CN105304799B - A kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material - Google Patents
A kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material Download PDFInfo
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- 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
- H01L33/48—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 body packages
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Abstract
The present invention is used as the LED encapsulation material of innovation by the use of metal nanometre cluster advanced luminescent material, realize constructing for high performance LED, and in particular to based on glow color is controllable, the LED of hyperfluorescence, the novel encapsulated material of the metal nanometre cluster package assembly of high stability is constructed.The method that more particularly to a kind of quick, simple, safety, high yield prepare high performance fluorescence metal nano-cluster package assembly：Be reduced directly by thiol molecule and stable metal nanometre cluster it is pre-prepared, ingredient proportion, reaction time and temperature between species, thiol molecule species, reactant by adjusting source metal etc., realize the nano-cluster package assembly of different glow colors, LED encapsulation material is eventually used for, constructing for high performance lED light source is realized.The present invention is easy to operate during preparation, assembling, encapsulation, dangerous small, and with good experimental repeatability.
Description
Technical field
The invention belongs to LED preparing technical fields, and in particular to one kind is prepared different based on metal nanometre cluster encapsulating material
Glow color LED method.
Background technology
Light emitting diode, abbreviation LED is referred to as forth generation light source, with energy-saving and environmental protection, safety, long lifespan, low-power consumption,
The features such as easy maintenance, it can be widely applied to the fields such as various instructions, display, decoration, liquid crystal screen backlight, illumination.At present,
The preparation for the commercial LED that in the market is produced now is broadly divided into two processes：(1) electroluminescent hair is prepared using InGaN/GaN materials
Light is the LED lamp (360-460nm) of blue light；(2) wick is packaged using the material with photoluminescent property.Its working machine
System can be simply interpreted as：When LED is powered, the blue light that wick is sent can excite the fluorescent material in encapsulating material, be excited production
Raw fluorescence and the blue light not being predominantly absorbed are combined, and difference is gone out by the encapsulating material final production for choosing different photoluminescent properties
Color LED light source.
In the development process of LED/light source, very crucial part is exactly the select permeability of the fluorescence encapsulating material of high-quality.It is excellent
The fluorescence encapsulating material of matter plays conclusive effect for final LED performance.Such as, stability, response time, color
Colour rendering, cost price, service life etc..At present, commercial the most frequently used fluorescence encapsulating material concentrates on the phosphorus of terres rares
Body of light material.However, the granular sensation of this material is stronger, the scattering of light is easily caused in encapsulation process so that luminous efficiency
Reduction.Meanwhile, the cost price of terres rares phosphor is few compared with high, earth storage level, and these shortcomings significantly limit LED hair
Exhibition.So, develop new fluorescence encapsulating material and increasingly obtain everybody concern and attention.
At present, fluorescence metal nano-cluster, the sight and of people is gradually entered into as a kind of new luminescent material
It is fast-developing.Metal nanometre cluster due to very small dimensions (<The luminosity of quasi-molecule state caused by 2nm).It is luminous with size
Dependence, the advantages of fluorescence quantum yield is high, while the price of the relative moderate of metal material and plentiful earth storage level, are
LED encapsulation material provides a kind of new selection.
The content of the invention
It is an object of the invention to provide a kind of side that different glow color LED are prepared based on metal nanometre cluster encapsulating material
Method.The present invention is by developing a kind of method that quick, high yield prepares high-performance fluorescence metal nano-cluster encapsulating material, to it from group
Dress behavior is regulated and controled, and realizes the metal nanometre cluster package assembly of stability height, color controllable, high fluorescence efficiency, for LED envelopes
Dress, realizes that New LED is constructed.
The LED light source chip that the present invention is used is commercial GaN base LED chip (transmitting peak position center is in 365nm).
Specifically, step of the invention is as follows：
1) preparation of fluorescence metal nano-cluster：At room temperature, metal salt is dissolved in organic solvent, preparing metal presoma is molten
Liquid, concentration range is 0.01~0.08mol/L；Then, under magnetic stirring, alkyl hydrosulfide reducing agent is added thereto, metal
The consumption mol ratio of salt and alkyl hydrosulfide is 1~8：5, (normal temperature, normal pressure) stirs 3~30min under temperate condition, obtains alkyl sulfide
The stable fluorescence metal nano-cluster solution of alcohol；
2) preparation of fluorescence metal nano-cluster encapsulating material：By the stable fluorescence metal nano-cluster solution of alkyl hydrosulfide 20
0.5~2h is handled at~100 DEG C, obtains relying on package assembly (including spherical, different-thickness flake-assembly mode structure, banding group
Assembling structure) different photoluminescent properties (green, yellow, orange or red light) fluorescence metal nano-cluster encapsulating material；For
The regulation and control of fluorescence metal nano-cluster package assembly, the nanoscale driving force being related to is mainly dredging between nano-cluster surface ligand
Aqueous phase interaction.Because the package assembly of different structure has distances different between different degree of compacting and interior metal, these
Factor directly affects the stability of fluorescence nano cluster, glow color, fluorescence quantum yield, so may finally be according to target fluorescent
Property realizes the controllable of encapsulating material performance by the assembling control of metal nanometre cluster；
3) preparation of the LED based on fluorescence metal nano-cluster encapsulating material：Fluorescence metal nano-cluster encapsulating material is air-dried
Powdered processing, then uniform with the blending of polydimethylsiloxane prepolymer thing, polydimethylsiloxane prepolymer thing and encapsulating material
Mass ratio be 15：5~8, it is then coated with GaN base LED chip, 2~5h is handled at 60~80 DEG C and realizes polymerisation,
Finally obtain packaged LED.Here it is possible to realize LED by the single metal nano clustered materials for choosing different glow colors
Preparation, again may be by different colours different types of metal nano clustered materials pass through the mixing of different ratio, realize
Color of object LED preparation.
Preferably, metal salt is the organic salt or inorganic salts of precious metal element or transition metal.
Preferably, metal is one kind in Pt, Ag, Au or Cu；Can be specifically CuCl2、CuBr、CuBr2、CuSO4、
Or Cu (C5H7O2)2One kind in (acetylacetone copper).
Preferably, organic solvent is benzyl ether, diphenyl ether, 1- octadecylenes or atoleine.
Preferably, reducing agent is the alkyl hydrosulfide (HSC of different C chain lengthsnH2n+1), wherein, n is 4~16 integer.
Preferably, reducing agent is HSC16H33(hexadecyl mercaptan), HSC12H25(lauryl mercaptan) or HSC8H17It is (pungent
Mercaptan).
Preferably, different glow colors can be realized by choosing the single metal nano clustered materials of different photoluminescent properties
LED preparation, the different types of metal nano clustered materials that again may be by different photoluminescent properties pass through the mixed of different ratio
Close, realize that (the transmitting light of LED chip excites the encapsulation of different photoluminescent properties as excitation source for the LED of color of object preparation
Material, realizes the preparation of LED modules with different colors).
Advantage is as follows compared with prior art by the present invention：
The raw material of the present invention all is from the chemical reagent of commercialization, it is not necessary to further processing, directly according to certain
Stoichiometric proportion, which is mixed, can obtain fluorescence metal nano-cluster.Because the package assembly of different structure has different compact
Spend and directly affect the stability of fluorescence nano cluster, glow color, fluorescence volume again different distances between interior metal, these factors
Sub- yield, so subsequent assembly and regulation process, it is only necessary to according to target capabilities such as the glow colors finally needed, changes metal
The experiment parameters such as rate of charge, reaction time and temperature between source category, reactant.So, whole assembly and regulation process
It is easy to operate, it is dangerous small, it is adapted to be prepared on a large scale.
Brief description of the drawings
Fig. 1 is the TEM that fluorescence color prepared by embodiment 1 is orange-red spherical package assembly Cu nano-cluster encapsulating materials
Picture (a) and be the wavelength 650nm at orange-red LED light spectrogram (b), luminous peak position as lighting of preparing of encapsulating material.
Fig. 2 is that fluorescence color prepared by embodiment 2 is lurid laminar package assembly Cu nano-cluster encapsulating materials
TEM pictures (a) and be the wavelength at lurid LED light spectrogram (b), luminous peak position as lighting of preparing of encapsulating material
558nm。
Fig. 3 is the TEM for the slab-like package assembly Cu nano-cluster encapsulating materials that fluorescence color prepared by embodiment 3 is green
Picture (a) and as LED light spectrogram (b) of the lighting of preparing of encapsulating material for green, the wavelength 524nm at luminous peak position.
Fig. 4 is the TEM figures for the wire package assembly Cu nano-cluster encapsulating materials that fluorescence color prepared by embodiment 4 is green
Piece (a) and as LED light spectrogram piece (b) of the lighting of preparing of encapsulating material for green, the wavelength 522nm at luminous peak position.
Fig. 5 is the TEM figures that fluorescence color prepared by embodiment 5 is red flake-assembly mode structure Au nano-cluster encapsulating materials
Piece (a) and be the wavelength 664nm at red LED light spectrogram (b), luminous peak position as lighting of preparing of encapsulating material.
Fig. 6 is the TEM figures that fluorescence color prepared by embodiment 6 is red flake-assembly mode structure Au nano-cluster encapsulating materials
Piece (a) and be the wavelength 658nm at red LED light spectrogram (b), luminous peak position as lighting of preparing of encapsulating material.
Fig. 7 is that fluorescence color prepared by embodiment 7 is orange-red spherical package assembly Cu nano-clusters encapsulating material, fluorescence
The slab-like package assembly that color is lurid laminar package assembly Cu nano-clusters encapsulating material and fluorescence color is green
Cu nano-cluster encapsulating materials, take quality 3mg, 1mg and 3mg to be lighted after being blended as prepared by encapsulating material to be white respectively
The spectrogram of LED/light source, emission spectrum is shown in 450-750nm visual fields well good transmitting.
Fig. 8 be embodiment 8 prepare fluorescence color be lurid laminar package assembly Cu nano-clusters encapsulating material and
Fluorescence color is green slab-like package assembly Cu nano-cluster encapsulating materials, and in hexichol ethereal solution, reducing agent is ten
Dialkyl group mercaptan, the red sheet package assembly Au nano-cluster encapsulating materials prepared take quality 3mg, 1mg and 3mg to be total to respectively
Mixed soldier is shown in 450- well as spectrogram of the lighting of preparing of encapsulating material for the LED/light source of white, emission spectrum
There is good transmitting 750nm visual fields.
Embodiment
With reference to embodiment, the present invention is further elaborated, rather than to be limited the invention with this.It is real
Apply example 1：
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O (metal precursors
Solution concentration is 0.01mol/L), under room temperature magnetic agitation, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for
3min, you can obtain the stable Cu nano-clusters of lauryl mercaptan.0.5h is stirred in maintenance at room temperature, can obtain diameter about
The spherical package assembly encapsulating material of 200nm Cu nano-clusters, the spherical package assembly encapsulating material of this Cu nano-clusters has
Fluorescent red-orange.Eventually pass centrifugation, drying, (product about 30mg, powder mesh number is 400), to take 5mg Cu for powdered processing
Piece package assembly encapsulating material, (mass ratio is 1 to the prepolymer blending with 15mg dimethyl silicone polymer:3), it is then coated with
In the LED chip of GaN base, it polymerize in 2h at 60 DEG C, that is, obtains packaged light as the LED/light source of orange light.
Embodiment 2：
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 1.6mmol CuCl2·2H2O (metal precursors
Solution concentration is 0.08mol/L), under room temperature magnetic agitation, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for
3min, you can obtain the stable Cu nano-clusters of lauryl mercaptan.1h is stirred in maintenance at room temperature, can obtain the thin of Cu nano-clusters
Piece (long 50~400nm, wide 50~400nm, thickness<5nm) package assembly encapsulating material, the thin slice assembling knot of this Cu nano-clusters
Structure encapsulating material has pale yellow fluorescent.Centrifugation, drying, powdered processing (product about 100mg) are eventually passed, takes 5mg's
The thin slice package assembly encapsulating material of Cu nano-clusters, (mass ratio is 1 to the prepolymer blending with 15mg dimethyl silicone polymer:
3), it is then coated with the LED chip of GaN base, polymerize in 5h at 80 DEG C, that is, obtains packaged light as pale yellow coloured light
LED/light source.
Embodiment 3：
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O, in room temperature magnetic force
Under stirring, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for 3min, you can obtain the stable Cu of lauryl mercaptan
Nano-cluster.Maintain 3h stir process at 50 DEG C, can obtain Cu nano-clusters sheet (long 100~400nm, wide 100~400nm,
Thickness>5nm) package assembly encapsulating material, the sheet package assembly encapsulating material of this Cu nano-clusters has green fluorescence.Finally
By centrifugation, dry, powdered processing (product about 30mg), 5mg Cu piece package assembly encapsulating materials are taken, it is poly- with 15mg
(mass ratio is 1 for the prepolymer blending of dimethyl siloxane:3), it is then coated with the LED chip of GaN base, it is poly- in 5h at 60 DEG C
Close, that is, obtain packaged light as the LED/light source of green light.
Embodiment 4：
5mL benzyl ether is added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O, is stirred in room temperature magnetic force
Mix down, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for 10min, you can obtain the stable Cu of lauryl mercaptan
Nano-cluster.1h stir process at 100 DEG C is maintained, the wire (wide 5~20nm, long 100~1000nm) of Cu nano-clusters can be obtained
Package assembly encapsulating material, this Cu pieces package assembly encapsulating material has green fluorescence.Eventually pass centrifugation, drying, powder
Change handles (product about 30mg), takes 5mg Cu piece package assembly encapsulating materials, the pre-polymerization with 15mg dimethyl silicone polymer
(mass ratio is 1 for thing blending:3), it is then coated with the LED chip of GaN base, polymerize in 2h at 80 DEG C, that is, obtain packaged
Light as the LED/light source of green glow.
Embodiment 5：
5mL benzyl ether is added in 20mL beaker, and dissolved with 0.4mmol HAuCl4·4H2O, is stirred in room temperature magnetic force
Mix down, the lauryl mercaptan for being dropwisely added 2mmol is kept stirring for 30min, you can obtain the stable Au of lauryl mercaptan
Nano-cluster.1h stir process at 100 DEG C is maintained, the sheet (roomy about 150nm, long 20~1000nm) of Au nano-clusters can be obtained
Package assembly encapsulating material, this Au pieces package assembly encapsulating material has red fluorescence.Eventually pass centrifugation, drying, powder
Change handles (product about 50mg), takes 5mg Au piece package assembly encapsulating materials, the pre-polymerization with 15mg dimethyl silicone polymer
(mass ratio is 1 for thing blending:3), it is then coated with the LED chip of GaN base, in polymerizeing 2h at 60 DEG C, that is, obtains packaged
Light as the LED/light source of feux rouges.
Embodiment 6：
5mL benzyl ether is added in 20mL beaker, and dissolved with 0.4mmol HAuCl4·4H2O, is stirred in room temperature magnetic force
Mix down, the hexadecyl mercaptan for being dropwisely added 2mmol is kept stirring for 30min, you can obtain the stable Au of lauryl mercaptan
Nano-cluster.Maintain 1h stir process at 100 DEG C, can obtain Au nano-clusters sheet (roomy 30~150nm, it is long by 50~
800nm) package assembly encapsulating material, this Au pieces package assembly encapsulating material has red fluorescence.Eventually pass centrifugation, do
Dry, powdered processing (product about 50mg), takes 5mg Au piece package assembly encapsulating materials, the polydimethylsiloxanes with 15mg
(mass ratio is 1 for the prepolymer blending of alkane:3), it is then coated with the LED chip of GaN base, polymerize in 2h at 60 DEG C, that is, obtain
Packaged lights as the LED/light source of feux rouges.
Embodiment 7：
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O, in room temperature magnetic force
Under stirring, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for 3min, you can obtain the stable Cu of lauryl mercaptan
Nano-cluster.10min is stirred in maintenance at room temperature, can obtain the diameter about 200nm spherical package assembly package material of Cu nano-clusters
Material, this Cu pieces assembly has fluorescent red-orange.
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O, in room temperature magnetic force
Under stirring, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for 3min, you can obtain the stable Cu of lauryl mercaptan
Nano-cluster.1h is stirred in maintenance at room temperature, can obtain thin slice (the long 50~400nm, wide 50~400nm, thickness of Cu nano-clusters<
5nm) package assembly, this Cu pieces package assembly encapsulating material has pale yellow fluorescent.
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O, in room temperature magnetic force
Under stirring, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for 3min, you can obtain the stable Cu of lauryl mercaptan
Nano-cluster.Maintain 3h stir process at 50 DEG C, can obtain Cu nano-clusters sheet (long 100~400nm, wide 100~400nm,
Thickness>5nm) package assembly, this Cu pieces package assembly encapsulating material has green fluorescence.
Eventually pass centrifugation, drying, powdered processing, take respectively the spherical package assembly encapsulating materials of the orange red Cu of 3mg,
The light yellow Cu thin slices package assembly encapsulating materials of 1mg and 3mg green Cu sheet package assembly encapsulating materials, the poly- diformazan with 20mg
The prepolymer blending of radical siloxane, is then coated with the LED chip of GaN base, polymerize in 2h at 60 DEG C, that is, obtain packaged
Light as the LED/light source of white light.
Embodiment 8：
5mL benzyl ether is added in 20mL beaker, and dissolved with 0.4mmol HAuCl4·4H2O, is stirred in room temperature magnetic force
Mix down, the lauryl mercaptan for being dropwisely added 2mmol is kept stirring for 30min, you can obtain the stable Au of lauryl mercaptan
Nano-cluster.1h stir process at 100 DEG C is maintained, the flake-assembly mode construction packages material of Au nano-clusters can be obtained (roomy about
150nm, long 20~1000nm), this Au pieces assembly has red fluorescence.
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O, in room temperature magnetic force
Under stirring, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for 3min, you can obtain the stable Cu of lauryl mercaptan
Nano-cluster.1h is stirred in maintenance at room temperature, can obtain thin slice group (the long 50~400nm, wide 50~400nm, thickness of Cu nano-clusters
<5nm) package material, this Cu pieces package assembly encapsulating material has pale yellow fluorescent.
5mL 1- octadecylenes are added in 20mL beaker, and dissolved with 0.2mmol CuCl2·2H2O, in room temperature magnetic force
Under stirring, the lauryl mercaptan for being dropwisely added 1mmol is kept stirring for 3min, you can obtain the stable Cu of lauryl mercaptan
Nano-cluster.Maintain 3h stir process at 50 DEG C, can obtain Cu nano-clusters sheet package assembly encapsulating material (it is long by 100~
400nm, wide 100~400nm, thickness>5nm), this Cu pieces package assembly encapsulating material has green fluorescence.
Eventually pass centrifugation, drying, powdered processing, take respectively the spherical package assembly encapsulating materials of the orange red Cu of 3mg,
The light yellow Cu thin slices assembly construction packages materials of 1mg and 3mg green Cu sheet package assembly encapsulating materials, poly- two with 20mg
The prepolymer blending of methylsiloxane, is then coated with the LED chip of GaN base, polymerize in 2h at 60 DEG C, that is, obtain packaged
Light as the LED/light source of white light.
Claims (9)
1. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material, its step is as follows：
1) preparation of fluorescence metal nano-cluster：At room temperature, metal salt is dissolved in organic solvent, preparing metal precursor solution,
Concentration range is 0.01~0.08mol/L；Then, under magnetic stirring, alkyl hydrosulfide reducing agent is added thereto, metal salt with
The consumption mol ratio of alkyl hydrosulfide is 1~8：5,3~30min is stirred under normal temperature and pressure, the stable fluorogold of alkyl hydrosulfide is obtained
Belong to nano-cluster solution；
2) preparation of fluorescence metal nano-cluster encapsulating material：By the stable fluorescence metal nano-cluster solution of alkyl hydrosulfide 20~
0.5~2h is handled at 100 DEG C, obtains relying on the fluorescence metal nano-cluster encapsulating material of the different photoluminescent properties of package assembly；
3) preparation of the LED based on fluorescence metal nano-cluster encapsulating material：Fluorescence metal nano-cluster encapsulating material is air-dried into powder
Change is handled, uniform with the blending of polydimethylsiloxane prepolymer thing, the mass ratio of polydimethylsiloxane prepolymer thing and encapsulating material
For 15：5~8, it is then coated with GaN base LED chip, 2~5h is handled at 60~80 DEG C and realizes polymerisation, is finally obtained
The LED of different glow colors.
2. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 1, its
It is characterised by：Metal salt is the organic salt or inorganic salts of precious metal element or transition metal.
3. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 2, its
It is characterised by：Metal is one kind in Pt, Ag, Au or Cu.
4. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 3, its
It is characterised by：Metal salt is CuCl2、CuBr、CuBr2、CuSO4Or Cu (C5H7O2)2In one kind.
5. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 1, its
It is characterised by：Organic solvent is benzyl ether, diphenyl ether, 1- octadecylenes or atoleine.
6. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 1, its
It is characterised by：The molecular formula of alkyl hydrosulfide is HSCnH2n+1, wherein, n is 4~16 integer.
7. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 1, its
It is characterised by：Reducing agent is HSC16H33、HSC12H25Or HSC8H17。
8. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 1, its
It is characterised by：By choosing the preparation that the single metal nano clustered materials of different photoluminescent properties realize the LED of different glow colors.
9. a kind of method that different glow color LED are prepared based on metal nanometre cluster encapsulating material as claimed in claim 1, its
It is characterised by：By different photoluminescent properties, different types of metal nano clustered materials by the mixing of different ratio, target is realized
The LED of color preparation.
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| EP3411334B1 (en) * | 2016-02-04 | 2021-05-26 | ExxonMobil Chemical Patents Inc. | Polyoxometalates comprising noble metals and corresponding metal clusters |
| CN105602554B (en) * | 2016-03-09 | 2018-01-05 | 吉林大学 | Copper nano-cluster self assembly fluorescent material, preparation method and its application in LED encapsulation of gold doping |
| CN106590635B (en) * | 2016-12-07 | 2019-03-26 | 吉林大学 | Yellow light or feux rouges copper cluster assembly fluorescent material, preparation method and its preparing the application in fine copper cluster white light LED part |
| CN107338042B (en) * | 2017-07-17 | 2019-07-09 | 吉林大学 | Full color emission copper cluster assembly fluorescent material, preparation method and its application in white light LED part of solvent regulation |
| CN110579828A (en) * | 2019-08-08 | 2019-12-17 | 深圳市华星光电技术有限公司 | metal dot color filter, manufacturing method thereof and liquid crystal display device |
| CN111014716B (en) * | 2019-12-10 | 2021-08-20 | 大连理工大学 | Method for macroscopic preparation of AIE copper nanoclusters by cysteamine |
| CN111909295B (en) * | 2020-07-01 | 2022-07-26 | 北京大学深圳研究生院 | Preparation method and application of photosensitization material |
| CN112080275B (en) * | 2020-09-21 | 2021-08-27 | 吉林大学 | Color temperature adjustable white light emitting copper cluster assembly fluorescent material and preparation method thereof |
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| CN101457403A (en) * | 2008-12-22 | 2009-06-17 | 中国科学院长春应用化学研究所 | Green synthetic method of controllable dimension semi-conductor nano cluster and nanocrystalline |
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