CN106367069B - Four-footed quantum dot, preparation method thereof and four-footed quantum dot light-emitting film - Google Patents
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Abstract
The invention discloses a four-footed quantum dot and a preparation method thereof and a four-footed quantum dot luminescent film, wherein the method comprises the following steps: preparing a cadmium precursor mixed solution, preparing a sulfur precursor mixed solution, injecting the sulfur precursor mixed solution into the cadmium precursor mixed solution, reacting for 5-120 s, and injecting zinc blende CdSe quantum dots; heating to 310-350 ℃, injecting anhydrous toluene after 5-25 min, and stopping heating; and after the reaction liquid is cooled to room temperature, repeatedly dissolving and precipitating the product, and centrifugally purifying to obtain the CdSe/CdS four-footed quantum dot. The invention adopts a two-step method to prepare the four-footed quantum dot with controllable size, effectively improves the luminous efficiency of the quantum dot and prolongs the service life of the quantum dot fluorescent film. Meanwhile, the four-footed quantum dot light-emitting film is expected to be applied to light-emitting diodes, solid-state lighting LEDs and the like due to the excellent fluorescence property of the four-footed quantum dots and the good machining property of organic silicon resin and epoxy resin.
Description
Technical Field
The invention relates to the field of fluorescent materials, in particular to a four-footed quantum dot, a preparation method thereof and a four-footed quantum dot light-emitting film.
Background
Semiconductor quantum dots are nano-sized particles with unique optical and electrical properties, and are currently in a wide range of research phases turning to applications including illumination, display, solar energy conversion, and molecular and cellular imaging. In recent years, quantum dots have been applied to the field of display devices, which can greatly improve the display effect, the color vividness, the color gamut, the color rendering index and the like, so that the color gamut of the display is increased from 70% NTSC to 110% NTSC. With the continuous improvement and promotion of the display technical requirements, the spherical nano particles are not easy to keep a dispersion state for a long time, so that the development of a material with a complex morphology and a stable dispersion state for a long time is very important.
The four-footed quantum dot is a nano-structure material consisting of a core and four-way extending equal-length feet, and the length and the diameter of the feet can be adjusted in the preparation process. The emitting source of the quadruped quantum dot is from the inner core, and the quadruped extending foot part of the quadruped quantum dot provides a better excitation channel. The absorption efficiency of the foot in the ultraviolet region is 300 times that of the core, i.e. excitons can be stored and can be transferred to the core, and finally the excitons are released in the form of emitted light energy. Due to the structural specificity of the four-footed quantum dot, the surface ligand is uniformly distributed, so that the four-footed quantum dot is easily dispersed in a matrix, and no agglomeration is formed to cause the loss of the luminescence property of the four-footed quantum dot.
Therefore, the four-footed quantum dots can be used to further improve the stability and display effect of the display device.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a quadruped quantum dot, a preparation method thereof and a quadruped quantum dot light-emitting film, which aim to solve the problem that the existing spherical nanoparticles are not easy to maintain a dispersed state for a long time.
The technical scheme of the invention is as follows:
a preparation method of a four-footed quantum dot, wherein the four-footed quantum dot takes a sphalerite CdSe quantum dot as a core to grow a cadmium sulfide nanorod, comprises the following steps:
A. preparing a cadmium precursor mixed solution: mixing a cadmium source, an organic ligand and a cadmium coating agent to obtain a mixed solution, heating the mixed solution to 110-180 ℃ in vacuum, degassing for 20-60 min, and heating the degassed mixed solution to 280-330 ℃ in an inert atmosphere until a clear and transparent solution is formed;
B. preparing a sulfur precursor mixed solution: under inert atmosphere, mixing and stirring a sulfur source and a sulfur coating agent at 45-55 ℃ for 25-35 min;
C. preparing CdSe/CdS four-footed quantum dots: injecting the prepared sulfur precursor mixed solution into the prepared cadmium precursor mixed solution at the temperature of 280-310 ℃; after reacting for 5-120 s, injecting the prepared sphalerite CdSe quantum dots; raising the temperature to 310-350 ℃, injecting anhydrous toluene after 5-25 min, and stopping heating; and after the reaction liquid is cooled to room temperature, repeatedly dissolving and precipitating the product, and performing centrifugal purification.
In the step A, the cadmium source is cadmium oxide, the organic ligand is a mixture of octadecyl phosphate and allyl diethyl phosphate, and the cadmium coating agent is trioctylphosphine oxide.
The preparation method of the four-footed quantum dot comprises the following step of mixing the cadmium oxide, the octadecyl phosphate, the allyl diethyl phosphate and the trioctylphosphine oxide in a molar ratio of (1-2) to (3-5) to (0.1-0.3) to (9-12).
The preparation method of the four-footed quantum dot comprises the step of mixing the cadmium oxide, the octadecyl phosphate, the allyl diethyl phosphate and the trioctylphosphine oxide in a molar ratio of 1.61:3.23:0.12: 9.18.
In the preparation method of the four-footed quantum dot, in the step B, the sulfur coating agent is trioctylphosphine.
The preparation method of the four-footed quantum dot comprises the step of mixing the sulfur powder and the trioctylphosphine in a molar ratio of 1:1-1: 5.
In the preparation method of the four-footed quantum dot, in the step C, the product is repeatedly dissolved by toluene and absolute ethyl alcohol.
A four-footed quantum dot is prepared by adopting the preparation method of the four-footed quantum dot.
A preparation method of a four-footed quantum dot luminescent film comprises the following steps:
E. mixing the four-footed quantum dots with organic silicon resin, and heating at 50-100 ℃ for 0.5-2 h to obtain a mixture;
F. and E, uniformly mixing the epoxy resin with the mixture obtained in the step E, removing bubbles, uniformly coating on the substrate, and curing at room temperature for 10-30 h to obtain the four-footed quantum dot light-emitting film.
The four-footed quantum dot light-emitting film is prepared by the preparation method of the four-footed quantum dot light-emitting film.
Has the advantages that: the invention adopts a two-step method to prepare the four-footed quantum dot with controllable size. The method can effectively improve the luminous efficiency of the quantum dots, thereby prolonging the service life of the quantum dot luminous film to a certain extent.
Drawings
Fig. 1 is a schematic diagram of a four-footed quantum dot light-emitting film of the present invention.
Detailed Description
The invention provides a quadruped quantum dot, a preparation method thereof and a quadruped quantum dot light-emitting film, and the invention is further explained in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a preparation method of a four-footed quantum dot, wherein the four-footed quantum dot takes zinc blende CdSe quantum dots as cores to grow cadmium sulfide nanorods, and the preparation method comprises the following steps:
A. preparing a cadmium precursor mixed solution: mixing cadmium source (such as cadmium oxide), organic ligand (such as mixture of octadecyl phosphate and allyl diethyl phosphate) and cadmium coating agent (such as trioctylphosphine oxide) to obtain mixed solution, heating the mixed solution to 110-180 deg.C (such as 120 deg.C) under vacuum, degassing for 20-60 min (such as 30 min), and placing the degassed mixed solution in inert atmosphere (such as N2Atmosphere) to 280-330 ℃ (e.g., 320 ℃) until a clear, transparent solution is formed;
preferably, in the step A, the mixing molar ratio of the cadmium oxide, the octadecyl phosphate, the allyl diethyl phosphate and the trioctyl phosphine oxide is (1-2): (3-5): (0.1-0.3): (9-12). More preferably, the molar ratio of cadmium oxide, stearyl phosphate, allyl diethyl phosphate, and trioctylphosphine oxide combined is 1.61:3.23:0.12: 9.18.
B. Preparing a sulfur precursor mixed solution: mixing and stirring a sulfur source (such as sulfur powder) and a sulfur coating agent (such as trioctylphosphine) at 45-55 ℃ (such as 50 ℃) for 25-35 min (such as 30 min) under inert atmosphere;
preferably, in the step B, the mixing molar ratio of the sulfur powder and the trioctylphosphine is 1:1-1: 5. More preferably, the molar ratio of the sulfur powder to trioctylphosphine is 1: 1.
C. Preparing CdSe/CdS four-footed quantum dots: injecting the prepared sulfur precursor mixed solution into the prepared cadmium precursor mixed solution at the temperature of 280-310 ℃ (such as 300 ℃); after reacting for 5-120 s (such as 40 s), injecting the prepared sphalerite CdSe quantum dots; increasing the temperature to 310-350 ℃ (315 ℃ for example), injecting anhydrous toluene after 5-25 min (20 min for example), and stopping heating (removing the heating sleeve); after the reaction liquid is cooled to room temperature, the product is repeatedly dissolved and precipitated by toluene and absolute ethyl alcohol, and then is centrifugally purified. The preparation of the sphalerite CdSe quantum dot has no special requirement, the preparation method of the sphalerite CdSe quantum dot has been described in detail in the prior art, and the invention is not repeated herein.
The invention adopts a two-step method to prepare the four-footed quantum dot with controllable size. The four-footed quantum dot prepared by the method has high light efficiency and excellent fluorescence performance.
The invention also provides the quadruped quantum dot which is prepared by adopting the preparation method of any quadruped quantum dot. By the method, the four-footed quantum dot with controllable size is obtained. Due to the particularity of this structure, holes are bound in three dimensions, and electrons are bound in two dimensions. Also, in this structure, the feet, arranged quadrupedly around the core, act as a perfect "antenna" that can efficiently capture photons from any direction without any polarization treatment, while passing them into the core and releasing the photon energy in the form of radiative transitions. Therefore, the method effectively improves the luminous efficiency of the quantum dots, thereby prolonging the service life of the quantum dot luminous film to a certain extent.
The invention provides a preparation method of a four-footed quantum dot luminescent film, which comprises the following steps:
E. mixing the quadruped quantum dots with the organic silicon resin, and heating for 0.5-2 h (such as 1 h) at 50-100 ℃ (such as 80 ℃) to obtain a mixture;
F. and E, uniformly mixing the epoxy resin with the mixture obtained in the step E, removing bubbles, uniformly coating the mixture on a substrate (such as a glass substrate) and curing the mixture at room temperature for 10-30 hours to obtain the four-footed quantum dot light-emitting film.
Fig. 1 is a schematic diagram of a four-footed quantum dot light-emitting film of the present invention, as shown in the figure, 1 is an organic silicon resin, 2 is a glass substrate, 3 is a four-footed quantum dot, and 4 is an epoxy resin. The four-footed quantum dot light-emitting film has high light-emitting efficiency and long service life and is expected to be applied to light-emitting diodes, solid-state lighting LEDs and the like.
The invention also provides a four-footed quantum dot light-emitting film which is prepared by adopting the preparation method of the four-footed quantum dot light-emitting film. The four-footed quantum dot light-emitting film has high light-emitting efficiency, thereby prolonging the light-emitting efficiency and the service life of the four-footed quantum dot light-emitting film to a certain extent. The four-footed quantum dot light-emitting film has adjustable fluorescence and high light-emitting efficiency. Meanwhile, the four-footed quantum dot light-emitting film is expected to be applied to light-emitting diodes, solid-state lighting LEDs and the like due to the excellent fluorescence property of the four-footed quantum dots and the good machining property of organic silicon resin and epoxy resin.
The moisture transmittance of the four-footed quantum dot light-emitting film is 1mg/m224h to 10E-4 mg/m2·24h。
The oxygen transmission rate of the four-footed quantum dot luminescent film is 2mL/m224h to 10E-5mL/m2·24h。
The present invention will be described in detail below with reference to examples.
Example 1
The preparation method of the four-footed quantum dot comprises the following steps:
(1) preparing a cadmium precursor mixed solution: 1.61mmol of Cadmium oxide (Cadmium oxide), 3.23mmol of octadecyl phosphate (octadecenylphosphonic acid), 0.12mmol of allyl Diethyl phosphate (Diethyl phosphate) and 9.18mmol of Trioctylphosphine oxide (Trioctylphosphine oxide) were placed in a 25mL three-neck flask and heated to 120 ℃ under vacuum and degassed for 30 min. Then in N2Heat to 320 ℃ under atmosphere until a clear, transparent solution is formed.
(2) Preparing a trioctylphosphine sulfide mixed solution: mixing sulfur powder (Sulphurpowder) and Trioctylphosphine (Trioctylphosphine) at 50 deg.C for 30min under inert gas atmosphere.
(3) Preparing CdSe/CdS four-footed quantum dots: and (3) injecting the prepared 1.61mmol of trioctylphosphine sulfide into the prepared cadmium precursor mixed solution at the temperature of 300 ℃. After 40s of reaction, 10 is added-8The mol sphalerite CdSe quantum dots are injected into the zinc blende CdSe quantum dots. The temperature was raised to 315 ℃, 10mL of anhydrous toluene was injected into the reaction solution after 20min, and the heating mantle was removed. The length and the diameter of the four feet in the reaction process are respectively regulated and controlled through the injection amount and the reaction time of the sphalerite CdSe quantum dots. After the reaction liquid is cooled to room temperature, the product is repeatedly dissolved and precipitated by toluene and absolute ethyl alcohol, and then is centrifugally purified.
The preparation method of the four-footed quantum dot light-emitting film comprises the following steps:
the prepared four-footed quantum dots are uniformly mixed with organic silicon resin and heated for 1h at the temperature of 80 ℃ to obtain a mixture. The moisture permeability of the gas barrier material is preferably 1mg/m224h to 10E-4mg/ m224h, more preferably 10E-1mg/m224h to 10E-2mg/m224h, oxygen transmission rate is preferably 2mL/m224h to 10E-5mL/m 2-24 h, more preferably 10E-2mL/m224h to 10E-3mL/m2·24h；
And (3) uniformly mixing the epoxy resin with the mixture, removing bubbles, uniformly coating on a glass substrate, and curing at room temperature for 20 hours to obtain the four-footed quantum dot light-emitting film.
Example 2
(1) Preparing a cadmium precursor mixed solution: 1.61mmol of Cadmium oxide (Cadmium oxide), 3.23mmol of octadecyl phosphate (octadecenylphosphonic acid), 0.12mmol of allyl Diethyl phosphate (Diethyl phosphate) and 9.18mmol of Trioctylphosphine oxide (Trioctylphosphine oxide) were placed in a 25mL three-neck flask and heated to 120 ℃ under vacuum and degassed for 30 min. Then in N2Heat to 320 ℃ under atmosphere until a clear, transparent solution is formed.
(2) Preparing a trioctylphosphine sulfide mixed solution: mixing sulfur powder (Sulphurpowder) and Trioctylphosphine (Trioctylphosphine) at 50 deg.C for 30min under inert gas atmosphere.
(3) Preparing CdSe/CdS four-footed quantum dots: and (3) injecting the prepared 1.61mmol of trioctylphosphine sulfide into the prepared cadmium precursor mixed solution at the temperature of 300 ℃. After 40s of reaction, 10 is added-8The mol sphalerite CdSe quantum dots are injected into the zinc blende CdSe quantum dots. The temperature was raised to 315 ℃, 10mL of anhydrous toluene was injected into the reaction solution after 8min, and the heating mantle was removed. The length and the diameter of the four feet in the reaction process are respectively regulated and controlled through the injection amount and the reaction time of the sphalerite CdSe quantum dots. After the reaction liquid is cooled to room temperature, the product is repeatedly dissolved and precipitated by toluene and absolute ethyl alcohol, and then is centrifugally purified.
The preparation method of the four-footed quantum dot light-emitting film comprises the following steps:
the prepared four-footed quantum dots are uniformly mixed with organic silicon resin and heated for 1h at the temperature of 80 ℃ to obtain a mixture. The moisture permeability of the gas barrier material is preferably 1mg/m224h to 10E-4mg/ m224h, more preferably 10E-1mg/m224h to 10E-2mg/m224h, oxygen transmission rate is preferably 2mL/m224h to 10E-5mL/m 2-24 h, more preferably 10E-2mL/m224h to 10E-3mL/m2·24h；
And (3) uniformly mixing the epoxy resin with the mixture, removing bubbles, uniformly coating on a glass substrate, and curing at room temperature for 20 hours to obtain the four-footed quantum dot light-emitting film.
Example 3
(1) Preparing a cadmium precursor mixed solution: 1.61mmol of Cadmium oxide (Cadmium oxide), 3.23mmol of octadecyl phosphate (octadecenylphosphonic acid), 0.12mmol of allyl Diethyl phosphate (Diethyl phosphate) and 9.18mmol of Trioctylphosphine oxide (Trioctylphosphine oxide) were placed in a 25mL three-neck flask and heated to 120 ℃ under vacuum and degassed for 30 min. Then in N2Heat to 320 ℃ under atmosphere until a clear, transparent solution is formed.
(2) Preparing a trioctylphosphine sulfide mixed solution: mixing sulfur powder (Sulphurpowder) and Trioctylphosphine (Trioctylphosphine) at 50 deg.C for 30min under inert gas atmosphere.
(3) Preparing CdSe/CdS four-footed quantum dots: and (3) injecting the prepared 1.61mmol of trioctylphosphine sulfide into the prepared cadmium precursor mixed solution at the temperature of 300 ℃. After 40s reaction, 5 x 10-8The mol sphalerite CdSe quantum dots are injected into the zinc blende CdSe quantum dots. The temperature was raised to 315 ℃, 10mL of anhydrous toluene was injected into the reaction solution after 20min, and the heating mantle was removed. The length and the diameter of the four feet in the reaction process are respectively regulated and controlled through the injection amount and the reaction time of the sphalerite CdSe quantum dots. After the reaction liquid is cooled to room temperature, the product is repeatedly dissolved and precipitated by toluene and absolute ethyl alcohol, and then is centrifugally purified.
The preparation method of the four-footed quantum dot light-emitting film comprises the following steps:
the prepared four-footed quantum dots are uniformly mixed with organic silicon resin and heated for 1h at the temperature of 80 ℃ to obtain a mixture. The moisture permeability of the gas barrier material is preferably 1mg/m224h to 10E-4mg/ m224h, more preferably 10E-1mg/m224h to 10E-2mg/m224h, oxygen transmission rate is preferably 2mL/m224h to 10E-5mL/m 2-24 h, more preferably 10E-2mL/m224h to 10E-3mL/m2·24h；
And (3) uniformly mixing the epoxy resin with the mixture, removing bubbles, uniformly coating on a glass substrate, and curing at room temperature for 20 hours to obtain the four-footed quantum dot light-emitting film.
In summary, the invention provides a four-footed quantum dot, a preparation method thereof and a four-footed quantum dot light-emitting film. The invention obtains the four-footed quantum dot with controllable size. Due to the particularity of this structure, holes are bound in three dimensions, and electrons are bound in two dimensions. Also, in this structure, the feet, arranged quadrupedly around the core, act as a perfect "antenna" that can efficiently capture photons from any direction without any polarization treatment, while passing them into the core and releasing the photon energy in the form of radiative transitions. Therefore, the method effectively improves the luminous efficiency of the quantum dots, thereby prolonging the service life of the quantum dot luminous film to a certain extent. Meanwhile, the four-footed quantum dot light-emitting film is expected to be applied to light-emitting diodes, solid-state lighting LEDs and the like due to the excellent fluorescence property of the four-footed quantum dots and the good machining property of organic silicon resin and epoxy resin.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (5)
1. A preparation method of four-footed quantum dots is characterized in that the four-footed quantum dots take sphalerite CdSe quantum dots as cores to grow cadmium sulfide nanorods, and comprises the following steps:
A. preparing a cadmium precursor mixed solution: mixing a cadmium source, an organic ligand and a cadmium coating agent to obtain a mixed solution, heating the mixed solution to 110-180 ℃ in vacuum, degassing for 20-60 min, and heating the degassed mixed solution to 280-330 ℃ in an inert atmosphere until a clear and transparent solution is formed;
B. preparing a sulfur precursor mixed solution: under inert atmosphere, mixing and stirring a sulfur source and a sulfur coating agent at 45-55 ℃ for 25-35 min;
C. preparing CdSe/CdS four-footed quantum dots: injecting the prepared sulfur precursor mixed solution into the prepared cadmium precursor mixed solution at the temperature of 280-310 ℃; after reacting for 5-120 s, injecting the prepared sphalerite CdSe quantum dots; raising the temperature to 310-350 ℃, injecting anhydrous toluene after 5-25 min, and stopping heating; after the reaction liquid is cooled to room temperature, repeatedly dissolving and precipitating the product, and centrifugally purifying;
the cadmium source is cadmium oxide, the organic ligand is a mixture of octadecyl phosphate and allyl diethyl phosphate, and the cadmium coating agent is trioctylphosphine oxide;
the mixing molar ratio of the cadmium oxide, the octadecyl phosphate, the allyl diethyl phosphate and the trioctylphosphine oxide is (1-2): 3-5): 0.1-0.3): 9-12;
the sulfur coating agent is trioctylphosphine; the mixing molar ratio of the sulfur powder to the trioctylphosphine is 1:1-1: 5.
2. The method for preparing the four-footed quantum dot according to claim 1, wherein the molar ratio of the cadmium oxide, the octadecyl phosphate, the allyl diethyl phosphate and the trioctylphosphine oxide is 1.61:3.23:0.12: 9.18.
3. The method for preparing the quadruped quantum dot according to the claim 1, wherein in the step C, the product is repeatedly dissolved by toluene and absolute ethyl alcohol.
4. A preparation method of a four-footed quantum dot luminescent film is characterized by comprising the following steps:
E. mixing the four-footed quantum dots with organic silicon resin, and heating at 50-100 ℃ for 0.5-2 h to obtain a mixture;
F. e, uniformly mixing epoxy resin with the mixture obtained in the step E, removing bubbles, uniformly coating the mixture on a substrate, and curing at room temperature for 10-30 hours to obtain the four-footed quantum dot light-emitting film;
the four-footed quantum dot is prepared by the preparation method of the four-footed quantum dot according to any one of claims 1 to 3.
5. A four-footed quantum dot luminescent film, which is prepared by the method for preparing the four-footed quantum dot luminescent film according to claim 4.
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