CN106367069A - Four-footed quantum dot, preparation method of four-footed quantum dot and four-footed quantum dot luminescent film - Google Patents
Four-footed quantum dot, preparation method of four-footed quantum dot and four-footed quantum dot luminescent film Download PDFInfo
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Abstract
The invention discloses a four-footed quantum dot, a preparation method of the four-footed quantum dot and a four-footed quantum dot luminescent film. The preparation method comprises preparing a cadmium precursor mixed solution, preparing a sulfur precursor mixed solution, pouring the sulfur precursor mixed solution into the cadmium precursor mixed solution, carrying out a reaction process for 5-120s, pouring sphalerite CdSe quantum dots into the reaction product, heating the mixture to a temperature of 310-350 DEG C, after heating for 5-25min, pouring anhydrous toluene into the heated product, then stopping heating, and repeatedly carrying out dissolution and deposition after the reaction solution is cooled to the room temperature, and carrying out centrifugation purification processes so that the CdSe/CdS four-footed quantum dots are obtained. The four-footed quantum dot with size controllability is prepared through a two-step method. The preparation method effectively improves quantum dot luminescence efficiency. The four-footed quantum dot prolongs a quantum dot luminescent film service life. The four-footed quantum dot has excellent fluorescence performances and good machining properties of the silicone resin and epoxy resin so that the four-footed quantum dot luminescent film can be used for a light emitting diode and solid state lighting LED.
Description
Technical field
The present invention relates to fluorescent material field, more particularly, to a kind of four-footed quantum dot and preparation method thereof and four-footed quantum dot
Light-emitting film.
Background technology
Semiconductor-quantum-point is that have the optical property of uniqueness and the nano size particles of electrology characteristic, is currently under model
During enclosing extensive conceptual phase steering application, application includes illumination, display, solar energy conversion and molecule and becomes with cell
Picture.In recent years, quantum dot is applied to field of display devices, can greatly improve display effect, improve colour vividness, colour gamut and
Color rendering index etc., makes the colour gamut of display bring up to 110%ntsc from 70%ntsc.With Display Technique require constantly improve with
Lifting, spherical nanoparticle is difficult to keep for a long time dispersity, therefore develops a kind of topographical height complexity, protects for a long time simultaneously
Keep steady and determine dispersity material and be particularly important.
Four-footed quantum dot be extended by core and four-way etc. the considerable nano structural material constituting, its sufficient length and diameter
Can be adjusted in preparation process.The transmitting of four-footed quantum dot is derived from its kernel, and the foot that its four-way extends provides more preferably
Excitation channel.The absorption efficiency in ultra-violet (UV) band for the foot is 300 times of core, you can to store exciton, again can swashing storage
Son is transferred to kernel, finally discharges exciton in the form of launching luminous energy.Due to the structural specificity of four-footed quantum dot, its surface is joined
Body is evenly distributed so as to be disperse easily in substrate, and will not be formed reunion lead to its luminescent properties lose.
Therefore, four-footed quantum dot can be used for improving display device stability and display effect further.
Content of the invention
A kind of in view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide four-footed quantum dot and preparation method thereof
With four-footed quantum dot light emitting thin film it is intended to solve the problems, such as that existing spherical nanoparticle is difficult to keep for a long time dispersity.
Technical scheme is as follows:
A kind of preparation method of four-footed quantum dot, wherein, described four-footed quantum dot is to be carried out with sphalerite cdse quantum dot for core
The growth of cadmium sulfide nano-stick, including step:
A, the preparation of cadmium presoma mixed liquor: cadmium source, organic ligand and cadmium covering are mixed, obtains mixed liquor, then will mix
Close liquid heating under vacuum to 110 ~ 180 DEG C and the 20 ~ 60min that deaerates, then the mixed liquor after degassing is heated under inert atmosphere
To 280 ~ 330 DEG C until forming clarification, clear solution；
B, the preparation of sulfur presoma mixed liquor: under inert atmosphere, by sulphur source and sulfur covering at 45 ~ 55 DEG C mix and blend 25 ~
35 min；
The preparation of c, cdse/cds four-footed quantum dot: when temperature is 280 ~ 310 DEG C, the above-mentioned sulfur presoma preparing is mixed
Liquid injects in the above-mentioned cadmium presoma mixed liquor preparing；After reaction 5 ~ 120s, inject the sphalerite cdse quantum dot got ready；Will
Temperature is increased to 310 ~ 350 DEG C, injects dry toluene after 5 ~ 25min, and stops heating；After question response liquid is cooled to room temperature, produce
Thing repeatedly dissolves, precipitates, centrifugation purification.
The preparation method of described four-footed quantum dot, wherein, in step a, described cadmium source is Aska-Rid., described organic ligand
For the mixture of phosphoric acid octadecyl ester and phosphoric acid pi-allyl diethylester, described cadmium covering is trioctyl phosphine oxide.
The preparation method of described four-footed quantum dot, wherein, described Aska-Rid., phosphoric acid octadecyl ester, phosphoric acid pi-allyl diethyl
The mol ratio of ester and trioctyl phosphine oxide mixing is (1 ~ 2): (3 ~ 5): (0.1 ~ 0.3): (9 ~ 12).
The preparation method of described four-footed quantum dot, wherein, described Aska-Rid., phosphoric acid octadecyl ester, phosphoric acid pi-allyl diethyl
The mol ratio of ester and trioctyl phosphine oxide mixing is 1.61:3.23:0.12:9.18.
The preparation method of described four-footed quantum dot, wherein, in step b, described sulfur covering is tri octyl phosphine.
The preparation method of described four-footed quantum dot, wherein, described sulphur powder and tri octyl phosphine mixing mol ratio be 1:1 ~
1:5.
The preparation method of described four-footed quantum dot, wherein, in step c, product passes through toluene and dehydrated alcohol is repeatedly molten
Solution.
A kind of four-footed quantum dot, wherein, the preparation method using as above arbitrary described four-footed quantum dot is prepared from.
A kind of preparation method of four-footed quantum dot light emitting thin film, wherein, including step:
E, four-footed quantum dot as described above is mixed with organic siliconresin, heat 0.5 ~ 2h at 50 ~ 100 DEG C, obtain mixture；
F, epoxy resin is mixed homogeneously with the mixture that step e obtains, removes bubble removing, be more uniformly coated on substrate and in
Solidify 10 ~ 30h under room temperature, obtain four-footed quantum dot light emitting thin film.
A kind of four-footed quantum dot light emitting thin film, wherein, using the preparation side of four-footed quantum dot light emitting thin film as above
Method is prepared from.
Beneficial effect: the present invention is prepared for a kind of controlled four-footed quantum dot of size using " two-step method ".The inventive method
The luminous efficiency of quantum dot can effectively be improved, thus extending the service life of quantum dot light emitting thin film to a certain extent.
Brief description
Fig. 1 is a kind of schematic diagram of present invention four-footed quantum dot light emitting thin film.
Specific embodiment
The present invention provides a kind of four-footed quantum dot and preparation method thereof and four-footed quantum dot light emitting thin film, for making the present invention's
Purpose, technical scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that this place is retouched
The specific embodiment stated only in order to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of preparation method of four-footed quantum dot, and wherein, described four-footed quantum dot is with sphalerite cdse
Quantum dot carries out the growth of cadmium sulfide nano-stick for core, including step:
A, the preparation of cadmium presoma mixed liquor: by cadmium source (as Aska-Rid .), organic ligand (as phosphoric acid octadecyl ester and phosphoric acid pi-allyl
The mixture of diethylester) and cadmium covering (as trioctyl phosphine oxide) mixing, obtain mixed liquor, then will add under mixed liquor vacuum
Heat to 110 ~ 180 DEG C (as 120 DEG C) and 20 ~ 60min(such as 30min that deaerates), then by deaerate after mixed liquor in inert atmosphere
(as n2Atmosphere) under be heated to 280 ~ 330 DEG C (as 320 DEG C) until forming clarification, till clear solution；
Preferably, in step a, Aska-Rid., phosphoric acid octadecyl ester, phosphoric acid pi-allyl diethylester and trioctyl phosphine oxide mixing mole
Than for (1 ~ 2): (3 ~ 5): (0.1 ~ 0.3): (9 ~ 12).It is highly preferred that Aska-Rid., phosphoric acid octadecyl ester, phosphoric acid pi-allyl diethylester
Mol ratio with trioctyl phosphine oxide mixing is 1.61:3.23:0.12:9.18.
B, the preparation of sulfur presoma mixed liquor: under inert atmosphere, by sulphur source (as sulphur powder) and sulfur covering (as trioctylphosphine
Phosphine) mix and blend 25 ~ 35min(such as 30min under 45 ~ 55 DEG C (as 50 DEG C))；
Preferably, in step b, the mol ratio of sulphur powder and tri octyl phosphine mixing is 1:1 ~ 1:5.It is highly preferred that sulphur powder and trioctylphosphine
The mol ratio of phosphine mixing is 1:1.
The preparation of c, cdse/cds four-footed quantum dot: when temperature is 280 ~ 310 DEG C (as 300 DEG C), prepare above-mentioned
Sulfur presoma mixed liquor inject the above-mentioned cadmium presoma mixed liquor preparing in；Reaction 5 ~ 120s(such as 40s) after, injection is got ready
Sphalerite cdse quantum dot；Temperature is increased to 310 ~ 350 DEG C (as 315 DEG C), 5 ~ 25min(such as 20min) inject afterwards anhydrous
Toluene, and stop heating (removing heating mantle)；After question response liquid is cooled to room temperature, product passes through toluene and dehydrated alcohol is repeatedly molten
Solution, precipitation, centrifugation purification.The preparing and have no special requirements of described sphalerite cdse quantum dot, prior art is to its preparation method
It is described in detail, here of the present invention is no longer repeated.
The present invention is prepared for a kind of controlled four-footed quantum dot of size using " two-step method ".The inventive method prepares
Four-footed quantum dot light emitting efficiency high, fluorescence property is excellent.
The present invention also provides a kind of four-footed quantum dot, and it adopts the preparation method system of as above arbitrary described four-footed quantum dot
Standby form.By the inventive method, obtain a kind of controlled four-footed quantum dot of size.Due to the particularity of this structure, hole
In bond on three-dimensional, electronics is in bond in the two-dimensional direction.Meanwhile, in the structure shown here, arrange around core in four-footed shape
Foot act as one perfect " antenna ", can effectively capture without any polarization manipulation, from any direction
Photon, passes it in core simultaneously, and discharges photon energy in the form of radiation transistion.Therefore, the inventive method is effective
Improve the luminous efficiency of quantum dot, thus extending the service life of quantum dot light emitting thin film to a certain extent.
The present invention provides a kind of preparation method of four-footed quantum dot light emitting thin film, and it includes step:
E, four-footed shape quantum dot as described above is mixed with organic siliconresin, under 50 ~ 100 DEG C (as 80 DEG C), heating 0.5 ~ 2h(is such as
1h), obtain mixture；
F, epoxy resin is mixed homogeneously with the mixture that step e obtains, remove bubble removing, be more uniformly coated in substrate (as glass
Glass substrate) solidify 10 ~ 30h above and at room temperature, obtain four-footed quantum dot light emitting thin film.
Fig. 1 is a kind of schematic diagram of present invention four-footed quantum dot light emitting thin film, as illustrated, 1 is organic siliconresin, 2 are
Glass substrate, 3 is four-footed quantum dot, and 4 is epoxy resin.The excellent fluorescence property of four-footed quantum dot and organic siliconresin, epoxy
The good machining property of resin, so that this four-footed quantum dot light emitting thin-film light emitting efficiency high, long service life, is expected to be answered
For light emitting diode, solid-state illumination led etc..
The present invention also provides a kind of four-footed quantum dot light emitting thin film, and it adopts four-footed quantum dot light emitting thin film as above
Preparation method be prepared from.Four-footed quantum dot light emitting efficiency high of the present invention, thus extend four-footed quantum dot to a certain extent send out
The luminous efficiency of optical thin film and service life.Four-footed quantum dot light emitting film fluorescence of the present invention is adjustable, and luminous efficiency is high.With
When, the excellent fluorescence property of four-footed quantum dot and the good machining property of organic siliconresin, epoxy resin are so that this four-footed
Quantum dot light emitting thin film is expected to be applied to light emitting diode, solid-state illumination led etc..
The moisture transmitance of four-footed quantum dot light emitting thin film of the present invention is 1mg/m224h to 10e-4mg/ m2·
24h.
The OTR oxygen transmission rate of four-footed quantum dot light emitting thin film of the present invention is 2ml/m224h to 10e-5ml/m2·
24h.
Below by embodiment, the present invention is described in detail.
Embodiment 1
The preparation of four-footed quantum dot, step is as follows:
(1) preparation of cadmium presoma mixed liquor: by 1.61mmol Aska-Rid. (cadmium oxide), 3.23mmol phosphoric acid 18
Ester (octadecylphosphonic acid), 0.12mmol phosphoric acid pi-allyl diethylester (diethyl allyl
Phosphate) and 9.18mmol trioctyl phosphine oxide (trioctylphosphine oxide) be placed in 25ml there-necked flask in
Heating under vacuum is to 120 DEG C and the 30min that deaerates.Then in n2It is heated to 320 DEG C until forming clarification, clear solution is under atmosphere
Only.
(2) preparation of trioctylphosphine sulfide mixed liquor: under inert gas atmosphere, by equimolar sulphur powder (sulphur
) and tri octyl phosphine (trioctylphosphine) mix and blend 30min at 50 DEG C powder.
(3) preparation of cdse/cds four-footed quantum dot: when temperature is 300 DEG C, by the above-mentioned 1.61mmol sulfur preparing
Change tri octyl phosphine to inject in the above-mentioned cadmium presoma mixed liquor preparing.After reaction 40s, by 10-8The sphalerite cdse quantum of mol
Point injection is wherein.Temperature is increased to 315 DEG C, injects the dry toluene of 10ml after 20min in reaction solution, and remove heating
Set.In course of reaction, the length of four-footed and diameter pass through the injection rate of sphalerite cdse quantum dot, response time realization tune respectively
Control.After question response liquid is cooled to room temperature, product passes through toluene and dehydrated alcohol repeatedly dissolves, precipitates, centrifugation purification.
The preparation of four-footed quantum dot light emitting thin film, step is as follows:
The four-footed quantum dot of above-mentioned preparation is mixed homogeneously with organic siliconresin, heats 1h at 80 DEG C, obtain its mixture.Described
Gas barrier material moisture transmitance is preferably 1mg/m224h to 10e-4mg/ m224h, more preferably 10e-1mg/m2·
24h to 10e-2mg/m224h, OTR oxygen transmission rate is preferably 2ml/m224h to 10e-5ml/m2 24h, more preferably
10e-2ml/m224h to 10e-3ml/m2·24h；
Epoxy resin is mixed homogeneously with said mixture, removes bubble removing, more uniformly coat on a glass substrate and in room temperature
Lower solidification 20 h, obtain four-footed quantum dot light emitting thin film.
Embodiment 2
(1) preparation of cadmium presoma mixed liquor: by 1.61mmol Aska-Rid. (cadmium oxide), 3.23mmol phosphoric acid 18
Ester (octadecylphosphonic acid), 0.12mmol phosphoric acid pi-allyl diethylester (diethyl allyl
Phosphate) and 9.18mmol trioctyl phosphine oxide (trioctylphosphine oxide) be placed in 25ml there-necked flask in
Heating under vacuum is to 120 DEG C and the 30min that deaerates.Then in n2It is heated to 320 DEG C until forming clarification, clear solution is under atmosphere
Only.
(2) preparation of trioctylphosphine sulfide mixed liquor: under inert gas atmosphere, by equimolar sulphur powder (sulphur
) and tri octyl phosphine (trioctylphosphine) mix and blend 30min at 50 DEG C powder.
(3) preparation of cdse/cds four-footed quantum dot: when temperature is 300 DEG C, by the above-mentioned 1.61mmol sulfur preparing
Change tri octyl phosphine to inject in the above-mentioned cadmium presoma mixed liquor preparing.After reaction 40s, by 10-8The sphalerite cdse quantum of mol
Point injection is wherein.Temperature is increased to 315 DEG C, injects the dry toluene of 10ml after 8min in reaction solution, and remove heating
Set.In course of reaction, the length of four-footed and diameter pass through the injection rate of sphalerite cdse quantum dot, response time realization tune respectively
Control.After question response liquid is cooled to room temperature, product passes through toluene and dehydrated alcohol repeatedly dissolves, precipitates, centrifugation purification.
The preparation of four-footed quantum dot light emitting thin film, step is as follows:
The four-footed quantum dot of above-mentioned preparation is mixed homogeneously with organic siliconresin, heats 1h at 80 DEG C, obtain its mixture.Described
Gas barrier material moisture transmitance is preferably 1mg/m224h to 10e-4mg/ m224h, more preferably 10e-1mg/m2·
24h to 10e-2mg/m224h, OTR oxygen transmission rate is preferably 2ml/m224h to 10e-5ml/m2 24h, more preferably
10e-2ml/m224h to 10e-3ml/m2·24h；
Epoxy resin is mixed homogeneously with said mixture, removes bubble removing, more uniformly coat on a glass substrate and in room temperature
Lower solidification 20 h, obtain four-footed quantum dot light emitting thin film.
Embodiment 3
(1) preparation of cadmium presoma mixed liquor: by 1.61mmol Aska-Rid. (cadmium oxide), 3.23mmol phosphoric acid 18
Ester (octadecylphosphonic acid), 0.12mmol phosphoric acid pi-allyl diethylester (diethyl allyl
Phosphate) and 9.18mmol trioctyl phosphine oxide (trioctylphosphine oxide) be placed in 25ml there-necked flask in
Heating under vacuum is to 120 DEG C and the 30min that deaerates.Then in n2It is heated to 320 DEG C until forming clarification, clear solution is under atmosphere
Only.
(2) preparation of trioctylphosphine sulfide mixed liquor: under inert gas atmosphere, by equimolar sulphur powder (sulphur
) and tri octyl phosphine (trioctylphosphine) mix and blend 30min at 50 DEG C powder.
(3) preparation of cdse/cds four-footed quantum dot: when temperature is 300 DEG C, by the above-mentioned 1.61mmol sulfur preparing
Change tri octyl phosphine to inject in the above-mentioned cadmium presoma mixed liquor preparing.After reaction 40s, by 5 10-8The sphalerite cdse of mol
Quantum dot injects wherein.Temperature is increased to 315 DEG C, injects the dry toluene of 10ml after 20min in reaction solution, and remove
Heating mantle.In course of reaction, the length of four-footed and diameter pass through the injection rate of sphalerite cdse quantum dot, response time in fact respectively
Now regulate and control.After question response liquid is cooled to room temperature, product passes through toluene and dehydrated alcohol repeatedly dissolves, precipitates, centrifugation purification.
The preparation of four-footed quantum dot light emitting thin film, step is as follows:
The four-footed quantum dot of above-mentioned preparation is mixed homogeneously with organic siliconresin, heats 1h at 80 DEG C, obtain its mixture.Described
Gas barrier material moisture transmitance is preferably 1mg/m224h to 10e-4mg/ m224h, more preferably 10e-1mg/m2·
24h to 10e-2mg/m224h, OTR oxygen transmission rate is preferably 2ml/m224h to 10e-5ml/m2 24h, more preferably
10e-2ml/m224h to 10e-3ml/m2·24h；
Epoxy resin is mixed homogeneously with said mixture, removes bubble removing, more uniformly coat on a glass substrate and in room temperature
Lower solidification 20 h, obtain four-footed quantum dot light emitting thin film.
In sum, a kind of four-footed quantum dot that the present invention provides and preparation method thereof and four-footed quantum dot light emitting thin film.
Present invention obtains a kind of controlled four-footed quantum dot of size.Due to the particularity of this structure, hole is restrainted on three-dimensional
Tie up, electronics is in bond in the two-dimensional direction.Meanwhile, in the structure shown here, the foot being in the arrangement of four-footed shape around core act as one
Perfectly " antenna ", can effectively capture without any polarization manipulation, from the photon of any direction, be transmitted simultaneously
To in core, and discharge photon energy in the form of radiation transistion.Therefore, the inventive method effectively raises the luminous of quantum dot
Efficiency, thus extend the service life of quantum dot light emitting thin film to a certain extent.Meanwhile, the excellent fluorescence property of four-footed quantum dot
And the good machining property of organic siliconresin, epoxy resin is so that this four-footed quantum dot light emitting thin film is expected to be applied to
Light emitting diode, solid-state illumination led etc..
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved according to the above description or to convert, all these modifications and variations all should belong to the guarantor of claims of the present invention
Shield scope.
Claims (10)
1. a kind of preparation method of four-footed quantum dot is it is characterised in that described four-footed quantum dot is with sphalerite cdse quantum dot
Carry out the growth of cadmium sulfide nano-stick for core, including step:
A, the preparation of cadmium presoma mixed liquor: cadmium source, organic ligand and cadmium covering are mixed, obtains mixed liquor, then will mix
Close liquid heating under vacuum to 110 ~ 180 DEG C and the 20 ~ 60min that deaerates, then the mixed liquor after degassing is heated under inert atmosphere
To 280 ~ 330 DEG C until forming clarification, clear solution；
B, the preparation of sulfur presoma mixed liquor: under inert atmosphere, by sulphur source and sulfur covering at 45 ~ 55 DEG C mix and blend 25 ~
35 min；
The preparation of c, cdse/cds four-footed quantum dot: when temperature is 280 ~ 310 DEG C, the above-mentioned sulfur presoma preparing is mixed
Liquid injects in the above-mentioned cadmium presoma mixed liquor preparing；After reaction 5 ~ 120s, inject the sphalerite cdse quantum dot got ready；Will
Temperature is increased to 310 ~ 350 DEG C, injects dry toluene after 5 ~ 25min, and stops heating；After question response liquid is cooled to room temperature, produce
Thing repeatedly dissolves, precipitates, centrifugation purification.
2. the preparation method of four-footed quantum dot according to claim 1 is it is characterised in that in step a, described cadmium source is oxygen
Cadmium, described organic ligand is the mixture of phosphoric acid octadecyl ester and phosphoric acid pi-allyl diethylester, and described cadmium covering is trioctylphosphine
Phosphine oxide.
3. the preparation method of four-footed quantum dot according to claim 2 is it is characterised in that described Aska-Rid., phosphoric acid 18
The mol ratio of ester, phosphoric acid pi-allyl diethylester and trioctyl phosphine oxide mixing is (1 ~ 2): (3 ~ 5): (0.1 ~ 0.3): (9 ~ 12).
4. the preparation method of four-footed quantum dot according to claim 3 is it is characterised in that described Aska-Rid., phosphoric acid 18
The mol ratio of ester, phosphoric acid pi-allyl diethylester and trioctyl phosphine oxide mixing is 1.61:3.23:0.12:9.18.
5. the preparation method of four-footed quantum dot according to claim 1 is it is characterised in that in step b, described sulfur covering
For tri octyl phosphine.
6. the preparation method of four-footed quantum dot according to claim 5 is it is characterised in that described sulphur powder and tri octyl phosphine mix
The mol ratio closed is 1:1 ~ 1:5.
7. the preparation method of four-footed quantum dot according to claim 1 is it is characterised in that in step c, product passes through toluene
Repeatedly dissolve with dehydrated alcohol.
8. a kind of four-footed quantum dot is it is characterised in that adopt the preparation side of described four-footed quantum dot as arbitrary in claim 1 ~ 7
Method is prepared from.
9. a kind of preparation method of four-footed quantum dot light emitting thin film is it is characterised in that include step:
E, four-footed quantum dot described in claim 8 is mixed with organic siliconresin, heat 0.5 ~ 2h at 50 ~ 100 DEG C, mixed
Thing；
F, epoxy resin is mixed homogeneously with the mixture that step e obtains, removes bubble removing, be more uniformly coated on substrate and in
Solidify 10 ~ 30h under room temperature, obtain four-footed quantum dot light emitting thin film.
10. a kind of four-footed quantum dot light emitting thin film is it is characterised in that adopt four-footed quantum dot light emitting as claimed in claim 9
The preparation method of thin film is prepared from.
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