CN114958369B - Organic silicon coated quantum dot material and preparation method and application thereof - Google Patents

Organic silicon coated quantum dot material and preparation method and application thereof Download PDF

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CN114958369B
CN114958369B CN202210677537.6A CN202210677537A CN114958369B CN 114958369 B CN114958369 B CN 114958369B CN 202210677537 A CN202210677537 A CN 202210677537A CN 114958369 B CN114958369 B CN 114958369B
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CN114958369A (en
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陈家立
陈锦全
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Guangdong Odiming Photoelectric Technology Co ltd
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Abstract

The invention relates to the field of photoelectric display materials, in particular to an organic silicon coated quantum dot material and a preparation method and application thereof. The organic silicon coated quantum dot material comprises the following components in percentage by mass: 0.01 to 1 percent of quantum dot kernel is coated with organosilicon polymer on the surface of the quantum dot kernel. The quantum dot material prepared by the method has excellent long-term preservation performance, avoids the loss phenomenon of the quantum dot material under the common condition, effectively isolates air and moisture, eliminates surface defects, greatly improves the chemical stability of the quantum dot material, has wider application range and application field, and is suitable for popularization in the photoluminescence field.

Description

Organic silicon coated quantum dot material and preparation method and application thereof
Technical Field
The invention relates to the field of photoelectric display materials, in particular to an organic silicon coated quantum dot material and a preparation method and application thereof.
Background
The quantum dot is a polymer composed of a certain number of atoms, the particle size of the quantum dot is small (1-100 nm), the quantum dot is influenced by small size effect, surface effect, quantum size effect, quantum confinement effect and the like, the quantum dot has good optical properties such as wide absorption peak, narrow emission peak, high luminous efficiency and the like, the application research of quantum dot materials is mainly in the fields of photoluminescence and electroluminescence, and quantum dot photoluminescence devices are being applied to high-color-quality illumination light sources and high-color-gamut display backlight sources. Especially in the display field, the emission spectrum of the quantum dot has narrow half-peak width, high color saturation and strong color reduction capability, thereby greatly improving the display color gamut and being one of the most potential luminescent materials at present.
However, the quantum dots are easily decomposed and reacted with oxygen and water under the irradiation of high temperature or ultraviolet light due to lattice defects on the surfaces of the quantum dots, so that the deterioration and failure of the quantum dots are caused, and the application of the quantum dots in the commercial field is limited.
The prior art (CN 201210264411.2) provides a method for preparing a photoluminescence quantum dot, which adopts solid residues obtained by squeezing soybeans as a raw material to prepare a carbon quantum dot, and mainly adopts a low-temperature heating carbonization method to prepare a photoluminescence quantum dot material, but the whole scheme does not effectively solve the problems that the carbon quantum dot material cannot be stored for a long time and the optical performance is damaged due to the problems of surface lattice defects and the like.
Therefore, in order to solve the above technical problems, the present application provides a quantum dot material coated with silicone.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a quantum dot material coated with silicone, which comprises the following components by mass: 0.01 to 1 percent of quantum dot core is coated with organosilicon polymer on the surface of the quantum dot core.
Preferably, the content of the quantum dot core is 0.03-0.5%.
Preferably, the content of the quantum dot core is 0.05-0.1%.
As a preferable scheme, the thickness of the organosilicon polymer coated on the surface of the quantum dot core is 1-100 μm; the content of the organic silicon polymer is 99.5-99.99% by mass percentage.
Preferably, the thickness of the organosilicon polymer coated on the surface of the quantum dot core is 1-50 μm.
Preferably, the thickness of the organosilicon polymer coated on the surface of the quantum dot core is 1-10 μm.
As a preferable scheme, the organosilicon polymer is coated on the surface of the quantum dot core by either a uniform-thickness shell layer or an amorphous shell layer.
As a preferable scheme, the organosilicon polymer is coated on the surface of the quantum dot core by a uniform-thickness shell layer.
Preferably, the quantum dot core is a compound nanocrystal composed of group II to group IV atoms with an average particle size of 1 to 100 nm.
Preferably, the quantum dot core is a compound nanocrystal consisting of group II to group IV atoms with the average particle diameter of 15 to 60 nm.
In a preferred embodiment, the compound composed of group II to group IV atoms is at least one of cesium halide, lead halide, tin halide, zinc halide, indium halide, cadmium halide, nickel halide, and technetium halide.
More preferably, the group II to group IV atomic composition compound includes at least PbBr 2 And MABr; the PbBr is 2 And MABr 2 The mass ratio of (A) to (B) is 1-2: 1 to 2.
As a most preferred embodiment, the group II to group IV atom compound is PbBr 2 CsBr/NiCl, MABr, the mass ratio of the three is 1.8: 2-2.5: 1.5 to 2.
In a preferred embodiment, the silicone monomer in the silicone polymer is at least one of trialkoxysilane, triethoxysilane, gamma-propyltrimethoxysilane, gamma-aminopropyltriethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, trifluoropropyltrimethoxysilane, vinyltrialkoxysilane, gamma-chloropropyltriethoxysilane, trialkoxychloromethylsilane, tetraethoxysilane, phenyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
As a preferred embodiment, the organosilicon monomer comprises at least a trifunctional silane and a dimer silane; the molar ratio of the trifunctional silane to the dimer silane is 1-200.
In a preferred embodiment, the molar ratio of the trifunctional silane to the dimeric silane is 1.
In a preferred embodiment, the organosilicon monomers are methyldiethylsiloxane and dimethylphenylsiloxane.
In the application, the uniform polymer shell layer of the quantum dot material is coated, the content of the quantum dot material and the monomer proportion in the polymer shell layer are further limited, the chemical stability of the quantum dot material is effectively improved, the storage stability of the quantum dot material is enhanced, the surface defects are repaired, the application environment of the quantum dot material is expanded, and the quantum dot material has excellent resin compatibility. The applicant believes that: the coating method of the organic silicon polymer with uniform thickness can effectively fill the surface defect pores of the quantum dot material, and is used as a protective layer to isolate air and moisture, so that the chemical potential energy of the surface of the quantum dot is eliminated, and the surface of the low-friction-coefficient composite particle with low surface energy is formed; on the other hand, the degree of spontaneous exothermic reaction in the preparation process of the composite quantum dot material is effectively controlled by adding the reaction raw materials, especially the quantum dots, and the proportion of the organic silicon monomer, so that the influence of local over-high temperature on the thermal decomposition of the quantum dot core is avoided, the effective proceeding of the reaction is ensured, and the generation of the final product is realized.
The invention provides a preparation method of the organic silicon coated quantum dot material, which comprises the following steps: (1) Putting the quantum dot kernel in an organic solvent, and heating for 1-10 hours at 25-180 ℃ to obtain a quantum dot solution; (2) Putting the quantum dot solution into deionized water, keeping the temperature and stirring for 1-20 minutes; (3) Adding and mixing organic silicon monomers, adding a catalyst, heating to 50-80 ℃, and stirring for 1-5 hours under heat preservation; (4) And after the reaction is finished, performing centrifugal separation, drying at low temperature, and removing water and the organic solvent to obtain the catalyst.
As a preferred scheme, a prehydrolyzed silicone monomer is also added in the step (2).
As a preferred scheme, the catalyst is an acidic or basic aqueous solution containing H + or OH-.
In a preferred embodiment, the catalyst is an alkaline solution with a pH greater than 10.
In a preferred embodiment, the organic solvent is any one of benzoyl peroxide, acetone, toluene, polyacrylamide, polyvinylpyrrolidone, polyvinyl alcohol, polyethylene oxide, and polyethylene glycol.
The invention provides an application of the organic silicon coated quantum dot material and a photoluminescence device comprising the organic silicon coated quantum dot material.
As a preferable scheme, the raw materials of the photoluminescence device at least comprise 0.1-1 wt% of the organosilicon coated quantum dot material.
The preparation method of the photoluminescence device comprises the following steps: (1) Fully mixing the organic silicon coated quantum dot material and the organic resin base material particle material according to the mass fraction ratio of 1; (2) After uniform mixing, pouring the mixture into an extruder, and heating the mixture in sections by a multi-section high-temperature machine barrel at 75-300 ℃ until the mixture is melted into a viscous state; (3) The viscous state mixture is shaped by a mould to form a sheet with the thickness of 0.1-10 mm; (4) And cutting the sheet material in sections after passing through a cooling frame to obtain the photoluminescence sheet material containing the quantum dot material coated by the organic silicon.
In a preferred embodiment, the organic resin substrate may be at least one of polycarbonate, polymethyl methacrylate, polystyrene, polyethylene, polypropylene, and polyethylene terephthalate.
As a preferred scheme, the photoluminescence device containing the organic silicon coated quantum dot material is prepared, and the organic silicon coated quantum dot material is coated between two sheets of materials, and the method comprises the following steps: (1) Fully mixing the quantum dot material coated with the organic silicon with a photocuring glue according to the mass fraction ratio of 1-10; (2) Coating glue containing the quantum dot material coated with the organic silicon between two sheets of sheet materials through a coating machine and compacting through a roller, wherein the thickness of the coating is 1-100 mu m; (3) Irradiating the sheet material for 10-1000 s by an ultraviolet machine to cure the glue; (4) And cutting the glue in sections after the glue is cured to obtain the photoluminescence sheet containing the quantum dot material coated by the organic silicon.
As a preferable scheme, the photo-curing glue is any one of polyurethane glue, polyacrylate glue and epoxy resin glue.
As a preferable mode, the sheet material may be any one of glass, polycarbonate, polymethyl methacrylate, polystyrene, polyethylene, polypropylene, and polyethylene terephthalate.
Has the beneficial effects that:
1. the quantum dot material coated with the organic silicon prepared in the application has excellent long-term storage performance, avoids the loss phenomenon of the quantum dot material under the common condition, effectively isolates air and moisture, eliminates surface defects, greatly improves the chemical stability of the quantum dot material, and has wider application range and application field.
2. According to the quantum dot material coated with the organic silicon, the uniform polymer shell layer of the quantum dot material is coated, the content of the quantum dot material and the proportion of monomers in the polymer shell layer are further limited, the chemical stability of the quantum dot material is effectively improved, the storage stability of the quantum dot material is enhanced, the surface defects are repaired, the application environment of the quantum dot material is expanded, and the quantum dot material has excellent resin compatibility.
3. The application also specifically provides a photoluminescence device containing the quantum dot material coated with the organic silicon, and the quantum dot material and the matrix resin material in the prepared photoluminescence device have excellent compatibility effect due to the hybridization phenomenon formed by the bonding effect, so that various optical properties of the photoluminescence device can be greatly improved.
Drawings
Fig. 1 is a schematic view of a core-shell structure of a quantum dot material prepared in the present application.
Fig. 2 is a schematic view of a multilayer structure of a sheet-like photoluminescent device comprising quantum dot material prepared according to the present application.
Fig. 3 is a schematic view of a single layer structure of a sheet-like photoluminescent device comprising quantum dot material prepared according to the present application.
In the figure: 1-quantum dot inner core, 2-organic silicon polymer, 3-organic silicon coated quantum dot material, 4-sheet organic base material, 5-supporting protective layer and 6-fluorescent glue layer.
Detailed Description
Example 1
Embodiment 1 provides in a first aspect a silicone coated quantum dot material, comprising, in mass percent: 0.5 percent of quantum dot kernel and 99.5 percent of organic silicon polymer with a uniform thickness shell layer coated on the surface of the quantum dot kernel.
The shell layer of the organosilicon polymer is 2 μm thick. The quantum dot kernel is PbBr with the average grain diameter of 25nm 2 Mixed quantum dot material of CsBr and MABr, pbBr 2 And the mass ratio of CsBr to MABr is 1.8:2:1.5.
the organic silicon monomer in the organic silicon polymer is methyl diethyl siloxane and dimethyl phenyl siloxane, and the molar ratio of the methyl diethyl siloxane to the dimethyl phenyl siloxane is 1:1.5.
in a second aspect of this embodiment, a method for preparing the above silicone-coated quantum dot material is provided, which includes the following steps: (1) 100ml of polyvinylpyrrolidone was heated to 40 ℃ and the quantum dot material: 1.8g of PbBr 2 、2gCsBr、1.5gMaBr 2 Putting the polyvinylpyrrolidone into the reactor for pre-reaction, and reacting for 1 hour under the condition of heat preservation to obtain a quantum dot solution; (2) Heating 10L of deionized water to 40 ℃, putting 10wt% of methyl diethylsiloxane and dimethyl phenylsiloxane into the deionized water, putting 60mL of ammonia water and stirring, and controlling the using amount of the ammonia water to enable an organic siloxane monomer to be subjected to prehydrolysis under the weak alkaline condition; (3) Putting the quantum dot solution obtained in the step (1) into the organic siloxane-containing deionized water obtained in the step (2) and stirring for 10 minutes; (4) The remaining methyldiethylsiloxane and dimethylphenylsiloxane are added slowly over 60 minutes and stirring is continued for 100 minutes; (5) And (4) filtering the mixed solution obtained in the step (4) through a 10000-mesh filter membrane, and conveying filter residues to a low-temperature dryer to remove residual water to obtain the filter cake.
Example 2
The embodiment of the present invention is different from embodiment 1 in that: the average grain diameter of the quantum dot material is 45nm, and the quantum dot material is PbBr 2 Mixed quantum dots of NiCl, MABrMaterial, pbBr 2 The mass ratio of NiCl to MABr is 1.8:2.5:2.
example 3
In a first aspect, this embodiment provides a photoluminescent device comprising the silicone-coated quantum dot material prepared in example 1, and the structure is shown in fig. 2, and includes two side supporting protective layers 5 and a middle fluorescent glue layer 6, where the thickness of the supporting protective layer 5 is 0.5mm, and the thickness of the fluorescent glue layer 6 is 200 μm.
A second aspect provides a method of making a photoluminescent device, the steps comprising: (1) Mixing an organosilicon-coated quantum dot material epoxy resin (EP, the epoxy equivalent is 205) iodonium salt cationic photoinitiator according to a mass fraction ratio of 1; (2) Injecting the photo-curing epoxy resin jelly obtained in the step (1) into a coating machine, coating the jelly between two sheets in a roller coating mode, compacting by an upper roller and a lower roller, setting the rotating speed to be 10r/min, and adjusting the discharging speed to enable the thickness of the coating to be 20 microns; (3) Irradiating the sheet material obtained in the step (2) for 20s through UV to enable the glue to be cured, and enabling Si-O and C-C to generate in-situ chemical crosslinking reaction; (4) And (4) cutting the sheet material obtained in the step (3) in a segmented manner to obtain the photoluminescence sheet material containing the quantum dot material coated by the organic silicon.
The sheet material is transparent polyethylene terephthalate.
Example 4
In a first aspect, this embodiment provides a photoluminescent device including the organic silicon-coated quantum dot material prepared in embodiment 1, and the structure of the photoluminescent device is as shown in fig. 3: the organosilicon-coated quantum dot material 3 is dispersed in a sheet-like organic base material 4.
A second aspect provides a method for preparing the above photoluminescent device, comprising the steps of: (1) Placing the organic silicon coated quantum dot material and the organic resin base material particle material into a throwing mixer according to the mass fraction ratio of 1; (2) Pouring the mixture obtained in the step (1) into a double-screw plastic extruder, and heating the mixture in a segmented manner by a multi-segment heating machine barrel, wherein the heating machine barrel is divided into 6-10 segments, and the ratio of the section of the machine barrel 1:120 ℃, barrel 2:150 ℃, barrel 3:180 ℃, barrel 4:220 ℃, barrel 5:210 ℃, barrel 6:190 ℃ until the mixture is melted into viscous state; (3) Extruding the viscous state mixture forwards through a screw to a die for extrusion, forming into viscous flow with the thickness of 2mm, and then cooling and extruding into a sheet through a three-roller structure; (4) And (4) cooling the sheet obtained in the step (3) to room temperature through a cooling rack, and cutting the sheet in sections to obtain the photoluminescence sheet containing the quantum dot material coated by the organic silicon.
Comparative example 1
This comparative example is similar to example 3, except that: in the organic silicon coated quantum dot material, the mass ratio of lead bromide to cesium bromide to MABr is 0.5:2:1.
comparative example 2
This comparative example is similar to example 3, except that: in the organic silicon coated quantum dot material, the organic silicon monomer is methyl diethyl siloxane.
Evaluation of Properties
And (3) aging test: the samples 3 and 4 were subjected to a spectrum test using SRC-600 spectrometer manufactured by Hangzhou remote corporation, and the samples were subjected to a constant temperature and humidity aging test to measure the external quantum efficiency thereof at regular intervals, and the average value of the test results was 10 times as shown in Table 1 below.
TABLE 1
Figure BDA0003695346830000091
Figure BDA0003695346830000101
Through the embodiment, the comparative example and the table 1, the organosilicon-coated quantum dot material provided by the invention has excellent long-term storage performance, avoids the loss phenomenon of the quantum dot material under the common condition, effectively isolates air and moisture, eliminates surface defects, greatly improves the chemical stability of the quantum dot material, has wider application range and application field, is suitable for popularization in the photoluminescence field, and has wide development prospect.

Claims (4)

1. A preparation method of an organosilicon-coated quantum dot material is characterized by comprising the following steps: the method comprises the following steps: (1) 100ml of polyvinylpyrrolidone was heated to 40 ℃ and the quantum dot material: 1.8g of PbBr 2 、2gCsBr、1.5gMaBr 2 Putting the polyvinylpyrrolidone into the reactor for pre-reaction, and reacting for 1 hour under the condition of heat preservation to obtain a quantum dot solution; (2) Heating 10L of deionized water to 40 ℃, adding 10wt% of organic siloxane monomer into the deionized water, adding 60mL of ammonia water, stirring, and controlling the using amount of the ammonia water to enable the organic siloxane monomer to be subjected to prehydrolysis under the alkalescent condition; (3) Putting the quantum dot solution obtained in the step (1) into the organic siloxane-containing deionized water obtained in the step (2) and stirring for 10 minutes; (4) Slowly adding the remaining organosiloxane monomer over 60 minutes and continuing to stir for 100 minutes; (5) Filtering the mixed solution obtained in the step (4) through a 10000-mesh filter membrane, and sending filter residues to a low-temperature dryer to remove residual moisture to obtain the filter cake;
the mass percentage content of the quantum dot material is 0.5%;
the organic siloxane monomer is methyl diethyl siloxane and dimethyl phenyl siloxane, and the mass ratio of the methyl diethyl siloxane to the dimethyl phenyl siloxane is 1.
2. The organosilicon-coated quantum dot material prepared by the method for preparing the organosilicon-coated quantum dot material according to claim 1.
3. Use of the silicone-coated quantum dot material of claim 2, wherein: application of a photoluminescence device comprising the organosilicon coated quantum dot material.
4. Use of the silicone-coated quantum dot material according to claim 3, characterized in that: the raw materials of the photoluminescence device at least comprise 0.1 to 1wt% of quantum dot materials coated by organic silicon.
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