CN112079955A - Quantum dot @ polymer composite material and preparation method thereof - Google Patents
Quantum dot @ polymer composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a quantum dot @ polymer composite material, which comprises a quantum dot material, a barrier material and a polymer material; the barrier material is coated outside the quantum dot material; the polymer material is coated outside the quantum dot material and the barrier material; the barrier material comprises nano-silicon, sub-silicon oxide and a carbon material. Among them, the carbon material is preferably graphene or CNT. The QD is coated with the nano-silicon, the silicon monoxide and the carbon, wherein the Si and the SiO are mainly combined with moisture and oxygen in the air to protect the quantum dots from being damaged by moisture and oxygen, and the C is mainly used for dissipating heat and resisting high temperature; the outermost polymer material plays a role in isolating water vapor and oxygen, and the main role of the outermost polymer material lies in that the quantum dots are convenient to fuse into the plastic film, the dispersibility and the bonding firmness of the quantum dots in the plastic film are improved, and the problems of precipitation and falling caused by poor fusion of the quantum dots and the plastic film are avoided.
Description
Technical Field
The invention relates to the technical field of quantum materials, in particular to a quantum dot @ polymer composite material and a preparation method and application thereof.
Background
Quantum dots are tiny semiconductor particles of several nanometers in size, with different optical and electronic properties than larger light emitting diode particles. The size of the quantum dots in three dimensions is less than 100nm, less than the Bohr radius of excitons, and can be constrained in three spatial directions so as to be limited in a nanometer space. Internal electron and hole transport is limited, the electron mean free path is short, the electron locality and coherence are enhanced, so that a quantum confinement effect is generated, and the electron energy level near the fermi level is split from continuous states into discrete levels. The forbidden band width can be adjusted by changing the size of the particles. The method has wide application in photodiodes, photodetectors, lasers, transistors and solar cells. An important advantage of quantum dots is that they are solution processable and therefore are typically fabricated into thin films by solution coating methods. However, the quantum dots are susceptible to oxygen, water vapor, high temperature and the like in the external environment, and are easily damaged and fail after being exposed to the natural environment for a long time.
In order to solve the technical problem, for example, chinese patent application CN111621287A proposes a quantum dot polymer composite film, in which a barrier film made of a high molecular polymer is respectively disposed on the upper and lower side surfaces of a quantum dot composite layer to isolate oxygen and water vapor. Although the scheme has the function of preventing the quantum dots from being rapidly attenuated due to environmental factors to a certain extent, the peripheral edge of the composite film loses the protection of the barrier film after being cut, so that the composite film fails to generate the problem of blue edges. In addition, the addition of the additional barrier film can make the thickness of the whole quantum dot polymer composite film larger, usually to about 350 um. The composite film can be normally used in larger products such as televisions and the like, but cannot be applied to thin/miniaturized equipment such as mobile phones, flat panels and the like. And the use of barrier films also leads to high material cost of the product, and according to investigation, the 3M quantum dot film is initially 300 dollars per square meter or so, and the price of 2016 is still as high as 150 dollars per square meter. Therefore, there is a need for an improved solution to the prior art.
Disclosure of Invention
Technical problem to be solved
In view of the above disadvantages and shortcomings of the prior art, the present invention provides a quantum dot @ polymer composite material and a preparation method thereof, which solves the technical problems that quantum dots are easily damaged and fail due to the influence of environmental factors such as high temperature, high humidity and oxygen, and the thickness of the quantum dot film is large and the quantum dot film is difficult to be applied to thin/miniaturized products due to the existing additionally arranged barrier film.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
in a first aspect, the present invention provides a quantum dot @ polymer composite comprising:
quantum dot materials, barrier materials, and polymeric materials;
the barrier material is coated outside the quantum dot material;
the polymer material is coated outside the quantum dot material and the barrier material;
the barrier material comprises nano-silicon, sub-silicon oxide and a carbon material.
According to a preferred embodiment of the present invention, the carbon material is graphite carbon, graphene or carbon nanotube; preferably graphene. Preferably, the carbon material is pre-modified with a coupling agent to enable it to better compatibilize with the external polymeric material. If the carbon material is CNT or graphene, not only the thermal conductivity coefficient is very high, but also a part of CNT extends the surface of the polymer material, further playing a role in thermal conduction and quantum dot protection.
According to the preferred embodiment of the invention, the mass ratio of the quantum dot material, the barrier material and the polymer material is 0.1-4:0.1-4: 8-30.
According to the preferred embodiment of the invention, the barrier material is composed of nano silicon, silicon monoxide and a carbon material, wherein the mass ratio of the nano silicon to the silicon monoxide to the carbon material is 1-2:2-3: 4-8.
According to a preferred embodiment of the invention, the polymeric material is PMMA (polymethylmethacrylate), EVOH (ethylene vinyl alcohol copolymer), PET (polyethylene terephthalate), PS (polystyrene), PVP (polyvinylpyrrolidone), LDPE (low density polyethylene) or PVDC (polyvinylidene chloride).
In another aspect, the present invention further provides a method for preparing a quantum dot @ polymer composite material, comprising:
dispersing a quantum dot material into an organic solution (liquid alcohol, such as ethanol and the like) containing a coupling agent, heating and stirring, filtering, and drying to obtain a surface modified quantum dot material;
step 2, adding a solution of water and a polymer monomer into a stirrer with a heating function, stirring and mixing uniformly, adding an oil-soluble initiator accounting for 0.5-5% of the total mass of the polymer monomer and a cross-linking agent accounting for 0.3-1%, stirring and mixing uniformly, heating to 55-100 ℃ for polymerization, and after prepolymerization is carried out for 0.5h, rapidly reducing the temperature of the system to below 30 ℃ by using an ice bath to obtain a prepolymer solution;
and step 3: adding the surface modified quantum dot material and the barrier material into a prepolymer solution, and fully stirring to uniformly mix; the barrier material comprises nano-silicon, sub-silicon oxide and a carbon material;
and 4, step 4: and (3) adding 0.1-0.8% of polyvinyl alcohol solution as a dispersing agent into the reaction system in the step (3), stirring and dispersing for 10-20 min at the rotating speed of 100-1500 rpm/min, heating to 60-100 ℃, curing for 12-24 h, and finally cooling, filtering, washing and drying to obtain the quantum dot @ polymer composite material.
Preferably, the mass ratio of the polymer monomer, the quantum dot material and the barrier material is 10-50: 0.1-5: 0.2-10; in the barrier material, the mass ratio of the nano silicon to the silicon monoxide to the carbon material is 1-2:2-3: 4-8.
In the step 1, the heating and stirring temperature is 40-60 ℃, and the time is 1-5 h; the coupling agent is one or more of KH550, KH560, KH570, KH792, DL602 and DL 171.
Preferably, the barrier material is also pre-treated with a coupling agent, the treatment method referring to the treatment method of the quantum dot material in step 1.
In step 2, the polymer monomer is a monomer of EVOH (EVOH is an ethylene/vinyl alcohol copolymer) or a monomer of PVDC (polyvinylidene chloride, the monomer of which is CCl2＝CH2). Preferably, the polymer monomer is one or a combination of more of acrylonitrile monomers, vinyl monomers, acrylates and acrylamide monomers.
EVOH is a high barrier material. EVOH is remarkably characterized by excellent barrier properties against gases and excellent processability, and is also excellent in transparency, gloss, mechanical strength, stretchability, abrasion resistance, cold resistance and surface strength. The PVDC plastic has strong intermolecular cohesive force and high crystallinity, chlorine atoms in PVDC molecules have hydrophobicity, hydrogen bonds cannot be formed, oxygen molecules and water molecules are difficult to move in the PVDC molecules, so that the PVDC plastic has excellent oxygen resistance and moisture resistance, and the oxygen resistance is not influenced by the humidity of the surrounding environment. Under any temperature or humidity condition, the plastic packaging material has excellent capability of blocking water vapor, oxygen, smell and fragrance, and is currently accepted as the plastic packaging material with the best combination of barrier property. Therefore, in the invention, the EVOH monomer or the PVDC monomer is preferably used for polymerization coating outside the quantum dot material.
In another aspect, the invention also relates to a preparation method of the plastic master batch containing the quantum dots, which comprises the following steps:
s1, stirring and mixing the quantum dot @ polymer composite material or the quantum dot @ polymer composite material prepared by the preparation method of claim 6 or 7, the master batch of the high molecular polymer material, the solvent, the light stabilizer and the surfactant to prepare a mixture;
and S2, adding the mixture into a screw extruder, and performing blending, extrusion and granulation to obtain the quantum dot-containing plastic master batch.
Preferably, the screw temperature in the screw extruder is controlled at 180 ℃ and 100 ℃, so as to avoid the carbon material in the barrier material from being oxidized due to overhigh temperature.
Preferably, the solvent is one or more of white oil, mineral oil, vegetable oil, paraffin oil and decalin.
Preferably, the surfactant is alkylolamide (6502), stearic acid, sodium dodecylbenzenesulfonate, Alkylglucoside (APG), triethanolamine, fatty acid glyceride, sorbitan fatty acid (span), polysorbate (tween), sodium dioctyl sulfosuccinate (aloso-OT), sodium dodecylbenzenesulfonate, sodium glycocholate, or the like.
Preferably, the light stabilizer is a Hindered Amine Light Stabilizer (HALS). The light stabilizer can eliminate or slow down the possibility of photochemical reaction of high molecular polymer under the radiation of light, and prevent or delay the process of photoaging, thereby achieving the purpose of prolonging the service life of the film. Function of light stabilizer: the light degradation and the light aging of the high polymer material under the light radiation, especially under the ultraviolet light can be prevented or slowed down, and the outdoor service life of the high polymer material can be greatly prolonged. The hindered amine light stabilizer has regeneration capability and can efficiently capture free radicals, so that the hindered amine light stabilizer has higher light aging resistance.
Preferably, in step S3, a light diffusing agent (e.g., MSE light diffusing agent, acrylate polymer with core-shell structure, etc.) and/or a light diffusing aid are further added. The light diffusing agent is a microsphere product developed by means of crosslinking, grafting functional groups and the like by utilizing a high molecular polymerization technology. The light diffusant and the light diffusion auxiliary agent are added into transparent resin such as PC, PVC, PS, PMMA, PET, epoxy resin and the like and LEDs (light emitting diodes), so that light scattering and transmission are increased, a light source and a glaring light source are shielded, the whole resin can emit softer, attractive and elegant light, and the light-transmitting and opaque comfortable effect is achieved.
(III) advantageous effects
Aiming at the problems that the quantum dot film is thicker and is difficult to be applied to thin products because the barrier films are additionally arranged at the upper side and the lower side of the quantum dot composite layer at present, the invention improves the following steps:
(1) the quantum dot structure adopts nano silicon Si, SiO and carbon C to coat QD (quantum dot) according to a certain proportion, wherein Si and SiO are mainly combined with moisture and oxygen in the air to protect the quantum dot from being damaged by moisture and oxygen, and C mainly plays a role in heat dissipation and high temperature resistance; the outermost polymer material plays a role in isolating water vapor and oxygen, and the main role of the outermost polymer material is to facilitate the fusion of the quantum dots into the plastic film, increase the dispersibility and the bonding firmness of the quantum dots in the plastic film and avoid the problems of precipitation and falling caused by poor fusion of the quantum dots (inorganic materials) and the plastic film.
The quantum dot @ polymer composite material is of a core-shell structure, wherein the core part is high Tg to achieve the effect of high temperature resistance of a product, and the shell is a low Tg polymer to improve the viscosity of the coated product so as to be mixed with plastic particles to provide conditions for manufacturing a quantum membrane.
(2) The invention prepares the quantum dot @ polymer composite material and plastic into plastic master batches in advance, and takes the plastic master batches with the quantum dots as product output. When the quantum dot diaphragm needs to be manufactured, the plastic master batch containing the quantum dots is only required to be directly manufactured into the diaphragm in an extrusion mode. The thickness of the membrane can be accurately controlled in different thicknesses of 50-300 mu m, and the prepared membrane belongs to a single-layer membrane and does not need to be additionally covered with barrier films on the upper surface and the lower surface for protection. The quantum dot film can be used for manufacturing a diffusion plate of a direct type backlight panel or a light guide plate of a side type backlight panel.
(3) When the plastic master batch is manufactured, a light stabilizer, a light diffusant and/or a light diffusion auxiliary agent are added, so that the prepared quantum dot film also has the characteristic of light aging resistance, and the light diffusant and/or the light diffusion auxiliary agent can increase the light scattering and transmission, shield a light source and a glaring light source, and enable the whole resin to emit softer, attractive and elegant light, so as to achieve the light-transmitting and opaque comfortable effect. The scheme of the invention is that the quantum dots are coated with nano-Si, SiO, carbon material for heat conduction and organic polymer material which are resistant to water vapor and oxygen, and then matched with the application of light stabilizer and light diffusant, so that the backlight plate with high color gamut and low attenuation can be obtained.
Drawings
Fig. 1 is a schematic structural diagram of a quantum dot @ polymer composite.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
As shown in fig. 1, the structure of the quantum dot @ polymer composite material is schematically shown. The quantum dot @ polymer composite comprises a quantum dot material 11, a barrier material 12 and a polymer material 13. Wherein, the barrier material 12 is coated outside the quantum dot material 11, and the polymer material 13 is coated outside the quantum dot material 11 and the barrier material 12. The barrier material 12 comprises nanosilicon 121, silica 122 and carbon material 123.
Preferably, carbon material 123 is graphitic carbon, graphene, or carbon nanotubes; preferably graphene 123. The graphene has extremely high heat transfer efficiency, is a two-dimensional material, and can play a good heat transfer role only by adding a small amount of graphene. Preferably, the polymeric material 13 is PMMA, EVOH, PET, PS, PVP, LDPE or PVDC. The quantum dot material 11 may be selected from CdSe, CdTe, ZnS, ZnSe, ZnTe, ZnO, HgS, HgSe, HgTe, MgSe, MgS, and binary compounds of mixtures thereof; or a ternary compound selected from the group consisting of CdSeS, CdSeTe, CdSTe, ZnSeS, ZnSTe, HgSeS, HgSeTe, HgSTe, CdZnS, CdZnSe, CdZnTe, CdHgS, CdHgSe, CdHgTe, HgZnS, HgZnSe, HgZnTe, MgZnSe, MgZnS, and mixtures thereof. Or a quaternary compound selected from the group consisting of HgZnTeS, CdZnSeS, CdZnSeTe, CdHgSeS, CdHgSeTe, CdHgSTe, HgZnSeS, HgZnSeTe, and mixtures thereof, and the like, but is not limited to the above list.
Preferably, the mass ratio of the quantum dot material 11, the barrier material 12 and the polymer material 13 is 0.1-4:0.1-4: 6-30. In the barrier material, the mass ratio of the nano-silicon 121 to the silicon monoxide 122 to the carbon material 123 is 1-2:2-3: 4-8.
For preparing the quantum dot @ polymer composite material, the following method can be referred to:
dispersing the quantum dot material into an organic solution (liquid alcohol, such as ethanol and the like) containing a coupling agent, heating and stirring, filtering, and drying to obtain the surface modified quantum dot material.
Wherein the heating and stirring temperature is 40-60 ℃, and the time is 1-5 h; the coupling agent is one or more of KH550, KH560, KH570, KH792, DL602 and DL 171.
And 2, adding water and a polymer monomer into a stirrer with a heating function, stirring and mixing uniformly, adding an oil-soluble initiator accounting for 0.5-5% of the total mass of the polymer monomer and a cross-linking agent accounting for 0.3-1%, stirring and mixing uniformly, heating to 55-100 ℃ for polymerization, prepolymerizing for 0.5h, and rapidly reducing the system temperature to below 30 ℃ by using an ice bath to obtain a prepolymer solution.
In the step 2, the polymer monomer is one or a combination of more of acrylonitrile, ethylene, acrylate and acrylamide monomers.
And step 3: adding the surface modified quantum dot material and the barrier material into a prepolymer solution, and fully stirring to uniformly mix; the barrier material comprises nano-silicon, sub-silicon oxide and a carbon material;
the mass ratio of the polymer monomer, the quantum dot material and the barrier material is 10-50: 0.1-5: 0.2-10; in the barrier material, the mass ratio of the nano silicon to the silicon monoxide to the carbon material is 1-2:2-3: 4-8.
And 4, step 4: and (3) adding 0.1-0.8% of polyvinyl alcohol solution as a dispersing agent into the reaction system in the step (3), stirring and dispersing for 10-20 min at the rotating speed of 100-1500 rpm/min, heating to 60-100 ℃, curing for 12-24 h, and finally cooling, filtering, washing and drying to obtain the quantum dot @ polymer composite material.
And (2) obtaining a prepolymer solution with a certain viscosity after prepolymerization, then adding the surface-modified quantum dot material and the barrier material into the solution to be wrapped and suspended by the prepolymer, so as to prevent the surface-modified quantum dot material and the barrier material from sinking, and then heating and curing the solution to obtain the composite microsphere, wherein the composite microsphere is a quantum dot @ polymer composite material.
Preferably, the barrier material is also pre-treated with a coupling agent, the treatment method referring to the treatment method of the quantum dot material in step 1.
The invention is further illustrated by the following specific examples, which are not to be construed as limiting the invention in any way.
Example 1
The preparation method of the quantum dot @ polymer composite material provided in this example is as follows:
step 1, dispersing 5g of quantum dot material CdSe into 30% KH570 ethanol solution, heating to 50 ℃, stirring for 3h, filtering, and drying to obtain the surface modified quantum dot material.
Step 2, adding 200g of water, 14g of ethylene and 22g of vinyl alcohol into a stirrer with a heating function, stirring and mixing uniformly, adding an oil-soluble initiator azobisisobutyronitrile accounting for 0.5 percent of the total mass of the monomers and a crosslinking agent polyethylene glycol 200 dimethacrylate accounting for 0.3 percent of the total mass of the monomers, stirring and mixing uniformly, heating to 62 ℃ for polymerization reaction, prepolymerizing for 30min, and rapidly reducing the temperature of the system to 20 ℃ by using an ice bath.
And step 3: and (3) adding 1g of the surface-modified quantum dot material CdSe and nano-silicon, 2g of silicon monoxide and 4g of graphene in the step (1) into the prepolymerization reactant, and fully stirring to uniformly mix.
And 4, step 4: and (3) adding 50ml of 0.5% polyvinyl alcohol solution serving as a dispersing agent into the reaction system in the step (3), stirring and dispersing for 20min at the rotating speed of 500rpm/min, heating to 90 ℃, curing for 12h, and finally cooling, filtering, washing and drying to obtain the quantum dot @ polymer composite material.
Example 2
The preparation method of the plastic masterbatch containing quantum dots provided in this embodiment is as follows:
firstly, stirring and mixing the quantum dot @ polymer composite material prepared by the method, PMMA master batch, white oil, Hindered Amine Light Stabilizer (HALS), MSE organic silicon light diffusant and surfactant sodium dodecyl benzene sulfonate to prepare a mixture. Wherein, the quantum dot @ polymer composite material: PMMA master batch: the mass ratio of the white oil to the white oil is 2:5: 10.
S2, adding the mixture into a screw extruder, and performing blending, extrusion and granulation to obtain the plastic master batch containing the quantum dots, wherein the screw temperature is controlled at 160-180 ℃, and the carbon material in the barrier material is prevented from being oxidized due to overhigh temperature.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A quantum dot @ polymer composite, comprising:
quantum dot materials, barrier materials, and polymeric materials;
the barrier material is coated outside the quantum dot material;
the polymer material is coated outside the quantum dot material and the barrier material;
the barrier material comprises nano-silicon, sub-silicon oxide and a carbon material.
2. Quantum dot @ polymer composite according to claim 1, wherein the carbon material is graphitic carbon, graphene or carbon nanotubes.
3. A quantum dot @ polymer composite as claimed in claim 1, wherein the mass ratio of the quantum dot material, the barrier material, and the polymer material is 0.1-4:0.1-4: 8-30.
4. Quantum dot @ polymer composite as claimed in claim 1, wherein the barrier material consists of nano silicon, silica and carbon material, and wherein the mass ratio of nano silicon, silica and carbon material is 1-2:2-3: 4-8.
5. Quantum dot @ polymer composite according to claim 1, characterized in that the polymer material is PMMA, EVOH, PET, PS, PVP, LDPE or PVDC.
6. A preparation method of a quantum dot @ polymer composite material is characterized by comprising the following steps:
dispersing a quantum dot material into an organic solution containing a coupling agent, heating and stirring, filtering, and drying to obtain a surface-modified quantum dot material;
step 2, adding a solution of water and a polymer monomer into a stirrer with a heating function, stirring and mixing uniformly, adding an oil-soluble initiator accounting for 0.5-5% of the total mass of the polymer monomer and a cross-linking agent accounting for 0.3-1%, stirring and mixing uniformly, heating to 55-100 ℃ for polymerization, prepolymerizing for 0.5-1h, and rapidly reducing the temperature of the system to below 30 ℃ by using an ice bath to obtain a prepolymer solution;
and step 3: adding the surface modified quantum dot material and the barrier material into a prepolymer solution, and fully stirring to uniformly mix; the barrier material comprises nano-silicon, sub-silicon oxide and a carbon material;
and 4, step 4: and (3) adding 0.1-0.8% of polyvinyl alcohol solution as a dispersing agent into the reaction system in the step (3), stirring and dispersing for 10-20 min at the rotating speed of 100-1500 rpm/min, heating to 60-100 ℃, curing for 12-24 h, and finally cooling, filtering, washing and drying to obtain the quantum dot @ polymer composite material.
7. The preparation method according to claim 6, wherein the mass ratio of the polymer monomer to the quantum dot material to the barrier material is 10-50: 0.1-5: 0.2-10; in the barrier material, the mass ratio of the nano silicon to the silicon monoxide to the carbon material is 1-2:2-3: 4-8.
8. The preparation method of the plastic master batch containing the quantum dots is characterized by comprising the following steps:
s1, stirring and mixing the quantum dot @ polymer composite material as defined in any one of claims 1-5 or the quantum dot @ polymer composite material as defined in claim 6 or 7, master batch of high molecular polymer material, solvent, light stabilizer and surfactant to prepare a mixture;
and S2, adding the mixture into a screw extruder, and blending, extruding and granulating through the extruder to obtain the plastic master batch containing the quantum dots.
9. The method according to claim 8, wherein a light stabilizer is further added in step S1, wherein the light stabilizer is a hindered amine light stabilizer.
10. The method according to claim 8 or 9, wherein a light diffusing agent and/or a light diffusing aid is further added in step S1.
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