CN106486571B - A kind of preparation method of high heat conduction quantum dot film - Google Patents
A kind of preparation method of high heat conduction quantum dot film Download PDFInfo
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- CN106486571B CN106486571B CN201610968220.2A CN201610968220A CN106486571B CN 106486571 B CN106486571 B CN 106486571B CN 201610968220 A CN201610968220 A CN 201610968220A CN 106486571 B CN106486571 B CN 106486571B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 bodies
- H01L33/04—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0083—Processes for devices with an active region comprising only II-VI compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 bodies
- H01L33/26—Materials of the light emitting region
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 bodies
- H01L33/26—Materials of the light emitting region
- H01L33/28—Materials of the light emitting region containing only elements of group II and group VI of the periodic system
Abstract
The invention discloses a kind of preparation methods of high heat conduction quantum dot film, including:Semiconductor-quantum-point, polymer matrix and the first organic solvent of S1 hybrid nanoscales, and polymer matrix is made to be dissolved completely in the first organic solvent, obtain quantum dot solution;Quantum dot solution is transferred in the syringe of electrospinning device by S2, and electrospun membrane is prepared using electrospinning device;S3 carries out hot pressing to electrospun membrane and obtains compacting electrospun membrane;S4 will be compacted electrospun membrane and immerse in LED packaging plastics, be taken out after vacuum defoamation, and heated solidification is to get to high heat conduction quantum dot film.Simple and effective, environmental protection and economy of the invention, significantly improves the heat conductivility for improving quantum dot film, so as to the heat dissipation performance for improving quantum dot LED and photochromic stability.
Description
Technical field
The invention belongs to quantum dot LED encapsulation technologies fields, more particularly, to a kind of system of high heat conduction quantum dot film
Preparation Method.
Background technology
LED (Light Emitting Diode) is a kind of electroluminescent light emitting semiconductor device, has service life
The advantages that length, environmental protection and energy saving, high colour developing coefficient, electro-optical efficiency be high, small, high reliability.Since LED is unique superior
Property, it is widely applied and rapidly develops in many fields, be considered most there is the next generation of foreground and importance to consolidate by industry
Body lighting source has huge market potential.
There is quantum dot LED component based on semiconductor-quantum-point (QD) color to be saturated, purity is high, monochromaticjty is good, color
It is adjustable and the advantages that simple solution manufacturing method is obtained and can be prepared on a large scale can be used.With the quantum of nucleocapsid
The defects of appearance of point, the photooxidation of nuclear quantum dot and photobleaching, is improved, photoluminescence quantum yield and optical stabilization
Property higher, the outer quantum yield of quantum dot LED component are greatly improved, become the luminescent device that currently attracts most attention it
One, and present fine application prospect.But very big heat is generated when quantum dot light emitting, since polymer matrix bulk thermal conductivities are low,
Traditional quantum dots-polymer film heat conductivility is poor, to which quantum dot film temperature is higher, causes quantum dot light emitting efficiency
Decline and color displacement, cause quantum dot LED heat performance and photochromic stability poor.
Invention content
The object of the present invention is to provide a kind of preparation methods of high heat conduction quantum dot film, can be by quantum dot using this method
The thermal conductivity of film is promoted from 0.2K/W or so to 0.9K/W or more.
In order to achieve the above objectives, the preparation method of high heat conduction quantum dot film provided by the invention, including step:
Semiconductor-quantum-point, polymer matrix and the first organic solvent of S1 hybrid nanoscales, and keep polymer matrix complete
Fully dissolved obtains quantum dot solution in the first organic solvent;
Quantum dot solution is transferred in the syringe of electrospinning device by S2, and electrospun membrane is prepared using electrospinning device;
S3 carries out hot pressing to electrospun membrane and obtains compacting electrospun membrane;
S4 will be compacted electrospun membrane and immerse in LED packaging plastics, be taken out after vacuum defoamation, heated solidification is led to get to height
Hot quantum dot film.
Further, semiconductor-quantum-point be CdSe/ZnS quantum dots, CdSe quantum dot, CdSe/CdS/ZnS quantum dots,
ZnO/CdS quantum dots, ZnSe/ZnS quantum dots, CuInS2Quantum dot or InP/ZnS quantum dots.
Further, polymer matrix is polystyrene (PS), polymethyl methacrylate (PMMA) or poly- terephthaldehyde
Sour glycol ester (PET).
Further, the first organic solvent is chloroform, toluene, hexane or dimethylbenzene.But the first organic solvent is not
It is limited to this, as long as the organic solvent of polymer matrix used by capable of dissolving.
Further, in quantum dot solution, the mass ratio of semiconductor-quantum-point and polymer matrix is 1:(50~200),
The mass concentration of polymer matrix is 10wt%~20wt%.
Further, syringe is glass or plastic material, and syringe needle is stainless steel.
Further, the hot pressing condition of step S3 is:Hot pressing temperature be 50 DEG C~100 DEG C, pressure limit be 5MPa~
20MPa, hot pressing time are 10 minutes~20 minutes.
Preferably, in step S3, before hot pressing, electrospun membrane is infiltrated using the second organic solvent, second is organic
The organic solvent that solvent selection does not dissolve polymer matrix and do not reacted with semiconductor-quantum-point.It is carried out using the second organic solvent
The purpose of infiltration is:So that electrospun membrane internal fiber is assembled, is easily formed dense film in hot pressing in this way
Second organic solvent is alcohol, ethylene glycol or isopropanol.
Further, LED packaging plastics are silica gel or epoxy resin.
Compared to the prior art, the present invention has following features and advantageous effect:
(1) the method for the present invention can prepare high heat conduction quantum dot film using simple common equipment and raw material, letter
It is single effective, environmental protection and economy.
(2) thermal conductivity of quantum dot film prepared by can reach 0.9K/W or more, and quantum dot-prepared by conventional method is poly-
The thermal conductivity only about 0.2K/W of object film is closed, the thermal conductivity of quantum dot film is significantly improved.The quantum dot of high heat conductance is thin
Film can effectively export the heat of quantum dot light emitting generation;The quantum dot film of the high heat conductance is used for quantum dot LED, can be promoted
The heat dissipation performance of quantum dot LED, while improving the photochromic stability of quantum dot LED.
Description of the drawings
Fig. 1 is the concrete technology flow process figure of the present invention;
Fig. 2 is the specific schematic diagram for preparing quantum dot solution;
Fig. 3 is the specific schematic diagram for preparing electrospun membrane;
Fig. 4 is the structural schematic diagram of electricity spinning fibre;
Fig. 5 is the specific schematic diagram of infiltration and the hot pressing of electrospun membrane;
Fig. 6 is the specific schematic diagram for filling LED packaging plastics;
Fig. 7 is the structural schematic diagram of high heat conduction quantum dot film prepared by the present invention.
In figure, 1- semiconductor-quantum-points, 2- quantum dot solutions, 3- magnetic stirring apparatus, 4- sealed membranes, 5- the first containers, 6-
Water, 7- high-voltage DC power supplies, 8- supporting tables, 9- syringe pumps, 10- syringes, 11- aluminium foils, 12- receiver boards, 13- draught cupboards, 14-
Electricity spinning fibre, 15- polymer matrixs, 16- electrospun membranes, 17- carriers, 18- alcohol, 19- pressing plates, 20- hot plates, 21- compactings
Electrospun membrane, 22-LED packaging plastics, 23- bubbles, 24- quantum dot films, 25- second containers.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
Embodiment 1
Referring to Fig. 1, a kind of high heat conduction quantum dot film preparation method comprising following steps:The system of S1 quantum dot solutions
Standby, S2 electrospun membranes preparation, the infiltration of S3 electrospun membranes and hot pressing, S4 filling LED packaging plastics simultaneously cure.These are walked below
Suddenly it is described in detail.
Referring to Fig. 2, in step S1, quantum dot solution 2 is prepared, semiconductor-quantum-point 1, polymer matrix 15 and first are had
Solvent is added in the first container 5, is sealed the first container for 5 mouthfuls with sealed membrane 4.The first container 5 is placed in 3 institute of magnetic stirring apparatus
It is filled with water in 6, carries out the magnetic agitation of 12 hours, obtain uniform quantum dot solution 2.In gained quantum dot solution, semiconductor
The mass ratio of quantum dot and polymer matrix is 1:100, mass concentration of the polymer matrix in quantum dot solution is 15wt%.
Referring to Fig. 3, in step S2, electrospun membrane is prepared, which carries out in draught cupboard 13, and draught cupboard 13 can provide photograph
Bright, ventilation and protective effect.Syringe pump 9 is fixed in supporting table 8, syringe pump 9 controls syringe 10.Quantum is housed in syringe 10
The syringe needle connection high-voltage DC power supply 7 of point solution 2, syringe 10 connects.Receiver board 12 is grounded, and 12 surface of receiver board has aluminium foil
11.Electricity spinning fibre 14 is attached directly to form electrospun membrane 16 on aluminium foil 11.
Referring to Fig. 4, electricity spinning fibre 14 is made of polymer matrix 15 and semiconductor-quantum-point 1, semiconductor-quantum-point 1 or
It is embedded in 15 surface of polymer matrix, or embedment polymer matrix 15.
Referring to Fig. 5, in step S3, in the infiltration and hot pressing of electrospun membrane, first by electrospun membrane 16 from aluminium foil 11
On remove, be transferred on smooth carrier 17, carrier 17 can be glass carrier or ceramic monolith.With alcohol 18 by electrospun membrane
Carrier 17 with electrospun membrane 16, is then placed on hot plate 20, smooth pressing plate 19 is used in combination to be pressed on electrospun membrane by 16 infiltrations
On 16, the hot pressing 20 minutes under 50 DEG C of temperature, 20Mpa pressure obtains the compacting electrospun membrane 21 being attached on carrier 17.Pressing plate 19
Flat, ceramic platen, aluminium alloy pressing plate or stainless steel platen can be used.
Referring to Fig. 6, in step S4, fill LED packaging plastics and it is cured during, first, will compacting electrospun membrane 21 from
It removes, is put into the second container 25 equipped with LED packaging plastics 22 on carrier 17.Then vacuum defoamation is carried out, by LED packaging plastics 22
In bubble 23 extract out.Then, the compacting electrospun membrane 21 for being mixed with LED packaging plastics 22 is taken out, is placed on carrier 17, carrier 17 is set
In on hot plate 20,60 minutes are heated to cure LED packaging plastics 22 to get to quantum dot film 24 in 80 DEG C of temperature.
Referring to Fig. 7, gained quantum dot film 24 is mainly made of electricity spinning fibre 14 and LED packaging plastics 22.
In the present embodiment, semiconductor-quantum-point is cadmium selenide/zinc sulphide (CdSe/ZnS) quantum dot of core/shell structure.
In the present embodiment, the first organic solvent is chloroform.
In the present embodiment, polymer matrix is polystyrene (PS).
In the present embodiment, LED packaging plastics are silica gel.
Each step of the present embodiment carries out under super-clean environment, i.e., is carried out in 100000 grades of ultra-clean chamber, and utensil used makes
With it is preceding cleaned with absolute ethyl alcohol and deionized water after in vacuum drying chamber it is dry.
Embodiment 2
The present embodiment and 1 method and step all same of embodiment, unlike:
In quantum dot solution prepared by step S1, the mass ratio of semiconductor-quantum-point and polymer matrix is 1:50, it is high
The mass concentration of copolymer matrix is 20wt%;
In step S3, hot pressing temperature is 80 DEG C, hot pressing pressure 10Mpa, and hot pressing time is 15 minutes;
In step S4, solidification temperature is 100 DEG C, and hardening time is 50 minutes;
Semiconductor-quantum-point is cadmium selenide (CdSe) quantum dot;
Polymer matrix is polymethyl methacrylate (PMMA);
LED packaging plastics are epoxy resin.
Each step of the present embodiment carries out under super-clean environment, i.e., is carried out in 100000 grades of ultra-clean chamber, and utensil used makes
With it is preceding cleaned with absolute ethyl alcohol and deionized water after in vacuum drying chamber it is dry.
Embodiment 3
The present embodiment and 1 method and step all same of embodiment, unlike:
In quantum dot solution prepared by step S1, the mass ratio of semiconductor-quantum-point and polymer matrix is 1:200, it is high
The mass concentration of copolymer matrix is 10wt%;
In step S3, hot pressing temperature is 100 DEG C, hot pressing pressure 5Mpa, and hot pressing time is 10 minutes;
In step S4, solidification temperature is 120 DEG C, and hardening time is 40 minutes;
Semiconductor-quantum-point is cadmium selenide/cadmium sulfide/zinc sulfide (CdSe/CdS/ZnS) quantum dot of core shell/shell structure;
Polymer matrix is polyethylene terephthalate (PET);
LED packaging plastics are epoxy resin.
Each step of the present embodiment carries out under super-clean environment, i.e., is carried out in 100000 grades of ultra-clean chamber, and utensil used makes
With it is preceding cleaned with absolute ethyl alcohol and deionized water after in vacuum drying chamber it is dry.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of high heat conduction quantum dot film, characterized in that including step:
Semiconductor-quantum-point, polymer matrix and the first organic solvent of S1 hybrid nanoscales, and keep polymer matrix completely molten
Solution obtains quantum dot solution in the first organic solvent;
Quantum dot solution is transferred in the syringe of electrospinning device by S2, and electrospun membrane is prepared using electrospinning device;
S3 carries out hot pressing to electrospun membrane and obtains compacting electrospun membrane;
S4 will be compacted electrospun membrane and immerse in LED packaging plastics, be taken out after vacuum defoamation, and heated solidification is to get to high heat conduction amount
Son point film.
2. the preparation method of high heat conduction quantum dot film as described in claim 1, it is characterized in that:
The semiconductor-quantum-point is CdSe/ZnS quantum dots, CdSe quantum dot, CdSe/CdS/ZnS quantum dots, ZnO/CdS
Quantum dot, ZnSe/ZnS quantum dots, CuInS2Quantum dot or InP/ZnS quantum dots.
3. the preparation method of high heat conduction quantum dot film as described in claim 1, it is characterized in that:
The polymer matrix is polystyrene, polymethyl methacrylate or polyethylene terephthalate.
4. the preparation method of high heat conduction quantum dot film as described in claim 1, it is characterized in that:
First organic solvent is chloroform, toluene, hexane or dimethylbenzene.
5. the preparation method of high heat conduction quantum dot film as described in claim 1, it is characterized in that:
In the quantum dot solution, the mass ratio of semiconductor-quantum-point and polymer matrix is 1:(50~200), high polymer base
The mass concentration of body is 10wt% ~ 20wt%.
6. the preparation method of high heat conduction quantum dot film as described in claim 1, it is characterized in that:
Hot pressing condition is in step S3:Hot pressing temperature is 50 DEG C ~ 100 DEG C, and pressure limit is 5MPa ~ 20MPa, and hot pressing time is
10 minutes ~ 20 minutes.
7. the preparation method of high heat conduction quantum dot film as described in claim 1, it is characterized in that:
In step S3, before hot pressing, electrospun membrane is infiltrated using the second organic solvent, the selection of the second organic solvent is insoluble
Solution polymer matrix and the organic solvent not reacted with semiconductor-quantum-point.
8. the preparation method of high heat conduction quantum dot film as claimed in claim 7, it is characterized in that:
Second organic solvent is alcohol, ethylene glycol or isopropanol.
9. the preparation method of high heat conduction quantum dot film as described in claim 1, it is characterized in that:
The LED packaging plastics are silica gel or epoxy resin.
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