CN111592849A - 一种半固化环氧胶膜及其制备方法 - Google Patents

一种半固化环氧胶膜及其制备方法 Download PDF

Info

Publication number
CN111592849A
CN111592849A CN202010632433.4A CN202010632433A CN111592849A CN 111592849 A CN111592849 A CN 111592849A CN 202010632433 A CN202010632433 A CN 202010632433A CN 111592849 A CN111592849 A CN 111592849A
Authority
CN
China
Prior art keywords
adhesive film
epoxy resin
parts
semi
curing agent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010632433.4A
Other languages
English (en)
Other versions
CN111592849B (zh
Inventor
侯志成
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qingdao Deju Bonding Technology Co ltd
Original Assignee
Qingdao Deju Bonding Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Qingdao Deju Bonding Technology Co ltd filed Critical Qingdao Deju Bonding Technology Co ltd
Priority to CN202010632433.4A priority Critical patent/CN111592849B/zh
Publication of CN111592849A publication Critical patent/CN111592849A/zh
Application granted granted Critical
Publication of CN111592849B publication Critical patent/CN111592849B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
    • C08G59/4014—Nitrogen containing compounds
    • C08G59/4021—Ureas; Thioureas; Guanidines; Dicyandiamides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
    • C08G59/4014—Nitrogen containing compounds
    • C08G59/4035—Hydrazines; Hydrazides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/44—Amides
    • C08G59/46—Amides together with other curing agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5006—Amines aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5026—Amines cycloaliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5046—Amines heterocyclic
    • C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
    • C08G59/5073—Amines heterocyclic containing only nitrogen as a heteroatom having two nitrogen atoms in the ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/56—Amines together with other curing agents
    • 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
    • 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
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • 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
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • 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
    • 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
    • C09J2400/00—Presence of inorganic and organic materials
    • 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
    • C09J2463/00—Presence of epoxy resin

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

本发明公开了一种半固化环氧胶膜及其制备方法。该环氧胶膜为单组份环氧树脂复合物，由环氧树脂、活性稀释剂、固化剂、颜填料、助剂等组成，在液体混合物状态时经压制或刮涂等方式形成薄膜状。该环氧胶膜经过一定程度的预固化后，具有一定的粘性和弹性，可自然贴附于电子、微电子行业的小型器件的两个部分中间，再经完全固化后起到粘接的作用，解决了目前市场上的胶膜需要热压贴附的问题。另该环氧胶膜固化物性能优异，玻璃化转变温度可达100℃以上，线膨胀系数低于50ppm/℃，剪切粘接强度（Al‑Al）可达20MPa以上。

Description

一种半固化环氧胶膜及其制备方法
技术领域
本发明涉及一种半固化环氧胶膜及其制备方法，属于高分子技术领域。
背景技术
环氧胶黏剂作为一种综合性能优越的工业产品，目前在诸多领域都有着广泛的应用，其中环氧胶膜作为其中一种比较特殊的形式近年来也受到越来越多的重视。环氧胶膜主要应用于电子、微电子行业的中小型电子元器件的真空封装、导电、粘接固定等。
常用的环氧胶膜采用固体或固体和液体树脂混合的形式作为主材料，添加有一定的潜伏性固化剂、填料、助剂等，常温状态下为不粘手的无弹性薄膜状，应用时采用加温加压的方式，使其具有一定的粘性、流动性，在充分润湿基材的情况下，再进行固化。
目前，市场上出现一种对于环氧胶膜新的需求，即环氧胶膜作为器件两个部分的中间粘接固定部分应用时，需要在常温下具有一定的粘性和弹性，具有保持形状能力、稳定性好的特点，应用时直接贴附于器件的一个组件之上，另一个组件自然压在其上并进行后固化即可，且固化后性能要求高，需要有较高的粘接强度和较低的线膨胀系数，以适应器件的耐久性测试。这种要求与市场上现有的环氧胶膜的特性有一定的偏差，开发难度大，应用前景广阔。
发明内容
针对现有技术的不足，本发明要解决的技术问题是提供一种半固化环氧胶膜及其制备方法，该材料具有常温下具有一定粘弹性、固化后性能优越等特点，可用于电子、微电子行业的小型器件的粘接固定。
本发明提出了一种半固化环氧胶膜，环氧胶膜为单组份环氧树脂复合物，由环氧树脂、活性稀释剂、固化剂、颜填料、助剂等组成，以上材料按重量比混合均匀后，经压制或刮涂制成薄层片材，于50-100℃条件下预固化得到可应用于电子、微电子行业器件的粘接。
优选地，所述的环氧树脂为双酚A型环氧树脂、双酚F型环氧树脂、脂环族环氧树脂、溴化环氧树脂、含萘环氧树脂、双环戊二烯型环氧树脂、柔韧性嵌段环氧树脂、酚醛环氧树脂、二聚酸改性环氧树脂中的一种或几种。
优选地，所述的活性稀释剂为正丁基缩水甘油醚、C12～C14烷基缩水甘油醚、苯基缩水甘油醚、聚丙二醇二缩水甘油醚中的一种或几种。
优选地，所述的固化剂包含潜伏性固化剂和常温固化剂，其中潜伏性固化剂为双氰胺、咪唑类、胺类、脲类、酰肼类、酚醛树脂类中的一种或几种，常温固化剂为聚醚胺、聚酰胺、脂肪胺、脂环胺中一种或几种。
优选地，所述的颜料是色膏，色膏为炭黑复合物；填料为硅微粉、氢氧化铝粉、核/壳橡胶粒子、碳酸钙中的一种或几种。
优选地，所述的助剂包含有消泡剂、偶联剂、分散剂等。消泡剂
为毕克化学的BYK-A530，BYK-A555，BYK-066N，BYK-141，BYK-1770中的一种或几种。偶联剂为带环氧基的硅烷偶联剂、γ-缩水甘油醚氧丙基三甲氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷的一种或几种。分散剂为毕克化学的BYK-W9010、BYK-W9011中的一种或几种。
优选地，所述的活性稀释剂用量为对应每100份环氧树脂使用2-6份。
优选地，所述的潜伏性固化剂用量为对应每100份环氧树脂使用3-20份；所述的常温固化剂的用量为对应每100份环氧树脂使用10-30份。
优选地，所述的颜料用量为对应每100份环氧树脂使用1-3份，填料用量为对应每100份环氧树脂使用100-200份。
优选地，所述的助剂用量为对应每100份环氧树脂使用0.2-1份。
与现有的技术相比，本发明的有益效果在于：
通过使用常规树脂、功能树脂复合并调整不同类型的树脂的比例，选用不同固化温度的固化剂并调整其比例，来控制半固化胶膜的固化程度和完全固化后的各项性能，最终得到了半固化阶段粘弹性合适且储存稳定性好、完全固化阶段性能优良的产品，可以同时满足在器件上应用的合适工艺性和最终作为粘接固定材料的优秀的物理性能和耐老化性能。
该环氧胶膜的粘手度好，第一法向应力差(80℃)在0.5MPa以上，完全固化后的产物玻璃化转变温度可达100℃以上，线膨胀系数低于50ppm/℃，剪切粘接强度(Al-Al)可达20MPa以上。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案。
如无具体说明，本发明的各种原料均可市售购得，或根据本领域的常规方法制备得到。
本实施例提供的一种半固化环氧胶膜的制备方法，包括如下步骤：
按重量份计，取混合树脂、活性稀释剂、颜料、助剂加入到反应釜中并高速搅拌混合均匀；
按重量份计，在之前步骤得到的混合料中缓慢加入填料，抽真空的情况下高速搅拌混合均匀；
按重量份计，在之前步骤得到的混合料中缓慢加入潜伏性固化剂，控制温度≤40℃以及抽真空的条件下高速搅拌混合均匀；
按重量份计，在之前步骤得到的混合料中加入常温固化剂，控制温度≤40℃以及抽真空的条件下高速搅拌混合均匀，得到所需的环氧胶膜用液体料；
将以上液体料通过涂布机辊涂，后经80℃/60min的预固化得到环氧胶膜。
以下实施例的半固化环氧胶膜均采用上述的制备方法得到。
实施例1
本实施例的一种半固化环氧胶膜，按重量份计，包括如下原料：
Figure BDA0002566209740000031
实施例2
本实施例的一种半固化环氧胶膜，按重量份计，包括如下原料：
Figure BDA0002566209740000032
Figure BDA0002566209740000041
实施例3
本实施例的一种半固化环氧胶膜，按重量份计，包括如下原料：
Figure BDA0002566209740000042
实施例4
本实施例的一种半固化环氧胶膜，按重量份计，包括如下原料：
Figure BDA0002566209740000043
对比例1
本对比例的一种半固化环氧胶膜，按重量份计，包括如下原料：
Figure BDA0002566209740000051
对比例2
本对比例的一种半固化环氧胶膜，按重量份计，包括如下原料：
Figure BDA0002566209740000052
对比例3
本对比例的一种半固化环氧胶膜，按重量份计，包括如下原料：
Figure BDA0002566209740000053
Figure BDA0002566209740000061
将实施例1-4和对比例1-3所制得的半固化环氧胶膜及其完全固化后的最终产物进行对比测试，实验结果如下：
Figure BDA0002566209740000062
由以上测试结果可以得知，两种不同固化温度的固化剂分别对半固化胶膜和完全固化后的性能有重要影响，在配合相应树脂的情况下，常温固化剂的用量在合理范围内可以提供良好的粘弹性，第一法向应力差可达到0.5MPa以上，低于范围则不具备较好的应用效果。潜伏性固化剂的用量可以对完全固化后的性能有很大改变，两种固化剂搭配得当，Tg可达到100℃以上，剪切粘接强度(Al-Al)高于20MPa。
填料的用量可以决定整个体系完全固化后的CTE(线膨胀系数)，其用量越多，则CTE越低，本发明的最终固化物CTE可低于50ppm/℃，但鉴于填料用量的增加对于混合难度也显著增大，因此需要控制在一定合理的范围内。
以上借助具体实施例对本发明做了进一步描述，但是应该理解的是，这里具体的描述，不应理解为对本发明的实质和范围的限定，本领域内的普通技术人员在阅读本说明书后对上述实施例做出的各种修改，都属于本发明所保护的范围。

Claims (8)

1.一种半固化环氧胶膜，其特征在于，由环氧树脂、活性稀释剂、潜伏性固化剂、常温固化剂、颜料、填料、助剂组成；
各组分之间的重量比为：以每100份环氧树脂计，活性稀释剂用量为2-6份；潜伏性固化剂用量为3-20份；常温固化剂的用量为10-30份；颜料用量为1-3份，填料用量为100-200份；助剂用量为0.2-1份。
2.如权利要求1所述的一种半固化环氧胶膜，其特征在于，所述的环氧树脂为双酚A型环氧树脂、双酚F型环氧树脂、脂环族环氧树脂、溴化环氧树脂、含萘环氧树脂、双环戊二烯型环氧树脂、柔韧性嵌段环氧树脂、酚醛环氧树脂、二聚酸改性环氧树脂中的一种或几种。
3.如权利要求1所述的一种半固化环氧胶膜，其特征在于，所述的活性稀释剂为正丁基缩水甘油醚、C12~C14烷基缩水甘油醚、苯基缩水甘油醚、聚丙二醇二缩水甘油醚中的一种或几种。
4.如权利要求1所述的一种半固化环氧胶膜，其特征在于，所述的固化剂包含潜伏性固化剂和常温固化剂，其中潜伏性固化剂为双氰胺、咪唑类、胺类、脲类、酰肼类、酚醛树脂类中的一种或几种，常温固化剂为聚醚胺、聚酰胺、脂肪胺、脂环胺中一种或几种。
5.如权利要求1所述的一种半固化环氧胶膜，其特征在于，所述的颜料是色膏，色膏为炭黑复合物。
6.如权利要求1所述的一种半固化环氧胶膜，其特征在于，所述的填料为硅微粉、氢氧化铝粉、核/壳橡胶粒子、碳酸钙中的一种或几种。
7.如权利要求1所述的一种半固化环氧胶膜，其特征在于，所述的助剂含有消泡剂、偶联剂、分散剂；消泡剂为毕克化学的BYK-A530，BYK-A555，BYK-066N，BYK-141，BYK-1770中的一种或几种；偶联剂为带环氧基的硅烷偶联剂、γ-缩水甘油醚氧丙基三甲氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷的一种或几种；分散剂为毕克化学的BYK-W9010、BYK-W9011中的一种或几种。
8.制备上述任一项权利要求所述的半固化环氧胶膜的方法，其特征在于，包括下列步骤：
（1）按重量份计，取100份的混合树脂、2-6份的活性稀释剂、1-3份的颜料、0.2-1份的助剂加入到反应釜中并高速搅拌混合均匀；
（2）在之前步骤得到的混合料中缓慢加入100-200份的填料，抽真空的情况下高速搅拌混合均匀；
（3）在之前步骤得到的混合料中缓慢加入3-20份的潜伏性固化剂，控制温度≤40℃以及抽真空的条件下高速搅拌混合均匀；
（4）在之前步骤得到的混合料中加入10-30份的常温固化剂，控制温度≤40℃以及抽真空的条件下高速搅拌混合均匀，得到环氧胶膜用液体料；
（5）将以上液体料通过涂布机辊涂，后经80℃/60min的预固化得到环氧胶膜。
CN202010632433.4A 2020-07-02 2020-07-02 一种半固化环氧胶膜及其制备方法 Active CN111592849B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010632433.4A CN111592849B (zh) 2020-07-02 2020-07-02 一种半固化环氧胶膜及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010632433.4A CN111592849B (zh) 2020-07-02 2020-07-02 一种半固化环氧胶膜及其制备方法

Publications (2)

Publication Number Publication Date
CN111592849A true CN111592849A (zh) 2020-08-28
CN111592849B CN111592849B (zh) 2022-04-08

Family

ID=72191835

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010632433.4A Active CN111592849B (zh) 2020-07-02 2020-07-02 一种半固化环氧胶膜及其制备方法

Country Status (1)

Country Link
CN (1) CN111592849B (zh)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112048271A (zh) * 2020-09-14 2020-12-08 深圳市安伯斯科技有限公司 一种单组份底部填充胶及其制备方法
CN112592503A (zh) * 2020-12-15 2021-04-02 佛山佛塑科技集团股份有限公司 一种风电叶片前缘防护材料及其制备方法和应用
CN113873767A (zh) * 2021-10-20 2021-12-31 南雄市科鼎化工有限公司 一种hdi电路板用棕化后塞孔树脂的制备方法及应用方法
CN115895549A (zh) * 2023-01-06 2023-04-04 拓迪化学(上海)有限公司 Uv延迟固化胶粘剂及其制备方法和应用
CN115960548A (zh) * 2023-01-18 2023-04-14 江苏科麦特科技发展有限公司 一种芯片包封用环氧树脂胶膜及其制备方法
CN116987476A (zh) * 2023-08-09 2023-11-03 惠州市帕克威乐新材料有限公司 一种冷压快速固化粘结膜及其制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001003015A (ja) * 1999-06-18 2001-01-09 Hitachi Chem Co Ltd 熱硬化性接着フィルム
JP2011046782A (ja) * 2009-08-25 2011-03-10 Panasonic Electric Works Co Ltd プリント配線板用エポキシ樹脂組成物、樹脂フィルム、プリプレグ、樹脂付き金属箔、フレキシブルプリント配線板
CN102977557A (zh) * 2012-12-11 2013-03-20 蓝星(北京)化工机械有限公司 一种室温固化环氧树脂组合物及其制备方法
CN103333623A (zh) * 2013-06-27 2013-10-02 烟台德邦科技有限公司 一种热压合胶膜及其制备方法
CN105670542A (zh) * 2016-01-22 2016-06-15 上海拜高高分子材料有限公司 一种低线膨胀系数的中低温固化的单组份环氧胶粘剂及制备方法
CN109321186A (zh) * 2018-10-15 2019-02-12 航天材料及工艺研究所 一种半固化环氧胶膜及其制备方法和使用
CN109535715A (zh) * 2018-11-28 2019-03-29 苏州生益科技有限公司 一种阻燃型树脂组合物及使用其制备的半固化片和层压板

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001003015A (ja) * 1999-06-18 2001-01-09 Hitachi Chem Co Ltd 熱硬化性接着フィルム
JP2011046782A (ja) * 2009-08-25 2011-03-10 Panasonic Electric Works Co Ltd プリント配線板用エポキシ樹脂組成物、樹脂フィルム、プリプレグ、樹脂付き金属箔、フレキシブルプリント配線板
CN102977557A (zh) * 2012-12-11 2013-03-20 蓝星(北京)化工机械有限公司 一种室温固化环氧树脂组合物及其制备方法
CN103333623A (zh) * 2013-06-27 2013-10-02 烟台德邦科技有限公司 一种热压合胶膜及其制备方法
CN105670542A (zh) * 2016-01-22 2016-06-15 上海拜高高分子材料有限公司 一种低线膨胀系数的中低温固化的单组份环氧胶粘剂及制备方法
CN109321186A (zh) * 2018-10-15 2019-02-12 航天材料及工艺研究所 一种半固化环氧胶膜及其制备方法和使用
CN109535715A (zh) * 2018-11-28 2019-03-29 苏州生益科技有限公司 一种阻燃型树脂组合物及使用其制备的半固化片和层压板

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
YOUNG GYU JEONG等: "Effects of mixed carbon filler composition on electric heating behavior of", 《COMPOSITES: PART A》 *
张在新: "环氧树脂胶粘剂近展", 《中国胶粘剂》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112048271A (zh) * 2020-09-14 2020-12-08 深圳市安伯斯科技有限公司 一种单组份底部填充胶及其制备方法
CN112592503A (zh) * 2020-12-15 2021-04-02 佛山佛塑科技集团股份有限公司 一种风电叶片前缘防护材料及其制备方法和应用
CN113873767A (zh) * 2021-10-20 2021-12-31 南雄市科鼎化工有限公司 一种hdi电路板用棕化后塞孔树脂的制备方法及应用方法
CN113873767B (zh) * 2021-10-20 2022-07-12 南雄市科鼎化工有限公司 一种hdi电路板用棕化后塞孔树脂的制备方法及应用方法
CN115895549A (zh) * 2023-01-06 2023-04-04 拓迪化学(上海)有限公司 Uv延迟固化胶粘剂及其制备方法和应用
CN115960548A (zh) * 2023-01-18 2023-04-14 江苏科麦特科技发展有限公司 一种芯片包封用环氧树脂胶膜及其制备方法
CN116987476A (zh) * 2023-08-09 2023-11-03 惠州市帕克威乐新材料有限公司 一种冷压快速固化粘结膜及其制备方法

Also Published As

Publication number Publication date
CN111592849B (zh) 2022-04-08

Similar Documents

Publication Publication Date Title
CN111592849B (zh) 一种半固化环氧胶膜及其制备方法
CN103797043B (zh) 结构粘着剂及其粘合应用
US9074041B2 (en) Curable epoxy resin compositions and composites made therefrom
KR100804293B1 (ko) 에폭시 수지용 경화제 및 에폭시 수지 조성물
CN107779147B (zh) 一种高强度环氧蜂窝胶及其制备方法
TW201531515A (zh) 柔軟性環氧樹脂組成物
KR20140009296A (ko) 에폭시 수지 조성물 및 그것을 사용한 반도체 봉지재
WO2013025304A2 (en) Curable resin compositions
CN103694637B (zh) 一种风电叶片用高韧性真空慢速环氧树脂及其制备方法
CN112341970B (zh) 一种环氧结构胶及其制备方法
CN114854347A (zh) 一种绝缘导热的胶粘剂及其制备方法和导热胶粘材料
KR20210152521A (ko) 경화성 2성분 수지계 시스템
WO2006005559A1 (en) Stable curable epoxy resin compositions and uses thereof
CN102504742B (zh) 一种室温快速固化粘接胶
CN112823177B (zh) 树脂组合物
CN101851395A (zh) 环氧树脂及其生产方法
CN115427529A (zh) 两部分导热性环氧粘合剂组合物
CN111675989A (zh) 一种低应力环氧灌封胶及其制备方法、使用方法
CN109438713A (zh) 适合非热压罐成型工艺的自粘性预浸料的制备方法及应用
WO2019065470A1 (ja) 硬化性エポキシ樹脂組成物、及びそれを用いた繊維強化複合材料
CN115322719B (zh) 可初步固定的环氧胶粘剂及其制备与使用方法
JP3354707B2 (ja) エポキシ樹脂組成物
CN117736499A (zh) 一种环氧树脂增韧剂及其制备方法
WO2023174891A1 (en) Epoxy resin adhesive
WO2024035866A1 (en) Epoxy-based composition for thermal interface materials

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant