WO2018121048A1 - 大功率led照明灯用耐高温封装胶及其制备方法 - Google Patents

大功率led照明灯用耐高温封装胶及其制备方法 Download PDF

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WO2018121048A1
WO2018121048A1 PCT/CN2017/109033 CN2017109033W WO2018121048A1 WO 2018121048 A1 WO2018121048 A1 WO 2018121048A1 CN 2017109033 W CN2017109033 W CN 2017109033W WO 2018121048 A1 WO2018121048 A1 WO 2018121048A1
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epoxy resin
power led
parts
active
temperature resistant
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PCT/CN2017/109033
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English (en)
French (fr)
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王行柱
肖军
吴卫平
肖启振
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苏州兴创源新材料科技有限公司
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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
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
    • H01L33/52—Encapsulations
    • H01L33/56—Materials, e.g. epoxy or silicone resin
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Definitions

  • the invention relates to a high temperature resistant encapsulant for high power LED illumination lamp and a preparation method thereof.
  • the density of electronic assembly has been greatly increased, electronic components have been reduced by thousands of times, and the computing speed has become faster and faster.
  • the heat generated by electronic components rapidly accumulates and increases, resulting in a decrease in the performance of the material.
  • the heat conductive polymer material plays an increasingly important role in heat dissipation, high precision and long life of high frequency microelectronic components.
  • the materials of the packaging technology currently on the market have problems such as poor high temperature resistance and poor compatibility in the preparation process.
  • the object of the present invention is to provide a high-temperature resistant package for a high-power LED illumination lamp and a preparation method thereof, which are prepared by using an epoxy resin F-44 and E-51, and simultaneously using a material such as a silane coupling agent to the surface of the silicon micropowder particles.
  • the modification and activation treatment is carried out, and the obtained encapsulant has moderate viscosity, long operation time, excellent mechanical processing performance, and no cracking after high and low temperature cyclic impact.
  • the technical solution of the present invention provides a high-temperature resistant package for high-power LED illumination lamps and a preparation method thereof, which are prepared by the following steps:
  • the encapsulant was obtained by curing at 100 ° C for 30 min.
  • the active toughening agent is epoxy resin D-410.
  • the curing agent is diethylenetriamine.
  • the promoter is an acid anhydride promoter.
  • the active filler is a silane coupling agent.
  • the invention has the advantages and beneficial effects that the epoxy resin D-410 active toughening agent is added, and the proportion of the ether network is greatly increased in the crosslinked network structure of the cured product, thereby greatly improving the mechanical properties and electrical insulation of the cured product.
  • the silane coupling agent is used as the active filler to effectively improve the adhesion between the resin and the quartz powder silicon powder and the interfacial hydrophobicity.
  • the package adhesive has moderate viscosity, long operation time, excellent machinability, and no cracking after high temperature and low temperature cycle impact.
  • epoxy resin E-51, 20-40 parts of epoxy resin F-44 are compounded in proportion; 10-20 parts of active toughening agent, 150-300 parts of active filler are added and stirred uniformly; and ground by a three-roll mill; After vacuum degassing, 20-25 parts of curing agent and 1-2 accelerator were added and uniformly mixed, and the bubbles were vacuum-purged and then poured into the reactor; and the encapsulant was obtained by curing at 100 ° C for 30 min.
  • epoxy resin E-51, 20-40 parts of epoxy resin F-44 are compounded in proportion; 18 parts of active toughening agent, 190 parts of active filler are added and stirred uniformly; after three-roll mill grinding; vacuum degassing bubble Thereafter, 35 parts of curing agent and 1 accelerator were added and uniformly mixed, and the bubbles were vacuum-purged and then poured into the reactor; and the packaged rubber was obtained by curing at 140 ° C for 40 minutes.

Abstract

一种大功率LED照明灯用耐高温封装胶及其制备方法，以环氧树脂为基体材料，添加活性增韧稀释剂、活性填料在一定的工艺条件下制成，包括环氧树脂、固化剂和促进剂。所述环氧树脂选择双酚A型环氧树脂E-51作为主体树脂，同时为了提高产品的耐高低温性能，同时采用环氧树脂F-44与E-51复配，由于F-44分子结构中含有2个以上环氧基团，活性大，其固化物的交联密度大，结构紧密，且耐热性、机械强度、耐化学品性能优良。同时采用硅烷偶联剂等材料对硅微粉颗粒表面进行改性活化处理，制得的封装胶粘度适中，可操作时间长，机械加工性能优良，经高低温循环冲击后不开裂。

Description

[根据细则37.2由ISA制定的发明名称]　大功率LED照明灯用耐高温封装胶及其制备方法 技术领域
本发明涉及一种大功率LED照明灯用耐高温封装胶及其制备方法。
背景技术
随着电子集成技术和印刷电路板技术的发展,电子组装的密度大幅提高,电子元器件在成千上万倍地缩小,同时运算速度也越来越快。在高频工作下,电子元器件产生的热量迅速积累、增加,造成材料的性能下降。导热高分子材料对于高频微电子元器件的散热,精度提高、延长寿命具有愈来愈重要的作用。但是目前市场上的封装技术的材料存在耐高温性能差，在制备过程中相容性差等问题。
发明内容
本发明的目的在于提供一种大功率LED照明灯用耐高温封装胶及其制备方法，采用环氧树脂F-44与E-51复配，同时采用硅烷偶联剂等材料对硅微粉颗粒表面进行改性活化处理，制得的封装胶粘度适中，可操作时间长，机械加工性能优良，经高低温循环冲击后不开裂。
为实现上述目的，本发明的技术方案是提供一种大功率LED照明灯用耐高温封装胶及其制备方法，通过如下步骤制备：
(1)、将100份环氧树脂E-51、20-40份环氧树脂F-44按比例复合；
(2)、加入10-20份活性增韧剂、150-300份活性填料搅拌均匀；
(3)、经过三辊研磨机研磨；
(4)、真空脱净气泡后加入20-25份固化剂和1-2促进剂混合均匀并真空脱净气泡后浇注到反应器内；
(5)、按100℃的固化条件进行固化30min后制得所述封装胶。
优选的，所述的活性增韧剂为环氧树脂D-410。
优选的，所述的固化剂为二乙烯三胺。
优选的，所述的促进剂为酸酐促进剂。
优选的，所述的活性填料为硅烷偶联剂。
本发明的优点和有益效果在于：加入环氧树脂D-410活性增韧剂，使固化物交联网络结构中，醚网络比例大大增加，大大提高了固化产物的机械力学性能和电气绝缘性，采用硅烷偶联剂作为活性填料，有效的提高树脂与石英粉硅微粉的粘结力和界面憎水性能，制得 的封装胶粘度适中，可操作时间长，机械加工性能优良，经高低温循环冲击后不开裂。
具体实施方式
下面结合实施例，对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
本发明具体实施的技术方案是：
实施例1：
将100份环氧树脂E-51、20-40份环氧树脂F-44按比例复合；加入10-20份活性增韧剂、150-300份活性填料搅拌均匀；经过三辊研磨机研磨；真空脱净气泡后加入20-25份固化剂和1-2促进剂混合均匀并真空脱净气泡后浇注到反应器内；按100℃的固化条件进行固化30min后制得所述封装胶。
实施例2：
将130份环氧树脂E-51、20-40份环氧树脂F-44按比例复合；加入16份活性增韧剂、180份活性填料搅拌均匀；经过三辊研磨机研磨；真空脱净气泡后加入30份固化剂和2促进剂混合均匀并真空脱净气泡后浇注到反应器内；按130℃的固化条件进行固化35min后制得所述封装胶。
实施例3：
将165份环氧树脂E-51、20-40份环氧树脂F-44按比例复合；加入18份活性增韧剂、190份活性填料搅拌均匀；经过三辊研磨机研磨；真空脱净气泡后加入35份固化剂和1促进剂混合均匀并真空脱净气泡后浇注到反应器内；按140℃的固化条件进行固化40min后制得所述封装胶。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (6)

  1. 一种大功率LED照明灯用耐高温封装胶及其制备方法，其特征在于，包括环氧树脂E-51、环氧树脂F-44、活性增韧剂、活性填料、固化剂和促进剂按照100:20-40:10-20:150-300:20-25:1-2的比例混合制得。
  2. 根据权利要求1所述的大功率LED照明灯用耐高温封装胶及其制备方法，其特征在于，通过如下步骤制备：
    (1)、将100份环氧树脂E-51、20-40份环氧树脂F-44按比例复合；
    (2)、加入10-20份活性增韧剂、150-300份活性填料搅拌均匀；
    (3)、经过三辊研磨机研磨；
    (4)、真空脱净气泡后加入20-25份固化剂和1-2促进剂混合均匀并真空脱净气泡后浇注到反应器内；
    (5)、按100℃的固化条件进行固化30min后制得所述封装胶。
  3. 根据权利要求2所述的大功率LED照明灯用耐高温封装胶及其制备方法，其特征在于，所述的活性增韧剂为环氧树脂D-410。
  4. 根据权利要求2所述的大功率LED照明灯用耐高温封装胶及其制备方法，其特征在于，所述的固化剂为二乙烯三胺。
  5. 根据权利要求2所述的大功率LED照明灯用耐高温封装胶及其制备方法，其特征在于，所述的促进剂为酸酐促进剂。
  6. 根据权利要求2所述的大功率LED照明灯用耐高温封装胶及其制备方法，其特征在于，所述的活性填料为硅烷偶联剂。
PCT/CN2017/109033 2016-12-27 2017-11-02 大功率led照明灯用耐高温封装胶及其制备方法 WO2018121048A1 (zh)

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CN112373149A (zh) * 2020-11-12 2021-02-19 西安航天三沃化学有限公司 一种可挠曲铝基板的制备方法
CN114196358A (zh) * 2021-12-24 2022-03-18 山东工业陶瓷研究设计院有限公司 一种环氧树脂粘结剂及其制备方法和应用
CN114196360A (zh) * 2021-12-28 2022-03-18 句容协鑫光伏科技有限公司 一种提高粘接效率的快干铁板胶及其制备方法
CN114773963A (zh) * 2022-04-01 2022-07-22 广州市雷曼兄弟电子科技有限公司 一种适用于手机膜的防静电两液混合硬化胶及其制备工艺
CN115160967A (zh) * 2022-07-29 2022-10-11 六和电子（江西）有限公司 一种环氧树脂灌封胶的制备方法及制备装置
CN115260958A (zh) * 2022-08-29 2022-11-01 厦门理工学院 一种Micro-LED用封装胶的制备工艺

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CN112373149A (zh) * 2020-11-12 2021-02-19 西安航天三沃化学有限公司 一种可挠曲铝基板的制备方法
CN114196358A (zh) * 2021-12-24 2022-03-18 山东工业陶瓷研究设计院有限公司 一种环氧树脂粘结剂及其制备方法和应用
CN114196360A (zh) * 2021-12-28 2022-03-18 句容协鑫光伏科技有限公司 一种提高粘接效率的快干铁板胶及其制备方法
CN114773963A (zh) * 2022-04-01 2022-07-22 广州市雷曼兄弟电子科技有限公司 一种适用于手机膜的防静电两液混合硬化胶及其制备工艺
CN115160967A (zh) * 2022-07-29 2022-10-11 六和电子（江西）有限公司 一种环氧树脂灌封胶的制备方法及制备装置
CN115260958A (zh) * 2022-08-29 2022-11-01 厦门理工学院 一种Micro-LED用封装胶的制备工艺

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