CN104263361A - AgInS2 quantum dot/PMMA (Polymethyl Methacrylate) composite luminescent material and application thereof - Google Patents
AgInS2 quantum dot/PMMA (Polymethyl Methacrylate) composite luminescent material and application thereof Download PDFInfo
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Abstract
The invention discloses an AgInS2 quantum dot/PMMA (Polymethyl Methacrylate) composite luminescent material and application thereof. A preparation method of the AgInS2 quantum dot/PMMA composite luminescent material comprises the following steps: (1) dissolving mononuclear AgInS2 quantum dots into normal hexane to obtain a quantum dot solution of which the concentration is 0.002-0.003mmol/ml; (2) adding (3-sulfydryl propyl)trimethoxy silane into the quantum dot solution obtained in the step (1) for modifying the surface of the solution to obtain a modified quantum dot solution; and (3) mixing the modified quantum dot solution obtained in the step (2) with methyl methacrylate in the volume ratio of 1:(1-20), and performing a polymerization reaction under the action of an initiator to obtain the AgInS2 quantum dot/PMMA composite luminescent material. The invention provides application of the AgInS2 quantum dot-PMMA composite luminescent material in manufacturing of white-light LEDs (Light-Emitting Diodes). The AgInS2 quantum dot/PMMA composite luminescent material prepared by using the method has high optical transparency and superior luminescence property; and when the AgInS2 quantum dot/PMMA composite luminescent material is used for encapsulating white-light LEDs of different structures, the color temperatures, color rendering indexes and the like of the white-light LEDs can be improved effectively.
Description
(1) technical field
The present invention relates to a kind of AgInS
2quantum dot/PMMA composite luminescent material and preparing the application in white light LEDs.
(2) background technology
Sony corporation of Japan has put on display the Bravia high-definition liquid crystal panel TV set of first use quantum techniques in the world at CES (Consumer Electronics Show) recently.This product has benefited from the excellent photoelectric properties of quantum dot, and the clear beautiful color technology of application Triluminos, makes the gamut extension 50% of televisor, and the more high definition that develops the color is dazzled color beautiful.The appearance of this product, shows that the research of quantum dot enters unprecedented fieriness, and it is at the applied research of photoelectric field especially in the efficient photoelectricity treater switching device LED center that focuses on of current researcher especially.
In recent years, new green environment protection I-III-VI race semiconductor nano AgInS
2be that quantum dot obtains significant progress, effectively can absorb the blue light that GaN chip sends, launch each coloured light that wavelength is accurately adjustable in visible-range, by AgInS
2be that quantum dot is applied on GaN base white light LEDs and can replaces Ce:YAG fluorescent material, red fluorescence powder and the application of Cd based quantum dot in this field, effectively improve the performances such as the colour temperature of GaN base white light LEDs, colour rendering index.
But due to AgInS
2the small size of quantum dot makes it have very high specific surface area, surface energy is high, easy reunion, semiconductor-quantum-point is normally got by organic polymer or the laminating one-tenth of micromolecular stabilizer package simultaneously, suffer to destroy the performance being just easy to affect quantum dot once these stablizers, make its unstable properties, the Colloidal Quantum Dots prepared at present cannot directly apply in white-light LED structure.There is investigator by AgIn
5s
8-ZnS quantum dot and silica gel (OE-6630A, B) be coated on blue-light LED chip after mixing, obtaining luminous efficiency is 53lm/W, colour rendering index is 74, corresponding colour temperature is white light LEDs [the Do Y R of 3700K, Hong S P, Park H K, et al.Comparisons of the Structural and Optical Properties of o-AgInS
2, t-AgInS
2, and c-AgIn
5s
8nanocrystals and their Solid-Solution Nanocrystals with ZnS.J.Mater.Chem., 2012,22:18939-18949.].
In order to make AgInS
2be that the excellent luminance performance of quantum dot is embodied in GaN base white light LEDs, apply with the form of body material after itself and polymkeric substance can being carried out being compounded to form polymer-based nano recombination luminescence block materials.Polymkeric substance has good processing characteristics and optical transparence, in the composite, not only can play carrier function, prevent the reunion of quantum dot, and can control size and the distribution of particle and improve stability.
PMMA (polymethylmethacrylate) is as a kind of water white thermoplastics.It has fabulous light transmission, and (visible light transmissivity reaches 92%, exceedes simple glass; Uv transmittance reaches 73%, far away higher than simple glass, infraredly can to pass through well at below 2800nm), physical strength is higher, has that certain heat-resistant is cold, erosion resistance, and insulating property are good, dimensional stabilizing, be easy to shaping, and nontoxic corrosion-free, cost is low, be widely used at present preparing in optical clear and fluorescence nano composite material.
Therefore, will there is the AgInS of excellent luminance performance
2be that quantum dot is with AgInS
2be that the form of quantum dot/PMMA composite luminescent material is applied in white light LEDs as luminescent layer, replace Ce:YAG fluorescent material, red fluorescence powder and the application of Cd based quantum dot in this field, break the patent monoply of Japan and other countries to white light LEDs, improve the overall innovation of China in LED field, realize the expectation of the people to high color rendering index (CRI) warm white LED light source, promote the great development of China's LED industry.
In addition, also relevant AgInS is not yet had both at home and abroad so far
2the report being quantum dot/PMMA recombination luminescence block materials and applying in GaN base white light LEDs.
(3) summary of the invention
First object of the present invention is to provide a kind of AgInS with the optical transparence of height and the luminescent properties of excellence
2quantum dot/PMMA composite luminescent material.
Second object of the present invention is to provide described AgInS
2quantum dot/PMMA composite luminescent material is preparing the application in white light LEDs.
Below the technical solution used in the present invention is illustrated.
The invention provides a kind of AgInS
2quantum dot/PMMA composite luminescent material, its preparation method comprises the steps:
(1) by monokaryon AgInS
2quantum dot is dissolved in normal hexane and obtains the quantum dot solution that concentration is 0.002 ~ 0.003mmol/mL;
(2) silane coupling agent is added in the quantum dot solution obtained in step (1)---(3-mercaptopropyi) Trimethoxy silane (MPS), to its modifying surface, obtains modified quantum dot solution; Wherein the volume ratio that feeds intake of MPS and quantum dot solution is 1:1 ~ 10;
(3) get the modified quantum dot solution that step (2) obtains to mix according to volume ratio 1:1 ~ 20 with methyl methacrylate (MMA), under initiator effect, carry out polyreaction, obtain AgInS
2quantum dot/PMMA composite luminescent material.
In step of the present invention (1), described monokaryon AgInS
2the preparation method of quantum dot can with reference to our early-stage Study: J.Mater.Chem.C, and 2013,1 (10): 2014-2020; J.Alloys Compd.10.1016/j.jallcom.2013.10.188; CN 103265948 A; CN 103265949 A; The present invention quotes in full above-mentioned document.Specifically, described monokaryon AgInS
2quantum dot be using Silver Nitrate as silver-colored source, indium chloride as indium source, oleic acid is surface capping agents, Dodecyl Mercaptan is surface ligand, sulphur powder is sulphur source, oleyl amine is prepared as the solvent dissolving sulphur powder by hot injection method, described preparation method comprises the steps:
A () adds AgNO in reaction vessel
3, InCl
3, oleic acid, Dodecyl Mercaptan and solvent octadecylene, obtain Ag, In presoma mixed solution, wherein AgNO
3, InCl
3, oleic acid, Dodecyl Mercaptan molar ratio be 1:1 ~ 6:1 ~ 10:10 ~ 40, AgNO
3with InCl
3molar ratio most preferably 1:4; AgNO
3be preferably 1:20 ~ 30 with the molar ratio of Dodecyl Mercaptan, most preferably be 1:30;
B () is got sulphur powder and is added in oleyl amine, heating makes sulphur powder fully dissolve, and obtains S precursor solution;
C Ag, In presoma mixed solution, under the protection of argon gas, is heated to 50 ~ 80 DEG C from room temperature and keeps 10 ~ 60min, with venting air by (); Be warming up to 100 ~ 120 DEG C, after stablizing 1 ~ 5min subsequently, inject S precursor solution, the mol ratio of control Ag:S is 1:2 ~ 10, reaction 5 ~ 90min;
D () sampling is also dissolved in normal hexane, obtain AgInS
2quantum dot solution;
E AgInS that () obtains in step (d)
2add dehydrated alcohol in quantum dot solution, centrifugation obtains monokaryon AgInS
2quantum dot.
Further, in step (1), the concentration of quantum dot solution is preferably 0.0025mmol/mL.
In step of the present invention (2), selection and the luminescent properties of its addition on gained matrix material with the silane coupling agent of amphiprotic group have very large impact.The present invention selects MPS as the properties-correcting agent of quantum dot solution, and it forms-Si-O-bridged bond by hydrolysis, connects the organic phase (AgInS that oleic acid, oleyl amine are coated
2quantum dot) and inorganic phase (MMA), effectively improve being separated between organic and inorganic phase interface, impel carrying out smoothly of its recombination process.This invention simplifies the step of the modification to quantum dot, only need directly to add MPS in quantum dot solution.Experimental result shows: if its addition is 0, namely quantum dot solution is without MPS modification, and the matrix material obtained is not luminous.When MPS addition within the specific limits time, gained Composite material transparent and luminosity is high.When its addition is too much, make polymerization velocity slowly, the transparency of matrix material declines and luminosity reduces.The AgInS that transparency is high in order to prepare in the short period of time, luminosity is strong
2quantum dot-PMMA composite luminescent material, the volume ratio that feeds intake of preferred MPS and quantum dot solution is 1:2 ~ 5, is more preferably 1:3 ~ 5.
In step of the present invention (3), the consumption of the quantum dot solution of doping has a great impact the polymerization velocity of composite luminescent material, transparency, luminosity.Doping content within the specific limits time, the luminosity of gained matrix material improves along with the increase of doping content, when exceeding a certain amount of, cannot be polymerized.The volume ratio of preferred quantum dots solution and MMA is 1:1 ~ 20.The performance of selection to gained composite luminescent material of initiator does not have great effect, generally can select AIBN, BPO etc.Because AIBN can form free radical through level of decomposition, initiated polymerization at relatively low temperatures, and AIBN is more stable, so the relatively more conventional AIBN of the bulk polymerization of MMA is as initiator.In the present invention, the mass ratio that feeds intake of initiator and MMA is 0.1 ~ 1.0:100, preferred 0.6:100.
Further, the polyreaction in step (3) preferably adopts classical two-stage polymerization method---the pre-polymerization process of short period of time and the Post isothermal treatment of long period, make the matrix material for preparing to obtain there is higher transparency.Specifically, preferred prepolymerization temperature is 70 ~ 90 DEG C, prepolymerization time 10 ~ 30min; Post isothermal treatment temperature is at 50 ~ 70 DEG C, and the Post isothermal treatment time is 24 ~ 72h.
In the present invention, by AgInS
2quantum dot-PMMA composite luminescent material is made bulk and can be completed in above-mentioned steps (3), namely after prepolymerization, pours in mould by gained mixture, carries out later stage pre-treatment subsequently, then takes out demoulding polishing and obtain transparent AgInS
2/ PMMA recombination luminescence block materials.
In one embodiment of the present invention, provide described AgInS
2quantum dot-PMMA composite luminescent material is preparing the application in white light LEDs, and described application is specially: by AgInS
2quantum dot-PMMA composite luminescent material makes bulk, the AgInS not homochromy by one or more
2the block composite luminescent material of quantum dot-PMMA mates with GaN chip, is packaged into white light LEDs.
In another embodiment of the invention, also provide described AgInS
2quantum dot-PMMA composite luminescent material is preparing the application in white light LEDs, and described application is specially: by AgInS
2quantum dot-PMMA composite luminescent material makes bulk, the AgInS not homochromy by one or more
2the block composite luminescent material of quantum dot-PMMA mates with Ce:YAG monocrystalline, GaN chip, is packaged into white light LEDs.
Compared with prior art, maximum advantage and difference are in the present invention: the AgInS 1) obtained by the present invention
2quantum dot/PMMA composite luminescent material has the optical transparence of height; 2) quantum dot is uniformly dispersed in PMMA, and remains the luminescent properties of quantum dot excellence, achieves AgInS
2the organic functional of quantum dot.3) luminescent properties of matrix material regulates by the performance of adopted quantum dot, the concentration etc. of doped quantum dot.4) only need add the modification that a certain amount of MPS can realize quantum dot solution in the present invention in quantum dot solution, simplify in prior art and need to carry out numerous and diverse steps such as stir process to it for a long time.5) the present invention is directly by AgInS
2quantum dot solution and MMA carry out mass polymerization, avoid after quantum dot being prepared into powder in current techniques and carry out compound, the phenomenon that fluorescence property reduces.6) under the exciting of near ultraviolet and blue light, glow peak is adjustable at 550 ~ 700nm, be applicable to each illumination field especially in GaN base white light LEDs, gained block materials is mated with GaN chip, optimize its packaging process, be packaged into the white light LEDs with different structure, effectively can improve the colour temperature, colour rendering index etc. of white light LEDs.7) the luminous block materials of gained mates with block Ce:YAG monocrystalline by the present invention, effectively solves the problems such as matching degree is low, packaging process is complicated, powder characteristic is unstable between block and commercially available Ce:YAG fluorescent powder.8) the present invention adopts the AgInS with different glow color
2-PMMA luminescent material directly combines or becomes white light LEDs with Ce:YAG monocrystalline combinations matches, has broken the external patent limitation to Ce:YAG fluorescent material, has achieved the white-light LED structure with independent intellectual property right.
(4) accompanying drawing explanation
Fig. 1: the AgInS obtained by different quantum dot-doped amount
2the luminous spectrum schematic diagram of quantum dot-PMMA composite luminescent material under GaN blue chip (460nm) excites.
Fig. 2 a is the transmittance curve figure of different silane coupling agent consumption gained matrix material.
Fig. 2 b is the luminous spectrograms of different silane coupling agent consumption gained matrix materials under GaN chip excites.
Fig. 3: by red AgInS
2quantum dot-PMMA composite luminescent material mates with gold-tinted Ce:YAG monocrystalline and is used for GaN white light LEDs schematic diagram.
Fig. 4: by gold-tinted AgInS
2quantum dot-PMMA composite luminescent material in order to replace Ce:YAG monocrystalline, and mates for encapsulating white light LEDs schematic diagram with GaN chip.
Fig. 5: by red yellowish green trichromatism AgInS
2quantum dot-PMMA composite luminescent material and GaN chip carry out mating for encapsulating white light LEDs schematic diagram.
(5) embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are described in detail: the present embodiment is implemented under premised on technical solution of the present invention, given detailed embodiment and process, are further illustrate of the present invention, instead of limit the scope of the invention.
Embodiment 1:AgInS
2the preparation (orange light) of quantum dot
The first step, takes 16.8mg (0.1mmol) AgNO
3, 88.7mg (0.4mmol) InCl
3, 170.8mg (0.6mmol) oleic acid and 609.2mg (3mmol) Dodecyl Mercaptan be placed in the three-necked bottle of 100mL, and add 8mL octadecylene solvent.
Second step, takes 26.1mg (0.8mmol) sulphur powder, is dissolved in 2mL oleyl amine, and is placed in 50 DEG C of water-baths and makes sulphur powder fully be dissolved in oleyl amine.
3rd step, under the condition of magnetic agitation and argon shield, is heated to 60 DEG C and keeps 30min, continue subsequently to be warming up to 110 DEG C, after stablize 2min, inject the S powder that second step is dissolved in oleyl amine, beginning timing by the precursor solution in the first step.
4th step is 30min sampling in the reaction times.Get 0.5mL reaction solution to be dissolved in 0.5mL normal hexane, prepare AgInS
2quantum dot solution.
5th step, the AgInS obtained in the 4th step
2add 3mL dehydrated alcohol in quantum dot, be placed in the centrifugal 5min of 8000rpm, after being gone by supernatant liquor, add the AgInS after the purification of 2mL n-hexane dissolution gained
2quantum dot sample, obtains the AgInS that concentration is 0.0025mmol/mL
2quantum dot solution saves backup.
The AgInS that 30min sampling obtains
2the fluorescence emission wavelengths of quantum dot is 621nm.
Embodiment 2:AgInS
2the preparation (ruddiness) of quantum dot
The feed molar ratio of selected precursor A g:In:Zn is 1:2:2, namely takes 17.6mg (0.1mmol) AgNO
3, 44.8mg (0.2mmol) InCl
3, 27.6mg (0.2mmol) ZnCl
2, selected implantation temperature is 170 DEG C, and other reaction conditionss, with embodiment 1, obtain the AgInS that concentration is 0.0025mmol/mL
2quantum dot solution saves backup.The AgInS that 30min sampling obtains
2the fluorescence emission wavelengths of quantum dot is 658nm.
Embodiment 3:AgInS
2the preparation (gold-tinted) of quantum dot
The feed ratio changing precursor A g:In:Zn is 1:5:5, takes 6.9mg (0.04mmol) AgNO
3, 44.5mg (0.2mmol) InCl
3, 27.5mg (0.2mmol) ZnCl
2, other reaction conditionss, with embodiment 2, obtain the AgInS that concentration is 0.0025mmol/mL
2quantum dot solution saves backup.The AgInS that 30min sampling obtains
2the fluorescence emission wavelengths of quantum dot is 572nm.
Embodiment 4:AgInS
2the preparation (green glow) of quantum dot
The feed ratio of mixing changing precursor A g:In:Zn is 1:10:10, takes 3.5mg (0.02mmol) AgNO
3, 44.5mg (0.2mmol) InCl
3, 27.5mg (0.2mmol) ZnCl
2, other reaction conditionss, with embodiment 2, obtain the AgInS that concentration is 0.0025mmol/mL
2quantum dot solution saves backup.The AgInS that 30min sampling obtains
2the fluorescence emission wavelengths of quantum dot is 533nm.
Embodiment 5:AgInS
2it is the original position mass polymerization (quantum dot-doped amount is 0.3mL) of quantum dot-PMMA recombination luminescence block materials
The first step: the reaction times in Example one is 30min, concentration is the AgInS of 0.0025mmol/mL
2quantum dot solution 0.30mL, adds 0.05mL silane coupling agent MPS thereupon, carries out modification to it.
Second step: take 0.5g methyl methacrylate (MMA:100.12, CP 98%, specific gravity 0.936) and be placed in glassware, add 0.003g initiator Diisopropyl azodicarboxylate (AIBN), concussion makes initiator dissolve slightly.
3rd step: the quantum dot solution of MPS modification in the first step is joined in above-mentioned MMA solution, be placed in 85 DEG C of oil baths and carry out prepolymerization, pour in mould after reaching certain viscosity (about 15min), and be placed in 50 DEG C of baking ovens and heat-treat, take out demoulding polishing after 24h and obtain AgInS
2-PMMA composite luminescent material.
As shown in Figure 1, gained matrix material highly transparent, effectively can be excited by GaN blue chip, launch orange light.
Embodiment 6:AgInS
2it is the original position mass polymerization (quantum dot-doped amount is 0.05 ~ 0.20 mL) of quantum dot-PMMA recombination luminescence block materials
The first step: the reaction times in Example 1 is 30min, concentration is the AgInS of 0.0025mmol/mL
2quantum dot solution 0.05 ~ 0.20mL, adds 0.05mL silane coupling agent MPS thereupon, carries out modification to it.
Second step: take 0.5g methyl methacrylate (MMA:100.12, CP 98%, specific gravity 0.936) and be placed in glassware, add 0.003g initiator Diisopropyl azodicarboxylate (AIBN), concussion makes initiator dissolve slightly.
3rd step: the quantum dot solution of MPS modification in the first step is joined in above-mentioned MMA solution, be placed in 85 DEG C of oil baths and carry out prepolymerization, pour in mould after reaching certain viscosity (about 15min), and be placed in 50 DEG C of baking ovens and heat-treat, take out demoulding polishing after 24h and obtain AgInS
2-PMMA composite luminescent material.
As shown in Figure 1, gained matrix material effectively can be excited by GaN blue chip, and along with the increase of quantum dot-doped amount, the faint red shift of glow peak of gained matrix material, luminous intensity strengthens.
Embodiment 7:AgInS
2it is the original position mass polymerization (silane coupling agent consumption is 0 ~ 0.1mL) of quantum dot-PMMA recombination luminescence block materials
The first step: the reaction times in Example one is 30min, concentration is the AgInS of 0.0025mmol/mL
2quantum dot solution 0.30mL, adds 0 ~ 0.1mL silane coupling agent MPS thereupon, carries out modification to it.
Second step: take 0.5g methyl methacrylate (MMA:100.12, CP 98%, specific gravity 0.936) and be placed in glassware, add 0.003g initiator Diisopropyl azodicarboxylate (AIBN), concussion makes initiator dissolve slightly.
3rd step: the quantum dot solution of MPS modification in the first step is joined in above-mentioned MMA solution, be placed in 85 DEG C of oil baths and carry out prepolymerization, pour in mould after reaching certain viscosity (about 15min), and be placed in 50 DEG C of baking ovens and heat-treat, take out demoulding polishing after 24h and obtain AgInS
2-PMMA composite luminescent material.
Be the transmittance curve figure of different silane coupling agent consumption gained matrix material as shown in Figure 2 a.Fig. 2 b is depicted as the luminous spectrogram of different silane coupling agent consumption gained matrix materials under GaN chip excites, as can be seen from the figure, when the consumption of silane coupling agent is 0, gained matrix material is not luminous, along with the increase of silane coupling agent consumption, matrix material luminosity first strengthens and then weakens to some extent.
Embodiment 8
Respectively with the reaction times that embodiment 2 is obtained be 30min, concentration is the AgInS of 0.0025mmol/mL
2the AgInS that quantum dot solution alternative embodiment 1 is obtained
2quantum dot solution, other reaction conditionss, with embodiment 5, obtain AgInS
2-PMMA composite luminescent material.Gained matrix material highly transparent, effectively can be excited by GaN blue chip, red-emitting.
Embodiment 9
Respectively with the reaction times that embodiment 3 is obtained be 30min, concentration is the AgInS of 0.0025mmol/mL
2the AgInS that quantum dot solution alternative embodiment 1 is obtained
2quantum dot solution, other reaction conditionss, with embodiment 5, obtain AgInS
2-PMMA composite luminescent material.Gained matrix material highly transparent, effectively can be excited by GaN blue chip, launches gold-tinted.
Embodiment 10
Respectively with the reaction times that embodiment 4 is obtained be 30min, concentration is the AgInS of 0.0025mmol/mL
2the AgInS that quantum dot solution alternative embodiment 1 is obtained
2quantum dot solution, other reaction conditionss, with embodiment 5, obtain AgInS
2-PMMA composite luminescent material.Gained matrix material highly transparent, effectively can be excited by GaN blue chip, transmitting green light.
Embodiment 11
By AgInS obtained for embodiment 5,8,9,10
2quantum dot-PMMA composite luminescent material makes bulk, it is mated with GaN chip, is packaged into white light LEDs.
The photoelectric parameter testing gained after ruddiness, orange light, gold-tinted, green glow matrix material mate with GaN chip is respectively shown in following table 1.As can be seen from the table, when test current is 20mA, matrix material all can be excited by blue light GaN chip.
Gained photoelectric parameter is tested after table 1 one-color fluorescence matrix material mates with blue chip
Embodiment 12
For optimizing the performance of light source further, by there is different colours luminescence matrix material simultaneously and blue chip, to the white light source that colour temperature is low, colour rendering index is high, light efficiency is high can be obtained.
By the AgInS obtained according to embodiment 5,8,9,10 method
2quantum dot-PMMA composite luminescent material makes bulk, gets two or three not homochromy AgInS
2mate with GaN blue chip again after the block composite luminescent material coupling of quantum dot-PMMA, be packaged into white light LEDs.The photoelectric parameter of matching way and corresponding white light LEDs is in table 2:
Gained photoelectric parameter is tested after table 2 multicolor fluorescence composite material combination mates with blue chip
As shown in Table 2, after being mated with assorted luminescent material by red fluorescence block materials, the performance of gained light source improves, and colour temperature reduces, and colour rendering index is improved, and light efficiency also enhances, and shows to prepare gained AgInS
2the potential application of-PMMA composite luminescent material in white light LEDs, and red fluorescence obtains white light to compound plays important effect.This result indicates the AgInS preparing gained
2be that quantum dot-PMMA composite luminescent material not only as the supplementary luminescent layer of red light district in white light LEDs, can will have the AgInS of assorted fluorescence simultaneously
2-PMMA composite luminescent material is as the structure building novel white-light LED.
In addition, can by experiment gained AgInS
2-PMMA composite luminescent material mates with commercially available yellow fluorescent powder or monocrystalline, the performance of further raising LED, by the matching parameter of the preparation technology and luminescent material and GaN chip that optimize material further, be expected to break the patent limitation to white-light LED structure such as Japan, the U.S., improve China to the integral innovative ability of white light LEDs.
Claims (6)
1. an AgInS
2quantum dot/PMMA composite luminescent material, its preparation method comprises the steps:
(1) by monokaryon AgInS
2quantum dot is dissolved in normal hexane and obtains the quantum dot solution that concentration is 0.002 ~ 0.003mmol/mL;
(2) add (3-mercaptopropyi) Trimethoxy silane in the quantum dot solution obtained in step (1) and, to its modifying surface, obtain modified quantum dot solution; Wherein the volume ratio that feeds intake of (3-mercaptopropyi) Trimethoxy silane and quantum dot solution is 1:1 ~ 10;
(3) get the modified quantum dot solution that step (2) obtains to mix according to volume ratio 1:1 ~ 20 with methyl methacrylate, under initiator effect, carry out polyreaction, obtain AgInS
2quantum dot/PMMA composite luminescent material.
2. AgInS as claimed in claim 1
2quantum dot/PMMA composite luminescent material, is characterized in that: the volume ratio that feeds intake of (3-mercaptopropyi) Trimethoxy silane and quantum dot solution is 1:2 ~ 5.
3. AgInS as claimed in claim 2
2quantum dot/PMMA composite luminescent material, is characterized in that: the volume ratio that feeds intake of (3-mercaptopropyi) Trimethoxy silane and quantum dot solution is 1:3 ~ 5.
4. the AgInS as described in one of claims 1 to 3
2quantum dot/PMMA composite luminescent material, is characterized in that: the polyreaction described in step (3) adopts two-stage polymerization method, and comprise prepolymerization and Post isothermal treatment, prepolymerization temperature is 70 ~ 90 DEG C, prepolymerization time 10 ~ 30min; Post isothermal treatment temperature is at 50 ~ 70 DEG C, and the Post isothermal treatment time is 24 ~ 72h.
5. AgInS as claimed in claim 1
2quantum dot-PMMA composite luminescent material is preparing the application in white light LEDs, it is characterized in that described application is specially: by AgInS
2quantum dot-PMMA composite luminescent material makes bulk, the AgInS not homochromy by one or more
2the block composite luminescent material of quantum dot-PMMA mates with GaN chip, is packaged into white light LEDs.
6. AgInS as claimed in claim 1
2quantum dot-PMMA composite luminescent material is preparing the application in white light LEDs, it is characterized in that described application is specially: by AgInS
2quantum dot-PMMA composite luminescent material makes bulk, the AgInS not homochromy by one or more
2quantum dot-PMMA composite luminescent material mates with Ce:YAG monocrystalline, GaN chip, is packaged into white light LEDs.
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