WO2018205336A1 - Led封装材料及制备方法 - Google Patents

Led封装材料及制备方法 Download PDF

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WO2018205336A1
WO2018205336A1 PCT/CN2017/087821 CN2017087821W WO2018205336A1 WO 2018205336 A1 WO2018205336 A1 WO 2018205336A1 CN 2017087821 W CN2017087821 W CN 2017087821W WO 2018205336 A1 WO2018205336 A1 WO 2018205336A1
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Prior art keywords
graphene
exchange resin
curing agent
mixed solution
accelerator
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English (en)
French (fr)
Inventor
王海军
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TCL China Star Optoelectronics Technology Co Ltd
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Shenzhen China Star Optoelectronics Technology Co Ltd
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Priority to US15/737,159 priority Critical patent/US10418531B2/en
Publication of WO2018205336A1 publication Critical patent/WO2018205336A1/zh
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/852—Encapsulations
    • H10H20/854—Encapsulations characterised by their material, e.g. epoxy or silicone resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01—Manufacture or treatment
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/8506—Containers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

Definitions

  • the invention relates to an LED packaging material, in particular to an LED packaging material with graphene and a preparation method of the packaging material.
  • LED is composed of chip, metal wire, bracket, conductive adhesive, packaging material, etc.
  • the main function of the packaging material is to prevent the chip from being affected by humidity, temperature, oxidation and the like to reduce the efficiency, thereby protecting the normal operation of the chip.
  • the encapsulating material also has the following functions: fixing the electronic device, avoiding changes in the device parameters caused by mechanical vibration or the like; reducing the refractive index between the LED chip and the air, improving the light emitting efficiency; and functioning as an LED chip Heat dissipation. Therefore, the LED packaging material not only has better sealing property, higher transmittance, but also superior bonding strength.
  • the current LED packaging materials mainly include epoxy resin, silicone and other materials.
  • epoxy resin has become a mainstream material for LED packaging because of its excellent adhesion, electrical insulation, sealing and dielectric properties, and low cost and easy molding.
  • Silicone materials have good transparency, high temperature resistance, weather resistance, insulation and strong hydrophobicity, making them ideal for LED packaging materials.
  • the epoxy resin itself has defects such as hygroscopicity, aging, poor heat resistance, easy discoloration under high temperature and short-wave illumination, and large internal stress of curing.
  • the unfavorable factors will greatly affect and shorten the service life of the LED device; while the silicone material itself does not have strong mechanical strength and high thermal expansion rate.
  • these unfavorable factors will have a serious impact on the performance of the LED packaging materials.
  • Embodiments of the present invention provide a novel LED packaging material formed by combining graphene with silane or epoxy resin to improve the defects of single silane or epoxy resin for preparing LED packaging materials by using the characteristics of graphene to improve The performance of LED packaging materials.
  • the present invention provides an LED package material of the first embodiment, which is made of the following materials by weight: curing agent 10%-40%, graphene 0.05%-1%, ring Oxygen resin 40%-60% and accelerator 0.5%-2%.
  • the curing agent is composed of one or more of the following materials: methyltetrahydrophthalic anhydride, divinyltriamine, aminoethylpiperazine, 1,2-diaminocyclohexane, tetraethylenepentamine , dimethylaminopropylamine, dihexyltriamine, methylene bisphenylenediamine.
  • the graphene has a hydroxyl group and/or a carboxyl group added to its surface by surface modification.
  • the accelerator is an accelerator that promotes mutual dispersion between the raw materials, or an accelerator that promotes mutual dissolution between the raw materials to promote mixing between the graphene and the epoxy resin.
  • the present invention provides a method for preparing an LED package material according to the first embodiment, comprising the following steps:
  • a mixed solution of graphene and a curing agent is sufficiently mixed by ultrasonication to form an LED encapsulating material formed by combining graphene and an epoxy resin.
  • the curing agent is composed of one or more of the following materials: methyltetrahydrophthalic anhydride, divinyltriamine, aminoethylpiperazine, 1,2-diaminocyclohexane, tetraethylenepentamine , dimethylaminopropylamine, dihexyltriamine, methylene bisphenylenediamine;
  • the graphene is added with a hydroxyl group and/or a carboxyl group on its surface by surface modification;
  • the accelerator promotes mutual dispersion between the raw materials The promoter, or an accelerator that promotes mutual dissolution between the materials, to promote mixing between the graphene and the epoxy resin.
  • the weight percentage of each component is as follows: curing agent 10%-40%, graphene 0.05%-1%, epoxy The resin is 40%-60% and the accelerator is 0.5%-2%.
  • the operation method of sufficiently mixing the curing agent with graphene is as follows: ultrasonically dispersing the mixed curing agent and graphene by using an ultrasonic disperser, wherein the ultrasonic power is 500 W-900 W, and the duration is 3-5. hour.
  • the method further comprises the steps of: first adding the mixed solution of graphene and a curing agent through a glass rod; The components in the mixed solution are uniformly distributed.
  • the method further comprises the steps of: adding the mixed solution thoroughly mixed by ultrasonic means into a vacuum oven, and at 60- Bake at 80 ° C for 1 hour to remove air bubbles from the mixed solution.
  • the present invention provides an LED package material according to a second embodiment, the LED package material being made of the following materials: silane, a control agent, a basic ion exchange resin, and graphene, wherein the alkalinity
  • the mass percentage of the ion exchange resin is from 5% to 10%
  • the mass percentage of the graphene is from 0.5% to 2%
  • the molar ratio of the silane to the control agent is from 1:0.3 to 1:1.
  • the controlling agent has a terminal hydroxyl group; and the basic ion exchange resin is a basic anion exchange resin or an alkaline cation exchange resin.
  • the present invention provides a method for preparing an LED package material according to a second embodiment, comprising the following steps:
  • Pre-dosing silane, control agent, basic ion exchange resin, and graphene are mixed and heated to form a package material sample;
  • the impurities in the sample of the encapsulating material are removed to obtain an LED encapsulating material.
  • the heating temperature is 30-80 ° C, and the heating time is 5-20 hours.
  • the impurities in the sample of the encapsulating material include a basic ion exchange resin remaining insufficiently reacted, and the residual basic ion exchange resin can be removed by filtration.
  • the impurities in the sample of the encapsulating material further comprise a low boiling point solvent, and the low boiling point solvent can be removed by decompression.
  • the mass percentage of the ion exchange resin is 5%-10%
  • the mass percentage of the graphene is 0.5%-2%
  • the molar ratio of the silane to the control agent is 1:0.3-1:1.
  • the controlling agent has a terminal hydroxyl group
  • the basic ion exchange resin is a basic anion exchange resin or an alkaline cation exchange Resin.
  • the LED package material provided in the embodiment of the present invention is formed by combining graphene with silane or epoxy resin to improve the defects of the LED package material prepared by using a single silane or epoxy resin by the characteristics of graphene to improve the LED package.
  • the properties of the material are described by combining graphene with silane or epoxy resin to improve the defects of the LED package material prepared by using a single silane or epoxy resin by the characteristics of graphene to improve the LED package.
  • FIG. 1 is a flow chart of a method for preparing an LED package material according to a first embodiment of the present invention.
  • FIG. 2 is a flow chart of a method for preparing an LED package material according to a second embodiment of the present invention.
  • connection In the description of the present invention, it should be noted that the terms “installation”, “connected”, and “connected” are to be understood broadly, and may be fixed or detachable, for example, unless otherwise explicitly defined and defined.
  • the ground connection, or the integral connection may be a mechanical connection; it may be directly connected, or may be indirectly connected through an intermediate medium, and may be internal communication between the two elements.
  • the ground connection or the integral connection; may be a mechanical connection; it may be directly connected, or may be indirectly connected through an intermediate medium, and may be internal communication between the two elements.
  • Embodiments of the present invention provide an LED package material and a preparation method thereof, which are formed by combining graphene with a silane or an epoxy resin to improve the appearance of an LED package material prepared from a single silane or an epoxy resin by virtue of the characteristics of graphene. Defects to improve the performance of LED packaging materials. The details are described below separately.
  • the LED package material of the first embodiment of the present invention is made of the following materials by weight: curing agent 10%-40%, graphene 0.05%-1%, epoxy resin 40%-60% and promotion The agent is 0.5% to 2%.
  • the curing agent may be one or more of the following materials: methyltetrahydrophthalic anhydride, divinyltriamine, aminoethylpiperazine, 1,2-diaminocyclohexane, Tetraethylene pentamine, dimethylaminopropylamine, dihexyltriamine, methylene bisphenylenediamine, and the like.
  • the type of the curing agent is not specifically limited herein.
  • the graphene may be surface-modified, for example, a group such as a hydroxyl group and/or a carboxyl group may be added to the surface thereof to enhance the properties of the graphene.
  • the type of the accelerator may be an accelerator that promotes mutual dispersion between the raw materials, or an accelerator that promotes mutual dissolution between the raw materials to promote the graphene and the epoxy resin. a mixture of things.
  • the type of the accelerator is not specifically limited in the present invention as long as it can promote thorough mixing between the graphene and the epoxy resin.
  • the LED packaging material provided by the embodiment can promote the formation of the LED packaging material by the combination of the graphene and the epoxy resin through the curing agent and the accelerator, so as to overcome the hygroscopicity, aging and resistance of the LED packaging material formed by the single epoxy resin.
  • the problems of defects such as poor heat, high temperature and short-wave illumination, such as easy discoloration and large internal stress, make the thermal conductivity, environmental stability and mechanical properties of the LED package material large. Great improvement.
  • FIG. 1 is a flow chart of a method for preparing an LED package material according to a first embodiment of the present invention, and the LED package material of the first embodiment described above can be prepared.
  • the method for preparing the LED package material includes at least the following steps.
  • Step 1 Providing a predetermined dose of a curing agent and graphene, and thoroughly mixing the curing agent with graphene.
  • the graphene is in a powder form to facilitate thorough mixing with the curing agent. Further, the graphene may be surface-modified before being mixed with a curing agent, and a group such as a hydroxyl group and/or a carboxyl group may be added to the surface thereof to enhance the performance of the graphene.
  • the curing agent may be one or more of the following materials: methyltetrahydrophthalic anhydride, divinyltriamine, aminoethylpiperazine, 1,2-diaminocyclohexane Alkane, tetraethylenepentamine, dimethylaminopropylamine, dihexyltriamine, methylenebisphenylenediamine, and the like.
  • the type of the curing agent is not specifically limited herein.
  • the method for sufficiently mixing the curing agent with graphene is as follows: ultrasonically treating the mixed curing agent and graphene with an ultrasonic disperser, wherein the ultrasonic power is 500 W-900 W, and the duration is It is 3-5 hours.
  • Step 2 Providing a dose of an epoxy resin and an accelerator, and adding it to a mixed solution of graphene and a curing agent.
  • the mixed solution contains a curing agent, graphene, an epoxy resin, and an accelerator.
  • the epoxy resin is the same as the epoxy resin material commonly used in existing LED packaging materials, and will not be described in detail herein.
  • the type of the accelerator may be an accelerator that promotes mutual dispersion between the raw materials, or an accelerator that promotes mutual dissolution between the raw materials to promote the graphene and the epoxy. Mixing between resins.
  • the type of the accelerator is not specifically limited in the present invention as long as it can promote thorough mixing between the graphene and the epoxy resin.
  • the weight percentage of each component in the mixed solution of the curing agent, graphene, epoxy resin and accelerator is as follows: curing agent 10%-40%, graphene 0.05%-1 %, epoxy resin 40%-60% and accelerator 0.5%-2%.
  • Step 3 The mixed solution after adding the graphene and the curing agent is thoroughly mixed by ultrasonication. To form an LED package material formed by combining graphene and epoxy resin.
  • the method before the step of sufficiently mixing the mixed solution of graphene and the curing agent by ultrasonication, the method further comprises the step of: adding the mixture of graphene and a curing agent by stirring with a glass rod.
  • the solution is such that the components in the mixed solution are uniformly distributed. After the components in the mixed solution were uniformly stirred by a glass rod, the components were thoroughly mixed by ultrasonication.
  • the length of time of stirring by means of a glass rod is 20 minutes, and the time of mixing by ultrasonication is usually 1 hour.
  • the method further comprises the steps of: adding the mixed solution thoroughly mixed by ultrasonic means to the vacuum oven. And baking at 60-80 ° C for 1 hour to remove air bubbles in the mixed solution.
  • the residual low-boiling solvent is volatilized into a gaseous state to form the bubbles, and therefore, the solvent can be volatilized into a gaseous state by vacuum (ie, The bubbles are removed, and the bubbles in the mixed solution can be eliminated.
  • the curing agent, the accelerator, the graphene and the epoxy resin are thoroughly mixed by means of ultrasonication, and the LED and the epoxy resin are combined to form the LED by the curing agent and the accelerator.
  • the encapsulating material can overcome the defects of hygroscopicity, aging, poor heat resistance, easy discoloration under high temperature and short-wave illumination, and large internal stress of solidification when forming an LED encapsulant from a single epoxy resin, so that the LED packaging material The thermal conductivity, environmental stability, mechanical properties, and thermal stability are greatly improved.
  • An LED package material which is made of the following materials: silane, a control agent, a basic ion exchange resin, and graphene, wherein the basic ion exchange resin has a mass percentage of 5%. -10%, the graphene has a mass percentage of 0.5% to 2%, and the molar ratio of the silane to the control agent is 1:0.3 to 1:1.
  • the silane type may be a silicone monomer such as methyltrichlorosilane, dimethyldichlorosilane, phenyltrichlorosilane or diphenyldichlorosilane, or may be other groups. Substituted silicone monomers, such as alkoxysilanes and the like. In the embodiment of the invention, the type of the silane is not specifically limited.
  • the specific type of the controlling agent is not limited as long as it has a terminal hydroxyl group, for example, a double-end hydroxypolysiloxane, a terminal hydroxyl polydimethylsiloxane, or the like.
  • the basic ion exchange resin is not limited in specific type, and may be a basic anion exchange resin or an alkaline cation exchange resin.
  • the LED packaging material provided by the embodiment promotes the combination of graphene and silane to form an LED packaging material by using a control agent and a basic ion exchange resin, so as to overcome the weak mechanical strength, high thermal expansion rate, etc. when forming the LED packaging material from a single silane. Disadvantages, as LED packaging materials, these unfavorable factors will cause more serious problems. Therefore, the LED package material of the present invention promotes the combination of graphene and silane to form an LED package material by a control agent and a basic ion exchange resin, so that thermal conductivity, environmental stability, mechanical properties, heat stability and the like are greatly improved.
  • FIG. 2 is a flow chart of a method for preparing an LED package material according to a second embodiment of the present invention, and the LED package material of the second embodiment described above can be prepared.
  • the method for preparing the LED package material includes at least the following steps.
  • Step 21 Mixing and heating a predetermined dose of silane, a controlling agent, a basic ion exchange resin, and graphene to form a sample of the encapsulating material.
  • the silane type may be a silicone monomer such as methyltrichlorosilane, dimethyldichlorosilane, phenyltrichlorosilane or diphenyldichlorosilane, or may be other groups.
  • the group-substituted silicone monomer, such as an alkoxysilane, etc., is not specifically limited herein.
  • the specific type of the controlling agent is not limited as long as it has a terminal hydroxyl group, for example, a double-end hydroxypolysiloxane, a terminal hydroxyl polydimethylsiloxane, or the like.
  • the basic ion exchange resin is not limited in specific type, and may be a basic anion exchange resin or an alkaline cation exchange resin.
  • the mass percentage of the basic ion exchange resin is 5%-10%
  • the mass percentage of the graphene is 0.5%-2%
  • the molar ratio of the silane to the control agent It is 1:0.3-1:1.
  • the heating temperature is 30-80 ° C, and the heating time is 5-20.
  • the package material sample is formed in an hour.
  • Step 22 removing impurities in the sample of the packaging material to obtain an LED packaging material.
  • the impurities in the sample of the encapsulating material include a basic ion exchange resin that remains insufficiently reacted. Therefore, the residual basic ion exchange resin can be removed by filtration.
  • the impurities in the sample of the encapsulating material further include a solvent having a lower boiling point contained in the sample of the encapsulating material, such as a solvent in a basic ion exchange resin. Therefore, the solvent having a lower boiling point can be removed by means of reduced pressure.
  • the specific principle is as follows: the solvent with a lower boiling point in the sample of the packaging material is easily volatilized into a gaseous state, and then the solvent which is volatilized into a gaseous state is removed by decompression, and the solvent having a lower boiling point in the sample of the packaging material can be removed.
  • the two impurities in the package sample may be sequentially removed by filtration and decompression.
  • the alkaline ion exchange resin and the control agent are used to promote the combination of graphene and silane to form an LED package material, which can overcome the weak mechanical strength and thermal expansion rate of the LED package material formed by the single silane. Higher problems have greatly improved the thermal conductivity, environmental stability, mechanical properties, and thermal stability of LED packaging materials.

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Abstract

本发明公开了一种LED封装材料，由石墨烯与硅烷或者环氧树脂复合形成，以借助石墨烯的特性来改善单一硅烷或者环氧树脂制备LED封装材料时存在的缺陷，以改善LED封装材料的性能。本发明还公开了一种LED封装材料的制备方法。本发明的LED封装材料及其制备方法，由石墨烯与硅烷或者环氧树脂复合形成，以借助石墨烯的特性来改善由单一硅烷或者环氧树脂制备LED封装材料时存在的缺陷，以改善LED封装材料的性能。

Description

LED封装材料及制备方法
本申请要求2017年05月12日递交的发明名称为“LED封装材料及制备方法”的申请号为201710334882.9的在先申请优先权，上述在先申请的内容以引入的方式并入本文本中。
技术领域
本发明涉及一种LED封装材料，尤其涉及一种具有石墨烯的LED封装材料及该种封装材料的制备方法。
背景技术
LED是由芯片、金属线、支架、导电胶、封装材料等组成，其中封装材料的主要作用是密封以防止芯片受到湿度、温度、氧化等影响而降低效率，从而保护芯片正常工作。另外，封装材料还具有以下功能：固定电子器件，避免电子器件因受到机械振动等冲击而造成器件参数的变化；降低LED芯片与空气之间的折射率，提高光发出效率；以及起到LED芯片散热作用。因此LED封装材料不仅要具有较好的密封性、较高的透过率，同时还有较优的粘结强度。目前的LED封装材料主要有环氧树脂、有机硅等材料。其中，环氧树脂因其具有优良的粘结性、电绝缘性、密封性和介电性能，且成本比较低、易成型等特性而成为LED封装的主流材料。而有机硅材料则具有良好的透明性、耐高低温性、耐候性、绝缘性及强的疏水性等，使其成为LED封装材料的理想选择。
然而，当采用上述两种材料制备LED封装材料时都存在技术缺陷：环氧树脂自身存在吸湿性、易老化、耐热性差、高温和短波光照下易变色、固化的内应力大等缺陷，这些不利因素将极大影响和缩短LED器件的使用寿命；而有机硅材料本身不具备较强的机械强度，且热膨胀率较高。显然，目前的LED封装材料，采用上述两种材料制备时，这些不利因素都会对LED封装材料的性能造成较严重的影响。
发明内容
本发明实施例提供一种新的LED封装材料，由石墨烯与硅烷或者环氧树脂复合形成，以借助石墨烯的特性来改善单一硅烷或者环氧树脂制备LED封装材料时存在的缺陷，以改善LED封装材料的性能。
第一方面，本发明提供了第一实施例的一种LED封装材料，所述LED封装材料由以下重量百分比的原料制成：固化剂10％-40％、石墨烯0.05％-1％、环氧树脂40％-60％和促进剂0.5％-2％。
其中，所述固化剂由以下材料中的一种或多种组成：甲基四氢苯酐、二乙烯基三胺、氨乙基哌嗪、1，2-二氨基环己烷、四乙烯五胺、二甲胺基丙胺、二己基三胺、亚甲基双苯二胺。
其中，所述石墨烯通过表面改性在其表面增加羟基和/或羧基。
其中，所述促进剂是促进各原料之间相互分散的促进剂，或者是促进各原料之间相互溶解的促进剂，用以促进所述石墨烯与环氧树脂之间的混合。
第二方面，本发明提供了第一实施例的一种LED封装材料的制备方法，包括以下步骤：
提供一预设剂量的固化剂与石墨烯，并将所述固化剂与石墨烯充分混合；
提供一预设剂量的环氧树脂及促进剂，并将其加入石墨烯与固化剂的混合溶液中；
将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合，形成由石墨烯与环氧树脂复合形成的LED封装材料。
其中，所述固化剂由以下材料中的一种或多种组成：甲基四氢苯酐、二乙烯基三胺、氨乙基哌嗪、1，2-二氨基环己烷、四乙烯五胺、二甲胺基丙胺、二己基三胺、亚甲基双苯二胺；所述石墨烯通过表面改性在其表面增加羟基和/或羧基；所述促进剂是促进各原料之间相互分散的促进剂，或者是促进各原料之间相互溶解的促进剂，用以促进所述石墨烯与环氧树脂之间的混合。
其中，所述固化剂、石墨烯、环氧树脂以及促进剂组成的所述混合溶液中，各组分的重量百分比如下：固化剂10％-40％、石墨烯0.05％-1％、环氧树脂40％-60％和促进剂0.5％-2％。
其中，所述将所述固化剂与石墨烯充分混合的操作方法如下：利用超声分散仪对相混合的固化剂与石墨烯进行超声处理，其中，超声功率为500W-900W，时长为3-5小时。
其中，所述将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之前，还包括以下步骤：可以先通过玻璃棒搅拌加入了石墨烯与固化剂的所述混合溶液，使所述混合溶液中各组分分布均匀。
其中，所述将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之后，还包括以下步骤：将通过超声的方式充分混合后的混合溶液加入真空烤箱中，并在60-80℃下烘烤1小时，以将所述混合溶液中的气泡排除。
第三方面，本发明提供了第二实施例的一种LED封装材料，所述LED封装材料由以下原料制成：硅烷、控制剂、碱性离子交换树脂以及石墨烯，其中，所述碱性离子交换树脂的质量百分比为5％-10％，所述石墨烯的质量百分比为0.5％-2％，所述硅烷与控制剂两者的摩尔比为1∶0.3-1∶1。
其中，所述控制剂具有端羟基；所述碱性离子交换树脂为碱性阴离子交换树脂或碱性阳离子交换树脂。
第四方面，本发明提供了第二实施例的一种LED封装材料的制备方法，包括以下步骤：
将预设剂量的硅烷、控制剂、碱性离子交换树脂以及石墨烯混合搅拌并加热以形成封装材料样品；
将所述封装材料样品中的杂质去除，得到LED封装材料。
其中，所述将预设剂量的硅烷、控制剂、碱性离子交换树脂以及石墨烯混合搅拌并加热的步骤中，加热温度为30-80℃，加热时长为5-20小时。
其中，所述封装材料样品中的杂质包括未充分反应而残留的碱性离子交换树脂，可通过过滤的方式去除所述残留的碱性离子交换树脂。
其中，所述封装材料样品中的杂质还包括低沸点溶剂，可通过减压的方式去除所述低沸点溶剂。
其中，所述离子交换树脂的质量百分比为5％-10％，所述石墨烯的质量百分比为0.5％-2％，所述硅烷与控制剂两者的摩尔比为1∶0.3-1∶1；所述控制剂具有端羟基；所述碱性离子交换树脂为碱性阴离子交换树脂或碱性阳离子交换 树脂。
本发明实施例中提供的LED封装材料由石墨烯与硅烷或者环氧树脂复合形成，以借助石墨烯的特性来改善由单一硅烷或者环氧树脂制备LED封装材料时存在的缺陷，以改善LED封装材料的性能。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术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，对于本领域普通技术人员来讲，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为本发明第一实施例提供的LED封装材料的制备方法流程图。
图2为本发明第二实施例提供的LED封装材料的制备方法流程图。
具体实施方式
下面将结合本发明实施方式中的附图，对本发明实施方式中的技术方案进行清楚、完整地描述。显然，所描述的实施方式是本发明的一部分实施方式，而不是全部实施方式。基在本发明中的实施方式，本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施方式，都应属在本发明保护的范围。
此外，以下各实施例的说明是参考附加的图示，用以例示本发明可用以实施的特定实施例。本发明中所提到的方向用语，例如，“上”、“下”、“前”、“后”、“左”、“右”、“内”、“外”、“侧面”等，仅是参考附加图式的方向，因此，使用的方向用语是为了更好、更清楚地说明及理解本发明，而不是指示或暗指所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。
在本发明的描述中，需要说明的是，除非另有明确的规定和限定，术语“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸地连接，或者一体地连接；可以是机械连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员 而言，可以具体情况理解上述术语在本发明中的具体含义。
此外，在本发明的描述中，除非另有说明，“多个”的含义是两个或两个以上。若本说明书中出现“工序”的用语，其不仅是指独立的工序，在与其它工序无法明确区别时，只要能实现所述工序所预期的作用则也包括在本用语中。另外，本说明书中用“～”表示的数值范围是指将“～”前后记载的数值分别作为最小值及最大值包括在内的范围。在附图中，结构相似或相同的单元用相同的标号表示。
本发明实施例提供了一种LED封装材料及其制备方法，其由石墨烯与硅烷或者环氧树脂复合形成，以借助石墨烯的特性来改善由单一硅烷或者环氧树脂制备LED封装材料时存在的缺陷，以改善LED封装材料的性能。以下分别进行详细说明。
本发明第一实施例的LED封装材料，该LED封装材料由以下重量百分比的原料制成：固化剂10％-40％、石墨烯0.05％-1％、环氧树脂40％-60％和促进剂0.5％-2％。
在本实施方式中，所述固化剂可以是以下材料中的一种或多种：甲基四氢苯酐、二乙烯基三胺、氨乙基哌嗪、1，2-二氨基环己烷、四乙烯五胺、二甲胺基丙胺、二己基三胺、亚甲基双苯二胺等。在此不对所述固化剂的类型作具体限定。
在本实施方式中，所述石墨烯可以进行表面改性，例如在其表面增加羟基和/或羧基等基团，以提升所述石墨烯的性能。
在本实施方式中，所述促进剂的类型可以是促进各原料之间相互分散的促进剂，或者是促进各原料之间相互溶解的促进剂，用以促进所述石墨烯与环氧树脂之间的混合。在本发明中不对所述促进剂的类型作具体限定，只要能促进所述石墨烯与环氧树脂之间充分混合即可。
本实施例提供的LED封装材料，通过固化剂与促进剂可促进石墨烯与环氧树脂复合形成LED封装材料，以克服由单一环氧树脂形成LED封装材料所存在的吸湿性、易老化、耐热性差、高温和短波光照下易变色、固化的内应力大等缺陷的问题，使得LED封装材料的导热性、环境稳定性、机械性能等大 大提高。
请参阅图1，图1为本发明第一实施例提供的LED封装材料的制备方法流程图，可制备出上述第一实施例的LED封装材料。在本实施例中，所述LED封装材料制备方法至少包括以下步骤。
步骤1、提供一预设剂量的固化剂与石墨烯，并将所述固化剂与石墨烯充分混合。
在本发明一实施方式中，所述石墨烯呈粉末状，便于与所述固化剂的充分混合。并且，所述石墨烯可以在与固化剂混合之前进行表面改性，在其表面增加羟基和/或羧基等基团，从而提升石墨烯的性能。
在本发明一实施方式中，所述固化剂可以是以下材料中的一种或多种：甲基四氢苯酐、二乙烯基三胺、氨乙基哌嗪、1，2-二氨基环己烷、四乙烯五胺、二甲胺基丙胺、二己基三胺、亚甲基双苯二胺等。在此不对所述固化剂的类型作具体限定。
在本发明一实施方式中，将所述固化剂与石墨烯充分混合的操作方法如下：利用超声分散仪对相混合的固化剂与石墨烯进行超声处理，其中，超声功率为500W-900W，时长为3-5小时。
步骤2、提供一定剂量的环氧树脂及促进剂，并将其加入石墨烯与固化剂的混合溶液中，此时，所述混合溶液包含固化剂、石墨烯、环氧树脂以及促进剂。
在本发明一实施方式中，所述环氧树脂与现有的LED封装材料中常用的环氧树脂材料相同，在此不再详细描述。
在本发明一实施方式中，所述促进剂的类型可以是促进各原料之间相互分散的促进剂，或者是促进各原料之间相互溶解的促进剂，用以促进所述石墨烯与环氧树脂之间的混合。在本发明中不对所述促进剂的类型作具体限定，只要能促进所述石墨烯与环氧树脂之间充分混合即可。
在本发明一实施方式中，所述固化剂、石墨烯、环氧树脂以及促进剂组成的混合溶液中，各组分的重量百分比如下：固化剂10％-40％、石墨烯0.05％-1％、环氧树脂40％-60％和促进剂0.5％-2％。
步骤3、将加入石墨烯与固化剂后的混合溶液通过超声的方式充分混合， 以形成由石墨烯与环氧树脂复合形成的LED封装材料。
在本发明一实施方式中，在将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之前，还包括以下步骤：通过玻璃棒搅拌加入了石墨烯与固化剂的所述混合溶液，使所述混合溶液中各组分分布均匀。通过玻璃棒将所述混合溶液中的各组分搅拌均匀后，再通过超声的方式使各组分之间充分混合。在本发明一实施方式中，通过玻璃棒搅拌的时长为20分钟，通过超声混合的时常为1小时。
在本发明一实施方式中，所述将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之后，还包括以下步骤：将通过超声的方式充分混合后的混合溶液加入真空烤箱中，并在60-80℃下烘烤1小时，以将所述混合溶液中的气泡排除。其中，所述加入石墨烯与固化剂后的混合液形成LED封装材料后，残留的低沸点溶剂挥发成气态而形成所述气泡，因此，可以通过真空的方式将挥发成气态的溶剂(即所述气泡)抽走，即可排除所述混合溶液中的气泡。
本实施例的LED封装材料的制备方法，借助超声的方式将所述固化剂、促进剂、石墨烯与环氧树脂充分混合，以通过固化剂与促进剂促进石墨烯与环氧树脂复合形成LED封装材料，可克服由单一环氧树脂形成LED封装材料时所存在的吸湿性、易老化、耐热性差、高温和短波光照下易变色、固化的内应力大等缺陷的问题，使得LED封装材料的导热性、环境稳定性、机械性能、受热稳定性等大大提高。
本发明第二实施例的LED封装材料，该LED封装材料由以下原料制成：硅烷、控制剂、碱性离子交换树脂以及石墨烯，其中，所述碱性离子交换树脂的质量百分比为5％-10％，所述石墨烯的质量百分比为0.5％-2％，所述硅烷与控制剂两者的摩尔比为1∶0.3-1∶1。
在本发明实施方式中，所述硅烷类型可为甲基三氯硅烷、二甲基二氯硅烷、苯基三氯硅烷、二苯基二氯硅烷等有机硅单体，也可为其他基团取代的有机硅单体，诸如烷氧基硅烷等。在本发明实施方式中，不对所述硅烷的类型做具体限定。
在本发明一实施方式中，所述控制剂的具体类型不限，只要具有端羟基即可，例如双端羟基聚硅氧烷、端羟基聚二甲基硅氧烷等。
在本发明一实施方式中，所述碱性离子交换树脂具体类型不限，可以为碱性阴离子交换树脂，也可以为碱性阳离子交换树脂。
本实施例提供的LED封装材料，通过控制剂与碱性离子交换树脂促进石墨烯与硅烷复合形成LED封装材料，以克服由单一硅烷形成LED封装材料时所存在的机械强度弱、热膨胀率较高等不利因素，作为LED封装材料，这些不利因素都会造成较严重的影响的问题。因此，本发明的LED封装材料通过控制剂与碱性离子交换树脂促进石墨烯与硅烷复合形成LED封装材料，使得其导热性、环境稳定性、机械性能、受热稳定性等大大提高。
请参阅图2，图2为本发明第二实施例提供的LED封装材料的制备方法流程图，可制备出上述第二实施例的LED封装材料。在本实施例中，所述LED封装材料制备方法至少包括以下步骤。
步骤21、将预设剂量的硅烷、控制剂、碱性离子交换树脂以及石墨烯混合搅拌并加热以形成封装材料样品。
在本发明一实施方式中，所述硅烷类型可为甲基三氯硅烷、二甲基二氯硅烷、苯基三氯硅烷、二苯基二氯硅烷等有机硅单体，也可为其他基团取代的有机硅单体，诸如烷氧基硅烷等，在此不对所述硅烷的类型做具体限定。
在本发明一实施方式中，所述控制剂的具体类型不限，只要具有端羟基即可，例如双端羟基聚硅氧烷、端羟基聚二甲基硅氧烷等。
在本发明一实施方式中，所述碱性离子交换树脂具体类型不限，可以为碱性阴离子交换树脂，也可以为碱性阳离子交换树脂。
在本发明一实施方式中，所述碱性离子交换树脂的质量百分比为5％-10％，所述石墨烯的质量百分比为0.5％-2％，所述硅烷与控制剂两者的摩尔比为1∶0.3-1∶1。
在本发明一实施方式中，所述将预设剂量的硅烷、控制剂、碱性离子交换树脂以及石墨烯混合搅拌并加热的步骤中，加热温度为30-80℃，加热时长为5-20小时，形成所述封装材料样品。
步骤22、将所述封装材料样品中的杂质去除，得到LED封装材料。
在本发明一实施方式中，所述封装材料样品中的杂质包括未充分反应而残留的碱性离子交换树脂。因此，可通过过滤的方式去除所述残留的碱性离子交换树脂。
在本发明一实施方式中，所述封装材料样品中的杂质还包括所述封装材料样品中所包含的沸点较低的溶剂，比如碱性离子交换树脂中的溶剂。因此，可以通过减压的方式去除沸点较低的所述溶剂。具体原理如下：封装材料样品中沸点较低的溶剂容易挥发成气态，然后通过减压的方式将挥发成气态的溶剂抽走，即可去除封装材料样品中沸点较低的溶剂。
可以理解，当所述封装料样品中的杂质同时包括未充分反应而残留的碱性离子交换树脂以及上述沸点较低的溶剂时，可以依次通过过滤与减压的方式依次去除上述两种杂质。
本实施例的LED封装材料的制备方法，通过碱性离子交换树脂与控制剂促进石墨烯与硅烷复合形成LED封装材料，可克服由单一硅烷形成LED封装材料时所存在的机械强度弱、热膨胀率较高等问题，使得LED封装材料的导热性、环境稳定性、机械性能、受热稳定性等大大提高。
在本说明书的描述中，参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含在本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上对本发明实施例所提供的LED封装材料及液晶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，对于本领域的一般技术人员，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LED封装材料，其中，所述LED封装材料由以下重量百分比的原料制成：固化剂10％-40％、石墨烯0.05％-1％、环氧树脂40％-60％和促进剂0.5％-2％。
  2. 如权利要求1所述的LED封装材料，其中，所述固化剂由以下材料中的一种或多种组成：甲基四氢苯酐、二乙烯基三胺、氨乙基哌嗪、1，2-二氨基环己烷、四乙烯五胺、二甲胺基丙胺、二已基三胺、亚甲基双苯二胺。
  3. 如权利要求1所述的LED封装材料，其中，所述石墨烯通过表面改性在其表面增加羟基和/或羧基。
  4. 如权利要求1所述的LED封装材料，其中，所述促进剂是促进各原料之间相互分散的促进剂，或者是促进各原料之间相互溶解的促进剂，用以促进所述石墨烯与环氧树脂之间的混合。
  5. 一种LED封装材料的制备方法，其中，包括以下步骤：
    提供一预设剂量的固化剂与石墨烯，并将所述固化剂与石墨烯充分混合；
    提供一预设剂量的环氧树脂及促进剂，并将其加入石墨烯与固化剂的混合溶液中；
    将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合，以形成由石墨烯与环氧树脂复合形成的LED封装材料。
  6. 如权利要求5所述的制备方法，其中，所述固化剂由以下材料中的一种或多种组成：甲基四氢苯酐、二乙烯基三胺、氨乙基哌嗪、1，2-二氨基环己烷、四乙烯五胺、二甲胺基丙胺、二已基三胺、亚甲基双苯二胺；所述石墨烯通过表面改性在其表面增加羟基和/或羧基；所述促进剂是促进各原料之间相互分散的促进剂，或者是促进各原料之间相互溶解的促进剂，用以促进所述石墨烯 与环氧树脂之间的混合。
  7. 如权利要求5所述的制备方法，其中，固化剂、石墨烯、环氧树脂以及促进剂组成的所述混合溶液中，各组分的重量百分比如下：固化剂10％-40％、石墨烯0.05％-1％、环氧树脂40％-60％和促进剂0.5％-2％。
  8. 如权利要求5所述的制备方法，其中，所述将所述固化剂与石墨烯充分混合的操作方法如下：利用超声分散仪对相混合的固化剂与石墨烯进行超声处理，其中，超声功率为500W-900W，时长为3-5小时。
  9. 如权利要求5所述的制备方法，其中，所述将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之前，还包括以下步骤：通过玻璃棒搅拌加入了石墨烯与固化剂的所述混合溶液，使所述混合溶液中各组分分布均匀。
  10. 如权利要求5所述的制备方法，其中，所述将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之后，还包括以下步骤：将通超声的方式充分混合后的混合溶液加入真空烤箱中，并在60-80℃下烘烤1小时，以将所述混合溶液中的气泡排除。
  11. 如权利要求7所述的制备方法，其中，所述将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之后，还包括以下步骤：将通超声的方式充分混合后的混合溶液加入真空烤箱中，并在60-80℃下烘烤1小时，以将所述混合溶液中的气泡排除。
  12. 如权利要求9所述的制备方法，其中，所述将加入石墨烯与固化剂的混合溶液通过超声的方式充分混合这一步骤之后，还包括以下步骤：将通超声的方式充分混合后的混合溶液加入真空烤箱中，并在60-80℃下烘烤1小时，以将所述混合溶液中的气泡排除。
  13. 一种LED封装材料，其中，所述LED封装材料由以下原料制成：硅烷、控制剂、碱性离子交换树脂以及石墨烯，其中，所述碱性离子交换树脂的质量百分比为5％-10％，所述石墨烯的质量百分比为0.5％-2％，所述硅烷与控制剂两者的摩尔比为1∶0.3-1∶1。
  14. 如权利要求13所述的LED封装材料，其中，所述控制剂具有端羟基；所述碱性离子交换树脂为碱性阴离子交换树脂或碱性阳离子交换树脂。
  15. 一种LED封装材料的制备方法，其中，包括以下步骤：
    将预设剂量的硅烷、控制剂、碱性离子交换树脂以及石墨烯混合搅拌并加热以形成封装材料样品；
    将所述封装材料样品中的杂质去除，得到LED封装材料。
  16. 如权利要求15所述的制备方法，其中，所述将预设剂量的硅烷、控制剂、碱性离子交换树脂以及石墨烯混合搅拌并加热的步骤中，加热温度为30-80℃，加热时长为5-20小时。
  17. 如权利要求15所述的制备方法，其中，所述封装材料样品中的杂质包括未充分反应而残留的碱性离子交换树脂，可通过过滤的方式去除所述残留的碱性离子交换树脂。
  18. 如权利要求15所述的制备方法，其中，所述封装材料样品中的杂质还包括低沸点溶剂，可通过减压的方式去除所述低沸点溶剂。
  19. 如权利要求15所述的制备方法，其中，所述离子交换树脂的质量百分比为5％-10％，所述石墨烯的质量百分比为0.5％-2％，所述硅烷与控制剂两者的摩尔比为1∶0.3-1∶1；所述控制剂具有端羟基；所述碱性离子交换树脂为碱性阴离子交换树脂或碱性阳离子交换树脂。
  20. 如权利要求16所述的制备方法，其中，所述离子交换树脂的质量百分比为5％-10％，所述石墨烯的质量百分比为0.5％-2％，所述硅烷与控制剂两者的摩尔比为1∶0.3-1∶1；所述控制剂具有端羟基；所述碱性离子交换树脂为碱性阴离子交换树脂或碱性阳离子交换树脂。
PCT/CN2017/087821 2017-05-12 2017-06-09 Led封装材料及制备方法 Ceased WO2018205336A1 (zh)

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