CN115537008B - Mixed quantum dot diffusion plate and preparation method thereof - Google Patents
Mixed quantum dot diffusion plate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a mixed quantum dot diffusion plate which is formed by mixing, melting and extruding mixed quantum dots and organic polymers. The mixed quantum dots are formed by mixing a plurality of quantum dots with different components and different sizes, and are uniformly dispersed in an organic polymer matrix. Cd of different sizes and different x-components for several quantum dots constituting a hybrid quantum dot 1‑x Zn x Se luminous core, znSe shell layer composition wrapped outside luminous core and Cd 1‑x Zn x In x in Se luminous core, 0<x≤1；Cd 1‑x Zn x The size of the Se light-emitting core is in the range of 2.7-nm-3.5-nm. By mixing quantum dot light emitting cores with various components and sizes in the diffusion plate, different excitation wavelengths and colors are obtained, and quantum dots with different components or sizes can be excited when blue light passes through the mixed quantum dot diffusion plate, so that different excitation peaks from green light to red light wave bands are obtained, and white light with higher color gamut is obtained.
Description
Technical Field
The invention belongs to the technical field of quantum dot optics, and particularly relates to a quantum dot diffusion plate and a preparation method thereof.
Background
The light diffusion plate generally uses chemical or physical means to make light encounter two mediums with different refractive indexes in the middle of the path, and the physical phenomena of refraction, reflection and scattering occur. By adding inorganic or organic light diffusion agent into the base material with good light transmittance high molecular polymer or artificially adjusting light rays through the array arrangement of micro-characteristic structures on the surface of the base material, the light rays are refracted, reflected and scattered in different directions, so that the light travelling route is changed, and the effect of fully scattering the incident light to generate optical diffusion is realized. Light diffusion plates are widely used in liquid crystal display, LED lighting and imaging display systems.
The stimulated emission of the quantum dots has the characteristics of narrow half-peak width of an emission line, high color purity, good light stability and the like, and can improve the optical performance of the diffusion plate. The quantum dot with the core-shell structure takes a material with a narrow forbidden band, such as CdSe, as a luminescent core, and takes a material with a relatively wide forbidden band, such as ZnSe, as a shell layer, so that the fluorescence quenching can be effectively reduced, and the quantum yield can be improved.
Disclosure of Invention
Based on the prior art, the invention aims to provide the mixed quantum dot diffusion plate, by changing the size and the components of the quantum dot luminous cores in the diffusion plate, different excitation wavelengths and colors can be obtained, white light with higher color gamut can be realized, and the luminous efficiency of the diffusion plate can be improved.
In order to achieve the above object, the present invention adopts the following technical scheme.
The invention provides a mixed quantum dot diffusion plate, wherein the mixed quantum dots are composed of quantum dots with different components and different sizes; the mixed quantum dot diffusion plate is composed of mixed quantum dots and organic polymers, is formed by mixing, melting and extruding the mixed quantum dots and the organic polymers, and the different components forming the mixed quantum dots and the quantum dots with different sizes are uniformly dispersed in the organic polymer matrix.
Wherein the organic polymer is selected from one or more of PC (polycarbonate), PVC (polyvinyl chloride), PS (polystyrene), PMMA (polymethyl methacrylate), PET (polyethylene terephthalate) or epoxy resin.
More specifically, the mixed quantum dot consists of Cd with different sizes and different x components 1-x Zn x Se luminous core and ZnSe shell layer wrapping the luminous core. Wherein the ZnSe shell has a thickness of 2-4 nm. Cd with different sizes and components in mixed quantum dots 1-x Zn x The Se luminous core can enable the mixed quantum dot luminous wave band in the diffusion plate to realize continuous regulation and control within the range of 460-680 and nm. And the mixed quantum dots with the optimal mixing ratio can be formed by controlling the process in the manufacturing process of the mixed quantum dot diffusion plate, so that the mixed quantum dots can be mixed with high-quality white light after being excited by blue light. Meanwhile, the coated ZnSe shell reduces dangling bonds on the surface of the core, passivates the luminous core and improves the quantum yield; on the other hand, cd in the core and Zn in the shell layer can generate ion exchange, and an alloy layer is formed at the interface, so that the lattice mismatch degree of the core/shell is reduced, the lattice stress is reduced, and the luminous efficiency of the quantum dot is improved.
Further, the different x components: refers to Cd 1-x Zn x The value of x in Se luminous core is continuously adjustable, wherein 0<x is less than or equal to 1; the different dimensions: meaning that the mixed quantum dot contains Cd with various sizes 1-x Zn x Cd of Se light-emitting core 1-x Zn x Se/ZnSe quantum dots, cd of said plurality of sizes 1-x Zn x The size of Se light-emitting core is in the range of 2.7-nm-3.5-nm.
More specifically, the molar ratio of the quantum dots of different x components in the mixed quantum dot is 0< x less than or equal to 0.3, and the molar ratio of the quantum dots in the mixed quantum dot is 20% -40%; x is less than or equal to 0.3 and less than or equal to 0.6, the ratio of the mixed quantum dots is 20-40%, x is less than or equal to 0.6 and less than or equal to 1, and the ratio of the mixed quantum dots is 20-40%.
Correspondingly, cd with different sizes in the mixed quantum dots 1-x Zn x Se/ZnSe quantum dots, cd thereof 1-x Zn x Size distribution of Se light-emitting core and Cd light-emitting core 1-x Zn x The x component of Se is related, specifically: when 0 is<When x is less than or equal to 0.3, more than 80 percent of Cd 1- x Zn x The size of Se luminous core is between 2.7 and 3.1 and nm; when 0.3<When x is less than or equal to 0.6, more than 80 percent of Cd 1-x Zn x The Se luminous core has a size of 3.0-3.4nm, 0.6<When x is less than or equal to 1, 80% or more of Cd 1-x Zn x The size of Se light-emitting core is 3.2-3.5. 3.5nm. According to repeated actual measurement of the inventor in the research, for the quantum dot luminous cores of the same component, the excitation wavelength can generate 50-10 nm red shift along with the increase of the size of the quantum dot in the parameter range of the invention.
In the mixed quantum dot diffusion plate, the mass ratio of the mixed quantum dots to the organic polymer is 0.15-0.225%.
Further, the thickness of the mixed quantum dot diffusion plate is 2-30mm.
The mixed quantum dot diffusion plate adopts Cd 1-x Zn x Quantum dot with Se/ZnSe core-shell structure and Cd 1- x Zn x Se is used as a luminescent core, compared with the conventional CdSe/ZnSe core-shell structure quantum dot, the quantum dot can reduce the lattice mismatch stress of a core/shell interface and improve the quantum yield. Further, by using Cd of different composition and different size in the diffusion plate 1-x Zn x Se/ZnSe mixed quantum dots to form quantum dot luminous cores with different components and sizes, and quantum dots with different excitation wavelengths and colors are obtained by mixing the quantum dots with various components and sizes in a diffusion plate. When blue light passes through the mixed quantum dot diffusion plate, cd with different x components and different sizes can be excited 1-x Zn x Se/ZnSe mixed quantum dots, so that different excitation peaks from green light to red light wave bands are obtained, and white light with higher color gamut is obtained.
The invention also provides a preparation method of the mixed quantum dot diffusion plate, which comprises the following steps:
s1, mixing Cd in quantum dots 1-x Zn x Preparation of Se-emitting core
S11 preparation of the first Se precursor
Mixing Se powder with Octadecene (ODE) in a proportion of 0.4mmol/ml, carrying out ultrasonic oscillation at 60 ℃ for 30 minutes, and dispersing to obtain a first Se precursor for later use.
S12. Cd of different composition and different size 1-x Zn x Preparation of Se luminous core stock solution
CdO and Zn (Ac) 2 Mixing according to a molar ratio of 1:1; then with Zn (Ac) 2 1mmol/ml, oleic Acid (OA) was added; vacuumizing to 5pa, and adding ODE according to the volume ratio of the ODE to the OA of 10:1; heating the mixed liquid to 240-300 ℃, and mixing according to the volume ratio of 1:1 part of the first Se precursor in the step S11 is added to start the reaction; at 4, 6, 8, 10, 15, 20, and 30 minutes after the start of the reaction, zn (Ac) was sequentially added to the reaction mixture 2 ratio/CdO (2-30): 1 molar ratio and adding OA-activated Zn (Ac) 2 After the complete reaction, the X component is obtained to be 0<Cd with size between 2.7 and 3.5nm and increasing gradually between x and 1 1-x Zn x Cd of Se/ZnSe mixed quantum dot 1-x Zn x Se luminescent nuclear stock solution;
wherein the OA-activated Zn (Ac) 2 The method comprises the following steps: in Zn (Ac) 2 In Zn (Ac) 2 1mmol/ml, OA was added.
S13.Cd 1-x Zn x Se luminous core stock solution purification
Firstly, taking the Cd prepared in the step S12 1-x Zn x Centrifuging Se luminous core stock solution in a high-speed centrifuge;
dissolving the supernatant in n-hexane, adding absolute ethanol to promote precipitation, centrifuging for 2-3 times, collecting supernatant, promoting precipitation, dissolving the precipitate in a small amount of n-hexane solution, and sealing for storage to obtain Cd 1-x Zn x Purifying the Se luminous core stock solution;
the synthesized Cd is subjected to the following cladding process 1-x Zn x The Se luminous core stock solution is subjected to purification treatment to remove redundant Zn and impurities in the nucleation reaction process.
S2. Cd 1-x Zn x Synthesis of Se/ZnSe core-shell mixed quantum dot
S21, preparation of second Se precursor
Mixing Se powder with tri-n-octyl phosphine (TOP) at a ratio of 1mmol/ml, loading into a closed container, vacuumizing to 5Pa, filling inert gas for protection, stirring and heating to 80 ℃ until the Se powder is completely dissolved, and cooling to room temperature to obtain a second Se precursor for later use.
S22. Cd 1-x Zn x Synthesis of Se/ZnSe mixed quantum dots
The Cd obtained in the step S13 1-x Zn x Adding ODE into Se luminous core purification stock solution to prepare Cd of 1 nmol/mL 1-x Zn x Stirring Se luminescent core ODE diluent for multiple times under the protection of argon/nitrogen, heating to 300 ℃, adding the second Se precursor, and preparing the Se luminescent core ODE diluent according to Cd 1-x Zn x Adding Se luminous core ODE diluent and a second Se precursor in a volume ratio of 1.3:1; then slowly adding Zn precursor dropwise at a dropwise speed of 4mL/h to finally generate Cd 1-x Zn x Se/ZnSe hybrid quantum dots. Wherein the thickness of the ZnSe shell is controlled to be 2-4nm by controlling the dripping time of the Zn precursor. Wherein the Zn precursor refers to 0.3M zinc oleate Zn (OA) 2 。
S3, preparing a mixed quantum dot diffusion plate
The Cd obtained in the step S22 1-x Zn x The Se/ZnSe mixed quantum dots are mixed and melted with one or more of PC, PVC, PS, PMMA, PET and epoxy resin in a mode of mechanical stirring and ultrasonic vibration, and a diffusion plate is formed by extrusion, wherein the thickness of the diffusion plate is 2-30mm.
Compared with the prior art, the invention has the following beneficial effects:
(1) The fluorescence emission wavelength of the alloy quantum dot is regulated and controlled by changing the components of chemical element compositions in the alloy quantum dot. Alloy structure Cd 1-x Zn x The lattice structure and the forbidden band width of the Se quantum dot core are between ZnSe and CdSe，Cd 1-x Zn x The Se/ZnSe core-shell structure has small lattice mismatch degree, and the stability and fluorescence quantum yield of the quantum dots are improved.
(2) When blue light passes through the diffusion plate, cd with different x components and different sizes is excited 1-x Zn x The Se/ZnSe mixed quantum dots can obtain different excitation peaks from green light to red light wave bands, and can obtain white light with higher color gamut.
Drawings
Fig. 1 is a schematic structural diagram of a mixed quantum dot diffusion plate according to various embodiments of the present invention.
Wherein 01 is mixed quantum dot and 02 is organic polymer.
Detailed Description
The invention is described in further detail below with reference to the attached drawings and detailed description:
example 1:
1. hybrid quantum dot core Cd 1-x Zn x Preparation of Se
(1) Preparation of first Se precursor
Mixing Se powder with Octadecene (ODE) in a proportion of 0.4mmol/ml, carrying out ultrasonic oscillation at 60 ℃ for 30 minutes, and dispersing to obtain a first Se precursor for later use.
(2) Cd of different composition and different size 1-x Zn x Preparation of Se quantum dot nuclear stock solution
CdO and Zn (Ac) 2 Mixing according to a molar ratio of 1:1; with Zn (Ac) 2 1mmol/ml, oleic Acid (OA) was added; vacuumizing to 5pa, and adding ODE according to the volume ratio of the ODE to the OA of 10:1; the temperature of the secondary liquid is raised to 240 ℃, and the volume ratio is 1:1 part of the first Se precursor is added, and after 4, 6, 8, 10, 15, 20 and 30 minutes from the start of the reaction, zn (Ac) is sequentially added 2 CdO ratio 2:1 molar ratio and adding OA-activated Zn (Ac) 2 After the last addition, the reaction was carried out for a further 2 minutes and ended, which is to give Cd having a different x-component and size 1-x Zn x Se mixed quantum dot nuclear stock solution. Wherein the OA-activated Zn (Ac) 2 The method comprises the following steps: in Zn (Ac) 2 In Zn (Ac) 2 1mmol/ml, addOA is entered.
Through test analysis, zn (Ac) after OA activation is added into the obtained mixed quantum dot at different time points 2 The composition and size distribution of the obtained mixed quantum dots are as follows:
(3)Cd 1-x Zn x se quantum dot nuclear stock solution purification
(the purification treatment is carried out on the synthesized CdZnSe nuclear quantum dots before the subsequent cladding process, so as to remove redundant Zn and impurities in the nucleation reaction process.) the prepared nuclear stock solution is firstly taken and centrifuged in a high-speed centrifuge. Then the supernatant is taken and dissolved in normal hexane, absolute ethyl alcohol is added to promote precipitation, and the obtained precipitate is dissolved in a small amount of normal hexane solution for sealing and preservation after 2-3 times of centrifugation.
2. Cd 1-x Zn x Synthesis of Se/ZnSe core-shell quantum dots
(1) Preparation of a second Se precursor
Mixing Se powder with tri-n-octyl phosphine (TOP) at a ratio of 1mmol/ml, loading into a closed container, vacuumizing to 5Pa, filling inert gas for protection, stirring and heating to 80 ℃ until the Se powder is completely dissolved, and cooling to room temperature to obtain a second Se precursor for later use.
（2）Cd 1-x Zn x Synthesis of Se/ZnSe quantum dots
Will have purified Cd 1-x Zn x Precipitating Se quantum dot nuclear stock solution to prepare ODE diluent with the concentration of 1 nmol/mL, stirring for multiple times under the protection of argon/nitrogen, heating to 300 ℃, taking the second Se precursor, and preparing the Se precursor according to Cd 1-x Zn x Adding Se luminous core ODE diluent and a second Se precursor in a volume ratio of 1.3:1; then 0.3M zinc oleate Zn (OA) is slowly added dropwise 2 Dropping speed is 4mL/h, and finally Cd is generated 1-x Zn x Se/ZnSe hybrid quantum dots. The thickness of the resulting ZnSe shell layer was about 2-4 a nm a.
3. Preparation of diffusion plate
The quantum dots are mixed and melted with one or a mixture of PC, PVC, PS, PMMA, PET and epoxy resin in a mode of mechanical stirring and ultrasonic vibration, and a diffusion plate is formed by extrusion, wherein the thickness of the diffusion plate is 2-30mm.
Example 2
1. Hybrid quantum dot core Cd 1-x Zn x Preparation of Se
(1) Preparation of first Se precursor
Mixing Se powder with Octadecene (ODE) in a proportion of 0.4mmol/ml, carrying out ultrasonic oscillation at 60 ℃ for 30 minutes, and dispersing to obtain a first Se precursor for later use.
(2) Preparation of Cd1-xZnxSe quantum dot core stock solutions with different components and different sizes
Mixing CdO and Zn (Ac) 2 according to a molar ratio of 1:1; oleic Acid (OA) was added in a proportion of Zn (Ac) 21 mmol/ml; vacuumizing to 5pa, and adding ODE according to the volume ratio of the ODE to the OA of 10:1; the temperature of the secondary liquid is raised to 240 ℃, and the volume ratio is 1:1 part of a first Se precursor is added, and after the reaction starts for 4, 6, 8, 10, 15, 20 and 30 minutes, the reaction is carried out according to a Zn (Ac) 2/CdO ratio of 15:1 molar ratio and adding OA-activated Zn (Ac) 2 After the last addition, the reaction is finished after 2 minutes of reaction, and Cd with different x components and sizes is finally obtained 1-x Zn x Se mixed quantum dot nuclear stock solution. Wherein the OA-activated Zn (Ac) 2 The method comprises the following steps: in Zn (Ac) 2 In Zn (Ac) 2 1mmol/ml, OA was added. Through test analysis, zn (Ac) after OA activation is added into the obtained mixed quantum dot at different time points 2 The composition and size distribution in the mixed quantum dots are as follows:
(3) Purification of Cd1-xZnxSe quantum dot nuclear stock solution
(the purification treatment is carried out on the synthesized CdZnSe nuclear quantum dots before the subsequent cladding process, so as to remove redundant Zn and impurities in the nucleation reaction process.) the prepared nuclear stock solution is firstly taken and centrifuged in a high-speed centrifuge. Then the supernatant is taken and dissolved in normal hexane, absolute ethyl alcohol is added to promote precipitation, and the obtained precipitate is dissolved in a small amount of normal hexane solution for sealing and preservation after 2-3 times of centrifugation.
2. Synthesis of Cd 1-xZnSe/ZnSe core-shell quantum dot
(1) Preparation of a second Se precursor
Mixing Se powder with tri-n-octyl phosphine (TOP) at a ratio of 1mmol/ml, loading into a closed container, vacuumizing to 5Pa, filling inert gas for protection, stirring and heating to 80 ℃ until the Se powder is completely dissolved, and cooling to room temperature to obtain a second Se precursor for later use.
(2) Synthesis of Cd 1-xZnSe/ZnSe quantum dots
Precipitating the core stock solution of the purified Cd1-xZnxSe quantum dot to prepare ODE diluent of 1 nmol/mL, stirring for multiple times under the protection of argon/nitrogen, heating to 300 ℃, taking the second Se precursor, and preparing the precursor according to Cd 1-x Zn x Adding Se luminous core ODE diluent and a second Se precursor in a volume ratio of 1.3:1; then 0.3M zinc oleate Zn (OA) is slowly added dropwise 2 Dropping speed is 4mL/h, and finally Cd is generated 1-x Zn x Se/ZnSe hybrid quantum dots. The thickness of the resulting ZnSe shell layer was about 2-4 a nm a.
3. Preparation of diffusion plate
The quantum dots are mixed and melted with one or a mixture of PC, PVC, PS, PMMA, PET and epoxy resin in a mode of mechanical stirring and ultrasonic vibration, and a diffusion plate is formed by extrusion, wherein the thickness of the diffusion plate is 2-30mm.
EXAMPLE 3
1. Preparation of mixed quantum dot core Cd1-xZnxSe
(1) Preparation of first Se precursor
Mixing Se powder with Octadecene (ODE) in a proportion of 0.4mmol/ml, carrying out ultrasonic oscillation at 60 ℃ for 30 minutes, and dispersing to obtain a first Se precursor for later use.
(2) Preparation of Cd1-xZnxSe quantum dot core stock solutions with different components and different sizes
Mixing CdO and Zn (Ac) 2 according to a molar ratio of 1:1; at a ratio of Zn (Ac) 21 mmol/mlFor example, oleic Acid (OA) was added; vacuumizing to 5pa, and adding ODE according to the volume ratio of the ODE to the OA of 10:1; the temperature of the secondary liquid is raised to 240 ℃, and the volume ratio is 1:1 part of the first Se precursor is added, and after 4, 6, 8, 10, 15, 20 and 30 minutes from the beginning of the reaction, zn (Ac) is added in sequence 2 / CdO 2 Ratio 30:1 molar ratio and adding OA-activated Zn (Ac) 2 After the last addition, the reaction is completed for 2 minutes to obtain Cd containing different x components and sizes 1-x Zn x Se mixed quantum dot nuclear stock solution. Wherein the OA-activated Zn (Ac) 2 The method comprises the following steps: in Zn (Ac) 2 In Zn (Ac) 2 1mmol/ml, OA was added. Through test analysis, zn (Ac) after OA activation is added into the obtained mixed quantum dot at different time points 2 The composition and size distribution in the mixed quantum dots are as follows:
(3)Cd 1-x Zn x se quantum dot nuclear stock solution purification
(the purification treatment is carried out on the synthesized CdZnSe nuclear quantum dots before the subsequent cladding process, so as to remove redundant Zn and impurities in the nucleation reaction process.) the prepared nuclear stock solution is firstly taken and centrifuged in a high-speed centrifuge. Then the supernatant is taken and dissolved in normal hexane, absolute ethyl alcohol is added to promote precipitation, and the obtained precipitate is dissolved in a small amount of normal hexane solution for sealing and preservation after 2-3 times of centrifugation.
2. Synthesis of Cd 1-xZnSe/ZnSe core-shell quantum dot
(1) Preparation of a second Se precursor
Mixing Se powder with tri-n-octyl phosphine (TOP) at a ratio of 1mmol/ml, loading into a closed container, vacuumizing to 5Pa, filling inert gas for protection, stirring and heating to 80 ℃ until the Se powder is completely dissolved, and cooling to room temperature to obtain a second Se precursor for later use.
（2）Cd 1-x Zn x Synthesis of Se/ZnSe quantum dots
Will have purified Cd 1-x Zn x Precipitating Se quantum dot nuclear stock solution to prepare ODE diluent with the concentration of 1 nmol/mL, stirring for multiple times under the protection of argon/nitrogen, heating to 300 ℃, taking the second Se precursor, and preparing the Se precursor according to Cd 1-x Zn x Adding Se luminous core ODE diluent and a second Se precursor in a volume ratio of 1.3:1; then 0.3M zinc oleate Zn (OA) is slowly added dropwise 2 Dropping speed is 4mL/h, and finally Cd is generated 1-x Zn x Se/ZnSe hybrid quantum dots. The thickness of the resulting ZnSe shell layer was about 2-4 a nm a.
3. Preparation of diffusion plate
The quantum dots are mixed and melted with one or a mixture of PC, PVC, PS, PMMA, PET and epoxy resin in a mode of mechanical stirring and ultrasonic vibration, and a diffusion plate is formed by extrusion, wherein the thickness of the diffusion plate is 2-30mm.
What has been described above is only a partial embodiment of the invention. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the structure of the present invention, and these should also be considered as the scope of the present invention, which does not affect the effect of the implementation of the present invention and the utility of the patent. The protection scope of the present application shall be subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (7)
1. The utility model provides a mixed quantum dot diffuser plate which characterized in that: the mixed quantum dot diffusion plate consists of the mixed quantum dots and an organic polymer, and is formed by mixing, melting and extruding the mixed quantum dots and the organic polymer; the mixed quantum dots are formed by mixing a plurality of quantum dots with different components and different sizes; and a plurality of quantum dots of different components and different sizes constituting the mixed quantum dot are uniformly dispersed in the organic polymer matrix;
wherein, a plurality of quantum dots in the mixed quantum dot are all Cd with different sizes and different x components 1-x Zn x A Se luminous core and a ZnSe shell layer wrapping the luminous core; wherein the different x components: refers to Cd 1-x Zn x The value of x in Se luminous core is continuously adjustable, wherein 0<x is less than or equal to 1; the different dimensions: refers to the Cd 1-x Zn x The size of Se luminous core is in the range of 2.7nm-3.5 nm;
the mixed quantum dot diffusion plate is prepared by the following steps:
s1, mixing Cd in quantum dots 1-x Zn x Preparation of Se-emitting core
S11, preparation of a first Se precursor
Mixing Se powder with octadecene in a proportion of 0.4mmol/ml, carrying out ultrasonic oscillation at 60 ℃ for 30 minutes, and dispersing to obtain a first Se precursor;
s12, cd with different components and different sizes 1-x Zn x Preparation of Se luminous core stock solution
CdO and Zn (Ac) 2 Mixing according to a molar ratio of 1:1; then with Zn (Ac) 2 1mmol/ml, oleic acid OA was added; vacuumizing to 5pa, and adding octadeceneode according to the volume ratio of the octadeceneode to the oleic acid OA of 10:1; heating the mixed liquid to 240-300 ℃, and mixing according to the volume ratio of 1:1 part of the first Se precursor in the step S11 is added to start the reaction; at 4, 6, 8, 10, 15, 20, and 30 minutes after the start of the reaction, zn (Ac) was sequentially added to the reaction mixture 2 ratio/CdO (2-30): 1 molar ratio and adding Zn (Ac) after OA activation of oleic acid 2 After the complete reaction, the X component is obtained to be 0<Cd with size between 2.7 and 3.5nm and increasing gradually between x and 1 1-x Zn x Cd of Se/ZnSe mixed quantum dot 1-x Zn x Se luminescent nuclear stock solution; wherein said oleic acid OA-activated Zn (Ac) 2 The method comprises the following steps: in Zn (Ac) 2 In Zn (Ac) 2 1mmol/ml, OA was added;
S13.Cd 1-x Zn x se luminous core stock solution purification
Firstly, taking the Cd prepared in the step S12 1-x Zn x Centrifuging Se luminous core stock solution in a high-speed centrifuge; dissolving the supernatant in n-hexane, adding absolute ethanol to promote precipitation, centrifuging for 2-3 times, collecting supernatant, and dissolving the precipitate in the final centrifugationSealing and preserving in a small amount of n-hexane solution to obtain Cd 1-x Zn x Purifying the Se luminous core stock solution;
S2.Cd 1-x Zn x synthesis of Se/ZnSe core-shell mixed quantum dot
S21, preparation of second Se precursor
Mixing Se powder with tri-n-octyl phosphine according to the proportion of 1mmol/ml, placing in a closed container, vacuumizing to 5Pa, filling inert gas for protection, stirring and heating to 80 ℃ until the Se powder is completely dissolved, and cooling to room temperature to obtain a second Se precursor;
S22.Cd 1-x Zn x synthesis of Se/ZnSe mixed quantum dots
The Cd obtained in the step S13 1-x Zn x Adding octadeceneode into Se luminous core purification stock solution to prepare Cd of 1 nmol/mL 1- x Zn x The Se luminous core ODE diluent is stirred for multiple times under the protection of argon/nitrogen, and the temperature is raised to 300 ℃; adding the second Se precursor according to Cd 1-x Zn x Adding Se luminous core ODE diluent and a second Se precursor in a volume ratio of 1.3:1; then slowly adding Zn precursor dropwise at a dropwise speed of 4mL/h to finally generate Cd 1-x Zn x Se/ZnSe hybrid quantum dots; wherein the Zn precursor refers to 0.3M zinc oleate Zn (OA) 2 ；
S3, preparing a mixed quantum dot diffusion plate
The Cd obtained in the step S22 1-x Zn x The Se/ZnSe mixed quantum dots are mixed and melted with one or more of PC, PVC, PS, PMMA, PET and epoxy resin in a mode of mechanical stirring and ultrasonic vibration, and a diffusion plate is formed by extrusion, wherein the thickness of the diffusion plate is 2-30mm.
2. The hybrid quantum dot diffusion plate of claim 1, wherein: the organic polymer is selected from one or more of PC, PVC, PS, PMMA, PET or epoxy resin.
3. The hybrid quantum dot diffusion plate of claim 1, wherein: wherein the ZnSe shell has a thickness of 2-4 nm.
4. The hybrid quantum dot diffusion plate of claim 1, wherein: the mole ratio of the quantum dots forming different x components of the mixed quantum dot is as follows: x is more than 0 and less than or equal to 0.3, and the ratio of the mixed quantum dots is 20% -40%; x is more than 0.3 and less than or equal to 0.6, and the ratio of the mixed quantum dots is 20-40%;
x is less than or equal to 1 and is 0.6 percent, and the ratio of the mixed quantum dots is 20-40 percent.
5. The hybrid quantum dot diffusion plate of claim 4, wherein: a plurality of quantum dots with different sizes forming the mixed quantum dot, and Cd thereof 1-x Zn x Size distribution of Se light-emitting core and Cd light-emitting core 1-x Zn x The x component of Se is related to: when 0 is<When x is less than or equal to 0.3, more than 80 percent of Cd 1-x Zn x The size of Se luminous core is between 2.7-3.1 nm; when 0.3<When x is less than or equal to 0.6, more than 80 percent of Cd 1-x Zn x Se luminous core size is 3.0-3.4nm, 0.6<When x is less than or equal to 1, 80% or more of Cd 1-x Zn x The size of Se luminous core is 3.2-3.5nm.
6. The hybrid quantum dot diffusion plate of claim 1, wherein: in the mixed quantum dot diffusion plate, the mass ratio of the mixed quantum dots to the organic polymer is 0.15-0.225%.
7. The hybrid quantum dot diffusion plate of claim 1, wherein: the thickness of the mixed quantum dot diffusion plate is 2-30mm.
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