WO2022032811A1 - 钡钛复合物及其制备方法与显示面板 - Google Patents

钡钛复合物及其制备方法与显示面板 Download PDF

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WO2022032811A1
WO2022032811A1 PCT/CN2020/116455 CN2020116455W WO2022032811A1 WO 2022032811 A1 WO2022032811 A1 WO 2022032811A1 CN 2020116455 W CN2020116455 W CN 2020116455W WO 2022032811 A1 WO2022032811 A1 WO 2022032811A1
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barium
titanium composite
titanium
preparing
quantum dots
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PCT/CN2020/116455
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English (en)
French (fr)
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孙小卫
王恺
周淼
杨鸿成
刘湃
徐冰
陈黎暄
李冬泽
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深圳市华星光电半导体显示技术有限公司
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Priority to US17/050,410 priority Critical patent/US11326095B2/en
Publication of WO2022032811A1 publication Critical patent/WO2022032811A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/006—Alkaline earth titanates
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
    • G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • G02F1/1336—Illuminating devices
    • G02F1/133614—Illuminating devices using photoluminescence, e.g. phosphors illuminated by UV or blue light
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
    • H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502—Wavelength conversion materials

Definitions

  • the present application relates to the field of display technology, in particular to a barium-titanium composite, a preparation method thereof, and a display panel.
  • quantum dots as a popular display material, have been widely studied, and some progress has been made in the display field, which has gradually entered the stage of industrial production. Compared with traditional phosphors, quantum dot displays have the advantages of high luminous efficiency and narrow half-peak width. Therefore, quantum dot optical films have high brightness, high color purity and wide color gamut.
  • Quantum dot optical films have good application prospects in mobile phone and TV backlights.
  • the preparation of quantum dot optical film requires mixing red and green quantum dots with glue, and then combining with blue light backlight to obtain a white light source.
  • energy resonance transfer is easy to occur, and more green quantum dots are required to achieve white balance. Therefore, additional brightness enhancement materials are required to improve the luminous brightness of quantum dots, thereby reducing the amount of quantum dots used. .
  • Barium titanate nanoparticles are conventional scattering particles.
  • the barium source for the synthesis of barium titanate nanoparticles by traditional methods is barium hydroxide.
  • the synthesized inorganic barium titanate nanoparticles are hydrophilic, which is not conducive to their dispersion in organic solvents. and acrylic organic glue, affecting its brightening effect in quantum dot optical films.
  • the present application provides a barium-titanium composite, a preparation method thereof, and a display panel.
  • the barium-titanium composite is prepared from an alkenoic acid barium salt, which can solve the problem of poor compatibility with organic glue, which leads to application in optical films The problem of poor scattering effect.
  • the present invention provides a preparation method of a barium-titanium composite, comprising the following steps:
  • barium source precursor is mixed with titanium source precursor and alkaline solution, obtains mixed solution to be reacted, and described barium source precursor is selected from alkenoic acid barium salt;
  • the number of carbon atoms in the barium source precursor is 2-20.
  • the barium source precursor is barium acrylate or barium crotonate.
  • the titanium source precursor is selected from titanate compounds.
  • the titanium source precursor is tetrabutyl titanate.
  • the molar ratio of barium element to titanium element is (1-3):2.
  • the molar ratio of the barium element to the titanium element is 1:1.
  • the pH value of the mixed solution to be reacted is 9-14.
  • the alkaline solution includes at least one of sodium hydroxide, potassium hydroxide, ammonium hydroxide, ethylenediamine and hydrazine hydrate.
  • the titanium source precursor in the S10, is first dispersed in an organic solvent, and then mixed with the alkaline solution.
  • the organic solvent is selected from at least one of ethanol or toluene.
  • the barium source precursor is first dispersed in water, and then mixed with the alkaline solution.
  • the water is ultrapure water.
  • the first condition includes performing a reaction in a closed reaction kettle at a reaction temperature of 100-2000°C.
  • the first time is 2-20 hours.
  • the present invention provides a barium-titanium composite.
  • the barium-titanium composite is prepared by the aforementioned preparation method of the barium-titanium composite.
  • the present invention provides a display panel, the display panel includes a color conversion layer, and the color conversion layer includes quantum dots and the aforementioned barium-titanium composite.
  • the quantum dots are selected from indium phosphide quantum dots, perovskite quantum dots, indium copper sulfide quantum dots, silver sulfide quantum dots, lead sulfide quantum dots, lead selenide quantum dots At least one of quantum dots and cadmium selenide quantum dots.
  • the color conversion layer further includes organic glue.
  • the organic glue is selected from acrylic glue.
  • the present invention provides a barium-titanium composite, a preparation method thereof, and a display panel.
  • the barium source is replaced by traditional barium hydroxide with an organic barium alkenoic acid salt.
  • the barium source makes the resulting product a barium-titanium composite containing organic groups.
  • it has better compatibility with organic glue, so that it can be better dispersed in In the quantum dot optical film, better scattering effect can be provided, the light-color conversion efficiency of quantum can be improved, and the brightness of the quantum dot optical film can be increased.
  • Fig. 1 is the schematic flow sheet of the preparation method of a kind of barium-titanium composite provided by the embodiment of the present invention
  • FIG. 2 is a high-angle annular dark-field scanning transmission microscope view of a barium-titanium composite provided by an embodiment of the present invention
  • FIG. 3 is a high-angle annular dark-field scanning transmission microscope view of another barium-titanium composite provided by an embodiment of the present invention.
  • Fig. 4 is the Fourier transform infrared spectrogram of a kind of barium-titanium composite provided by the embodiment of the present invention.
  • FIG. 5 is a photoluminescence spectrum diagram of an optical film prepared from particles of a barium-titanium composite provided by an embodiment of the present invention.
  • An embodiment of the present invention provides a method for preparing a barium-titanium composite. For specific steps, please refer to the flow chart provided in FIG. 1 , which will be described in detail below.
  • the preparation method comprises the following steps:
  • the barium source is replaced by the traditional barium hydroxide with the organic barium source of the alkenoic acid barium salt, so that the generated product is a barium-titanium composite containing organic groups, compared with the traditional barium-titanium compound.
  • Inorganic barium titanate nanoparticles have better compatibility with organic glue, so that they can be better dispersed in the quantum dot optical film, so as to provide better scattering effect and improve the light color of quantum dots Conversion efficiency increases the brightness of quantum dot optical films.
  • the number of carbon atoms in the barium source precursor is 2-20, for example, the barium source is barium acrylate or barium crotonate, and the hydrogen atoms in the barium alkenoate salt Can also be substituted by other common groups.
  • the titanium source precursor is selected from titanate-based compounds, for example, the titanate-based compound is tetrabutyl titanate.
  • the molar ratio of barium element to titanium element is (1-3): 2.
  • the molar ratio of the titanium element and the barium element is The ratio is 1:1.
  • the pH value of the mixed solution to be reacted is 9-14, wherein the alkaline solution includes sodium hydroxide, potassium hydroxide, hydroxide At least one of ammonium, ethylenediamine and hydrazine hydrate acts as a mineralizer, thereby promoting the formation of the barium-titanium composite particles.
  • the titanium source precursor is first dispersed in an organic solvent, for example, it can be dispersed in a common organic solvent such as ethanol or toluene, and the barium source precursor is dispersed in water.
  • a common organic solvent such as ethanol or toluene
  • the barium source precursor is dispersed in water.
  • the first condition includes performing calcination in a closed reaction kettle at a reaction temperature of 100-2000°C, and the first time is 2-20 hours.
  • the reaction temperature is high, the reaction time is corresponding
  • the reaction time increases accordingly.
  • Another embodiment of the present invention provides a barium-titanium composite, which is prepared by the preparation method of the barium-titanium composite provided in the foregoing embodiment.
  • Another embodiment of the present invention also provides a display panel, the display panel includes a color conversion layer, and the color conversion layer includes quantum dots and the aforementioned barium-titanium composite particles.
  • the color conversion layer is usually made of organic glue as a base material, wherein by adding the barium-titanium composite particles containing organic groups as a scattering example, according to a similar compatibility principle, the barium-titanium composite particles can be uniformly dispersed in In the color conversion layer, by increasing the brightness of the color conversion film, the amount of quantum dots used can be reduced, and at the same time, the absorption of the backlight can be increased.
  • the quantum dots can be selected from indium phosphide quantum dots, perovskite quantum dots, indium copper sulfide quantum dots, silver sulfide quantum dots, lead sulfide quantum dots, lead selenide quantum dots, and cadmium selenide quantum dots.
  • Tetrabutyl titanate (dispersed in ethanol) and barium acrylate monomer (dispersed in ultrapure water), wherein the molar ratio of barium and titanium elements is 1:1, and then add sodium hydroxide solution (1mol/L) , so that the pH of the solution to be reacted is 12, and after stirring evenly, it is placed in a high-temperature and high-pressure reaction at 200°C for 10 hours, and the corresponding barium-titanium composite powder is obtained after separation and purification.
  • the green light alloy quantum dots and the acrylic glue were mixed in a mass ratio of 1:100, and 5.0 wt % of the prepared barium-titanium composite powder was added at the same time, and a 120-micron optical film was coated by a coating equipment.
  • the obtained barium-titanium composite powder was tested by high-angle annular dark-field scanning transmission microscope (HADDF-STEM).
  • the scattering effect on light is improved, thereby increasing the light-color conversion efficiency and luminous brightness of the quantum dot film.
  • the prepared barium-titanium composite powder was tested by infrared spectrum Fourier transform infrared spectrum.
  • the test chart is shown in Figure 4. It can be seen from the figure that there is an absorption peak at 2910cm -1 , which is the characteristic absorption peak of CH. It is proved that the barium-titanium composite powder contains organic groups.
  • Tetrabutyl titanate (dispersed in ethanol) and barium acrylate monomer (dispersed in ultrapure water), wherein the molar ratio of barium and titanium elements is 1:1, and then add sodium hydroxide solution (1mol/L) , so that the pH of the solution to be reacted is 12, and after stirring evenly, it is placed in a high-temperature and high-pressure reaction at 200°C for 10 hours, and the corresponding barium-titanium composite powder is obtained after separation and purification.
  • the green light alloy quantum dots and acrylic glue were mixed in a mass ratio of 1:100, and 10.0 wt % of the prepared barium-titanium composite powder was added at the same time, and a 120-micron optical film was coated with a coating equipment.
  • the obtained barium-titanium composite powder was tested by high-angle annular dark-field scanning transmission microscope (HADDF-STEM).
  • Tetrabutyl titanate (dispersed in ethanol) and barium crotonate monomer (dispersed in ultrapure water), wherein the molar ratio of barium and titanium element is 1:1, and then add potassium hydroxide solution (1mol/ L), so that the pH of the solution to be reacted is 12, and after stirring evenly, it is placed in an autoclave at 200° C. for high-temperature and high-pressure reaction for 10 hours, and the corresponding barium-titanium composite powder is obtained after separation and purification.
  • the green light alloy quantum dots and acrylic glue were mixed in a mass ratio of 1:100, and 5.0 wt% of the prepared barium-titanium composite powder was added at the same time, and a 120-micron optical film was coated with a coating equipment.
  • Tetrabutyl titanate (dispersed in ethanol) and barium crotonate monomer (dispersed in ultrapure water), wherein the molar ratio of barium and titanium element is 1:1, and then add potassium hydroxide solution (1mol/ L), so that the pH of the solution to be reacted is 12, and after stirring evenly, it is placed in an autoclave at 200° C. for high-temperature and high-pressure reaction for 10 hours, and the corresponding barium-titanium composite powder is obtained after separation and purification.
  • the green light alloy quantum dots and acrylic glue were mixed in a mass ratio of 1:100, and 10.0 wt % of the prepared barium-titanium composite powder was added at the same time, and a 120-micron optical film was coated with a coating equipment.
  • the green light alloy quantum dots and acrylic glue were mixed according to the mass ratio of 1:100, and the optical film of 120 ⁇ m was coated by coating equipment.
  • the green light alloy quantum dots and the acrylic glue were mixed in a mass ratio of 1:100, and 5.0 wt % of barium titanate nanoparticles were added at the same time, and a 120 ⁇ m optical film was coated by a coating equipment.
  • optical films prepared by the above-mentioned Examples 1-4 and Comparative Examples 1-2 were subjected to a brightness test under the backlight of 450 nm blue light, and the results are shown in the following table:
  • Example 1 842.64
  • Example 2 890.78
  • Example 3 892.81
  • Example 4 963.42 Comparative Example 1 597.30 Comparative Example 2 832.69
  • the barium-titanium composite prepared by the preparation method provided by the present invention can be used as scattering particles, effectively improving the brightness of the prepared optical film, and compared with the traditional one prepared by using barium hydroxide as a barium source.
  • Inorganic barium titanate nanoparticles with higher brightening effect can be used as scattering particles, effectively improving the brightness of the prepared optical film, and compared with the traditional one prepared by using barium hydroxide as a barium source.
  • FIG. 5 for the photoluminescence spectrum of the optical film prepared in the above-mentioned Example 1 for the brightness test. It can be seen from the figure that there are two peaks at about 450 nm and about 530 nm, respectively. The blue light backlight and the green quantum dots formed by the luminescence.

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Abstract

一种钡钛复合物及其制备方法与显示面板，制备方法包括：将钡源前驱体与钛源前驱体以及碱性溶液混合，得到待反应混合溶液，钡源前驱体选自烯酸类钡盐（S10）；以及将待反应混合溶液在第一条件下反应第一时间，分离提纯后即得到钡钛复合物（S20）。

Description

钡钛复合物及其制备方法与显示面板 技术领域
本申请涉及显示技术领域，具体涉及钡钛复合物及其制备方法与显示面板。
背景技术
近年来，量子点作为一种热门的显示材料，得到广泛的研究，同时在显示领域取得一定的进展，已经逐步进入工业化生产的阶段。与传统的荧光粉相比，量子点显示具备发光效率高，半峰宽窄的优点，因此，量子点光学膜具备高亮度、高色纯度以及宽色域。
量子点光学膜在手机和电视背光具备良好的应用前景。量子点光学膜的制备需要将红绿量子点和胶水混合，使用时再结合蓝光背光，即可获得白光光源。但是，量子点的粒径小，容易产生能量共振转移，将需要更多的绿光量子点才能达到白平衡，因此，需要额外加入亮度增强材料来提高量子点的发光亮度，进而减少量子点的用量。
钛酸钡纳米粒子为先有的常规的散射粒子，传统方法合成钛酸钡纳米颗粒的钡源为氢氧化钡，合成的无机钛酸钡纳米颗粒为亲水性，不利于其分散在有机溶剂和丙烯酸类有机胶水中，影响其在量子点光学薄膜中的增亮效果。
技术问题
本申请提供一种钡钛复合物及其制备方法与显示面板，所述钡钛复合物由烯酸类钡盐制备而成，可解决与有机胶水相容性较差，而导致应用于光学膜时的散射效果不佳的问题。
技术解决方案
为解决上述问题，第一方面，本发明提供一种钡钛复合物的制备方法，包括如下步骤：
S01:将钡源前驱体与钛源前驱体以及碱性溶液混合，得到待反应混合溶 液，所述钡源前驱体选自烯酸类钡盐；以及
S02:将所述待反应混合溶液在第一条件下反应第一时间，分离提纯后即得到所述钡钛复合物。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述钡源前驱体中碳原子个数为2-20。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述钡源前驱体为丙烯酸钡或丁烯酸钡。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述钛源前驱体选自钛酸酯类化合物。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述钛源前驱体为钛酸四丁酯。
在本发明实施例提供的一种钡钛复合物的制备方法中，在所述钡源前驱体与钛源前驱体中，钡元素与钛元素的摩尔比为(1-3):2。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述钡元素与钛元素的摩尔比为1:1。
在本发明实施例提供的一种钡钛复合物的制备方法中，在所述S10中，通过加入所述碱性溶液，使得所述待反应混合溶液的pH值为9-14。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述碱性溶液包括氢氧化钠、氢氧化钾、氢氧化铵、乙二胺以及水合肼中的至少一者。
在本发明实施例提供的一种钡钛复合物的制备方法中，在所述S10中，先将所述钛源前驱体分散于有机溶剂中，再与所述碱性溶液进行混合。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述有机溶剂选自乙醇或甲苯中的至少一者。
在本发明实施例提供的一种钡钛复合物的制备方法中，在所述S10中，先将将所述钡源前驱体分散于水中，再与所述碱性溶液进行混合。
在本发明实施例提供的一种钡钛复合物的制备方法中，所述水为超纯水。
在本发明实施例提供的一种钡钛复合物的制备方法中，在所述S20中，所述第一条件包括在密闭的反应釜中以100-2000℃作为反应温度进行反应。
在本发明实施例提供的一种钡钛复合物的制备方法中，在所述S20中，所 述第一时间为2-20小时。
第二方面，本发明提供一种钡钛复合物所述钡钛复合物由前述的钡钛复合物的制备方法制备而得。
第三方面，本发明提供一种显示面板，所述显示面板包括色转换层，所述色转换层中包括量子点以及前述的钡钛复合物。
在本发明实施例提供的一种显示面板中，所述量子点选自磷化铟量子点、钙钛矿量子点、硫化铟铜量子点、硫化银量子点、硫化铅量子点、硒化铅量子点、硒化镉量子点中的至少一者。
在本发明实施例提供的一种显示面板中，所述色转换层还包括有机胶水。
在本发明实施例提供的一种显示面板中，所述有机胶水选自丙烯酸类胶水。
有益效果
相较于现有技术，本发明提供了一种钡钛复合物及其制备方法与显示面板，在所述制备方法中，将钡源由传统的氢氧化钡替换为烯酸类钡盐的有机钡源，使得生成的产物为包含有机基团的钡钛复合物，相较传统的无机钛酸钡纳米颗粒，与有机胶水之间具有更好的相容性，使得其能更好地分散于所述量子点光学膜中，从而能提供更好的散射效果，提升量子的光色转换效率，增加量子点光学膜的亮度。
附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是本发明实施例提供的一种钡钛复合物的制备方法的流程示意图；
图2是本发明实施例提供一种钡钛复合物的高角环形暗场扫描透射显微镜图；
图3是本发明实施例提供另一种钡钛复合物的高角环形暗场扫描透射显微镜图；
图4是本发明实施例提供一种钡钛复合物的傅里叶红外光谱图；
图5是本发明实施例提供一种由钡钛复合物的颗粒制备而得的光学膜的光致发光谱图。
本发明的实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
在本申请中，“示例性”一词用来表示“用作例子、例证或说明”。本申请中被描述为“示例性”的任何实施例不一定被解释为比其它实施例更优选或更具优势。为了使本领域任何技术人员能够实现和使用本发明，给出了以下描述。在以下描述中，为了解释的目的而列出了细节。应当明白的是，本领域普通技术人员可以认识到，在不使用这些特定细节的情况下也可以实现本发明。在其它实例中，不会对公知的结构和过程进行详细阐述，以避免不必要的细节使本发明的描述变得晦涩。因此，本发明并非旨在限于所示的实施例，而是与符合本申请所公开的原理和特征的最广范围相一致。
本发明实施例提供了一种钡钛复合物的制备方法，具体步骤请参阅图1提供的流程图，以下分别进行详细说明。
所述制备方法包括如下步骤：
S01:将钡源前驱体与钛源前驱体以及碱性溶液混合，得到待反应混合溶液，所述钡源前驱体选自烯酸类钡盐；以及
S02:将所述待反应混合溶液在第一条件下反应第一时间，分离提纯后即得到所述钡钛复合物。
在本实施例提供的制备方法中，将钡源由传统的氢氧化钡替换为烯酸类钡盐的有机钡源，使得生成的产物为包含有机基团的钡钛复合物，相较传统的无机钛酸钡纳米颗粒，与有机胶水之间具有更好的相容性，使得其能更好地分散 于所述量子点光学膜中，从而能提供更好的散射效果，提升量子的光色转换效率，增加量子点光学膜的亮度。
在一些实施例中，所述钡源前驱体中碳原子个数为2-20，示例性地，所述钡源为丙烯酸钡或丁烯酸钡，所述烯酸类钡盐中的氢原子也可被其他的常见基团取代。
在一些实施例中，所述钛源前驱体选自钛酸酯类化合物，示例性地，所述钛酸酯类化合物为钛酸四丁酯。
在一些实施例中，在所述钡源前驱体与钛源前驱体中，钡元素与钛元素的摩尔比为(1-3):2，通常情况下，所述钛元素、钡元素的摩尔比为1：1。
在一些实施例中，通过加入所述碱性溶液，使得所述待反应混合溶液的pH值为9-14，其中，在所述碱性溶液中，包括氢氧化钠、氢氧化钾、氢氧化铵、乙二胺以及水合肼中的至少一者，作为矿化剂，从而促使生成所述钡钛复合物颗粒。
在一些实施例中，先将所述钛源前驱体分散于有机溶剂中，例如可分散在乙醇或甲苯等常用的有机溶剂中，以及将所述钡源前驱体分散于水中，为减少杂质，通常分散于超纯水中，再与所述碱性溶液进行混合。
在一些实施例中，所述第一条件包括在密闭的反应釜中以100-2000℃作为反应温度进行煅烧反应，所述第一时间为2-20小时，当反应温度高时，反应时间相应地减小，当反应温度低时，反应时间相应地增加。
本发明的另一实施例提供了一种钡钛复合物，由前述实施例所提供的钡钛复合物的制备方法制备而得。
本发明的另一实施例还提供了一种显示面板，所述显示面板包括色转换层，所述色转换层中包括量子点以及前述的钡钛复合物颗粒。所述色转换层通常由有机胶水作为基材，其中通过添加所述包含有机基团的钡钛复合物颗粒作为散射例子，根据相似相容原理，所述钡钛复合物颗粒可均匀地分散于所述色转换层中，以此增加色转换膜的亮度，即可降低量子点的用量，同时，增加对背光的吸收。所述量子点可选自磷化铟量子点、钙钛矿量子点、硫化铟铜量子点、硫化银量子点、硫化铅量子点、硒化铅量子点、硒化镉量子点。
以下结合具体的实施例进行进一步说明：
实施例1
将钛酸四丁酯(分散在乙醇中)和丙烯酸钡单体(分散在超纯水中)，其中钡和钛元素的摩尔比为1:1，再加入氢氧化钠溶液(1mol/L)，使得待反应溶液的pH为12，搅拌均匀后将其置于高压反应釜中200℃高温高压反应10h，分离提纯后获得相应的钡钛复合物粉末。将绿光合金量子点和丙烯酸类胶水按照1:100的质量比例混合，同时加入5.0wt％的所制备的钡钛复合物粉末，利用涂膜设备涂成120微米的光学膜。
对所获得的钡钛复合物粉末进行高角环形暗场扫描透射显微镜(HADDF-STEM)测试，测试图片请参阅图2，从测试图片可看出该钡钛复合物具有疏松多孔的结构，有利于提高其对光线的散射效应，从而增加量子点薄膜的光色转换效率与发光亮度。
另外还对所制备的钡钛复合物粉末进行红外光谱傅里叶红外光谱测试，测试图请参见图4，从图中可看出2910cm -1存在吸收峰，为C-H的特征吸收峰，以此证明该钡钛复合物粉末中包括有机基团。
实施例2
将钛酸四丁酯(分散在乙醇中)和丙烯酸钡单体(分散在超纯水中)，其中钡和钛元素的摩尔比为1:1，再加入氢氧化钠溶液(1mol/L)，使得待反应溶液的pH为12，搅拌均匀后将其置于高压反应釜中200℃高温高压反应10h，分离提纯后获得相应的钡钛复合物粉末。将绿光合金量子点和丙烯酸类胶水按照1:100的质量比例混合，同时加入10.0wt％的所制备的钡钛复合物粉末，利用涂膜设备涂成120微米的光学膜。
对所获得的钡钛复合物粉末进行高角环形暗场扫描透射显微镜(HADDF-STEM)测试，测试图片请参阅图3，从测试图片可看出该钡钛复合物具有疏松多孔的结构。
实施例3
将钛酸四丁酯(分散在乙醇中)和丁烯酸钡单体(分散在超纯水中)，其中钡和钛元素的摩尔比为1:1，再加入氢氧化钾溶液(1mol/L)，使得待反应溶液的pH为12，搅拌均匀后将其置于高压反应釜中200℃高温高压反应10h，分离提纯后获得相应的钡钛复合物粉末。将绿光合金量子点和丙烯酸类胶水按照1:100的质量比例混合，同时加入5.0wt％的所制备的钡钛复合物粉末，利用涂 膜设备涂成120微米的光学膜。
实施例4
将钛酸四丁酯(分散在乙醇中)和丁烯酸钡单体(分散在超纯水中)，其中钡和钛元素的摩尔比为1:1，再加入氢氧化钾溶液(1mol/L)，使得待反应溶液的pH为12，搅拌均匀后将其置于高压反应釜中200℃高温高压反应10h，分离提纯后获得相应的钡钛复合物粉末。将绿光合金量子点和丙烯酸类胶水按照1:100的质量比例混合，同时加入10.0wt％的所制备的钡钛复合物粉末，利用涂膜设备涂成120微米的光学膜。
对比例1
将绿光合金量子点和丙烯酸类胶水按照1:100的质量比例混合，利用涂膜设备涂成120μm的光学膜。
对比例2
将绿光合金量子点和丙烯酸类胶水按照1:100的质量比例混合，同时加入5.0wt％的钛酸钡纳米颗粒，利用涂膜设备涂成120μm的光学膜。
将上述实施例1-4以及对比例1-2所制备的光学膜，在450nm的蓝光背光照射下，进行亮度测试，结果如下表所示：
样品 亮度(cd/m 2)
实施例1 842.64
实施例2 890.78
实施例3 892.81
实施例4 963.42
对比例1 597.30
对比例2 832.69
经验证可得，由本发明所提供的制备方法制备而得的钡钛复合物可作为散射粒子，有效提升所制备而得的光学膜亮度，且相较传统的由氢氧化钡作为钡源制备的无机钛酸钡纳米颗粒，具有更高的增亮效果。
另外，上述实施例1中所制备的光学膜进行亮度测试的光致发光图谱请参 阅图5，从图中可看出约450nm与约530nm处各有一个波峰，分别由蓝光背光以及绿色量子点所发光形成。
在上述实施例中，对各个实施例的描述都各有侧重，某个实施例中没有详述的部分，可以参见上文针对其他实施例的详细描述，此处不再赘述。
以上对本发明实施例所提供的一种钡钛复合物及其制备方法与显示面板进行了详细介绍，本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本发明的限制。

Claims (20)

  1. 一种钡钛复合物的制备方法，其中，包括如下步骤：
    S01:将钡源前驱体与钛源前驱体以及碱性溶液混合，得到待反应混合溶液，所述钡源前驱体选自烯酸类钡盐；以及
    S02:将所述待反应混合溶液在第一条件下反应第一时间，分离提纯后即得到所述钡钛复合物。
  2. 如权利要求1所述的钡钛复合物的制备方法，其中，所述钡源前驱体中碳原子个数为2-20。
  3. 如权利要求2所述的钡钛复合物的制备方法，其中，所述钡源前驱体为丙烯酸钡或丁烯酸钡。
  4. 如权利要求1所述的制备方法，其中，所述钛源前驱体选自钛酸酯类化合物。
  5. 如权利要求4所述的制备方法，其中，所述钛源前驱体为钛酸四丁酯。
  6. 如权利要求1所述的钡钛复合物的制备方法，其中，在所述钡源前驱体与钛源前驱体中，钡元素与钛元素的摩尔比为(1-3):2。
  7. 如权利要求6所述的钡钛复合物的制备方法，其中，所述钡元素与钛元素的摩尔比为1:1。
  8. 如权利要求1所述的钡钛复合物的制备方法，其中，在所述S10中，通过加入所述碱性溶液，使得所述待反应混合溶液的pH值为9-14。
  9. 如权利要求8所述的钡钛复合物的制备方法，其中，所述碱性溶液包括氢氧化钠、氢氧化钾、氢氧化铵、乙二胺以及水合肼中的至少一者。
  10. 如权利要求1所述的钡钛复合物的制备方法，其中，在所述S10中，先将所述钛源前驱体分散于有机溶剂中，再与所述碱性溶液进行混合。
  11. 如权利要求10所述的钡钛复合物的制备方法，其中，所述有机溶剂选自乙醇或甲苯中的至少一者。
  12. 如权利要求1所述的钡钛复合物的制备方法，其中，在所述S10中，先将将所述钡源前驱体分散于水中，再与所述碱性溶液进行混合。
  13. 如权利要求12所述的钡钛复合物的制备方法，其中，所述水为超纯水。
  14. 如权利要求1所述的钡钛复合物的制备方法，其中，在所述S20中，所 述第一条件包括在密闭的反应釜中以100-2000℃作为反应温度进行反应。
  15. 如权利要求1所述的钡钛复合物的制备方法，其中，在所述S20中，所述第一时间为2-20小时。
  16. 一种钡钛复合物，其中，所述钡钛复合物由权利要求1所述的钡钛复合物的制备方法制备而得。
  17. 一种显示面板，其中，所述显示面板包括色转换层，所述色转换层中包括量子点以及权利要求16所述的钡钛复合物。
  18. 如权利要求17所述的显示面板，其中，所述量子点选自磷化铟量子点、钙钛矿量子点、硫化铟铜量子点、硫化银量子点、硫化铅量子点、硒化铅量子点、硒化镉量子点中的至少一者。
  19. 如权利要求17所述的显示面板，其中，所述色转换层还包括有机胶水。
  20. 如权利要求19所述的显示面板，其中，所述有机胶水选自丙烯酸类胶水。
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