CN101580684A - Low-temperature fast curing underfill adhesive and preparation method thereof - Google Patents

Low-temperature fast curing underfill adhesive and preparation method thereof Download PDF

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Publication number
CN101580684A
CN101580684A CNA2009100163239A CN200910016323A CN101580684A CN 101580684 A CN101580684 A CN 101580684A CN A2009100163239 A CNA2009100163239 A CN A2009100163239A CN 200910016323 A CN200910016323 A CN 200910016323A CN 101580684 A CN101580684 A CN 101580684A
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resin
low
mixing
solidifying agent
temperature
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CNA2009100163239A
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CN101580684B (en
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周建忠
王建斌
解海华
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Yantai Darbond Technology Co Ltd
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Yantai Darbond Technology Co Ltd
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Abstract

The invention discloses a low-temperature fast curing underfill adhesive, which is characterized by comprising the following raw materials by weight portion: 40 to 65 portions of resin, 0.5 portion of colorant, 20 to 25 portions of curing agent, 1 to 6 portions of accelerant, 0.1 to 3 portions of coupler and 15 to 25 portions of epoxy active diluents. The preparation method comprises the following steps: firstly, uniformly mixing the resin and color paste for 20 to 40 minutes at 20 to 30 DEG C; secondly, adding the curing agent and the accelerant by three times, uniformly mixing the materials with a three-roller at 20 to 30 DEG C under a condition of chilling drying with cooling water kept at 15 DEG C for 3 times, adding the uniformly mixed materials into a reaction kettle and completely vacuumizing the reaction kettle for 15 minutes; and finally, after the resin and the curing agent are mixed uniformly, adding the coupler and the epoxy active diluents, mixing the materials in the reaction kettle, and completely vacuumizing for 30 minutes to obtain the product. The product is low in curing temperature, high in curing speed and good in storage stability, simple, easy and environmentally-friendly in preparation process, low in cost and wide in application range.

Description

A kind of low-temperature fast curing underfill adhesive and preparation method thereof
Technical field:
The present invention relates to filling technique field, bottom, is a kind of low-temperature fast curing underfill adhesive and preparation method thereof specifically.
Background technology:
Bottom filling technique the seventies in last century is risen in IBM Corporation, has become the important integral part of electronics manufacturing industry at present.Originally this The Application of Technology scope is only limited to ceramic substrate, carries out the transition to organic (lamination) substrate up to industry member from ceramic substrate, and the bottom filling technique just obtains large-scale application, and the use of organic bottom packing material is decided as industrial standards.The bottom fill system that uses can be divided three classes at present: the kapillary bottom fills, helps weldering (non-current) type bottom to fill and four jiaos or an angle-bottom fill system.Every class bottom fill system all has its benefit and limitation, but at present the most widely used be the kapillary underfill.The range of application that fill the kapillary bottom comprises flip-chip (FCiP) in FCOB (FCOB) and the encapsulation.Fill stress that can the dispersed chip surface bears and then the reliability that has improved whole prod by adopting the bottom.The technology of using the kapillary bottom to fill in conventional flip chip and chip size packages (CSP) is similar.At first, flow again afterwards, so just formed alloy interconnect chip attach position of solder paste deposited to the substrate.After chip is finished upside-down mounting, adopt dispersion technology underfill to be injected into one or two limits of CSP.Material below encapsulation, flow and filling CSP and populated circuit board between the space.Problems such as there is the solidification value height mostly in underfill at present, and curing speed is slow, and stability in storage is bad, and be difficult to meet the demands at high-speed, the present underfill of high-level efficiency of electron production.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of low-temperature fast curing underfill adhesive is provided.
Another object of the present invention provides a kind of preparation method of low-temperature fast curing underfill adhesive.
Problems such as the present invention mainly solves existing underfill solidification value height, curing speed is slow, stability in storage is bad.
In order to achieve the above object, the present invention is achieved in that a kind of low-temperature fast curing underfill adhesive, and its special character is that it is made up of the following weight proportion raw material: resin 40-65 part, 0.5 part in colorant, solidifying agent 20-25 part, promotor 1-6 part, coupling agent 0.1-3 part, epoxy active diluent 15-25 part; Resin is bisphenol A-type, bisphenol f type epoxy resin; Colorant is carbon black T4, earlier colorant carbon black T4 is become color with mixed with resin; Solidifying agent is modified imidazole and derivative thereof, modified amine curing agent, can be one or more mixing; Promotor is modified imidazole; Coupling agent is aminopropyl triethoxysilane (KH550), γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane (KH560), γ-methacryloxypropyl trimethoxy silane (KH570), can be one or more mixing, epoxy active diluent is an aliphatics monocycle oxygen activity thinner.
A kind of low-temperature fast curing underfill adhesive of the present invention, described resin is bisphenol A-type, bisphenol f type epoxy resin, as bisphenol F epoxy resin 830LVP, big Japanese ink company produces, liquid bisphenol A epoxide resin 828EL, the U.S. Shell Oil Co. produce, and liquid resin is given glued membrane high cohesive strength, and some heat-resistant resins can improve the Tg point solution heat resistance after the glue curing.
A kind of low-temperature fast curing underfill adhesive of the present invention, described colorant is carbon black T4, mixing at first with colorant and electronic-grade dihydroxyphenyl propane epoxy resin (828EL) or electronic-grade bisphenol F epoxy resin (830LVP), because the difficult dispersion of colorant, need in advance it to be mixed in proportion, scattered standby with three-roller.
A kind of low-temperature fast curing underfill adhesive of the present invention, described solidifying agent comprises the composition of following one or more materials, modified imidazole and derivative thereof, modified amine curing agent, as modified amine curing agent 1020, Fuji's chemical production, modified amine curing agent PN23, Japan's aginomoto production, modified imidazole class solidifying agent 2,4 methylimidazoles, selected solidifying agent is a latent, fineness is at 5-10 μ, has the low temperature fast setting, stability in storage is good, stifled syringe needle during this sampling point glue.
A kind of low-temperature fast curing underfill adhesive of the present invention, described promotor is modified imidazole, as PN-H, Japanese aginomoto production.
A kind of low-temperature fast curing underfill adhesive of the present invention, described epoxy active diluent AGE are H8 aliphatics monocycle oxygen activity thinner, and U.S.'s shell is produced.
The preparation method of low-temperature fast curing underfill adhesive of the present invention, its special character is that it comprises following processing step: earlier colorant and mixed with resin are made color, again residual resin and color are mixed, time 20-40min, temperature 20-30 ℃, add solidifying agent (dividing three addings) then, curing catalyst, three-roller mixes, temperature 20-30 ℃, under the cooling drying condition, mix, cold water is controlled at 15 ℃, mixes three times, mixes the back and adds full vacuum 15min in the reactor, after mixing, resin and solidifying agent add coupling agent, epoxide diluent mixes, full vacuum 30min.
A kind of low-temperature fast curing underfill adhesive of the present invention, its performance test be, sampling should be controlled in 7 minutes with 120 ℃ of following curing speeds of DSC test, and shearing resistance is tested by the GB/T7124-1986 standard.Glue is placed on 7-24h in 40 ℃ of baking ovens, the assessment stability in storage.
Compared with the prior art a kind of low-temperature fast curing underfill adhesive of the present invention and preparation method thereof has outstanding substantive distinguishing features and marked improvement: 1, this adhesive curing temperature is low 120 ℃, the fast DSC of curing speed is less than 7 minutes, set time was less than 20 minutes in the actual production, velocity of flow is fast, velocity of flow between 25 micron gap is greater than 12mm/s, stable storing, the refrigerator 2-8 ℃ shelf lives is more than 6 months; 2, preparation technology's simple environment protection, cost is low, and is applied widely.
Embodiment:
In order to understand better and to implement, describe a kind of low-temperature fast curing underfill adhesive of the present invention and preparation method thereof in detail below in conjunction with embodiment.
Embodiment 1, take by weighing resin 828EL (shell) 13.2g, resin 830LVP (big Japanese ink) 39.2g, (Degussa carbon black T4 and 828EL are mixed in proportion colorant 0.5g, concrete part by weight is 2: 8, be mixed into color), solidifying agent fujicure fxr 1020 25g, promotor PN-H (Japanese aginomoto) 5g, coupling agent KH560 0.56g, epoxy active diluent AGE (shell H8) 20g, solidifying agent is a latent, fineness is 5-10 μ; Resin 830LVP is toasted a night down at 70-75 ℃, then resin 828EL, resin 830LVP, color mixes, time 30min, 25 ℃ of temperature, add solidifying agent (dividing three addings) then, promotor, three-roller mixes, 25 ℃ of temperature, under the cooling drying condition, mix, cold water is controlled at 15 ℃, mixes three times, mixes the back and adds full vacuum 15min in the reactor, after mixing, resin and solidifying agent add coupling agent, epoxide diluent mixes, full vacuum 30min obtains sample, through survey its solidification value be 120 ℃ 15 minutes, the velocity of flow 14mm/s of velocity of flow between 25 micron gap, shearing resistance is 7Mpa; 40 ℃ of shelf liveves surpass 10h, and its 2-8 ℃ shelf lives is 10 months.
The comparative example 1, takes by weighing E-51 resin 39.2g, adds E-44 resin 13.2g, black cream 0.5g, dicy-curing agent 4.2g, F101S curing catalyst 0.4gE-20, coupling agent KH560:0.56g, AGE (shellH8) 20g, by above working method, obtain sample, through survey its solidification value be 120 ℃ 30 minutes, the velocity of flow 10mm/s of velocity of flow between 25 micron gap, shearing resistance is 7Mpa; 40 ℃ of shelf liveves surpass 10h, and its 2-8 ℃ shelf lives is 10 months.
Embodiment 1 compares with comparative example 1, two kinds of situation prescriptions are basic identical, difference is: embodiment 1 uses a kind of latent curing agent, curing catalyst to form perfect curing system, the viscosity of the overall glue that the cooperation of Resins, epoxy makes is not high, wettability to base material is splendid, the velocity of flow excellence, and solidification value is low, and curing speed is fast.And the viscosity height of comparative example's 1 glue, velocity of flow is slow, and curing speed is slow, is difficult to satisfy the electronic industry of current emphasis efficient.
Embodiment 2, take by weighing resin 828EL (shell) 25g, resin 830LVP (big Japanese ink) 40g, (Degussa carbon black T4 and 828EL are mixed in proportion colorant 0.5g, concrete part by weight is 2: 8, is mixed into color), solidifying agent fujicure fxr 1020 10g, the solidifying agent PN23 10g that Japan's aginomoto is produced, promotor PN-H (Japanese aginomoto) 1g, coupling agent KH550 0.1g, epoxy active diluent (shellH8) 15g, solidifying agent is a latent, and fineness is 5-10 μ; Resin 830LVP is toasted a night down at 70-75 ℃, then resin 828EL, resin 830LVP, color are mixed, time 20min, 30 ℃ of temperature, add solidifying agent (dividing three addings), promotor then, three-roller mixes, 20 ℃ of temperature, mix under the cooling drying condition, cold water is controlled at 15 ℃, mixes three times, mix the back and add full vacuum 15min in the reactor, after resin and solidifying agent mix, add coupling agent, epoxide diluent mixes, full vacuum 30min obtains product.
Embodiment 3, take by weighing resin 828EL (shell) 20g, resin 830LVP (big Japanese ink) 20g, (Degussa carbon black T4 and 830LVP are mixed in proportion colorant 0.5g, concrete part by weight is 2: 8, be mixed into color), solidifying agent fujicure fxr 1020 and modified imidazole class solidifying agent 2,4 methylimidazole 25g, promotor PN-H (Japanese aginomoto) 6g, coupling KH570 2g, coupling KH560 1g, epoxy active diluent (shell H8) 25g, solidifying agent is a latent, fineness is 5-10 μ; Resin 830LVP is toasted a night down at 70-75 ℃, then resin 828EL, resin 830LVP, color are mixed, time 40min, 20 ℃ of temperature, add solidifying agent (dividing three addings), promotor then, three-roller mixes, 30 ℃ of temperature, mix under the cooling drying condition, cold water is controlled at 15 ℃, mixes three times, mix the back and add full vacuum 15min in the reactor, after resin and solidifying agent mix, add coupling agent, epoxide diluent mixes, full vacuum 30min obtains product.

Claims (3)

1, a kind of low-temperature fast curing underfill adhesive is characterized in that it is made up of the following weight proportion raw material: resin 40-65 part, 0.5 part in colorant, solidifying agent 20-25 part, promotor 1-6 part, coupling agent 0.1-3 part, epoxy active diluent 15-25 part; Resin is the mixing of bisphenol A-type, bisphenol f type epoxy resin; Colorant is carbon black T4; Solidifying agent is modified imidazole and derivative thereof, modified amine curing agent, can be one or more mixing; Promotor is modified imidazole; Coupling agent is aminopropyl triethoxysilane, Y-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, can be one or more mixing, and epoxy active diluent is an aliphatics monocycle oxygen activity thinner.
2, a kind of low-temperature fast curing underfill adhesive according to claim 1 is characterized in that described solidifying agent is a latent, and fineness is 5-10 μ.
3, the preparation method of the low-temperature fast curing underfill adhesive of aforesaid right requirement, it is characterized in that it comprises following processing step: even resin and coloring material for mixing, time 20-40min, temperature 20-30 ℃, add solidifying agent, promotor then, dividing three times adds, three-roller mixes, and temperature 20-30 ℃, mixes under the cooling drying condition, cold water is controlled at 15 ℃, mix three times, mix the back and add full vacuum 15min in the reactor, add coupling agent, epoxide diluent mixing when resin and solidifying agent mix the back, full vacuum 30min promptly gets product.
CN2009100163239A 2009-06-05 2009-06-05 Low-temperature fast curing underfill adhesive and preparation method thereof Expired - Fee Related CN101580684B (en)

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101880514A (en) * 2010-06-28 2010-11-10 深圳市库泰克电子材料技术有限公司 Single-component under-filler with favorable repairing property and preparation method thereof
CN102010686A (en) * 2010-09-30 2011-04-13 烟台德邦电子材料有限公司 Double-solidification system fast-flowing underfill and preparation method thereof
CN102102001A (en) * 2010-12-03 2011-06-22 烟台德邦科技有限公司 High thermal conductivity graphene-based epoxy resin adhesive and preparation method thereof
CN102250556A (en) * 2010-05-20 2011-11-23 松扬电子材料(昆山)有限公司 Lightproof polyimide back glue film
CN101724368B (en) * 2009-11-24 2013-03-27 烟台德邦科技有限公司 Anti-impact epoxy structural rubber and preparation method thereof
CN103087664A (en) * 2013-01-29 2013-05-08 深圳市宝力科技有限公司 Relay liquid state epoxy resin pouring sealant and preparation method thereof
CN103709983A (en) * 2013-12-23 2014-04-09 东莞市亚聚电子材料有限公司 High temperature resisting bottom filler glue and preparation method thereof
CN103725240A (en) * 2013-12-27 2014-04-16 烟台德邦科技有限公司 Underfill adhesive with storage stability and fast mobility and preparation method of underfill adhesive
CN103740060A (en) * 2013-12-23 2014-04-23 东莞市亚聚电子材料有限公司 Low-halogen underfill adhesive and preparation method thereof
CN103756612A (en) * 2013-12-23 2014-04-30 东莞市亚聚电子材料有限公司 Low-temperature setting underfill adhesive and preparation method thereof
CN104212122A (en) * 2014-09-02 2014-12-17 中国林业科学研究院木材工业研究所 Additive of phenolic resin as well as preparation method and application of additive
CN104979225A (en) * 2015-05-19 2015-10-14 深圳创维-Rgb电子有限公司 Bottom filling method for preventing cold solder joint of BGA IC
CN104974698A (en) * 2015-07-17 2015-10-14 苏州新区华士达工程塑胶有限公司 Novel plastic adhesive
CN105440998A (en) * 2015-11-26 2016-03-30 河南豫冠化工科技开发有限公司 Low-temperature fast-curing epoxy resin adhesive and preparation method thereof
CN106753143A (en) * 2016-12-21 2017-05-31 南京诺邦新材料有限公司 A kind of low-temperature setting underfill with heat conduction function and preparation method thereof
CN106928891A (en) * 2015-12-30 2017-07-07 卡本复合材料(天津)有限公司 A kind of high-strength adhesive of epoxies low temperature curing type
CN107394004A (en) * 2017-06-28 2017-11-24 中国电子科技集团公司第十研究所 A kind of bottom filling method of multispectral dual chip infrared detector
CN109880564A (en) * 2019-01-23 2019-06-14 甘肃省交通规划勘察设计院股份有限公司 A kind of fortified resins and its preparation method and application

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101724368B (en) * 2009-11-24 2013-03-27 烟台德邦科技有限公司 Anti-impact epoxy structural rubber and preparation method thereof
CN102250556A (en) * 2010-05-20 2011-11-23 松扬电子材料(昆山)有限公司 Lightproof polyimide back glue film
CN101880514A (en) * 2010-06-28 2010-11-10 深圳市库泰克电子材料技术有限公司 Single-component under-filler with favorable repairing property and preparation method thereof
CN101880514B (en) * 2010-06-28 2012-06-27 深圳市库泰克电子材料技术有限公司 Single-component under-filler with favorable repairing property and preparation method thereof
CN102010686A (en) * 2010-09-30 2011-04-13 烟台德邦电子材料有限公司 Double-solidification system fast-flowing underfill and preparation method thereof
CN102102001A (en) * 2010-12-03 2011-06-22 烟台德邦科技有限公司 High thermal conductivity graphene-based epoxy resin adhesive and preparation method thereof
CN102102001B (en) * 2010-12-03 2013-04-17 烟台德邦科技有限公司 High thermal conductivity graphene-based epoxy resin adhesive and preparation method thereof
CN103087664A (en) * 2013-01-29 2013-05-08 深圳市宝力科技有限公司 Relay liquid state epoxy resin pouring sealant and preparation method thereof
CN103756612B (en) * 2013-12-23 2015-12-30 东莞市亚聚电子材料有限公司 A kind of low-temperature curing underfill and preparation method thereof
CN103709983A (en) * 2013-12-23 2014-04-09 东莞市亚聚电子材料有限公司 High temperature resisting bottom filler glue and preparation method thereof
CN103740060A (en) * 2013-12-23 2014-04-23 东莞市亚聚电子材料有限公司 Low-halogen underfill adhesive and preparation method thereof
CN103756612A (en) * 2013-12-23 2014-04-30 东莞市亚聚电子材料有限公司 Low-temperature setting underfill adhesive and preparation method thereof
CN103709983B (en) * 2013-12-23 2015-12-30 东莞市亚聚电子材料有限公司 A kind of high temperature resistant underfill and preparation method thereof
CN103725240A (en) * 2013-12-27 2014-04-16 烟台德邦科技有限公司 Underfill adhesive with storage stability and fast mobility and preparation method of underfill adhesive
CN104212122A (en) * 2014-09-02 2014-12-17 中国林业科学研究院木材工业研究所 Additive of phenolic resin as well as preparation method and application of additive
CN104979225A (en) * 2015-05-19 2015-10-14 深圳创维-Rgb电子有限公司 Bottom filling method for preventing cold solder joint of BGA IC
CN104974698A (en) * 2015-07-17 2015-10-14 苏州新区华士达工程塑胶有限公司 Novel plastic adhesive
CN105440998A (en) * 2015-11-26 2016-03-30 河南豫冠化工科技开发有限公司 Low-temperature fast-curing epoxy resin adhesive and preparation method thereof
CN105440998B (en) * 2015-11-26 2018-06-26 河南豫冠化工科技开发有限公司 A kind of preparation method of low-temperature fast-curing epoxyn
CN106928891A (en) * 2015-12-30 2017-07-07 卡本复合材料(天津)有限公司 A kind of high-strength adhesive of epoxies low temperature curing type
CN106753143A (en) * 2016-12-21 2017-05-31 南京诺邦新材料有限公司 A kind of low-temperature setting underfill with heat conduction function and preparation method thereof
CN107394004A (en) * 2017-06-28 2017-11-24 中国电子科技集团公司第十研究所 A kind of bottom filling method of multispectral dual chip infrared detector
CN107394004B (en) * 2017-06-28 2018-11-20 中国电子科技集团公司第十一研究所 A kind of bottom filling method of multispectral dual chip infrared detector
CN109880564A (en) * 2019-01-23 2019-06-14 甘肃省交通规划勘察设计院股份有限公司 A kind of fortified resins and its preparation method and application
CN109880564B (en) * 2019-01-23 2021-06-25 甘肃省交通规划勘察设计院股份有限公司 Reinforced resin and preparation method and application thereof

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