WO2016015410A1 - 功能材料及其制备方法、封接材料、显示面板 - Google Patents
功能材料及其制备方法、封接材料、显示面板 Download PDFInfo
- Publication number
- WO2016015410A1 WO2016015410A1 PCT/CN2014/091854 CN2014091854W WO2016015410A1 WO 2016015410 A1 WO2016015410 A1 WO 2016015410A1 CN 2014091854 W CN2014091854 W CN 2014091854W WO 2016015410 A1 WO2016015410 A1 WO 2016015410A1
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- WO
- WIPO (PCT)
- Prior art keywords
- functional material
- modified layer
- oxide
- inorganic powder
- sealing material
- Prior art date
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 239000003566 sealing material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 54
- 150000004985 diamines Chemical class 0.000 claims abstract description 33
- 238000007789 sealing Methods 0.000 claims abstract description 30
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000292 calcium oxide Substances 0.000 claims abstract description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 4
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- 229910001947 lithium oxide Inorganic materials 0.000 claims abstract description 4
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001950 potassium oxide Inorganic materials 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
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- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 4
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- 230000008018 melting Effects 0.000 claims description 8
- -1 hexafluoro dianhydride Chemical compound 0.000 claims description 7
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 6
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 6
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- C—CHEMISTRY; METALLURGY
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L9/00—Disinfection, sterilisation or deodorisation of air
- A61L9/16—Disinfection, sterilisation or deodorisation of air using physical phenomena
- A61L9/22—Ionisation
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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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
- C09K11/02—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
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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
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/676—Aluminates; Silicates
-
- 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
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/842—Containers
- H10K50/8426—Peripheral sealing arrangements, e.g. adhesives, sealants
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/87—Passivation; Containers; Encapsulations
- H10K59/871—Self-supporting sealing arrangements
- H10K59/8722—Peripheral sealing arrangements, e.g. adhesives, sealants
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/02—Antibacterial glass, glaze or enamel
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2205/00—Compositions applicable for the manufacture of vitreous enamels or glazes
Definitions
- a display panel of the type such as an organic light emitting diode (OLED) display panel includes two display substrates (for example, an array substrate 11 and a package substrate 12) that are joined together on the outer side of the display area of the two display substrates.
- a sealing structure 2 is disposed between the regions, and the sealing structure 2 is used for connecting the two display substrates together, and prevents external moisture, oxygen, and the like from entering the display area to affect the display structure of the organic light emitting diode 19 or the like therein.
- the sealing structure 2 is usually formed of a sealing material, and the sealing material generally includes components such as a low-melting glass frit, a cellulose resin, a solvent, an additive (such as an antifoaming agent, an adhesion promoter).
- 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 sealing material further includes an additive, and in the case where the quality of the modified layer of the functional material is not calculated, the mass percentage of each component in the sealing material is:
- the inorganic powder of the functional material has a mass percentage in the sealing material of 0.1 to 2.0% without calculating the quality of the modified layer of the functional material.
- the inorganic powder of the functional material has a mass percentage in the sealing material of 0.1 to 1.8% without calculating the quality of the modified layer of the functional material.
- the inorganic powder surface of the functional material of the present invention has a modified layer which allows the inorganic powder to be well incorporated into the sealing structure, and also improves the ability of the inorganic powder to emit far infrared rays and negative ions.
- the sealing structure of the display panel of the present invention includes the above-mentioned functional materials, so that it can continuously emit far infrared rays and negative ions during use, and is environmentally friendly.
- 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 diamine contains, for example, at least one phenyl or non-phenyl six-membered carbocyclic ring (e.g., cyclohexyl), which is preferably 3-aminobenzylamine, 2,2'-difluoro-4,4'-( 9-indenyl)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-double (3-Aminophenyl)hexafluoropropane, 2,2-bis(4-aminophenyl)hexafluoropropane, 2,7-dia
- 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.
- a reaction between the dibasic anhydride and the diamine can be made to form a modified layer on the surface of the inorganic powder; wherein the stepwise heating is mainly to prevent the reaction from being too intense.
- the low-melting glass is a main component for forming a sealing structure, and may be boron oxide-zinc oxide-vanadium oxide glass, vanadium oxide-zinc oxide-yttria glass, or the like, and has a particle diameter of 500 nm to 6 ⁇ m.
- the additive is used to improve the performance of different aspects of the sealing material, and may include an adhesion promoter, an antifoaming agent, a wetting leveling agent, and the like.
- the solvent is used to dissolve and disperse other components to form a uniform and stable system, which may be a conventional organic solvent such as a ketone, an ester, an ether, an aliphatic hydrocarbon, a cycloalkane, an aromatic hydrocarbon or the like.
- the sealing material is prepared by using the above functional materials in the proportions of the following table, wherein the components can be uniformly mixed without using a specific feeding sequence and mixing method.
- the low-melting glass is uniformly selected from vanadium oxide-boron oxide-zinc oxide glass
- the cellulose resin is uniformly selected from the cellulose resin of the type Ethyl Cellulose A186
- the solvent is uniformly selected from diethylene glycol butyl ether acetate; Use the defoamer type BYK-A555.
- the embodiment further provides a display panel including a first substrate (such as an array substrate) and a second substrate (such as a package substrate) that are opposite to each other.
- a display panel including a first substrate (such as an array substrate) and a second substrate (such as a package substrate) that are opposite to each other.
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Abstract
本发明提供一种功能材料及其制备方法、封接材料、显示面板,属于显示技术领域,其可解决现有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反应生成。本发明封接材料包括上述功能材料。本发明的显示面板中包括由上述功能材料形成的封接结构。
Description
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、封接材料、显示面板。
如图1所示,在有机发光二极管(OLED)显示面板等类型的显示面板包括两块对合在一起的显示基板(如阵列基板11和封装基板12),在两显示基板的显示区的外侧区域之间设有封接结构2,封接结构2用于将两显示基板连接在一起,并防止外界的水分、氧气等进入显示区而影响其中的有机发光二极管19等显示结构。封接结构2通常由封接材料形成,封接材料中通常括低熔点玻璃粉、纤维素树脂、溶剂、添加剂(如消泡剂、附着力促进剂)等成分。
但是,现有的显示装置在使用中不可避免的会产生一定的电磁辐射污染,影响人体健康。
发明内容
本发明针对现有显示装置存在污染的问题,提供一种可解决以上问题的功能材料及其制备方法、封接材料、显示面板。
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反应生成。
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:
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改性层。
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。
解决本发明技术问题所采用的技术方案是一种封接材料,其包括:
低熔点玻璃粉;
纤维素树脂;
溶剂;和
上述的功能材料。
例如,所述封接材料还包括添加剂,且在不计算所述功能材料的改性层质量的情况下,所述封接材料中各组分的质量百分含量为:
低熔点玻璃粉:10~50%;
纤维素树脂:10~30%;
溶剂:15~75%;
添加剂:0.2~5%。
其中,“在不计算功能材料的改性层质量的情况下,封接材料中某物质的质量百分含量”是指以封接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、纤维素树脂、溶剂、添加剂等)的质量之和为100%时,某物质的含量。
例如,在不计算所述功能材料的改性层质量的情况下,所述功能材料的无机粉末在所述封接材料中的质量百分含量在0.1~2.5%。
优选的是,在不计算所述功能材料的改性层质量的情况下,所述功能材料的无机粉末在所述封接材料中的质量百分含量在0.1~2.0%。
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,所述功能材料的无机粉末在所述封接材料中的质量百分含量在0.1~1.8%。
解决本发明技术问题所采用的技术方案是一种显示面板,其包括相互对盒的第一基板和第二基板,所述第一基板和第二基板间通过封接结构连接,
所述封接结构由上述的封接材料形成。
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,该改性层可使无机粉末良好的融入封接结构中,并且还可提高该无机粉末发射远红外线和负离子的能力。
本发明的显示面板的封接结构中包括上述的功能材料,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。
图1为现有显示面板的剖面结构示意图;
图2为本发明实施例的功能材料的制备方法的流程图。
其中,附图标记为:11、阵列基板;12、封装基板;19、有机发光二极管;2、封接结构。
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反应生成。
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。
经研究发现,上述的二元酐和二元胺反应后生成的改性层可最好的改善无机粉末的性质。
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改性层。
具体的,如图2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(实际为改性层),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,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改性层;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、反应结束后用经冷藏的溶剂使反应物冷却至室温(约10~30℃)。
S06、蒸干剩余溶剂或将粉末从中分离出来,得到带有改性层的无机粉末,即得到功能材料。
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,加热也可只为一段等。总之,只要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封接材料,其包括:低熔点玻璃粉;纤维素树脂;溶剂;上述的功能材料。
封接材料用于在显示面板中形成封接结构,从而将两显示基板连接,并阻止水分、氧气进入显示区。
例如,封接材料还包括添加剂,且在不计算功能材料的改性层质量的情况下,所述封接材料中各组分的质量百分含量为:
低熔点玻璃粉:10~50%;
纤维素树脂:10~30%;
溶剂:15~75%;
添加剂:0.2~5%。
也就是说,在以封接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、纤维素树脂、溶剂、添加剂等)的质量为100%时,各组分的含量如上。
其中,低熔点玻璃是用于形成封接结构的主要成分,其可为氧化硼-氧化锌-氧化钒玻璃、氧化钒-氧化锌-氧化钡玻璃等,粒径可在500nm~6μm。
其中,纤维素树脂用于作为载体材料使封接材料初步固化为所需的形状,以便用其形成封接结构。具体的,纤维素树脂可选自甲基纤维素、乙基纤维素、羧乙基纤维素、羧甲基纤维素、羧甲基羟乙基纤维素等;且其优选的含量在10~25%,进一步优选在10~20%。
在封接材料中还含有上述功能材料,故由其制成的封接结构可发出远红外线和负离子;在不计算功能材料的改性层质量的情况下,封接材料中功能材料的无机粉末的质量百分含量例如在0.1~2.5%,优选在0.1~2.0%,进一步优选在0.1~1.8%。
其中,添加剂用于改善封接材料不同方面的性能,其可包括附着力促进剂、消泡剂、润湿流平剂等。
其中,溶剂用于将其他组分溶解、分散,以形成均匀、稳定的体系,其可为常规的有机溶剂,如酮、酯、醚、脂肪烃、环烷烃、芳香烃等。
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。
表1、功能材料的相关参数(含量单位均为质量份数)
用以上的功能材料按照下表的比例配制封接材料,其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。
在各实施例中,低熔点玻璃统一选用氧化钒-氧化硼-氧化锌玻璃,纤维素树脂统一选用型号为Ethyl Cellulose A186的纤维素树脂,溶剂统一选用二乙二醇丁醚醋酸酯;添加剂统一选用型号为BYK-A555的消泡剂。
其中,在封接材料中,除功能材料外均为常规组分,故在此为了结果的可比性,其他的组分选用了统一的物质。
之后,通过丝网印刷工艺将封接材料施加在基板的所需区域中,之后在380℃温度下固化烧结90min,使封接材料初步固化;之后将另一基板对盒,并用激光照射初步固化的封接材料使其熔融,从而形成厚度为5μm、宽度为700μm的封接结构。
之后,按照GB/T 7287-2008标准测试封接结构的红外线比辐射率,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;再用扫描电镜观察封接结构的封接截面。
表2、封接材料及封接结构的相关参数(含量单位均为质量份数)
实施例 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
功能材料的无机粉末量 | 0.1 | 0.4 | 0.6 | 2.5 | 0.8 | 1.2 | 1 | 2 | 1.8 | 1.4 |
低熔点玻璃粉量 | 45 | 12 | 38 | 40 | 35 | 38 | 40 | 45 | 40 | 43 |
纤维素树脂量 | 30 | 14 | 20 | 25 | 19 | 20 | 25 | 28 | 25 | 25 |
溶剂量 | 19.9 | 68.6 | 37.4 | 32.3 | 41.7 | 39 | 31.2 | 24.5 | 32.4 | 29.4 |
添加剂量 | 5 | 5 | 4 | 0.2 | 3.5 | 1.8 | 2.8 | 0.5 | 0.8 | 1.2 |
远红外线比辐射率(%) | 50 | 62 | 83 | 96 | 91 | 93 | 92 | 95 | 94 | 92 |
负离子浓度(个/cm3) | 135 | 480 | 765 | 2100 | 950 | 1510 | 1100 | 1980 | 1820 | 1600 |
封接截面形态 | 致密 | 致密 | 致密 | 致密 | 致密 | 致密 | 致密 | 致密 | 致密 | 致密 |
可见,各实施例的封接材料均有较高的红外线比辐射率和负离子浓度,证明其可产生远红外线和负离子,从而达到改善环境的作用。同时,封接结构的封接截面形态致密,表示其密封性能也好,证明功能材料的加入对其本身性能未产生不良影响。
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融入封接结构中,并且还可提高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显示面板,其包括相互对盒的第一基板(如阵列基板)和第二基板(如封装基板)。
第一基板和第二基板间通过封接结构相互连接,该封接结构位于两基板的显示区外侧的区域之间,可起到阻止水分、氧气等进入显示区的作用。
其中,封接结构由上述封接材料形成,其具体可为先将封接材料通过丝网印刷等工艺施加在封装基板上,之后加热烧结使其初步固化,再将阵列基板对盒,并用激光照射使初步固化的封接材料熔融形成封接结构;或者,也可在使封接材料初步固化后将其从基板上取下,并加工成条状等合适形式,再次设于所需的位置,之后进行激光熔融以形成封接结构。
其中,形成封接结构的具体方法是已知的,在此不再详细描述。但通常而言,其固化的温度可在280~550℃;固化的时间可在50~120min;而激光照射的参数根据材料和设备别而定;最终所得封接结构的厚度通常在3.5μm~5.5μm,宽度在500μm~1.0mm。
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201410367032.5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)
- 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反应生成。
- 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。
- 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。
- 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。
- 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。
- 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。
- 一种制备权利要求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: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改性层。
- 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。
- 根据权利要求7所述的功能材料的制备方法,其中,所述加热分为两步进行:在35~70℃的温度下加热20~40min;在70~100℃的温度下加热20~40min。
- 一种封接材料,其包括:低熔点玻璃粉;纤维素树脂;溶剂;和权利要求1至6中任意一项所述的功能材料。
- 根据权利要求10所述的封接材料,其中,所述封接材料还包括添加剂,且在不计算所述功能材料的改性层质量的情况下,所述封接材料中各组分的质量百分含量为:低熔点玻璃粉:10~50%;纤维素树脂:10~30%;溶剂:15~75%;添加剂:0.2~5%。
- 根据权利要求10或11所述的封接材料,其中,在不计算所述功能材料的改性层质量的情况下,所述功能材料的无机粉末在所述封接材料中的 质量百分含量在0.1~2.5%。
- 根据权利要求12所述的封接材料,其中,在不计算所述功能材料的改性层质量的情况下,所述功能材料的无机粉末在所述封接材料中的质量百分含量在0.1~2%。
- 根据权利要求13所述的封接材料,其中,在不计算所述功能材料的改性层质量的情况下,所述功能材料的无机粉末在所述封接材料中的质量百分含量在0.1~1.8%。
- 一种显示面板,包括相互对盒的第一基板和第二基板,所述第一基板和第二基板间通过封接结构连接,其中,所述封接结构由权利要求10至14中任意一项所述的封接材料形成。
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