CN109825281A - A kind of processing method of quanta point material, high stable quanta point material and application - Google Patents
A kind of processing method of quanta point material, high stable quanta point material and application Download PDFInfo
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Abstract
The invention discloses a kind of processing method of quanta point material, high stable quanta point material and applications, contain element sulphur in the surface of the quanta point material, the processing method of the quanta point material obtains metal salt stock solution the following steps are included: (1) takes metal salt to be scattered in solvent under an inert atmosphere；(2) the metal salt stock solution is added under an inert atmosphere and is reacted for the dispersion liquid for taking or preparing quanta point material.The present invention contains the quantum dot of element sulphur for surface, it is reacted by metal salt with the element sulphur of quantum dot surface, introduce a kind of metal sulfide cation of strong binding force, terminate quantum dot can continued growth reactivity, improve the chemical stability of quantum dot, quantum dot fluorescence yield with higher is being illuminated with display field with good application prospect.
Description
Technical field
The present invention relates to material processing technical fields, processing method, high stable more particularly, to a kind of quanta point material
Quanta point material and application.
Background technique
Colloidal semiconductor quantum dot (Colloidal quantum dots, QDs) is a kind of with high efficiency luminescence efficiency, height
The nano luminescent material of stability, includes that colour purity is good, luminous efficiency is high, light emission luminance is high, light is steady compared to Conventional luminescent material
Qualitative strong and luminous color is continuously adjustable, is widely used in highly effective quantum point luminescent diode (Quantum Dots Light
Emitting Diode, QLEDs) novel illumination and display technology, there is high-luminous-efficiency, few energy consumption, high stability and length
Many advantages, such as service life is illumination and display technology most with prospects.
There are mainly two types of the technology paths of compound Colloidal Quantum Dots preparation at present: first is that preparing in water phase, that is, distinguishing
The water phase precursor liquid for preparing nonmetalloid and metallic element, hybrid reaction generates quantum dot under oxygen-free environment；Second is that
It is prepared in organic system, i.e., in the organic solvent environment with Coordinate property, utilizes metallo-organic compound and nonmetallic member
Plain hybrid reaction, grows into nano particle.The above existing colloid method prepares fluorescence quantum, has synthesis temperature lower, instead
The higher feature of activity is answered, prepares fluorescence quantum conducive to efficient batch.But fluorescence quantum is in the preparation, generallys use cooling
Stop the growth of quantum dot with the mode for reducing reactant concentration, quantum dot own face still has compared with high reaction activity, makes
It is poor at itself chemical stability, lead to purifying, using processing and when device application work, it will usually due to use solvent or
Atmosphere is impure, impurity introduce and by fluorescence quantum adsorption, and then cause fluorescence quantum formed non-radiative recombination routes,
Its fluorescent yield is reduced, to be dfficult to apply in the white light QLEDs of efficient stable, constrains it in illumination and display field
Application.In addition, fluorescence quantum is when with encapsulation glue hybrid package, monomer active site occurs under the action of catalyst
Crosslinking, active site are easy that ligand exchange occurs with quantum dot, will also result in the decline of fluorescence quantum yield.
For the stability for improving quantum dot, the prior art mainly uses the protection thinking of outer enclosure to avoid water oxygen etc. miscellaneous
The erosion of confrontation quantum dot, it is lazy using high-purity in the application generally by the forms such as polymer overmold and exterior barrier encapsulation
Property atmosphere avoid causing fluorescence to fail quantum dot, but the mode of said external encapsulation is there are cumbersome, after encapsulation
Quantum point grain diameter can significantly increase, the problem of outer enclosure Effect of Materials Internal Quantum point fluorescent yield.
Summary of the invention
Aiming at the shortcomings in the prior art, the object of the present invention is to provide a kind of processing methods of quanta point material, Gao Wen
Determine quanta point material and application, the quantum dot of element sulphur is contained for surface, there is height by metal salt and quantum dot surface
The reaction of reactivity element sulphur introduces a kind of metal sulfide cation of strong binding force, and terminating quantum dot can continued growth
Reactivity improves the chemical stability of quantum dot, quantum dot fluorescence yield with higher.
The technical solution used in the present invention is:
The present invention provides a kind of processing method of quanta point material, and element sulphur is contained on the surface of the quanta point material, packet
Include following steps:
(1) it takes metal salt to be scattered in solvent under an inert atmosphere, obtains metal salt stock solution；
(2) the metal salt stock solution is added under an inert atmosphere and carries out instead for the dispersion liquid for taking or preparing quanta point material
It answers.
Used the purpose of inert atmosphere in step (1) is that protection reactant is not oxidized.In order to equal more easily by metal salt
It is even to be scattered in solvent, it can specifically be selected according to the metal salt of addition using decentralized processing is carried out under heating conditions
Heating temperature is selected, if heating temperature can be 20~500 DEG C.
The thinking of the application is that the quanta point material for containing element sulphur for surface is handled, can be existing above-mentioned
Metal salt stock solution is directly added into after quantum dot preparation to complete the treatment process, to save point for individually preparing quanta point material
The process of dispersion liquid and the efficiency prepared conducive to raising integral material, can also have the quantum dot prepared to be scattered in solvent with enchashment
It is prepared into the dispersion liquid of quanta point material, is then reacted again with metal salt stock solution.Step (2) is under heating conditions more
Conducive to reacting for quanta point material and metal salt, the temperature of heating depends on the solvent of reaction system, preferably heating temperature range
The upper limit be no more than using solvent boiling spread.
Preferably, the metallic element in the metal salt be selected from I B race, II B race element, V group Ⅴ element, alkaline-earth metal,
At least one of scandium, yttrium and lanthanide series.
Further, the metallic element is selected from least one of silver, mercury, zinc, copper, gold, cadmium, nickel, platinum.
In some preferred embodiments, the metal salt is selected from least one of silver salt, mercury salt, zinc salt.Into one
In the embodiment of step, the silver salt is selected from silver oxide, silver acetate or silver chlorate.
Preferably, the quanta point material is metal sulfide nanocrystalline Colloidal Quantum Dots or surface containing metal sulfide
Nanocrystalline colloid quantum dot.The quanta point material is including but not limited to cadmiumsulfide quantum dot, ZnS quantum dots.
Preferably, the concentration of metal salt is 0.001mmol/L~10mol/L in the metal salt stock solution.
Preferably, the solvent is corrdination type solvent or noncoordinating type solvent；It is preferred that the corrdination type nonpolar solvent is
The acid of carbon atom number >=6, the preferably described noncoordinating type solvent are at least one of carbon atom number >=9 alkane, alkene, ester.
Further, the corrdination type solvent is selected from least one of tetradecylic acid, oleic acid, stearic acid, lauric acid；It is described
Noncoordinating type solvent is selected from least one of atoleine, octadecylene, octadecane.
The present invention also provides a kind of high stable quanta point materials, are obtained by the processing method of above-mentioned quanta point material.
Application of the above-mentioned high stable quanta point material in illumination or display.Pass through the processing method of above-mentioned quanta point material
The quanta point material of acquisition chemical stability with higher, illumination or display field with good application prospect.
Preferably, the application is the application in QLEDs illumination or backlight display.
The beneficial effects of the present invention are:
Fluorescence quantum is in luminescence generated by light application, since quantum dot continues working under high temperature high-energy environment, table
Face is easy to happen photooxidation reaction, is directed to surface and contains for the quantum dot of element sulphur, such as the sulphur member in ZnS quantum dots
Element is easily oxidized to sulfate ion or sulfur dioxide, and quantum-dot structure is caused to be destroyed, and fluorescence quantum yield is caused to reduce.
The present invention provides a kind of processing method of quantum dot, uses and carries out terminating surface of the reaction to reduce quantum dot to quantum dot surface
The quantum dot chemical stability with higher that chemically active thinking obtains processing contains sulphur member specifically to surface
The quantum dot of element, is reacted by metal salt with the element sulphur of quantum dot surface, and a kind of metal vulcanization of strong binding force is introduced
Object cation, can terminate quantum dot can continued growth reactivity, enhance the ability of quantum dot anti-photooxidation, improve
The chemical stability of quantum dot is being illuminated with display field with good application prospect.
Detailed description of the invention
Fig. 1 is in effect example 2 to cadmium selenide/zinc sulphide alloy structure quantum dot fluorescence volume of heat treatment front and back
Son point yield test result figure；
Fig. 2 is the fluorescence in effect example 2 to the quanta point material handled in the embodiment 1 of heat treatment front and back
Quantum dot yield test result figure；
Fig. 3 is the ageing test result figure in effect example 3.
Specific embodiment
It is clearly and completely described below with reference to technical effect of the embodiment to design and generation of the invention, with
It is completely understood by the purpose of the present invention, feature and effect.Obviously, described embodiment is that a part of the invention is implemented
Example, rather than whole embodiments, based on the embodiment of the present invention, those skilled in the art is not before making the creative labor
Other embodiments obtained are put, the scope of protection of the invention is belonged to.
Embodiment 1
The present embodiment provides a kind of high stable quanta point materials, and processing obtains according to the following steps:
(1) it prepares quantum dot dispersion liquid: 0.6g cadmium selenide/zinc sulphide alloy structure quantum dot being taken to disperse under an inert atmosphere
In 15mL oleic acid, save；
(2) it prepares silver oxide stock solution: taking 0.05g silver oxide, 10mL oleic acid is added, is placed in reaction unit and in inertia
Under atmosphere protection range, 90 DEG C are heated to, dispersion obtains silver oxide stock solution；
(3) the quantum dot dispersion liquid in step (1) is placed in reaction unit and under inert protective atmosphere, is warming up to
320 DEG C, the silver oxide stock solution of step (2) preparation is added, uniform stirring dispersion reacts 10min, obtains fluorescence quantum.
Specifically used silver salt is silver oxide in the present embodiment, and the silver salt that actually can be used is including but not limited to oxidation
Silver, silver acetate, silver chlorate, silver carbonate etc..
Embodiment 2
The present embodiment provides a kind of high stable quanta point materials, and processing obtains according to the following steps:
(1) it prepares quantum dot dispersion liquid: 0.3g cadmium selenide/zinc sulphide alloy structure quantum dot being taken to disperse under an inert atmosphere
In 10mL oleic acid, save；
(2) it prepares mercury oxide stock solution: taking 0.01g mercury oxide, 15mL lauric acid is added, is placed in reaction unit and lazy
Under property atmosphere protection range, 90 DEG C are heated to, mercury oxide stock solution is prepared；
(3) the quantum dot dispersion liquid in step (1) is placed in reaction unit and under inert protective atmosphere, is warming up to
300 DEG C, the mercury oxide stock solution of step (2) preparation is added, uniform stirring dispersion reacts 10min, obtains fluorescence quantum.
Embodiment 3
The present embodiment provides a kind of high stable quanta point materials, and processing obtains according to the following steps:
(1) it prepares quantum dot dispersion liquid: containing according to being prepared the step of embodiment 1 in patent document CN107686731A
The dispersion liquid of CdSe@ZnCdS/ZnS alloy quantum dot；
(2) before not cooling down after the completion of the quantum dot preparation of step (1), the silver oxide being prepared in embodiment 1 is added
Stock solution reacts 10min, obtains fluorescence quantum.
Effect example 1
Take the quantum dot handled in untreated cadmium selenide/zinc sulphide alloy structure quantum dot and embodiment 1
Material is cleaned respectively, specific cleaning process are as follows: isometric n-hexane is added in initial quantum point solution, dispersion shakes up
Afterwards, the dehydrated alcohol of 3 times of volumes is added, continues dispersion and shakes up, centrifugal treating 2min, is precipitated under the conditions of 10000rpm
Object continuously adds n-hexane and repeats above-mentioned cleaning process.
Quantum dot to above-mentioned initial quantum point and Jing Guo cleaning process carries out the test of fluorescence quantum yield, detailed process
Are as follows: it disperses quantum dot to be measured in n-hexane, absorbance uses equipment shore 0.7 or so to adjustment concentration at 300 nm wavelength
Loose Quantaurus-QY C11347-12 is to test at 450nm in excitation wavelength.Test result is as shown in table 1.
The fluorescence quantum yield of quantum dot is handled in 1 cadmium selenide of table/zinc sulphide alloy structure quantum dot and embodiment 1
As it can be seen from table 1 without cadmium selenide/zinc sulphide alloy structure quantum dot of metal salt treatment by multiple
Fluorescence quantum yield declines rapidly after cleaning, and the quanta point material fluorescence quantum yield that handles in embodiment 1 is obvious
To promotion, and after being cleaned multiple times, fluorescence quantum yield is barely affected, the reason is that metal salt can be with quantum
The element sulphur on point surface combines the metal sulfosalt for forming strong binding force, avoids environment to the shadow of quantum dot fluorescence quantum yield
It rings, improves the chemical stability of quantum dot, solve the sulphur of original metal sulfide in the element sulphur and quantum dot not being coordinated
It is oxidized, the problem of quantum dot fluorescence quantum yield declines caused by ion exchange, the results show contains surface
There is the quantum dot of element sulphur, can be improved the chemical stability of such quantum dot using metal salt treatment.
Effect example 2
Take the quantum dot handled in untreated cadmium selenide/zinc sulphide alloy structure quantum dot and embodiment 1
Material is respectively heated processing, specific as follows: oleic acid is added in quanta point material, heating mantle heats are used in there-necked flask,
Heating interval is 50 DEG C of 5min, 100 DEG C of 5min, 150 DEG C of 5min, 200 DEG C of 10min, 300 DEG C of 10min, 320 DEG C of 10min respectively.
After completing heating process, it is cooled to room ambient conditions.To the above-mentioned cadmium selenide by before and after high-temperature heating treatment/vulcanization kirsite
Quanta point material in structure quantum point and embodiment 1 carries out the test of fluorescence quantum yield, detailed process are as follows: by quantum to be measured
Point is scattered in n-hexane, and absorbance uses equipment shore pine Quantaurus- 0.7 or so to adjustment concentration at 300 nm wavelength
QY C11347-12 is to test at 450nm in excitation wavelength.To cadmium selenide/zinc sulphide alloy structure quantum of heat treatment front and back
Test results are shown in figure 1 for point, the test result to the quanta point material handled in the embodiment 1 of heat treatment front and back
As shown in Figure 2.
It will be seen from figure 1 that untreated cadmium selenide/zinc sulphide alloy structure quantum dot is after heat treatment
Test fluorescence spectrum has apparent red shift situation, and the quanta point material by the application processing is by adding as can be seen from Figure 2
Fluorescence spectrum is tested after heat treatment is not evident that spectral shift situation.The reason is that metal salt can be high with having for quantum dot
The element sulphur reaction bonded of reactivity is at the metal sulfosalt with strong binding force, so as to avoid sulphur member in the case of high-temperature heating
The phenomenon that element is oxidized to form quantum dot surface vacancy, and quantum dot reunion is caused to further cause quantum dot fluorescence spectral shift.
The experimental results showed that the chemistry that can be improved such quantum dot using metal salt treatment is steady for the quantum dot containing element sulphur
Qualitative and dispersion stabilization.
Effect example 3
It takes to handle in untreated cadmium selenide/zinc sulphide alloy structure quantum dot (before processing) and embodiment 1 and obtain
Quanta point material (after processing) carry out LED glue dispensing and packaging respectively and carry out burn-in test, specifically: by quantum dot and UV glue
Mixing, after vacuum rotating deaeration, dispensing enters in 2835 blue chip LED.After ultraviolet light 30s glue curing, put
Enter and carry out burn-in test in high temperature and humidity accelerated ageing case, puts light current 20mA.After per a few houres persistently light, take out using remote
Square ATA-500 integrating sphere is tested, and the decay situation of quantum dot fluorescence spectrum is calculated, as a result as shown in Figure 3.
From figure 3, it can be seen that untreated cadmium selenide/zinc sulphide alloy structure quantum dot is passing through long-time high temperature
After high humidity lights aging, the rate of decay is very fast.In contrast, the quanta point material handled by embodiment 1 is in square one
Under be smoothly to decay.The reason is that the unstable element sulphur of metal salt and quantum dot forms the metal sulfosalt of strong binding force, keep away
Having exempted from quantum dot surface, element sulphur in the case where high temperature and humidity is oxidized by water oxygen, and quantum dot is caused to form vacancy and decomposition
Problem.The results show using metal salt treatment can be improved such quantum dot for the quantum dot containing element sulphur
Antioxidative stabilizer.
Claims (10)
1. a kind of processing method of quanta point material, which is characterized in that element sulphur is contained on the surface of the quanta point material, including
Following steps:
(1) it takes metal salt to be scattered in solvent under an inert atmosphere, obtains metal salt stock solution；
(2) the metal salt stock solution is added under an inert atmosphere and is reacted for the dispersion liquid for taking or preparing quanta point material.
2. the processing method of quanta point material according to claim 1, which is characterized in that the metal member in the metal salt
Element is selected from least one of I B race, II B race element, V group Ⅴ element, alkaline-earth metal, scandium, yttrium and lanthanide series.
3. the processing method of quanta point material according to claim 2, which is characterized in that the metallic element be selected from silver,
At least one of mercury, zinc, copper, gold, cadmium, nickel, platinum.
4. the processing method of quanta point material according to claim 1, which is characterized in that the quanta point material is metal
The nanocrystalline colloid quantum dot of sulfide nanocrystalline Colloidal Quantum Dots or surface containing metal sulfide.
5. the processing method of quanta point material described in -4 according to claim 1, which is characterized in that in the metal salt stock solution
The concentration of metal salt is 0.001mmol/L~10mol/L.
6. the processing method of quanta point material described in -4 according to claim 1, which is characterized in that the solvent is that corrdination type is molten
Agent or noncoordinating type solvent；It is preferred that the corrdination type nonpolar solvent is the acid of carbon atom number >=6, the preferably described noncoordinating type is molten
Agent is at least one of carbon atom number >=9 alkane, alkene, ester.
7. the processing method of quanta point material according to claim 6, which is characterized in that the corrdination type solvent is selected from ten
At least one of tetracid, oleic acid, stearic acid, lauric acid；The noncoordinating type solvent is selected from atoleine, octadecylene, 18
At least one of alkane.
8. a kind of high stable quanta point material, which is characterized in that pass through the described in any item quanta point materials of claim 1-7
Processing method obtains.
9. application of the high stable quanta point material according to any one of claims 8 in illumination or display.
10. application according to claim 9, which is characterized in that the application is in QLEDs illumination or backlight display
Using.
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| CN201910236499.9A CN109825281A (en) | 2019-03-27 | 2019-03-27 | A kind of processing method of quanta point material, high stable quanta point material and application |
| PCT/CN2019/082410 WO2020191821A1 (en) | 2019-03-27 | 2019-04-12 | Quantum dot material processing method, highly stable quantum dot material and application thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106701060A (en) * | 2016-12-22 | 2017-05-24 | Tcl集团股份有限公司 | Passivation quantum dot film and preparation method thereof |
| CN108441221A (en) * | 2018-05-10 | 2018-08-24 | 河北工业大学 | One kind core-shell quanta dots material compatible with packaging silicon rubber height and preparation method thereof |
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| KR20180099784A (en) * | 2015-12-31 | 2018-09-05 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | Composite particles comprising quantum dots and method for producing the same |
| CN106566529A (en) * | 2016-11-10 | 2017-04-19 | Tcl集团股份有限公司 | Passivated quantum dot and preparation method thereof |
| CN108807608B (en) * | 2017-05-02 | 2020-06-12 | Tcl科技集团股份有限公司 | Preparation method of oxide-coated quantum dot LED |
| CN107384371B (en) * | 2017-08-08 | 2019-10-11 | 中国科学院合肥物质科学研究院 | CuGaS-ZnS nuclear shell structure quantum point material and preparation method thereof |
| CN108441207B (en) * | 2018-02-22 | 2021-03-02 | 苏州星烁纳米科技有限公司 | Quantum dot composite and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106701060A (en) * | 2016-12-22 | 2017-05-24 | Tcl集团股份有限公司 | Passivation quantum dot film and preparation method thereof |
| CN108441221A (en) * | 2018-05-10 | 2018-08-24 | 河北工业大学 | One kind core-shell quanta dots material compatible with packaging silicon rubber height and preparation method thereof |
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