed in the NaOH solution that concentration is 0.8mol/L again 13 minutes, removes deoxidation
Layer is cleaned with distilled water;It anneals 4 hours in 450 DEG C later, it is cooling;Then at 0 DEG C, it is placed in volume ratio [V (C2H5OH): V
(HClO4)=3:1] mixed solution in constant pressure electrochemical polish, voltage 12V, polish 6 minutes, in order that improve surfacing
Degree.
B. anodic oxidation: by pretreated Al substrate 130, using 0 DEG C, concentration is the oxalic acid (H of 0.2mol/L2C2O)
Solution does electrolyte, and stereotype does cathode, and voltage 45V carries out oxidation 4.5 hours for the first time;At 56 DEG C, H is first used3PO4(quality
Score 5%) and H2CrO4The mixing vacuole of (mass fraction 1.5%) 2.5 hours, the removal oxidation film that oxidation is formed for the first time,
Carry out second of oxidation 2.5 hours under the same conditions again.
C. it removes Al substrate 130: thering is the Al substrate 130 of aluminum oxide film to handle growth, remove Al substrate 130.
3rd embodiment
Shown in Figure 10, the present embodiment provides a kind of quantum dot conversion of white light LED300 comprising lead frame 310,
LED blue chip 320 in lead frame 310 in lead frame 310 and is covered on LED blue chip 320
Fluorescent powder glue-line 330 and quantum dot film lens 200.Quantum dot film lens 200 include 210 He of lens in hat
Quantum dot AAO curved surface film 100.Quantum dot AAO curved surface film 100 includes porous array anodic aluminum oxide film in curved surface
110, the radius of curvature of porous array anodic aluminum oxide film 110 is equal to the radius of curvature of 210 inner surface of lens, porous array sun
The duct of pole aluminum oxide film 110 is embedded with quantum dot nano crystalline substance 120;Quantum dot AAO curved surface film 100 passes through layer of silica gel 220
Fit in the inner surface of lens 210.Quantum dot film lens 200 are covered in the opening of lead frame 310, and quantum dot AAO is bent
Face film 100 is towards in the opening of lead frame 310, and encapsulating has silicon between lead frame 310 and quantum dot film lens 200
Glue 340.
The embodiment of the present invention is thin using the porous array anodised aluminium (AAO) that radius of curvature agrees with 210 inner surface of lens
Film is uniformly embedded into the quantum dot AAO curved surface film 100 formed after quantum dot nano crystalline substance 120 in duct, can be by quanta point material
It is solidificated in the nano-array pipe of porous array anodic aluminum oxide film 110.The quantum dot conversion of white light eventually formed
LED300 forms chain structure, effectively contains hot Cluster Phenomenon since quanta point material is cured in nano-array pipe, and
And quantum dot conversion of white light LED300, when working, oxygen and moisture largely act on the quantum dot particle at chain structure both ends,
Intermediate quantum dot particle is effectively protected, to keep the light conversion efficiency of quantum dot, improves quantum dot conversion of white light
The thermal stability of LED300 enhances device reliability.
Referring to shown in Fig. 1 to Figure 10, the present embodiment also provides the encapsulation side of above-mentioned quantum dot conversion of white light LED300
Method comprising following steps:
S301, growth forms porous array anodic aluminum oxide film 110, Al on the Al substrate 130 in curved surface of outer surface
The radius of curvature of 130 outer surface of substrate is equal to the radius of curvature of 210 inner surface of lens.
S302, using spin coating proceeding, be uniformly embedded into quantum dot in the duct of porous array anodic aluminum oxide film 110 and receive
Rice crystalline substance 120, forms quantum dot AAO curved surface film 100.
S303, the inner surface spin coating a thin layer silica gel in lens 210 form layer of silica gel 220;Again by quantum dot AAO curved surface
Film 100 fits in the inner surface of lens 210, and solidification forms quantum dot thin film lens 200.
S304, quantum dot film lens 200 are placed in the opening of lead frame 310, quantum dot AAO curved surface film 100
Towards in the opening of lead frame 310, make to form closed space between quantum dot film lens 200 and lead frame 310,
Encapsulating silica gel 340 in space, solidification form quantum dot conversion of white light LED300.
Wherein, the growing method of porous array anodic aluminum oxide film 110 are as follows:
A. it pre-processes: taking the Al substrate 130 of purity 99.999%, it is super with the acetone soln that mass fraction is 97% first
Sound oil removing 15 minutes, next used distilled water flushing;It is placed in the NaOH solution that concentration is 1.2mol/L again 8 minutes, removes deoxidation
Layer is cleaned with distilled water;It anneals 3 hours in 520 DEG C later, it is cooling;Then at 0 DEG C, it is placed in volume ratio [V (C2H5OH): V
(HClO4)=4:1] mixed solution in constant pressure electrochemical polish, voltage 8V, polish 4 minutes, in order that improve surfacing
Degree.
B. anodic oxidation: by pretreated Al substrate 130, using 0 DEG C, concentration is the oxalic acid (H of 0.4mol/L2C2O)
Solution does electrolyte, and stereotype does cathode, and voltage 35V carries out oxidation 3.5 hours for the first time;At 62 DEG C, H is first used3PO4(quality
Score 7%) and H2CrO4The mixing vacuole of (mass fraction 2%) 1.5 hours, the removal oxidation film that oxidation is formed for the first time, then
Second of oxidation 3.5 hours is carried out under the same conditions.
C. it removes Al substrate 130: thering is the Al substrate 130 of aluminum oxide film to handle growth, remove Al substrate 130.
In conclusion the quantum dot AAO curved surface film of the embodiment of the present invention can encapsulate quantum dot wherein, while can mention
The radiating efficiency of high quantum dot;The simple process of the preparation method of quantum dot AAO curved surface film, can be made quantum dot encapsulating it
In curved surface film;Quantum dot film lens form quantum dot conversion of white light LED for encapsulating;The preparation of quantum dot film lens
The simple process of method;Quantum dot conversion of white light LED's is highly reliable;The packaging method of quantum dot conversion of white light LED is simple, can
It is strong by property.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of quantum dot AAO curved surface film, which is characterized in that quantum dot AAO curved surface film includes in curved surface
Or the porous array anodic aluminum oxide film of plane, the radius of curvature of the porous array anodic aluminum oxide film are equal in lens
The radius of curvature on surface, the duct of the porous array anodic aluminum oxide film are embedded with quantum dot nano crystalline substance, and quantum dot AAO is bent
The preparation method of face film the following steps are included:
In outer surface, Al grown on substrates in curved surface forms porous array anodic aluminum oxide film, the Al outer surface of substrate
Radius of curvature is equal to the radius of curvature of inner surface of the lens;
Quantum dot nano crystalline substance is uniformly embedded into the duct of the porous array anodic aluminum oxide film,
Wherein, the growing method of the porous array anodic aluminum oxide film are as follows:
The Al substrate for taking purity >=99.999% deoils, oxide layer, polishing, obtains pretreated Al substrate;
Pretreated Al substrate is subjected to anodic oxidation twice, obtains the Al substrate that growth has aluminum oxide film;
There is the Al substrate of aluminum oxide film to handle growth, removes Al substrate.
2. the preparation method of quantum dot AAO curved surface film according to claim 1, which is characterized in that pretreated mode
It is: Al substrate first with acetone soln ultrasound 15~25 minutes that mass fraction is 92%~97%, is secondly rushed with distilled water
It washes;It is placed in the NaOH solution that concentration is 0.8~1.2mol/L 8~13 minutes, is cleaned with distilled water again;Later in 450~520
It is DEG C annealing 3~4 hours, cooling;Then at 0 DEG C, it is placed in volume ratio [V (C2H5OH): V (HClO4)=3~4:1] mixing it is molten
Constant pressure electrochemical polish in liquid, 8~12V of voltage are polished 4~6 minutes.
3. the preparation method of quantum dot AAO curved surface film according to claim 1, which is characterized in that anodic oxidation twice
Method be: using 0 DEG C, concentration is the H of 0.2~0.4mol/L2C2O solution does electrolyte, and stereotype does cathode, and voltage 35~
45V carries out oxidation 3.5~4.5 hours for the first time;At 56~62 DEG C, H is first used3PO4And H2CrO4Mixing vacuole 1.5~
2.5 hours, then second of oxidation 2.5~3.5 hours is carried out under the same conditions.
4. the preparation method of quantum dot AAO curved surface film according to claim 1, which is characterized in that removal Al substrate
Method is:
At 0 DEG C, the corrosive liquid that copper sulphate and hydrochloric acid form is poured into glass container, plastic filter screen is fixed on the glass and is held
In device, there is the Al substrate of aluminum oxide film to be placed on the plastic filter screen growth, the Al substrate is located in corrosive liquid, until
Al substrate disappears, and obtains porous oxidation aluminium sheet;
At 30 DEG C or at room temperature, the barrier layer on the porous oxidation aluminium sheet is removed using phosphoric acid solution.
5. a kind of quantum dot film lens, which is characterized in that it includes the lens in hat, and as described in claim 1
Quantum dot AAO curved surface film, the film adhered inner surface in the lens of quantum dot AAO curved surface.
6. a kind of preparation method of quantum dot film lens as claimed in claim 5, which is characterized in that it includes following step
It is rapid:
In the inner surface spin coating a thin layer silica gel of the lens;It is again that the quantum dot AAO curved surface is film adhered in the lens
Inner surface, solidification.
7. a kind of quantum dot conversion of white light LED, which is characterized in that it includes lead frame, the LED in the lead frame
Blue chip, and quantum dot film lens as claimed in claim 5, the quantum dot film lens cover is in the lead
The opening of frame, and the quantum dot AAO curved surface film is towards in the opening of the lead frame, the lead frame with it is described
Encapsulating has silica gel between quantum dot film lens.
8. a kind of packaging method of quantum dot conversion of white light LED as claimed in claim 7, which is characterized in that it includes following
Step:
The quantum dot film lens are placed in the opening of the lead frame, the quantum dot AAO curved surface film is towards institute
It states in the opening of lead frame, makes to form closed space between the quantum dot film lens and the lead frame, in institute
Encapsulating silica gel in space is stated, is solidified.
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