CN103756612B - A kind of low-temperature curing underfill and preparation method thereof - Google Patents
A kind of low-temperature curing underfill and preparation method thereof Download PDFInfo
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- CN103756612B CN103756612B CN201310719566.5A CN201310719566A CN103756612B CN 103756612 B CN103756612 B CN 103756612B CN 201310719566 A CN201310719566 A CN 201310719566A CN 103756612 B CN103756612 B CN 103756612B
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Abstract
The present invention relates to electronics glue technical field, refer in particular to a kind of low-temperature curing underfill and preparation method thereof, the thinner of the dihydroxyphenyl propane of scientific formula or bisphenol F epoxy resin and low-temperature curing, promotor, coupling agent, stablizer is adopted in underfill of the present invention, by composition proportion and the preparation method of the present invention of science, underfill of the present invention have low-temperature curing and set time short feature, low-temperature curing, can energy consumption be reduced, meet the electronic product demand being not suitable for high temperature; Fast setting, meets high-level efficiency electronic product assembling demand, and has moderate cost, the feature of stable performance.
Description
Technical field
The present invention relates to electronics glue technical field, refer in particular to a kind of low-temperature curing underfill and preparation method thereof.
Background technology
Underfill technology last century the seventies rise in IBM Corporation, become at present electronic manufacture industry important make part.The underfill system of current use can be divided three classes: kapillary underfill, no-reflow underfill, a premolding (angle-underfill system.Every type systematic has its benefit and limitation, but the most widely used be at present kapillary underfill system, its range of application comprise FCOB (FCOB) and encapsulation in flip-chip (FCiP).Can the surperficial stress born of dispersed chip and then the reliability improving whole product by employing underfill.In order to the requirement of the slimming of satisfied digital mobile product, miniaturization, high performance, at the BGA(BallGridArray that IC encapsulation field is highly integrated) and the QFP that CSP(ChipSize/ScalePackage) etc. instead of in the past, be rapidly spread popularization.
BGA with CSP utilizes tin ball and the electrode on wiring board to carry out being connected.But can be subject to temperature shock after actual load, and wiring board such as to bend at the impact of the internal stress produced, make BGA, the reliability connected between CSP and wiring board can not get good guarantee.This problem has been got more and more concern in recent years.Underfill promptly can be impregnated into BGA and CSP etc. between chip and wiring board, has excellent filling characteristic; Can play after solidification and relax temperature shock and absorb internal stress, the effect of the connection of reinforcement BGA and substrate, and then the trustworthiness greatly enhancing connection.
At present in underfill, could solidify under generally at least needing the high temperature of 120 DEG C, and temperature is lower, set time is longer, is difficult to the high-level efficiency requirement of the Full-automatic spot gluing rapid-assembling electronics of automatic production.
Summary of the invention
The invention reside in and there is for current underfill the problem that solidification value is high, set time is long, and a kind of low-temperature curing underfill overcome the above problems and preparation method thereof is provided.
For achieving the above object, the present invention adopts following technical scheme:
A kind of low-temperature curing underfill, composition and the Parts by Ingredients of described filling glue are as follows:
Epoxy resin: dihydroxyphenyl propane and bisphenol F epoxy resin be a kind of or its combination wherein, containing 49.0 ~ 69.0 parts;
Thinner: glyceryl ether, containing 5.0 ~ 20.0 parts;
Promotor: PN23J imidazole adducts, 2,4,6-tri-(dimethylamino methyl) phenol, benzyldimethylamine, glyoxal ethyline urea be a kind of or arbitrary combination wherein, containing 3.0 ~ 8.0 parts;
Coupling agent: silane coupling agent, γ-chloropropyl triethoxysilane, titanate coupling agent, aluminate coupling agent is a kind of or arbitrary combination wherein, containing 0.5 ~ 1.0 part;
Filler: talcum powder, silicon powder, gas-phase silica, activated Calcium carbonate be a kind of or arbitrary combination wherein, containing 13.0 ~ 33.0 parts;
Pigment: carbon black, containing 0.5 ~ 1.0 part;
Stablizer: three (2,4 di-tert-butyl-phenyl) phosphorous acid ester, four [β (3,5-di-t-butyl 4-hydroxy-pheny) propionic acid] pentaerythritol ester, triphenyl phosphite be a kind of or arbitrary combination wherein, containing 0.5 ~ 3.0 part;
Solidifying agent: Dyhard RU 100,2-heptadecyl imidazole, glyoxal ethyline, Succinic anhydried, diethylenetriamine be a kind of or arbitrary combination wherein, containing 10.0 ~ 20.0 parts.
Preferably, bisphenol A epoxide resin in described epoxy resin is bisphenol A epoxide resin 827, bisphenol A epoxide resin 828, bisphenol A epoxide resin 828EL wherein a kind of or arbitrary combination, and bisphenol F epoxy resin is bisphenol F epoxy resin 862, bisphenol F epoxy resin YDF170, bisphenol F epoxy resin YDF175 wherein a kind of or arbitrary combination.
Preferably, glyceryl ether is one in polypropylene glycol diglycidyl ether, glycidyl allyl ether, n-butyl glycidyl ether, diglycidylether, butanediol diglycidyl ether or arbitrary combination.
The preparation method of described low-temperature curing underfill, comprises following processing step:
(1) successively epoxy resin, thinner, pigment are added in vacuum double planetary mixer, high-speed stirring speed 1000r/min ± 50r/min, stirring at low speed speed 50r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 30 ± 2min, temperature controls at 40 ± 5 DEG C, and dispersed with stirring is even;
(2) successively stablizer, promotor, coupling agent, filler are added again, high-speed stirring speed 1250r/min ± 50r/min, stirring at low speed speed 60r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 120 ± 5min, temperature controls at 25 ± 5 DEG C, and dispersed with stirring is even;
(3) solidifying agent is added again, high-speed stirring speed 1000r/min ± 50r/min, stirring at low speed speed 40r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 60 ± 5min, temperature controls at 20 ± 5 DEG C, and namely dispersed with stirring evenly obtains described underfill.
Beneficial effect of the present invention is: adopt the dihydroxyphenyl propane of scientific formula or the thinner of bisphenol F epoxy resin and low-temperature curing in underfill of the present invention, promotor, coupling agent, stablizer, by composition proportion and the preparation method of the present invention of science, the promotor of the present invention's formula, coupling agent, the selection of solidifying agent and proportioning, promotor and coupling agent accelerate curing reaction, reduce solidification value, shorten set time, also physical and mechanical property can be improved, the underfill of underfill of the present invention have low-temperature curing and set time short feature, low-temperature curing, energy consumption can be reduced, meet the electronic product demand being not suitable for high temperature, fast setting, meets high-level efficiency electronic product assembling demand, and has moderate cost, the feature of stable performance.
Embodiment
Below in conjunction with embodiment, the present invention is further described:
Embodiment 1:
The underfill of the present embodiment is made up of the component containing following weight part:
Embodiment 2:
The underfill of the present embodiment is made up of the component containing following weight part:
Embodiment 3:
The underfill of the present embodiment is made up of the component containing following weight part
Embodiment 4:
The underfill of the present embodiment is made up of the component containing following weight part:
The preparation method of low-temperature curing underfill of the present invention, comprises following processing step:
(1) successively epoxy resin, thinner, pigment are added in vacuum double planetary mixer, high-speed stirring speed 1000r/min ± 50r/min, stirring at low speed speed 50r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 30 ± 2min, temperature controls at 40 ± 5 DEG C, and dispersed with stirring is even;
(2) successively stablizer, promotor, coupling agent, filler are added again, high-speed stirring speed 1250r/min ± 50r/min, stirring at low speed speed 60r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 120 ± 5min, temperature controls at 25 ± 5 DEG C, and dispersed with stirring is even;
(3) solidifying agent is added again, high-speed stirring speed 1000r/min ± 50r/min, stirring at low speed speed 40r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 60 ± 5min, temperature controls at 20 ± 5 DEG C, and namely dispersed with stirring evenly obtains described underfill.
The underfill of underfill of the present invention have low-temperature curing and set time short feature, low-temperature curing, can reduce energy consumption, meets the electronic product demand being not suitable for high temperature; Fast setting, meets high-level efficiency electronic product assembling demand, and has moderate cost, the feature of stable performance
Detect by experiment, the form of the detection Data Comparison of the present invention four embodiment and conventional underfill set time used under different solidification values can significantly be found out: the underfill of underfill of the present invention have good low-temperature curing and set time short feature:
Table 1 detects Data Comparison table
The above embodiment, just preferred embodiments of the present invention, be not limit practical range of the present invention, therefore all equivalences done according to structure, feature and the principle described in the present patent application the scope of the claims change or modify, and all should be included in patent claim of the present invention.
Claims (4)
1. a low-temperature curing underfill, is characterized in that, composition and the Parts by Ingredients of described filling glue are as follows:
Epoxy resin: bisphenol A epoxide resin and bisphenol F epoxy resin be a kind of or its combination wherein, containing 49.0 ~ 69.0 parts;
Thinner: glyceryl ether, containing 5.0 ~ 20.0 parts;
Promotor: PN23J imidazole adducts, 2,4,6-tri-(dimethylamino methyl) phenol, benzyldimethylamine, glyoxal ethyline urea be a kind of or arbitrary combination wherein, containing 3.0 ~ 8.0 parts;
Coupling agent: γ-chloropropyl triethoxysilane, titanate coupling agent, aluminate coupling agent be a kind of or arbitrary combination wherein, containing 0.5 ~ 1.0 part;
Filler: talcum powder, silicon powder, gas-phase silica, activated Calcium carbonate be a kind of or arbitrary combination wherein, containing 13.0 ~ 33.0 parts;
Pigment: carbon black, containing 0.5 ~ 1.0 part;
Stablizer: three (2,4 di-tert-butyl-phenyl) phosphorous acid ester, four [β (3,5-di-t-butyl 4-hydroxy-pheny) propionic acid] pentaerythritol ester, triphenyl phosphite be a kind of or arbitrary combination wherein, containing 0.5 ~ 3.0 part;
Solidifying agent: Dyhard RU 100,2-heptadecyl imidazole, glyoxal ethyline, Succinic anhydried, diethylenetriamine be a kind of or arbitrary combination wherein, containing 10.0 ~ 20.0 parts.
2. low-temperature curing underfill according to claim 1, it is characterized in that: described bisphenol A epoxide resin is bisphenol A epoxide resin 827, bisphenol A epoxide resin 828, bisphenol A epoxide resin 828EL wherein a kind of or arbitrary combination, described bisphenol F epoxy resin is bisphenol F epoxy resin 862, bisphenol F epoxy resin YDF170, bisphenol F epoxy resin YDF175 wherein a kind of or arbitrary combination.
3. low-temperature curing underfill according to claim 1, is characterized in that: described glyceryl ether is one in polypropylene glycol diglycidyl ether, glycidyl allyl ether, n-butyl glycidyl ether, butanediol diglycidyl ether or arbitrary combination.
4. the preparation method of the low-temperature curing underfill according to claim 1-3 any one, comprises following processing step:
(1) successively epoxy resin, thinner, pigment are added in vacuum double planetary mixer, high-speed stirring speed 1000r/min ± 50r/min, stirring at low speed speed 50r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 30 ± 2min, temperature controls at 40 ± 5 DEG C, and dispersed with stirring is even;
(2) successively stablizer, promotor, coupling agent, filler are added again, high-speed stirring speed 1250r/min ± 50r/min, stirring at low speed speed 60r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 120 ± 5min, temperature controls at 25 ± 5 DEG C, and dispersed with stirring is even;
(3) solidifying agent is added again, high-speed stirring speed 1000r/min ± 50r/min, stirring at low speed speed 40r/min ± 5r/min, vacuum tightness 0.06-0.09MPa, time 60 ± 5min, temperature controls at 20 ± 5 DEG C, and namely dispersed with stirring evenly obtains described underfill.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104559884B (en) * | 2014-12-16 | 2016-08-24 | 惠州力王佐信科技有限公司 | A kind of polymeric adhesion material |
| CN105349077A (en) * | 2015-11-24 | 2016-02-24 | 太仓市金锚新材料科技有限公司 | Novel underfill 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 |
| CN108977145A (en) * | 2017-05-31 | 2018-12-11 | 烟台信友新材料股份有限公司 | A kind of high moisture-proof temperature curing epoxy low glue and preparation method thereof |
| CN112852305A (en) * | 2021-01-07 | 2021-05-28 | 东莞市新懿电子材料技术有限公司 | High-performance polyurethane solid filling adhesive and preparation method thereof |
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| CN101358121A (en) * | 2008-09-10 | 2009-02-04 | 武汉科技学院 | A kind of preparation method that can cure high temperature resistant epoxy resin adhesive at room temperature |
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| CN103232828A (en) * | 2013-05-16 | 2013-08-07 | 常州博美新材料科技有限公司 | High-adhesion and heat-resistant epoxy resin adhesive and using method thereof |
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| JP2009256466A (en) * | 2008-04-16 | 2009-11-05 | Sekisui Chem Co Ltd | Adhesive for electronic part |
| JP5875888B2 (en) * | 2012-02-17 | 2016-03-02 | 日本曹達株式会社 | SUS substrate adhesive |
| CN102627929B (en) * | 2012-03-22 | 2013-10-23 | 连云港华海诚科电子材料有限公司 | Underfill flowable at room temperature and rapidly solidified at low temperature, and preparation method thereof |
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| CN101358121A (en) * | 2008-09-10 | 2009-02-04 | 武汉科技学院 | A kind of preparation method that can cure high temperature resistant epoxy resin adhesive at room temperature |
| CN101580684A (en) * | 2009-06-05 | 2009-11-18 | 烟台德邦科技有限公司 | Low-temperature fast curing underfill adhesive and preparation method thereof |
| CN101928539A (en) * | 2010-09-10 | 2010-12-29 | 烟台德邦科技有限公司 | High-temperature resistant single-component epoxy structure glue, preparation method and using method thereof |
| CN102031081A (en) * | 2010-11-26 | 2011-04-27 | 烟台德邦电子材料有限公司 | Liquid epoxy encapsulating material and preparation method thereof |
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