阅读说明：本技术 一种钙钛矿量子点胶水的制备方法 (Preparation method of perovskite quantum dot glue ) 是由 曾凡龙 杨纯莉 彭洪尚 于 2019-11-14 设计创作，主要内容包括：本发明涉及一种钙钛矿量子点胶水的制备方法,该钙钛矿量子点胶水的制备方法,包括如下步骤S1：将丙烯酸酯类聚合物加入有机溶剂中溶解形成第一前驱溶液；S2：将表面含有Si-OH基团的钙钛矿量子点荧光粉加入第一前驱溶液中混合形成第二前驱溶液；S3：将十七氟癸基三甲氧基硅烷加入到第二前驱溶液中混合反应,使十七氟癸基三甲氧基硅烷包覆在钙钛矿量子点荧光粉表面形成致密阻水层,即得到具有阻水效果的钙钛矿量子点胶水。上述钙钛矿量子点胶水应用到钙钛矿量子点膜后,可以有效提升膜材的稳定性。(The invention relates to a preparation method of perovskite quantum dot glue, which comprises the following steps of S1: adding an acrylate polymer into an organic solvent to dissolve to form a first precursor solution; s2: adding perovskite quantum dot fluorescent powder with Si-OH groups on the surface into the first precursor solution and mixing to form a second precursor solution; s3: and adding heptadecafluorodecyltrimethoxysilane into the second precursor solution for mixing reaction, so that the heptadecafluorodecyltrimethoxysilane is coated on the surface of the perovskite quantum dot fluorescent powder to form a compact water-blocking layer, and thus obtaining the perovskite quantum dot glue with the water-blocking effect. After the perovskite quantum dot glue is applied to a perovskite quantum dot film, the stability of the film material can be effectively improved.)

1. The preparation method of the perovskite quantum dot glue is characterized by comprising the following steps:

s1: adding an acrylate polymer into an organic solvent to dissolve to form a first precursor solution;

s2: adding perovskite quantum dot fluorescent powder with Si-OH groups on the surface into the first precursor solution and mixing to form a second precursor solution;

s3: and adding heptadecafluorodecyltrimethoxysilane into the second precursor solution for mixing reaction, so that the heptadecafluorodecyltrimethoxysilane is coated on the surface of the perovskite quantum dot fluorescent powder to form a compact water-blocking layer, and thus obtaining the perovskite quantum dot glue with the water-blocking effect.

2. The preparation method of the perovskite quantum dot glue according to claim 1, wherein tetraethoxysilane is further added into the first precursor solution.

3. The preparation method of the perovskite quantum dot glue according to claim 1, wherein the acrylate polymer at least comprises one of polymethyl methacrylate and polyethyl methacrylate.

4. The preparation method of the perovskite quantum dot glue according to claim 1, wherein the organic solvent at least comprises one of toluene and xylene.

5. The preparation method of the perovskite quantum dot glue according to claim 2, characterized in that, according to the parts by weight, the acrylic polymer is 20-40 parts by weight, the organic solvent is 50-60 parts by weight, the perovskite quantum dot phosphor is 1.5-4.5 parts by weight, the ethyl orthosilicate is 6.5-9.5 parts by weight, and the heptadecafluorodecyltrimethoxysilane is 0.5-4.5 parts by weight.

6. The preparation method of the perovskite quantum dot glue according to claim 5, wherein 30 parts by mass of an acrylic polymer, 60 parts by mass of an organic solvent, 3 parts by mass of perovskite quantum dot phosphor, 8 parts by mass of ethyl orthosilicate and 2 parts by mass of heptadecafluorodecyltrimethoxysilane are used.

7. The preparation method of the perovskite quantum dot glue according to claim 1, wherein the acrylate polymer in S1 is added into an organic solvent, and stirred at 40-60 ℃ until the acrylate polymer is completely dissolved; s2, adding the perovskite quantum dot fluorescent powder with the surface containing Si-OH groups into the first precursor solution, stirring and mixing for 3-5 hours; seventeen-decafluorodecyltrimethoxysilane in the S3 is added into the second precursor solution to be stirred and mixed for reaction, and the mixing reaction time is 1.5-2.5 h.

Technical Field

The invention relates to the technical field of optical films, in particular to a preparation method of perovskite quantum dot glue.

Background

Quantum dots are nano-scale semiconductors that emit light of a specific frequency by applying a certain electric field or light pressure to the nano-semiconductor material, and the frequency of the emitted light varies with the size of the semiconductor, so that the color of the emitted light can be controlled by adjusting the size of the nano-semiconductor, which is called quantum dots because the nano-semiconductor has the property of confining electrons and electron holes, which is similar to atoms or molecules in the natural world.

Since quantum dots are easily corroded by water and oxygen in the air, in the using process of the quantum dot material, the quantum dot material needs to be prepared into a quantum dot film with a water and oxygen barrier function. The glue commonly used for preparing the quantum dot film comprises curing agent-containing photocuring glue or photoinitiator-containing thermocuring glue, and perovskite quantum dot raw materials are mixed with the glue to form mixed glue for later use.

Disclosure of Invention

The invention provides a preparation method of perovskite quantum dot glue to make up for the defects of the prior art, and solves the problems in the prior art.

The technical scheme adopted by the invention for solving the technical problems is as follows:

a preparation method of perovskite quantum dot glue comprises the following steps:

s1: adding an acrylate polymer into an organic solvent to dissolve to form a first precursor solution;

s2: adding perovskite quantum dot fluorescent powder with Si-OH groups on the surface into the first precursor solution and mixing to form a second precursor solution;

s3: and adding heptadecafluorodecyltrimethoxysilane into the second precursor solution for mixing reaction, so that the heptadecafluorodecyltrimethoxysilane is coated on the surface of the perovskite quantum dot fluorescent powder to form a compact water-blocking layer, and thus obtaining the perovskite quantum dot glue with the water-blocking effect.

Further, tetraethoxysilane is added into the first precursor solution.

Further, tetraethoxysilane is added into the precursor solution, the tetraethoxysilane is added before heptadecafluorodecyltrimethoxysilane, and the heptadecafluorodecyltrimethoxysilane is coated on the surface of the perovskite quantum dot fluorescent powder through tetraethoxysilane.

Further, the acrylic polymer contains at least one of polymethyl methacrylate and polyethyl methacrylate.

Further, the organic solvent contains at least one of toluene and xylene.

Furthermore, according to the parts by weight, the acrylic polymer accounts for 20-40 parts by weight, the organic solvent accounts for 50-60 parts by weight, the perovskite quantum dot fluorescent powder accounts for 1.5-4.5 parts by weight, the ethyl orthosilicate accounts for 6.5-9.5 parts by weight, and the heptadecafluorodecyltrimethoxysilane accounts for 0.5-4.5 parts by weight.

Further, 30 parts by mass of an acrylic polymer, 60 parts by mass of an organic solvent, 3 parts by mass of perovskite quantum dot phosphor, 8 parts by mass of ethyl orthosilicate and 2 parts by mass of heptadecafluorodecyltrimethoxysilane.

Further, adding the acrylic polymer in S1 into an organic solvent, and stirring at 40-60 ℃ until the acrylic polymer is completely dissolved; s2, adding the perovskite quantum dot fluorescent powder with the surface containing Si-OH groups into the first precursor solution, stirring and mixing for 3-5 hours; seventeen-decafluorodecyltrimethoxysilane in the S3 is added into the second precursor solution to be stirred and mixed for reaction, and the mixing reaction time is 1.5-2.5 h.

The perovskite quantum dot film is prepared by adopting the perovskite quantum dot glue water obtained by the preparation method, and the specific preparation method comprises the following steps:

d1: coating the perovskite quantum dot glue water obtained by the preparation method of S1-S3 on a drainage oxygen barrier film, and placing the drainage oxygen barrier film in a drying box for drying to obtain a barrier double layer of a drainage oxygen barrier layer and a perovskite quantum dot layer;

d2: and (3) attaching the blocking double layer to the lower water oxygen blocking film coated with the UV curing glue and curing under an ultraviolet lamp to obtain the perovskite quantum dot film of the lower water oxygen blocking layer, the perovskite quantum dot layer, the UV glue layer and the upper water oxygen blocking layer.

Wherein, the drying conditions in D1 are as follows: drying at 50 deg.C for 0.5h, drying at 80 deg.C for 0.5h, coating thickness of perovskite quantum dot layer is 200 μm, and coating thickness of UV glue layer is 10 μm.

In the preparation process of the perovskite quantum dot film, perovskite quantum dot glue is firstly adopted and then UV curing glue is adopted, and the perovskite quantum dot glue is coated between the upper water oxygen barrier film and the lower water oxygen barrier film and is dried together, so that the perovskite quantum dot glue is poor in curing effect and generates air holes, and the effect of the film is influenced. The two-step process is favorable for the volatilization of the organic solvent, and the UV curing glue does not influence the luminous effect of the perovskite quantum dots.

The invention adopts the structure, and has the advantages that:

1. wherein the acrylate polymer acts as a matrix for uniformly dispersing the perovskite quantum dot phosphor therein. As shown by comparing example 1 with example 6, the stability of the film material can be effectively improved by adding heptadecafluorodecyltrimethoxysilane. The heptadecafluorodecyltrimethoxysilane contains Si-OH groups after hydrolysis and is condensed with Si-OH groups on the surface of the perovskite quantum dot fluorescent powder, so that the heptadecafluorodecyltrimethoxysilane is coated on the perovskite quantum dot fluorescent powder and forms a compact water-blocking layer on the surface of the perovskite quantum dot fluorescent powder, the water-blocking layer formed by the heptadecafluorodecyltrimethoxysilane with a hydrophobic effect directly blocks water in the air outside the water-blocking layer, the water in the air is prevented from directly contacting with the perovskite quantum dot fluorescent powder, and the stability of the perovskite quantum dot fluorescent powder is ensured. And the group contained in the heptadecafluorodecyltrimethoxysilane is a nonpolar group, so that the heptadecafluorodecyltrimethoxysilane is compatible with the perovskite quantum dot fluorescent powder.

2. As can be seen by comparing the data of example 3 and example 5, the addition sequence of ethyl orthosilicate and heptadecafluorodecyltrimethoxysilane obviously influences the performance of the perovskite quantum dot glue, thereby influencing the stability of the perovskite quantum dot film. The reason is that when glue is prepared, the added ethyl orthosilicate is hydrolyzed and then condensed with Si-OH on the surface of the perovskite quantum dot fluorescent powder, so that more Si-OH can be formed on the surface of the perovskite quantum dot fluorescent powder material, and the heptadecafluorodecyltrimethoxysilane can grow to the surface of the perovskite quantum dot fluorescent powder material in a large area, so that the water resistance is improved.

Drawings

FIG. 1 is a schematic diagram of the structure of a perovskite quantum dot film prepared by the invention.

In the figure, 1, an upper barrier layer, 2, a PET matrix, 3, UV curing glue, 4, a perovskite quantum dot layer, 5 and a lower barrier layer.

Detailed Description

In order to more clearly explain the overall concept of the present application, the following detailed description is given by way of example. In the following description, specific details are given to provide a more thorough understanding of the present application. It will be apparent, however, to one skilled in the art, that the present application may be practiced without one or more of these specific details. In other instances, well-known features of the art have not been described in order to avoid obscuring the present application.

The perovskite quantum dot fluorescent powder with the surface containing Si-OH groups is self-made, and the preparation method comprises the following steps:

(1) and (3) mixing and dissolving 0.1mmol of PbBr2, 0.2mmol of CH3NH3Br and 0.2mmol of APTS in DMF to form a mixed solution a, and injecting the obtained mixed solution a into rapidly stirred toluene to generate precipitation, thereby obtaining a solution sample of the organic-inorganic hybrid perovskite quantum dots. (2) 3mL of ethanol, 3mL of Tetraethylorthosilicate (TEOS), 3mL of water, and 20. mu.L of acetic acid were mixed and stirred uniformly and left to stand for one day to form a mixed solution b. (3) Dissolving 0.01mmol of CH3NH3Br in 20 μ L of water, and injecting into the mixed solution b to obtain the required silica sol. (4) Stirring the obtained organic-inorganic hybrid perovskite quantum dot solution sample for 12h, centrifuging (2500rpm, 5min), re-dispersing the centrifuged solid into 2mL of ethanol, injecting the ethanol into the obtained silica sol, drying at 85 ℃ for 120h to obtain perovskite quantum dot doped silica dry glue which is a blocky solid, and grinding to form quantum dot fluorescent powder, namely the organic-inorganic hybrid perovskite quantum dot based fluorescent material, namely the perovskite quantum dot fluorescent powder with Si-OH groups on the surface.

The PET water oxygen barrier film in fig. 1 is composed of a PET substrate 2 and an upper barrier layer 1 or a lower barrier layer 5.

The perovskite quantum dot glue provided by the following embodiments is prepared by the following method respectively: