CN103937433B - A kind of high reliability environment-friendly type underfill and preparation method thereof - Google Patents
A kind of high reliability environment-friendly type underfill and preparation method thereof Download PDFInfo
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- CN103937433B CN103937433B CN201410125587.9A CN201410125587A CN103937433B CN 103937433 B CN103937433 B CN 103937433B CN 201410125587 A CN201410125587 A CN 201410125587A CN 103937433 B CN103937433 B CN 103937433B
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Abstract
The present invention relates to a kind of high reliability environment-friendly type underfill and preparation method thereof, in the percentage composition of raw material gross weight, be made up of following raw material: bisphenol-type epoxy resin 30 ~ 50 parts, cycloaliphatic epoxy resin 1 ~ 10 part, toughner 10 ~ 20 parts, thinner 5 ~ 10 parts, 5 ~ 15 parts, solidifying agent, silane coupling agent 0.1 ~ 5 part, dispersion agent 0.01 ~ 1 part, defoamer 0.01 ~ 1 part, filler 25 ~ 35 parts, pigment 0.1 ~ 1 part.Underfill prepared by the present invention, there is low halogen, normal temperature flow fast, middle temperature fast setting, cold-hot impact property are superior, with the advantage such as various tin cream film of flux residue compatibility is good, be applicable to the encapsulation such as BGA, CSP.
Description
Technical field
The present invention relates to a kind of high reliability environment-friendly type underfill and preparation method thereof, belong to sizing agent field.
Background technology
Along with the fast development of electronic industry, closely-related Electronic Encapsulating Technology is also more and more advanced with it.The Main Trends of The Development intelligent, lightweight, volume is little, speed is fast, function is strong, good reliability etc. becomes electronic product.Meanwhile, encapsulation industry is also unwilling to be outshone, and the Advanced Packagings such as BGA (Ball Grid Array), Flip Chip, CSP (Chip Scale Package) become main flow.Underfill is one of critical electronic material required in the microelectronics Packaging such as high-density flip-chip BGA, CSP, and its Main Function is protection high-density soldered ball node and chip, and ensure that BGA, the reliability of CSP device and life-time service.
It is high all to there is content of halogen in current most of underfill, does not meet the requirement of environmental protection; With tin cream film of flux residue poor compatibility, part glue may be caused not solidify; Reliability is low, and use properties is poor, can not meet the demand that encapsulation technology develop rapidly now brings.
Summary of the invention
The object of the invention is the deficiency overcoming above-mentioned prior art, a kind of high reliability environment-friendly type underfill and preparation method thereof is provided, underfill prepared by the present invention has low halogen, normal temperature flows fast, middle temperature fast setting, cold-hot impact property are superior, with the advantage such as various tin cream film of flux residue compatibility is good.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of high reliability environment-friendly type underfill, in the percentage composition of raw material gross weight, be made up of following raw material: bisphenol-type epoxy resin 30 ~ 50 parts, cycloaliphatic epoxy resin 1 ~ 10 part, toughner 10 ~ 20 parts, thinner 5 ~ 10 parts, silane coupling agent 0.1 ~ 5 part, 5 ~ 15 parts, solidifying agent, dispersion agent 0.01 ~ 1 part, defoamer 0.01 ~ 1 part, filler 25 ~ 35 parts, pigment 0.1 ~ 1 part.
Further, described bisphenol-type epoxy resin is one in the bisphenol A-type of low halogen, bisphenol-f type, phenol aldehyde modified epoxy resin or any several mixing.
Further, described cycloaliphatic epoxy resin is one or both mixing in 3,4-epoxycyclohexyl-methyl-3,4-epoxycyclohexyl manthanoate, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester.
Further, described toughner is one in core shell rubbers epoxy resin, nucleocapsid structure silicone rubber particles modified epoxy or any two kinds of mixing.
Further, described thinner is the C of low halogen
12-14one or both mixing in alkyl glycidyl ether (Japanese ADEKA), tertiary carbonic acid glycidyl ester (U.S. HEXION).
Further, described silane coupling agent is one in aminopropyl triethoxysilane (KH550), γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane (KH560), γ-methacryloxypropyl trimethoxy silane (KH570) or any several mixing.
Further, described solidifying agent is that aromatic amine, modified imidazole and derivative thereof, modified amine curing agent are as modified amine curing agent 1020(Japanese fuji chemistry), modified imidazole class solidifying agent PN40(Japan aginomoto), 2-ethyl-4-methylimidazole (Japanese four countries change into), selected solidifying agent is latent, fineness at 5-10 μ, have low-temperature fast-curing, stability in storage good.
Further, described dispersion agent is the one in BYK-9076, BYK-W9010, BYK-W985 of German Bi Ke chemistry.
Further, described defoamer is the one in BYK-A530, BYK-A535, BYK-S706, BYK-077 of German Bi Ke chemistry.
Further, described filler is 4um, 10um ball-shaped silicon micro powder (the handsome that in Wuhan) one or both mixing.
Further, described pigment is low halogen black color (Poly one).
The invention has the beneficial effects as follows: high reliability environment-friendly type underfill prepared by the present invention, low halogen, can room temperature flow fast, middle temperature fast setting, and good with various tin cream film of flux residue compatibility, cold-hot impact property is superior, and reliability is high.
The preparation method of the underfill that a kind of stable storing of the present invention flows fast, comprising:
1) in the percentage composition of raw material gross weight, take 30 ~ 50 parts of bisphenol-type epoxy resins, 1 ~ 10 part of cycloaliphatic epoxy resin, 10 ~ 20 parts of toughner, 5 ~ 10 parts of thinners, 0.1 ~ 5 part of silane coupling agent, 0.01 ~ 1 part of dispersion agent, 0.01 ~ 1 part of defoamer, 0.1 ~ 1 part of pigment, drop in reactor, be uniformly mixed;
2) take 25 ~ 35 parts of silicon powder fillers, be divided into equivalent three batches and join in the reactor of step 1), often criticizing the joining day is spaced apart 20 minutes, is uniformly mixed;
3) temperature controls to take 5 ~ 15 parts of solidifying agent at 20 ~ 30 DEG C and joins step 2) reactor in, rotating speed 300 revs/min, cooling water temperature control is built in 15 DEG C, and vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, get product.
Embodiment
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
embodiment 1
Take bisphenol f type epoxy resin 830lvp (large Japanese ink) 32g, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester (the new scape in the Hubei) 6g of cycloaliphatic epoxy resin, toughner core shell rubbers epoxy resin MX-125(Japan Zhong Yuan) 10g, thinner C
12-14alkyl glycidyl ether ED-502S(Japan ADEKA) 6g, coupling agent KH-560 1g, dispersant B YK-9076 0.6g, defoamer BYK-A530 0.7g, black color (Poly one) 0.5g, drop in reactor, be uniformly mixed; Add 10 um ball-shaped silicon micro powders (the handsome that in Wuhan) 25 grams again, divide and add for three times, add latent curative PN40(Japan aginomoto subsequently) 15 g, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
embodiment 2
Take bisphenol f type epoxy resin YL-983U (Mitsubishi Chemical) 40g, cycloaliphatic epoxy resin 3,4-epoxycyclohexyl-methyl-3,4-epoxycyclohexyl manthanoate (Daicel) 4g, nucleocapsid structure silicone rubber particles modified epoxy ALBIDUR EP2240A(Germany EVONIK) 12g, thinner tertiary carbonic acid glycidyl ester (U.S. HEXION) 6g, coupling agent KH-560 1g, dispersant B YK-W9010 0.8g, defoamer BYK-A535 0.9g, black color (Poly one) 0.5g, drops in reactor, is uniformly mixed; Add 4 um ball-shaped silicon micro powders (the handsome that in Wuhan) 30 grams again, divide and add for three times, add latent curative 1020(Japanese fuji chemistry subsequently) 12g, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
embodiment 3
Take bisphenol A type epoxy resin JF-9955A (Suzhou Ju Feng) 30g, cycloaliphatic epoxy resin 3,4-epoxycyclohexyl-methyl-3,4-epoxycyclohexyl manthanoate (Japanese Daicel) 9g, nucleocapsid structure silicone rubber particles modified epoxy ALBIDUR EP5340(Germany EVONIK) 14g, thinner C
12-14alkyl glycidyl ether ED-502S(Japan ADEKA) 6g, coupling agent kh-570 1g, dispersant B YK-W985 1g, defoamer BYK-A535 0.9g, black color (Poly one) 0.5g, drops in reactor, is uniformly mixed; Add 10 um ball-shaped silicon micro powders (the handsome that in Wuhan) 30 grams again, divide and add for three times, add latent curative 2-ethyl-4-methylimidazole (Japanese four countries change into) 8 g subsequently, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
embodiment 4
Take bisphenol f type epoxy resin 830lvp (large Japanese ink) 46g, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester (the new scape in the Hubei) 8g of cycloaliphatic epoxy resin, toughner core shell rubbers epoxy resin MX-125(Japan Zhong Yuan) 17g, thinner C
12-14alkyl glycidyl ether ED-502S(Japan ADEKA) 5g, coupling agent KH-550 0.8g, dispersant B YK-9076 0.5g, defoamer BYK-A530 1g, black color (Poly one) 1g, drop in reactor, be uniformly mixed; Add 10 um ball-shaped silicon micro powders (the handsome that in Wuhan) 35 grams again, divide and add for three times, add latent curative PN40(Japan aginomoto subsequently) 15 g, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
embodiment 5
Take bisphenol f type epoxy resin YL983U (Mitsubishi chemistry) 30g, cycloaliphatic epoxy resin 3,4-epoxycyclohexyl-methyl-3,4-epoxycyclohexyl manthanoate (Japanese Daicel) 10g, nucleocapsid structure silicone rubber particles modified epoxy ALBIDUR EP5340(Germany EVONIK) 14g, thinner C
12-14alkyl glycidyl ether ED-502S(Japan ADEKA) 6g, coupling agent KH-550 0.5g, dispersant B YK-9076 0.4g, defoamer BYK-A535 0.5g, black color (Poly one) 1g, drop in reactor, be uniformly mixed; Add 4 um ball-shaped silicon micro powders (the handsome that in Wuhan) 30 grams again, divide and add for three times, add latent curative 1020(Japanese fuji chemistry subsequently) 14 g, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
comparative example 1
Common bottom fills the curing mode of glue formula-traditional, take resin 828EL 14g, ball-type silicon powder 20g, carbon black 0.5g mixes, and then adds solidifying agent PN-23 25g, mixes under 25 DEG C of conditions, then vacuum 15 minutes are expired, add coupling agent KH560 0.56g, epoxy active diluent AGE (shell H8) 20g subsequently to mix, full vacuum 30 minutes, obtains sample.
concrete test example
By the performance of the underfill of experimental test the above embodiment of the present invention 1-5 below and comparative example.
test example 1content of halogen is tested
X fluorescence spectrum analyzes chlorine, bromine content
test example 2flowing property is tested
BGA exemplar: 10mm × 10mm, pitch are 0.4mm, soldered ball permutation is three-back-shaped, " I " type point glue;
Temperature: 25 DEG C
test example 3curing performance is tested
DSC cure profile, temperature rise rate 60 DEG C/min, 130 DEG C of isothermal cures.
test example 4thermal shock is tested
Latter-40 DEG C-85 DEG C of assembling chip solidification, every section keeps 30min, judging criterion: soldered ball resistance raises 10%.
test example 5the compatibility test of tin cream residue
For the tin cream that soldering flux existing BGA, CSP use, carry out assembling chip, last slice analysis, observe filling situation and solidification situation.
Test result as shown in Table 1 below.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example | |
| Halogen (chlorine+bromine)/ppm | 460 | 690 | 580 | 410 | 638 | 8470 |
| Curing speed/min | 6.78 | 7.02 | 7.56 | 6.03 | 7.56 | 10.54 |
| Velocity of flow/s | 54 | 57 | 60 | 72 | 78 | 124 |
| Thermal shock circulation/time | 1408 | 1369 | 1570 | 1468 | 1484 | 864 |
| Compatible | Good | Good | Good | Good | Good | Difference |
Data as can be seen from table 1, underfill prepared by the present invention, in the feature of environmental protection, curing speed, velocity of flow, reliability and tin cream soldering flux are compatible etc., more traditional underfill all has a clear superiority in, and is more applicable to the requirement of modern packaging process.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. a high reliability environment-friendly type underfill, it is characterized in that, take bisphenol f type epoxy resin 830lvp: large Japanese ink 32g, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester of cycloaliphatic epoxy resin: the new scape 6g in Hubei, toughner core shell rubbers epoxy resin MX-125: Japanese clock deep 10g, thinner C
12-14alkyl glycidyl ether ED-502S: Japanese ADEKA 6g, coupling agent KH-560 1g, dispersant B YK-9076 0.6g, defoamer BYK-A530 0.7g, black color: Poly one 0.5g, drops in reactor, is uniformly mixed; Add 10 um ball-shaped silicon micro powders again: the handsome that 25 grams in Wuhan, divide and add for three times, add latent curative PN40 subsequently: Japanese aginomoto 15 g, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
2. a high reliability environment-friendly type underfill, it is characterized in that, take bisphenol A type epoxy resin JF-9955A: Suzhou Ju Feng 30g, cycloaliphatic epoxy resin 3,4-epoxycyclohexyl-methyl-3,4-epoxycyclohexyl manthanoate: Japanese Daicel 9g, nucleocapsid structure silicone rubber particles modified epoxy ALBIDUR EP5340: German EVONIK 14g, thinner C
12-14alkyl glycidyl ether ED-502S: Japanese ADEKA 6g, coupling agent kh-570 1g, dispersant B YK-W985 1g, defoamer BYK-A535 0.9g, black color: Poly one 0.5g, drops in reactor, is uniformly mixed; Add 10 um ball-shaped silicon micro powders again: the handsome that 30 grams in Wuhan, divide and add for three times, add latent curative 2-ethyl-4-methylimidazole subsequently: Japanese four countries change into 8 g, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
3. a high reliability environment-friendly type underfill, it is characterized in that, take bisphenol f type epoxy resin 830lvp: large Japanese ink 46g, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester of cycloaliphatic epoxy resin: the new scape 8g in Hubei, toughner core shell rubbers epoxy resin MX-125: Japanese clock deep 17g, thinner C
12-14alkyl glycidyl ether ED-502S: Japanese ADEKA 5g, coupling agent KH-550 0.8g, dispersant B YK-9076 0.5g, defoamer BYK-A530 1g, black color: Poly one 1g, drops in reactor, is uniformly mixed; Add 10 um ball-shaped silicon micro powders again: the handsome that 35 grams in Wuhan, divide and add for three times, add latent curative PN40 subsequently: Japanese aginomoto 15 g, temperature 25 DEG C, mixes under cooling drying condition, and cold water controls at 15 DEG C, mix three times, vacuum tightness-0.08 MPa ~-0.05MPa, stirs 1 ~ 2 hour, gets product.
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| JP6489274B1 (en) | 2018-08-10 | 2019-03-27 | 千住金属工業株式会社 | Flux composition, solder paste, solder joint and solder joint method |
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| CN110128982B (en) * | 2019-04-01 | 2021-07-06 | 矽时代材料科技股份有限公司 | Normal-temperature fast-curing structural adhesive and preparation method thereof |
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| CN114214017B (en) * | 2021-11-29 | 2023-05-23 | 烟台德邦科技股份有限公司 | Bio-based epoxy underfill with high Tg and excellent thermal stability and preparation method thereof |
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