WO2016015409A1 - 功能材料及其制备方法、配向材料、液晶显示基板 - Google Patents

功能材料及其制备方法、配向材料、液晶显示基板 Download PDF

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WO2016015409A1
WO2016015409A1 PCT/CN2014/091838 CN2014091838W WO2016015409A1 WO 2016015409 A1 WO2016015409 A1 WO 2016015409A1 CN 2014091838 W CN2014091838 W CN 2014091838W WO 2016015409 A1 WO2016015409 A1 WO 2016015409A1
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functional material
inorganic powder
oxide
alignment
modified layer
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PCT/CN2014/091838
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English (en)
French (fr)
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杨久霞
白峰
郭振鹏
苏京
刘建涛
冯鸿博
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京东方科技集团股份有限公司
北京京东方光电科技有限公司
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Priority claimed from CN201410366432.4A external-priority patent/CN104277500B/zh
Application filed by 京东方科技集团股份有限公司, 北京京东方光电科技有限公司 filed Critical 京东方科技集团股份有限公司
Priority to EP14882167.1A priority Critical patent/EP3176226A4/en
Priority to US14/769,586 priority patent/US9796928B2/en
Publication of WO2016015409A1 publication Critical patent/WO2016015409A1/zh

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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • 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
    • G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
    • 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
    • G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
    • G02F1/133711—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by organic films, e.g. polymeric films
    • G02F1/133719—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by organic films, e.g. polymeric films with coupling agent molecules, e.g. silane
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    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • G—PHYSICS
    • G02—OPTICS
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    • 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
    • G02F1/1337—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers
    • G02F1/133711—Surface-induced orientation of the liquid crystal molecules, e.g. by alignment layers by organic films, e.g. polymeric films
    • G02F1/133723—Polyimide, polyamide-imide
    • 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
    • G02F2203/00—Function characteristic
    • G02F2203/11—Function characteristic involving infrared radiation

Definitions

  • the present invention relates to the field of display technologies, and in particular, to a functional material, a preparation method thereof, an alignment material, and a liquid crystal display substrate.
  • the alignment layer is one of important structures, and after irradiation or ultraviolet light irradiation, a specific orientation structure can be generated, so that liquid crystal molecules in contact therewith are aligned (ie, oriented) in a specific direction, and liquid crystal is realized. Filter the purpose.
  • the alignment layer is usually located in a liquid crystal display substrate (such as an array substrate or a color filter substrate) and covers all other display structures (such as a thin film transistor array, a pixel electrode, a color filter film, etc.).
  • the alignment layer is formed by curing the alignment material, and the alignment material contains polyimide, a crosslinking agent, a solvent, and the like.
  • the invention aims to solve the problem that the existing liquid crystal display device is polluted, and provides a functional material which can play a health care role and is environmentally friendly, a preparation method thereof, an alignment material, and a liquid crystal display substrate.
  • the technical solution adopted to solve the technical problem of the present invention is a functional material comprising an inorganic powder having a modified layer on its surface, the inorganic powder comprising:
  • the modified layer is obtained by dehydration ring closure of a reaction product of a dibasic anhydride and a diamine.
  • the ratio of the amount of the dibasic anhydride to the diamine used to form the modified layer is (0.85 to 1.05):1.
  • the ratio of the amount of the dibasic anhydride to the diamine used to form the modified layer is (0.92 to 1.05):1.
  • the dibasic anhydride used to form the modified layer contains at least one phenyl group;
  • the diamine forming the modified layer contains at least one phenyl or non-phenyl six-membered carbocyclic ring.
  • the dianhydride used to form the modified layer is selected from the group consisting of pyromellitic dianhydride, trimellitic anhydride, benzophenone dianhydride, biphenyl dianhydride, diphenyl ether dianhydride, and hexafluoro dianhydride.
  • any one of the diamines used to form the modified layer is selected from the group consisting of 3-aminobenzylamine, 2,2'-difluoro-4,4'-(9-fluorenylene)diphenylamine, 2, 2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane, hexahydro-m-xylylenediamine, 1,4-bis(aminomethyl)cyclohexane, 2,2-bis[4 -(4-Aminophenoxy)benzene]hexafluoropropane, 2,2-bis(3-amino-4-methylphenyl)hexafluoropropane, 2,2-bis(3-aminophenyl)hexafluoropropane, 2,2-bis(4-aminophenyl)hexafluoropropane, 2,7-diaminopurine, m-xylylenediamine, 4,4'-methylenebis(2-eth
  • the inorganic powder has a particle diameter of from 1 to 5,000 nm.
  • the technical solution adopted to solve the technical problem of the present invention is a method for preparing the above functional material, which comprises:
  • the ratio of the mass of the inorganic powder to the mass of the substance formed by the reaction of the dibasic anhydride and the diamine is (20 to 1):1.
  • the heating in the step S2 is carried out in two steps, specifically: heating at a temperature of 35 to 70 ° C for 20 to 40 minutes; heating at a temperature of 70 to 100 ° C for 20 to 40 minutes.
  • the heating in the step S3 is: heating at a temperature of 50 to 300 ° C for 30 to 60 minutes.
  • the mass percentage of each component in the alignment material is: polyimide: 1 to 20%; coupling agent: 0.1 to 5 %; solvent: 72.5 to 98%; inorganic powder of functional material: 0.1 to 2.5%.
  • the inorganic powder of the functional material in the alignment material has a mass percentage of 0.1 to 2%.
  • the inorganic powder of the functional material in the alignment material has a mass percentage of 0.1 to 1.8% without calculating the quality of the modified layer of the functional material.
  • the mass percentage of a substance in the alignment material means all the substances other than the modified layer of the functional material except the functional layer (functional material)
  • the mass percentage of a substance when the mass of the inorganic powder, polyimide, coupling agent, solvent, etc. is 100%.
  • a technical solution adopted to solve the technical problem of the present invention is a liquid crystal display substrate including an alignment layer, and
  • the alignment layer is obtained by curing the above alignment material.
  • the functional material of the invention can emit far infrared rays and negative ions; the far infrared rays can be absorbed by the human body to resonate water molecules in the body, activate water molecules, enhance the intermolecular binding force, thereby activating biological macromolecules such as proteins, so that the living cells are at the highest vibration.
  • the inorganic powder surface of the functional material of the present invention has a modified layer which can be well fused with the main component (polyimide) of the alignment material, so that the functional material can be stably distributed in the alignment layer;
  • the modified layer also improves the ability of the inorganic powder to emit far infrared rays and negative ions.
  • the liquid crystal display substrate of the present invention has an alignment layer formed of the above alignment material, it can continuously emit far infrared rays and negative ions during use, and is environmentally friendly.
  • FIG. 1 is a flow chart of a method of preparing a functional material according to an embodiment of the present invention.
  • This embodiment provides a functional material and a preparation method thereof.
  • the functional material includes an inorganic powder having a modified layer on the surface, and the inorganic powder includes alumina, magnesia, zinc oxide, zirconium oxide, silicon dioxide, titanium oxide, boron oxide, ferric oxide, calcium oxide, potassium oxide, Any one or more of sodium oxide and lithium oxide;
  • the modified layer is obtained by dehydration ring closure of a reaction product of a dibasic anhydride and a diamine.
  • the inorganic powder has a particle diameter on the order of nanometers to micrometers, specifically, for example, 1 to 5000 nm, preferably 10 to 500 nm.
  • the particle size can be measured, for example, using a Malvern laser particle size analyzer.
  • the dibasic anhydride refers to a substance having at least two acid anhydride groups in a molecular structure
  • the diamine is a substance having at least two amine groups (or amino groups) in a molecular structure.
  • the dibasic anhydride contains, for example, at least one phenyl group, and is preferably any one of pyromellitic dianhydride, trimellitic anhydride, benzophenone dianhydride, biphenyl dianhydride, diphenyl ether dianhydride, and hexafluoro dianhydride.
  • pyromellitic dianhydride trimellitic anhydride
  • benzophenone dianhydride biphenyl dianhydride
  • diphenyl ether dianhydride diphenyl ether dianhydride
  • hexafluoro dianhydride hexafluoro dianhydride.
  • the diamine contains, for example, at least one phenyl or non-phenyl six-membered carbocyclic ring (e.g., cyclohexane group), which is preferably 3-aminobenzylamine, 2,2'-difluoro-4,4' -(9-fluorenylene)diphenylamine, 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane, hexahydro-m-xylylenediamine, 1,4-bis(carbamyl) Cyclohexane, 2,2-bis[4-(4-aminophenoxy)benzene]hexafluoropropane, 2,2-bis(3-amino-4-methylphenyl)hexafluoropropane, 2,2 - bis(3-aminophenyl)hexafluoropropane, 2,2-bis(4-aminophenyl)hexafluoropropane,
  • the ratio of the amount of the dibasic anhydride to the diamine is, for example, (0.85 to 1.05):1; preferably at (0.92 to 1.05):1.
  • a layer of a product is formed on the surface of the inorganic powder, and the layer product is subjected to dehydration ring closure to obtain the modified layer.
  • the modified layer can be well fused with the main component (polyimide) in the alignment material, so that the functional material can be stably distributed in the alignment layer; and the modified layer can also improve the inorganic powder to emit far infrared rays and negative ions.
  • the functional material of the embodiment can emit far infrared rays and negative ions; the far infrared rays can be absorbed by the human body to resonate water molecules in the body, activate water molecules, enhance the intermolecular binding force, thereby activating biological macromolecules such as proteins, so that the living cells are at the highest level.
  • Vibration energy level; and far infrared heat can be transmitted to the deep part of the skin, so that the subcutaneous deep temperature rises, expands the capillaries, promotes blood circulation, strengthens the metabolism between tissues, enhances the ability of tissue regeneration, improves the body immunity, and regulates An abnormal state of mental excitement; and negative ions have decomposition and oxidation effects on bacteria and organic matter, and can have an effect of sterilizing and purifying and purifying ambient air quality; therefore, the functional materials of the present embodiment can serve as a health care function.
  • Environmentally friendly is an effect of sterilizing and purifying and purifying ambient air quality
  • the preparation method of the above functional material comprises: uniformly mixing the inorganic powder, the dibasic anhydride, the diamine, the initiator, and the solvent; heating to react the dibasic anhydride with the diamine, forming the middle on the surface of the inorganic powder. a product layer; heating the inorganic powder with the intermediate product layer to dehydrate the intermediate product layer to obtain the functional material.
  • the foregoing preparation method may include:
  • each of the raw materials is pulverized into a powder and then uniformly mixed in proportion, or the raw materials are uniformly mixed in proportion and then pulverized to obtain an inorganic powder.
  • the dispersing agent can be selected from the conventional dispersing agent such as BYK 161 produced by BYK of Germany, Solsperse 32500 and Solsperse 22000 produced by Lubrizol; the pulverization can be carried out by conventional methods such as ball milling and grinding; The method is therefore not described in detail here.
  • an initiator of 1/4 to 1/3 of the total amount and a diamine of 1/4 to 1/3 of the total amount are dissolved in a solvent for use.
  • the ratio of the mass of the inorganic powder to the mass of the substance formed by the reaction of the dibasic anhydride and the diamine is (20 to 1):1.
  • the amount of the dibasic anhydride and the diamine is determined as follows: It is assumed that the dibasic anhydride and the diamine can be completely reacted to obtain a product, and if the mass of the product is 1, the quality of the inorganic powder is Between 1 and 20; such an amount ensures that a modified layer of a suitable thickness is finally obtained on the inorganic powder.
  • an initiator is used to initiate the reaction, which is, for example, a nitrogen-based initiator, preferably azobisisobutyronitrile, 2,2'-bisazo-(2,4-dimethylvaleronitrile), azodi Any of dimethyl isobutyrate and azobisisovaleronitrile.
  • a nitrogen-based initiator preferably azobisisobutyronitrile, 2,2'-bisazo-(2,4-dimethylvaleronitrile), azodi Any of dimethyl isobutyrate and azobisisovaleronitrile.
  • the solvent may be selected from the group consisting of fatty alcohols, glycol ethers, ethyl acetate, methyl ethyl ketone, methyl isobutyl ketone, monomethyl ether glycol ester, ⁇ -butyrolactone, and 3-ethyl ether ethyl propionate.
  • a conventional organic solvent such as butyl carbitol, butyl carbitol acetate, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, cyclohexane, xylene, or isopropanol. Since the action of the solvent is only to disperse the respective substances, propylene glycol monomethyl ether acetate is uniformly used as a solvent in the process of specifically preparing the functional materials in the respective examples.
  • heating is started to carry out a reaction, and the intermediate product layer is formed on the surface of the inorganic powder; For example, it can be carried out in two steps, and specifically comprises: first heating at a temperature of 35 to 70 ° C for 20 to 40 minutes; and then continuing to heat at a temperature of 70 to 100 ° C for 20 to 40 minutes.
  • a reaction between the dibasic anhydride and the diamine can be made to form an intermediate product layer on the surface of the inorganic powder; wherein the stepwise heating is mainly to prevent the reaction from being too intense.
  • the reaction in this step is carried out, for example, under a nitrogen atmosphere, and stirring is maintained, for example, during the reaction.
  • the amount of the solvent in each step is determined by uniformly dispersing and dissolving the substance therein, and the amount of the initiator is based on the reaction, which can be adjusted by a person skilled in the art according to actual conditions, and will not be described in detail herein. .
  • the mass ratio (referred to as the total amount) of the inorganic powder, the initiator, and the solvent is 1: (0.25 to 0.4): (1 to 1.5), and in order to unify, the process of specifically preparing the functional material in each of the examples In the above, the mass ratio of the inorganic powder, the initiator, and the solvent was unified to 1:0.3:1.4.
  • the inorganic powder with the intermediate layer is separated from the solution by filtration, evaporation of the solvent, or the like.
  • the inorganic powder is continuously heated to cause a dehydration ring-closing reaction of the intermediate layer to obtain a modified layer which is well compatible with the polyimide.
  • the heating in this step is carried out at a temperature of 50 to 300 ° C for 30 to 60 minutes.
  • dibasic anhydride, diamine, initiator, etc. may be dissolved in the solvent at one time; for example, the heating in step S04 may also be Wait a while.
  • the heating in step S04 may also be Wait a while.
  • This embodiment also provides an alignment material.
  • the alignment material is used to form an alignment layer in the liquid crystal display substrate, which contains polyimide, a solvent, a coupling agent, and the above functional materials.
  • the components of the alignment material are The mass percentage is: polyimide: 1 to 20%; coupling agent: 0.1 to 5%; solvent: 72.5 to 98%; inorganic powder of functional material: 0.1 to 2.5%.
  • the mass percentage of the functional material is more preferably 0.1 to 2%, still more preferably 0.1 to 1.8%.
  • the components are The content is as above.
  • polyimide is a main material for forming an alignment layer, and its content is, for example, 1 to 15%, preferably 1 to 10%.
  • the coupling agent is used to crosslink the polyimide to form a solid alignment layer;
  • the coupling agent may be a silane coupling agent, a nitrogen silane coupling agent, or a phenoxysilane coupling agent such as ethylene.
  • the solvent is used to dissolve and disperse the components in the alignment material to form a uniform and stable system.
  • the solvent may be selected from organic solvents such as N-methyl-2-pyrrolidone, m-cresol, ⁇ -butyrolactone, N,N-dimethylacetamide, N,N-dimethylformamide, N-methylcaprolactam, dimethyl sulfoxide, ⁇ -butyrolactam, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol Monobutyl ether, diethylene glycol monoethyl ether, butyl carbitol, ethyl carbitol acetate, ethylene glycol, and the like.
  • the functional material is the above-mentioned functional material, and after adding it to the alignment material, the environmental friendliness of the alignment material can be improved.
  • the resulting functional material is used to continue to prepare the alignment material according to the parameters in the following table, and the preparation may be carried out by uniformly mixing the components without using a specific addition sequence and mixing method.
  • the infrared specific radiance of each alignment material was tested in accordance with the GB/T 7287-2008 standard, and the amount of negative ions generated by the air negative ion analyzer (for example, KEC-900 type of Japan KEC Corporation) was measured, and the results are shown in the following table.
  • the air negative ion analyzer for example, KEC-900 type of Japan KEC Corporation
  • the alignment material is cured to form an alignment layer, and the voltage retention rate thereof is tested.
  • the alignment material is spin-coated on a substrate having an indium tin oxide (ITO) layer on the surface, and pre-baked at 80 ° C for 2 min, at 220.
  • ITO indium tin oxide
  • the liquid crystal cell was composed of the substrate, and then the pulse cell voltage (5 V, 60 ⁇ ) was applied to charge the liquid crystal cell, and then the high-voltage voltmeter was used to measure the change of the cell voltage in 16.7 ms to remain The ratio of the voltage is taken as the voltage holding ratio.
  • polyimide of JSROPTMER AL23201 manufactured by JSR Co., Ltd. was uniformly used for the polyimide; ⁇ -aminopropyltriethoxysilane was uniformly used as the coupling agent; and ⁇ -butane was uniformly used for the solvent. Ester; Since the above components are all conventional components in the alignment material, for the comparability of the results, the above substances are uniformly tested here.
  • the alignment materials of the embodiments have higher infrared specific emissivity and negative ion concentration, and the voltage retention ratio of the alignment layer formed by the same is also good, which proves that the performance of the alignment layer itself is not affected, and at the same time, it can generate far Infrared and negative ions help to improve the environment.
  • the inorganic powder surface of the functional material of the present embodiment has a modified layer which allows the inorganic powder to be well compatible with the alignment material and also enhances the ability of the inorganic powder to emit far infrared rays and negative ions.
  • the embodiment further provides a liquid crystal display substrate including an alignment layer formed of the above alignment material.
  • the liquid crystal display substrate may be an array substrate or a color film substrate, and may further include other display structures such as a thin film transistor array, a pixel electrode, a color filter film, and the like, and the alignment layer covers other display structures.
  • the alignment material is mainly formed by heat curing to form an alignment layer, and specific curing methods, parameters and the like are known, and thus will not be described in detail herein.
  • the liquid crystal display substrate of the present embodiment has an alignment layer formed of the above alignment material, so that it can continuously emit far infrared rays and negative ions during use, and is environmentally friendly.

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Abstract

本发明提供一种功能材料及其制备方法、配向材料、液晶显示基板，属于显示技术领域，其可解决现有液晶显示装置存在污染的问题。本发明的功能材料包括表面带有改性层的无机粉末，无机粉末包括氧化铝、氧化镁、氧化锌、氧化锆、二氧化硅、二氧化钛、氧化硼、三氧化二铁、氧化钙、氧化钾、氧化钠、氧化锂中的任意一种或多种；改性层由二元酐和二元胺的反应产物经脱水闭环而得。本发明的配向材料包括上述功能材料。本发明的液晶显示基板包括由上述配向材料形成的配向层。

Description

功能材料及其制备方法、配向材料、液晶显示基板 技术领域
本发明涉及显示技术领域，尤其涉及一种功能材料及其制备方法、配向材料、液晶显示基板。
背景技术
在液晶显示装置中，配向层是重要的结构之一，其经过摩擦或紫外光照射后可产生特定的取向结构，从而使与其接触的液晶分子按照特定的方向排列(即取向)，实现用液晶进行滤光的目的。
其中，配向层通常位于液晶显示基板(如阵列基板、彩膜基板)中，并覆盖在所有其他的显示结构(如薄膜晶体管阵列、像素电极、彩色滤光膜等)上。配向层由配向材料固化而成，配向材料中含有聚酰亚胺、交联剂、溶剂等。
在液晶显示装置使用时，不可避免的会产生一些电磁辐射，从而对人体健康造成不良影响。
发明内容
本发明针对现有液晶显示装置会产生污染的问题，提供一种可起到医疗保健作用且对环境友好的功能材料及其制备方法、配向材料、液晶显示基板。
解决本发明技术问题所采用的技术方案是一种功能材料，其包括表面带有改性层的无机粉末，所述无机粉末包括：
氧化铝、氧化镁、氧化锌、氧化锆、二氧化硅、二氧化钛、氧化硼、三氧化二铁、氧化钙、氧化钾、氧化钠、氧化锂中的任意一种或多种；
所述改性层由二元酐和二元胺的反应产物经脱水闭环而得。
例如，用于生成所述改性层的二元酐与二元胺的物质的量的比在(0.85～1.05)∶1。
进一步优选的是，用于生成所述改性层的二元酐与二元胺的物质的量的比在(0.92～1.05)∶1。
例如，所述用于生成所述改性层的二元酐中含有至少一个苯基；所述用 于生成所述改性层的二元胺中含有至少一个苯基或非苯基的六元碳环。
进一步优选的是，用于生成所述改性层的二元酐选自均苯四甲酸二酐、偏苯三酸酐、二苯酮二酐、联苯二酐、二苯醚二酐、六氟二酐中的任意一种；用于生成所述改性层的二元胺选自3-氨基苄胺、2,2'-二氟-4,4'-(9-亚芴基)二苯胺、2,2-双(3-氨基-4-羟苯基)六氟丙烷、六氢-间苯二甲基二胺、1,4-二(氨甲基)环己烷、2,2-双[4-(4-氨基苯氧基)苯]六氟丙烷、2,2-双(3-氨基-4-甲苯基)六氟丙烷、2,2-双(3-氨基苯基)六氟丙烷、2,2-双(4-氨基苯基)六氟丙烷、2,7-二氨基芴、间苯二甲胺、4,4'-亚甲基双(2-乙基-6-甲基苯胺)中的任意一种。
例如，所述无机粉末的粒径在1～5000nm。
解决本发明技术问题所采用的技术方案是一种制备上述功能材料的方法，其包括：
S1、将所述无机粉末、二元酐、二元胺与引发剂、溶剂混合均匀；
S2、加热使所述二元酐与二元胺反应，在无机粉末表面形成所述中间产物层；
S3、对带有中间产物层的无机粉末进行加热，使中间产物层脱水闭环，得到所述功能材料。
例如，所述无机粉末的质量与二元酐、二元胺反应后生成的物质的质量的比为(20～1)∶1。
例如，所述步骤S2中的加热分为两步进行，其具体为：在35～70℃的温度下加热20～40min；在70～100℃的温度下加热20～40min。
例如，所述步骤S3中的加热为：在50～300℃的温度下加热30～60min。
解决本发明技术问题所采用的技术方案是一种配向材料，其包括：
聚酰亚胺；
偶联剂；
溶剂；和
上述的功能材料。
例如，在不计算所述功能材料的改性层质量的情况下，所述配向材料中各组分的质量百分含量为：聚酰亚胺：1～20％；偶联剂：0.1～5％；溶剂：72.5～98％；功能材料的无机粉末：0.1～2.5％。
进一步优选的是，在不计算所述功能材料的改性层质量的情况下，所述 配向材料中功能材料的无机粉末的质量百分含量在0.1～2％。
进一步优选的是，在不计算所述功能材料的改性层质量的情况下，所述配向材料中功能材料的无机粉末的质量百分含量在0.1～1.8％。
其中，“在不计算功能材料的改性层质量的情况下，配向材料中某物质的质量百分含量”是指以配向材料中除功能材料的改性层之外的其余全部物质(功能材料的无机粉末、聚酰亚胺、偶联剂、溶剂等)的质量为100％时，某物质的质量百分含量。
解决本发明技术问题所采用的技术方案是一种液晶显示基板，其包括配向层，且
所述配向层是由上述配向材料固化得到的。
本发明的功能材料可发出远红外线和负离子；远红外线被人体吸收后可使体内水分子共振，活化水分子，增强分子间结合力，从而活化蛋白质等生物大分子，使生物体细胞处于最高振动能级；且远红外热量可传递到皮下较深的部分，使皮下深层温度上升，扩张毛细血管，促进血液循环，强化各组织之间的新陈代谢，增强组织再生能力，提高机体免疫力，调节精神异常兴奋状态；而负离子对细菌和有机物有分解和氧化作用，可起到杀菌消毒和净化环境空气质量的效果；因此，该功能材料可起到医疗保健作用，对环境友好。
本发明的功能材料的无机粉末表面具有改性层，该改性层可与配向材料的主要成分(聚酰亚胺)良好的融合，从而使功能材料可稳定的分布在配向层中；并且该改性层还可改善无机粉末发出远红外线和负离子的能力。
本发明的液晶显示基板具有由上述配向材料生成的配向层，故其在使用过程中可持续发出远红外线和负离子，对环境友好。
附图说明
图1为本发明实施例的功能材料的制备方法的流程图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合附图和具体实施方式对本发明作进一步详细描述。
本实施例提供一种功能材料及其制备方法。
该功能材料包括表面带有改性层的无机粉末，该无机粉末包括氧化铝、氧化镁、氧化锌、氧化锆、二氧化硅、二氧化钛、氧化硼、三氧化二铁、氧化钙、氧化钾、氧化钠、氧化锂中的任意一种或多种；且
所述改性层由二元酐和二元胺的反应产物经脱水闭环而得。
其中，无机粉末的粒径在纳米量级至微米量级，具体例如在1～5000nm，优选在10～500nm。粒径例如可采用马尔文激光粒度仪进行测量。
其中，二元酐是指分子结构中含有至少两个酸酐基团的物质；而二元胺是指分子结构中含有至少两个胺基(或氨基)的物质。
其中，二元酐中例如含有至少一个苯基，其优选为均苯四甲酸二酐、偏苯三酸酐、二苯酮二酐、联苯二酐、二苯醚二酐、六氟二酐中的任意一种。
其中，二元胺中例如含有至少一个苯基或非苯基的六元碳环(例如环己烷基)，其优选为3-氨基苄胺、2,2'-二氟-4,4'-(9-亚芴基)二苯胺、2,2-双(3-氨基-4-羟苯基)六氟丙烷、六氢-间苯二甲基二胺、1,4-二(氨甲基)环己烷、2,2-双[4-(4-氨基苯氧基)苯]六氟丙烷、2,2-双(3-氨基-4-甲苯基)六氟丙烷、2,2-双(3-氨基苯基)六氟丙烷、2,2-双(4-氨基苯基)六氟丙烷、2,7-二氨基芴、间苯二甲胺、4,4'-亚甲基双(2-乙基-6-甲基苯胺)中的任意一种。
其中，二元酐与二元胺的物质的量的比例如为(0.85～1.05)∶1；优选在(0.92～1.05)∶1。
其中，二元酐和二元胺反应后可在无机粉末表面生成一层产物(中间产物层)，该层产物再经过脱水闭环，即可得到上述改性层。该改性层可与配向材料中的主要成分(聚酰亚胺)良好的融合，从而使功能材料可稳定的分布在配向层中；并且该改性层还可改善无机粉末发出远红外线和负离子的能力。
本实施例的功能材料可发出远红外线和负离子；远红外线被人体吸收后可使体内水分子共振，活化水分子，增强分子间结合力，从而活化蛋白质等生物大分子，使生物体细胞处于最高振动能级；且远红外热量能传递到皮下较深的部分，使皮下深层温度上升，扩张毛细血管，促进血液循环，强化各组织之间的新陈代谢，增强组织再生能力，提高机体免疫力，调节精神异常兴奋状态；而负离子对细菌和有机物有分解和氧化作用，可起到杀菌消毒和净化环境空气质量的效果；因此，本实施例的功能材料可起到医疗保健作用， 对环境友好。
上述功能材料的制备方法包括：将所述无机粉末、二元酐、二元胺与引发剂、溶剂混合均匀；加热使所述二元酐与二元胺反应，在无机粉末表面形成所述中间产物层；对带有中间产物层的无机粉末进行加热，使中间产物层脱水闭环，得到所述功能材料。
具体的，如图1所示，上述制备方法可包括：
S01、在使用分散剂的情况下，将各原料分别粉碎为粉末后按比例混合均匀，或将各原料按比例混合均匀后再粉碎，得到无机粉末。
其中，分散剂可选用德国毕克公司生产的BYK 161、路博润公司生产的Solsperse 32500、Solsperse 22000等常规分散剂；粉碎可采用球磨、研磨等常规方式；由于得到无机粉末可采用已知的方法，故在此不再详细描述。
S02、将占总量1/4～1/3的引发剂及占总量1/4～1/3的二元胺溶解在溶剂中备用。
其中，无机粉末的质量与二元酐、二元胺反应后生成的物质的质量的比为(20～1)∶1。
也就是说，二元酐、二元胺的用量按照如下的方式确定：假设二元酐与二元胺可完全反应并得到生成物，若该生成物的质量为1，则无机粉末的质量就在1～20之间；这样的用量可保证最终在无机粉末上得到厚度合适的改性层。
其中，引发剂用于引发反应，其例如为氮类引发剂，优选为偶氮二异丁腈、2,2'-双偶氮-(2,4-二甲基戊腈)、偶氮二异丁酸二甲酯、偶氮二异戊腈中的任意一种。
其中，溶剂可选自脂肪醇、乙二醇醚、乙酸乙酯、甲乙酮、甲基异丁基酮、单甲基醚乙二醇酯、γ-丁内酯、丙酸-3-乙醚乙酯、丁基卡必醇、丁基卡必醇醋酸酯、丙二醇单甲基醚、丙二醇单甲基醚醋酸酯、环己烷、二甲苯、异丙醇等常规的有机溶剂。由于溶剂的作用只是分散各物质，故在各实施例具体制备功能材料的过程中，统一采用丙二醇单甲基醚醋酸酯作溶剂。
S03、将无机粉末加入反应容器(如四口瓶)中，并开始搅拌、震荡、摇动等；之后加入二元酐、溶剂，以及剩余的引发剂、二元胺，溶解均匀。
S04、开始加热以进行反应，在无机粉末表面形成所述中间产物层；其 例如分为两步进行，具体可包括：先在35～70℃的温度下加热20～40min；之后继续在70～100℃的温度下加热20～40min。
以上的加热过程中，可使二元酐与二元胺间发生反应，从而在无机粉末表面生成中间产物层；其中，之所以分步加热，主要是为了防止反应过于剧烈。
在反应过程中，逐渐将上述溶解有引发剂和二元胺的溶液逐渐滴加到四口瓶中；之所以这样加入，是为了防止反应过于剧烈。
其中，本步反应例如在氮气保护下进行，且在反应过程中例如一直保持搅拌。
其中，各步骤中溶剂的用量以能将其中的物质均匀的分散、溶解为准，而引发剂用量以能引发反应为准，这些可由本领域技术人员根据实际情况调整，在此不再详细描述。但通常而言，无机粉末、引发剂、溶剂的质量比(均指总量)为1∶(0.25～0.4)∶(1～1.5)，为了统一，故在各实施例具体制备功能材料的过程中，统一使无机粉末、引发剂、溶剂的质量比为1∶0.3∶1.4。
S05、反应结束后将粉末分离出来，得到带有中间产物层的无机粉末。
也就是说，通过过滤、蒸干溶剂等方式，将带有中间产物层的无机粉末从溶液中分离出来。
S06、对带有中间产物层的无机粉末进行加热，使中间产物层脱水闭环而形成改性层，得到所述功能材料。
也就是说，继续对无机粉末进行加热，使其中间产物层发生脱水闭环反应，得到可与聚酰亚胺良好相容的改性层。
例如，本步骤中的加热为在50～300℃的温度下加热30～60min。
当然，应当理解，以上所述的制备方法还可进行许多变化，例如，二元酐、二元胺、引发剂等可一次都溶解在溶剂中；再如，步骤S04中的加热也可只为一段等。总之，只要最终能使二元酐与二元胺反应并在无机粉末表面形成改性层即可。
本实施例还提供一种配向材料。
配向材料用于在液晶显示基板中形成配向层，其含有聚酰亚胺、溶剂、偶联剂和上述的功能材料。
例如，在不计算功能材料的改性层质量的情况下，配向材料中各组分的 质量百分含量为：聚酰亚胺：1～20％；偶联剂：0.1～5％；溶剂：72.5～98％；功能材料的无机粉末：0.1～2.5％。
其中，在不计算功能材料的改性层质量的情况下，功能材料(中的无机粉末)的质量百分含量更优选在0.1～2％，进一步优选在0.1～1.8％。
也就是说，以配向材料中除功能材料的改性层之外的其余全部物质(功能材料的无机粉末、聚酰亚胺、偶联剂、溶剂)的质量为100％时，各组分的含量如上。
其中，聚酰亚胺是生成配向层的主要材料，其含量例如在1～15％，优选在1～10％。
其中，偶联剂用于使聚酰亚胺发生交联以生成固态的配向层；该偶联剂可为硅烷偶联剂、氮硅烷偶联剂、或者苯氧基硅烷偶联剂，例如乙烯基硅烷、氨基硅烷、环氧基硅烷、巯基硅烷和甲基丙烯酰氧基硅烷等；其含量例如在0.1～5％，优选在0.1～3％。
溶剂用于使配向材料中的各组分溶解、分散，从而形成均匀、稳定的体系。该溶剂可选自有机溶剂，如N-甲基-2-吡咯酮、间-甲酚、γ-丁内酯、N,N-二甲基乙酰胺、N,N-二甲基甲酰胺、N-甲基己内酰胺、二甲基亚砜、γ-丁内酰胺、乙二醇单甲醚、乙二醇单乙醚、乙二醇单丙基醚、乙二醇单丁醚、二乙二醇单丁基醚、二乙二醇单乙基醚、丁基卡必醇、乙酸乙基卡必醇酯、乙二醇等。
其中，功能材料为上述的功能材料，将其添加到配向材料中后，可改善配向材料的环境友好度。
按照上述的制备方法，依照以下表格中的参数制备各实施例的功能材料。
之后，用所得功能材料继续按照以下表格中的参数制备配向材料，其制备中只要将各组分混合均匀即可，而不必采用特定的加料顺序及混合方法。
之后，按照GB/T 7287-2008标准测试各配向材料的红外线比辐射率，并用空气负离子测定仪(例如日本KEC公司的KEC-900型)测量其产生的负离子数量，结果如下表所示。
最后，用该配向材料固化形成配向层，并测试其电压保持率，具体为：将配向材料旋涂在表面具有氧化铟锡(ITO)层的基板上，在80℃下前烘2min，在220℃下后烘20min，然后以转速1200rpm、平台移动速度50mm/s的参数 进行定向摩擦，压入深度为0.3mm；用该基板组成液晶盒，之后施加脉冲电压(5V，60μ)对液晶盒充电，再用高速电压计测量16.7ms内液晶盒电压的变化，以仍保持的电压的比例作为电压保持率。
在各实施例中，聚酰亚胺统一采用JSR株式会社制造的型号为JSROPTMER AL23201的聚酰亚胺；偶联剂统一采用γ-氨丙基三乙氧基硅烷；溶剂统一采用γ-丁内酯；由于以上组分均是配向材料中的常规组分，故为了结果的可比性，此处统一采用以上物质进行试验。
表1、功能材料及配向材料的相关参数(含量单位均为质量份数)
Figure PCTCN2014091838-appb-000001
可见，各实施例的配向材料均具有较高的红外线比辐射率和负离子浓度，且由其生成的配向层的电压保持率也好，证明配向层本身的性能未受到影响，且同时可产生远红外线和负离子，从而达到改善环境的作用。
本实施例的功能材料的无机粉末表面具有改性层，该改性层可使无机粉末良好的与配向材料相容，并且还可提高该无机粉末发射远红外线和负离子的能力。
本实施例还提供一种液晶显示基板，其中包括由上述配向材料形成的配向层。
其中，液晶显示基板可为阵列基板或彩膜基板，其中还可包括薄膜晶体管阵列、像素电极、彩色滤光膜等其他显示结构，而配向层覆盖在其他的显示结构上。
配向材料主要通过加热固化而形成配向层，其具体的固化方法、参数等是已知的，故在此不再详细描述。
本实施例的液晶显示基板具有由上述配向材料生成的配向层，故其在使用过程中可持续发出远红外线和负离子，对环境友好。
可以理解的是，以上实施方式仅仅是为了说明本发明的原理而采用的示例性实施方式，然而本发明并不局限于此。对于本领域内的普通技术人员而言，在不脱离本发明的精神和实质的情况下，可以做出各种变型和改进，这些变型和改进也视为本发明的保护范围。
本申请要求于2014年7月29日递交的中国专利申请第201410366432.4号的优先权，在此全文引用上述中国专利申请公开的内容以作为本申请的一部分。

Claims (15)

  1. 一种功能材料，其包括表面带有改性层的无机粉末，所述无机粉末包括：
    氧化铝、氧化镁、氧化锌、氧化锆、二氧化硅、二氧化钛、氧化硼、三氧化二铁、氧化钙、氧化钾、氧化钠、氧化锂中的任意一种或多种；
    所述改性层由二元酐和二元胺的反应产物经脱水闭环而得。
  2. 根据权利要求1所述的功能材料，其中，
    用于生成所述改性层的二元酐与二元胺的物质的量的比在(0.85～1.05)∶1。
  3. 根据权利要求2所述的功能材料，其中，
    用于生成所述改性层的二元酐与二元胺的物质的量的比在(0.92～1.05)∶1。
  4. 根据权利要求1所述的功能材料，其中，
    所述用于生成所述改性层的二元酐中含有至少一个苯基；
    所述用于生成所述改性层的二元胺中含有至少一个苯基或非苯基的六元碳环。
  5. 根据权利要求4所述的功能材料，其中，
    用于生成所述改性层的二元酐选自均苯四甲酸二酐、偏苯三酸酐、二苯酮二酐、联苯二酐、二苯醚二酐、六氟二酐中的任意一种；
    用于生成所述改性层的二元胺选自3-氨基苄胺、2,2'-二氟-4,4'-(9-亚芴基)二苯胺、2,2-双(3-氨基-4-羟苯基)六氟丙烷、六氢-间苯二甲基二胺、1,4-二(氨甲基)环己烷、2,2-双[4-(4-氨基苯氧基)苯]六氟丙烷、2,2-双(3-氨基-4-甲苯基)六氟丙烷、2,2-双(3-氨基苯基)六氟丙烷、2,2-双(4-氨基苯基)六氟丙烷、2,7-二氨基芴、间苯二甲胺、4,4'-亚甲基双(2-乙基-6-甲基苯胺)中的任意一种。
  6. 根据权利要求1至5中任意一项所述的功能材料，其中，
    所述无机粉末的粒径在1～5000nm。
  7. 制备权利要求1至6中任意一项所述的功能材料的方法，所述制备方法包括：
    S1、将所述无机粉末、二元酐、二元胺与引发剂、溶剂混合均匀；
    S2、加热使所述二元酐与二元胺反应，在无机粉末表面形成所述中间产物层；
    S3、对带有中间产物层的无机粉末进行加热，使中间产物层脱水闭环，得到所述功能材料。
  8. 根据权利要求7所述的功能材料的制备方法，其中，
    所述无机粉末的质量与二元酐、二元胺反应后生成的物质的质量的比为(20～1)∶1。
  9. 根据权利要求7所述的功能材料的制备方法，其中，所述步骤S2中的加热分为两步进行：
    在35～70℃的温度下加热20～40min；
    在70～100℃的温度下加热20～40min。
  10. 根据权利要求7所述的功能材料的制备方法，其中，所述步骤S3中的加热为：
    在50～300℃的温度下加热30～60min。
  11. 一种配向材料，其包括：
    聚酰亚胺；
    偶联剂；
    溶剂；和
    权利要求1至6中任意一项所述的功能材料。
  12. 根据权利要求11所述的配向材料，其中，在不计算所述功能材料的改性层质量的情况下，所述配向材料中各组分的质量百分含量为：
    聚酰亚胺：1～20％；
    偶联剂：0.1～5％；
    溶剂：72.5～95％；
    功能材料的无机粉末：0.1～2.5％。
  13. 根据权利要求11或12所述的配向材料，其中，
    在不计算所述功能材料的改性层质量的情况下，所述配向材料中功能材料的无机粉末的质量百分含量在0.1～2.0％。
  14. 根据权利要求13所述的配向材料，其中，
    在不计算所述功能材料的改性层质量的情况下，所述配向材料中功能材料的无机粉末的质量百分含量在0.1～1.8％。
  15. 一种液晶显示基板，包括配向层，其中，
    所述配向层是由权利要求11至14中任意一项所述的配向材料固化得到的。
PCT/CN2014/091838 2014-07-29 2014-11-21 功能材料及其制备方法、配向材料、液晶显示基板 WO2016015409A1 (zh)

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