CN102010686B - Double-solidification system fast-flowing underfill and preparation method thereof - Google Patents
Double-solidification system fast-flowing underfill and preparation method thereof Download PDFInfo
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- CN102010686B CN102010686B CN 201010297440 CN201010297440A CN102010686B CN 102010686 B CN102010686 B CN 102010686B CN 201010297440 CN201010297440 CN 201010297440 CN 201010297440 A CN201010297440 A CN 201010297440A CN 102010686 B CN102010686 B CN 102010686B
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- 238000007711 solidification Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000003822 epoxy resin Substances 0.000 claims abstract description 31
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 31
- 239000003999 initiator Substances 0.000 claims abstract description 16
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 125000002091 cationic group Chemical group 0.000 claims abstract description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229920005862 polyol Polymers 0.000 claims abstract description 6
- 150000003077 polyols Chemical class 0.000 claims abstract description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 17
- -1 phenol aldehyde Chemical class 0.000 claims description 17
- 229920005989 resin Polymers 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 14
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 11
- 239000004593 Epoxy Substances 0.000 claims description 8
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- 229930185605 Bisphenol Natural products 0.000 claims description 5
- 235000011037 adipic acid Nutrition 0.000 claims description 5
- 239000001361 adipic acid Substances 0.000 claims description 5
- WNLRTRBMVRJNCN-UHFFFAOYSA-N hexanedioic acid Natural products OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims description 4
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 4
- 229920001610 polycaprolactone Polymers 0.000 claims description 4
- 239000004632 polycaprolactone Substances 0.000 claims description 4
- 229920005906 polyester polyol Polymers 0.000 claims description 4
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract 2
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 abstract 2
- 238000012360 testing method Methods 0.000 description 16
- 239000000047 product Substances 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 150000005839 radical cations Chemical class 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 150000002118 epoxides Chemical group 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- VNSAGKHMOVSDFB-UHFFFAOYSA-N [O-][NH+](C1CC2OC2CC1)OCC1CC2OC2CC1 Chemical compound [O-][NH+](C1CC2OC2CC1)OCC1CC2OC2CC1 VNSAGKHMOVSDFB-UHFFFAOYSA-N 0.000 description 1
- 150000001279 adipic acids Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006059 cover glass Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Epoxy Resins (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a double-solidification system fast-flowing underfill and a preparation method thereof. The underfill comprises the following raw materials in parts by weight: 30-80% of epoxy resin, 10-50% of epoxy acrylate, 5-30% of acrylate, 2-20% of polyol, 1-20% of silane coupling agent, 0.3-4% of cationic initiator, 0.1-3% of radical initiator and 0.1-0.5% of carbon black; and the preparation method comprises the following steps of: weighing the epoxy resin and the cationic initiator in the proportion, putting in a reaction kettle and stirring into a uniform solution; weighing the epoxy acrylate, the acrylate, the polyol, the silane coupling agent, the radical initiator and the carbon black in the proportion, putting in the reaction kettle in sequence, mixing and stirring to obtain the finished product of the double-solidification system fast-flowing underfill.
Description
Technical field
The present invention relates to a kind of Double-solidification system fast-flowing underfill and preparation method thereof, be applicable to the encapsulation such as chip size packages (CSP), BGA Package (BGA) and fill with the bottom, belong to the 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, that volume is little, speed is fast, function is strong, good reliability etc. becomes electronic product.For the development that adapts to this trend has produced flip-chip technology.The main advantage of flip-chip comprises can reduce and save the space, also has in addition that interconnection vias is shorter and inductance is lower, high I/O density, does over again and the autoregistration ability.Concerning radiating management, the performance of flip-chip is also very outstanding.And underfill is high-density flip-chip BGA, and CSP reaches one of crucial electronic material required in the SIP microelectronics Packaging; its Main Function is protection high-density soldered ball node and chip; and BGA, processibility, reliability and the life-time service of CSP and SIP device have been guaranteed.
The underfill of cationic system has lot of advantages, and the rear smell of, curing low such as shrinking percentage is little etc.But also there are some defectives simultaneously, because the consistency of glue and some soldering flux is not good enough, the phenomenon that may cause part glue not solidify.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of radical cation Double-solidification system fast-flowing underfill and preparation method thereof is provided, do not solidify to avoid running into some soldering flux, the purpose of the characteristics such as reach good stability, can keep in repair.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of radical cation Double-solidification system fast-flowing underfill is comprised of each raw material of following weight percent: Resins, epoxy 30～80%, acrylic acid epoxy resin 10～50%, acrylate 5～30%, polyvalent alcohol 2～20%, silane coupling agent 1～20%, cationic initiator 0.3～4%, radical initiator 0.1～3%, carbon black 0.1～0.5%.
The invention has the beneficial effects as follows: Double-solidification system fast-flowing underfill of the present invention, shrinking percentage is low, has effectively guaranteed the reliability of encapsulation components and parts; Smell is little after solidifying, and has complied with the trend of environmental protection; Velocity of flow is fast, adapts to the requirement of high density packing; Middle temperature fast setting meets high efficiency beat in the modern production; Stability in storage is good, can keep in repair, and is applied widely.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described Resins, epoxy is a kind of or any several mixture in cycloaliphatic epoxy resin, bisphenol A type epoxy resin, bisphenol f type epoxy resin and the phenol aldehyde type epoxy resin.
Adopt the beneficial effect of above-mentioned further scheme to be, select dissimilar Resins, epoxy to cooperate, can be so that curing speed, cohesive strength etc. reach a trim point, excellent combination property.
Further, described cycloaliphatic epoxy resin is 3,4-epoxycyclohexyl methyl-3,4-epoxycyclohexyl manthanoate and two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester; Described 3,4-epoxycyclohexyl methyl-3, the structural formula of 4-epoxycyclohexyl manthanoate is:
The structural formula of described two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid esters is:
Further, the structural formula of described bisphenol A type epoxy resin is represented by following formula I:
Wherein, n=0～19.
Further, the structural formula of described bisphenol f type epoxy resin is represented by following general formula II:
Wherein, n=0～1.
Further, the structural formula of described phenol aldehyde type epoxy resin is represented by following general formula III:
Wherein, n=1～3.
Further, described acrylic acid epoxy resin is that an end of molecular chain is two keys, and the other end is epoxide group, i.e. the cationically polymerizable resin of free redical polymerization again, and its structural formula is represented by following general formula IV:
Adopt the beneficial effect of above-mentioned further scheme to be, acrylic acid epoxy resin is the bridge of positively charged ion, free radical two individual system combinations, so that the mutual supplement with each other's advantages of two individual system, obtains a kind of have fast, the middle temperature fast setting of velocity of flow, filling glue that reliability is high.
Further, described acrylate is a kind of or any several mixture in butyl acrylate, Isooctyl acrylate monomer, the lauryl methacrylate(LMA).
Further, described polyvalent alcohol is a kind of or any several mixture in polyester polyol, polyether glycol, polycaprolactone polyol, the BDO.
Adopt the beneficial effect of above-mentioned further scheme to be, the curing speed that the adding of polyalcohols namely can regulation system, toughness and any surface finish planeness that can regulate again cured article.
Further, described silane coupling agent is a kind of or any several mixture in β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-glycidoxypropyltrimewasxysilane, γ mercaptopropyitrimethoxy silane, the γ-aminopropyl triethoxysilane.
Adopt the beneficial effect of above-mentioned further scheme to be, silane coupling agent is conducive to improve fills glue to the wettability of base material, improves liquidity.
Further, described cationic initiator is hexafluoro antimonate.
Further, described radical initiator is a kind of or any several mixture in benzoyl peroxide, Diisopropyl azodicarboxylate, di-tert-butyl peroxide, the peroxidation-2-ethyl acid tert-butyl ester.
Another technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of radical cation Double-solidification system fast-flowing underfill, comprise by following weight percent and take by weighing Resins, epoxy 30～80%, cationic initiator 0.3～4%, it is dropped in the reactor, mixed 30 minutes at 30～35 ℃, make it dissolving and become uniform solution, and then take by weighing acrylic acid epoxy resin 10～50%, acrylate 5～30%, polyvalent alcohol 2～20%, silane coupling agent 1～20%, radical initiator 0.1～3% and carbon black 0.1～0.5%, add successively in the reactor, in 15～20 ℃ of temperature, vacuum tightness-0.08～-0.05MPa, 500～1000 rev/mins of rotating speeds, mix 1～2 hour, namely get product.
Embodiment
Below principle of the present invention and feature are described, institute only gives an actual example and to be used for explanation the present invention, is not be used to limiting scope of the present invention.
Embodiment 1
Accurately take by weighing following various raw material, 3,4-epoxycyclohexyl methyl-3,4-epoxycyclohexyl manthanoate 40g, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester 40g, hexafluoro antimonate are that the Super XC-7231 0.5g of U.S. King company drops in the reactor, mixed 30 minutes at 30 ℃, make it dissolving and become uniform solution, then add acrylic acid epoxy resin 10g, butyl acrylate 5g, 1,4-butyleneglycol 3g, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane 1g, benzoyl peroxide 0.3g, carbon black 0.2g.The control temperature is at 15 ℃, and vacuum tightness be-0.05MPa, and revolution is 500 rev/mins, and vacuum stirring mixing 2 hours obtains the homogeneous product.
Embodiment 2
Accurately take by weighing following various raw material, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester 50g, bisphenol A type epoxy resin 20g, hexafluoro antimonate is that the K-PURE CXC-1612 3g of U.S. king company drops in the reactor, mixed 30 minutes at 35 ℃, making it dissolving becomes uniform solution, then adds acrylic acid epoxy resin 10g, Isooctyl acrylate monomer 8g, polycaprolactone polyol 6.5g, γ-glycidoxypropyltrimewasxysilane 2g, Diisopropyl azodicarboxylate 0.3g, carbon black 0.2g; The control temperature is at 15 ℃, and vacuum tightness be-0.05MPa, and revolution is 1000 rev/mins, and vacuum stirring mixing 2 hours obtains the homogeneous product.
Wherein, the structural formula of described bisphenol A type epoxy resin is:
N is the mixture of 0,1,2～18,19 compounds that form.
Embodiment 3
Accurately take by weighing following various raw material, two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester 30g, hexafluoro antimonate is that the K-PURE CXC-1612 1g of U.S. king company drops in the reactor, mixed 30 minutes at 30 ℃, making it dissolving becomes uniform solution, then adds acrylic acid epoxy resin 15g, lauryl methacrylate(LMA) 30g, polyester polyol 20g, γ mercaptopropyitrimethoxy silane 3g, di-tert-butyl peroxide 0.5g, carbon black 0.5g; The control temperature is at 15 ℃, and vacuum tightness be-0.07MPa, and revolution is 700 rev/mins, and vacuum stirring mixing 2 hours obtains the homogeneous product.
Embodiment 4
Accurately take by weighing following various raw material, 3,4-epoxycyclohexyl methyl-3,4-epoxycyclohexyl manthanoate 50g, phenol aldehyde type epoxy resin 15g, hexafluoro antimonate is that the Super XC-7231 2g of U.S. King company drops in the reactor, mixed 30 minutes at 35 ℃, making it dissolving becomes uniform solution, then adds acrylic acid epoxy resin 15g, butyl acrylate 5g, polyester polyol 9.5g, γ-aminopropyl triethoxysilane 3g, peroxidation-2-ethyl acid tert-butyl ester 0.3g, carbon black 0.2g; The control temperature is at 15 ℃, and vacuum tightness be-0.07MPa, and revolution is 1000 rev/mins, and vacuum stirring mixing 2 hours obtains the homogeneous product.
Wherein, the structural formula of described phenol aldehyde type epoxy resin is:
N is the composition of 1,2 or 3 compounds that consist of.
Embodiment 5
Accurately take by weighing following various raw material, bisphenol A type epoxy resin 15g, bisphenol f type epoxy resin 15g, hexafluoro antimonate is that the Super XC-7231 4g of U.S. King company drops in the reactor, mixed 30 minutes at 30 ℃, make it dissolving and become uniform solution, then add acrylic acid epoxy resin 45g, lauryl methacrylate(LMA) 10g, polycaprolactone polyol 5g, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane 5g, benzoyl peroxide 0.5g, carbon black 0.5g; The control temperature is at 15 ℃, and vacuum tightness be-0.05MPa, and revolution is 1000 rev/mins, and vacuum stirring mixing 2 hours obtains the homogeneous product.
The comparative example 1
Common bottom is filled glue prescription-traditional curing mode, take by weighing resin 828EL 13.2g, resin 830LVP 39.2g, colorant 0.5g, solidifying agent fujicure fxr 1020 25g, promotor PN-H 5g, coupling agent KH5600.56g, epoxy active diluent AGE 20g toasts resin 830LVP one night under 70-75 ℃, then resin 828EL, resin 830LVP, color mixes, 30 minutes time, then 25 ℃ of temperature add solidifying agent, promotor, three-roller mixes, 25 ℃ of temperature, mix under the cooling drying condition, cold water is controlled at 15 ℃, mixes three times, mix and expire vacuum 15 minutes in the rear adding reactor, adding coupling agent after resin and solidifying agent mix, epoxide diluent mixes, and full vacuum 30 minutes obtains sample.
Concrete test example
The performance of the Double-solidification system fast-flowing underfill by following experimental test the above embodiment of the present invention 1-5 and comparative example.
The test of test example 1 curing performance
The DSC cure profile, 60 ℃/minute of temperature rise rates, 130 ℃ of curing of constant temperature.
The test of test example 2 flowing propertys
24mm * 24mm testing plate, cover glass and slide glass form, and the slit is 25 microns, the velocity of flow that (simulation packaged chip) is 25 ℃.
Test example 3 thermal expansivity tests (CTE)
The TMA test, 10 ℃/minute of temperature rise rates, the μ m/m of unit ℃
Test according to ASTM D696
The test of test example 4 shearing resistances
The AL/AL shearing resistance, 130 ℃ of conditions of cure, 2 hours.
Test according to GB/T7124-1986.
Test result is shown in following table 1.
The sample that table 1 embodiment 1-5 makes and comparative example's sample common bottom are filled colloidality and can be contrasted
Test result
Data from table 1 can find out that Double-solidification system fast-flowing underfill of the present invention all has a clear superiority at more traditional underfills in aspect such as curing speed, velocity of flow, thermal expansivity, shearing resistances; When having higher reliability, more be fit to the requirement of fast beat packaging process.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. Double-solidification system fast-flowing underfill, it is characterized in that, formed by each raw material of following weight percent: Resins, epoxy 30～80%, acrylic acid epoxy resin 10～50%, acrylate 5～30%, polyvalent alcohol 2～20%, silane coupling agent 1～20%, cationic initiator 0.3～4%, radical initiator 0.1～3%, carbon black 0.1～0.5%.
2. Double-solidification system fast-flowing underfill according to claim 1, it is characterized in that, described Resins, epoxy is a kind of or any several mixture in cycloaliphatic epoxy resin, bisphenol A type epoxy resin, bisphenol f type epoxy resin and the phenol aldehyde type epoxy resin.
3. Double-solidification system fast-flowing underfill according to claim 2, it is characterized in that, described cycloaliphatic epoxy resin is 3,4-epoxycyclohexyl methyl-3,4-epoxycyclohexyl manthanoate and two (7-oxabicyclo [4.1.0] 3-methyl in heptan) adipic acid ester.
4. Double-solidification system fast-flowing underfill according to claim 2 is characterized in that, the structural formula of described bisphenol A type epoxy resin is represented by following general formula I:
Wherein, n=0～19.
5. Double-solidification system fast-flowing underfill according to claim 2 is characterized in that, the structural formula of described bisphenol f type epoxy resin is represented by following general formula I I:
Wherein, n=0～1.
6. Double-solidification system fast-flowing underfill according to claim 2 is characterized in that, the structural formula of described phenol aldehyde type epoxy resin is represented by following general formula I II:
Wherein, n=1～3.
7. Double-solidification system fast-flowing underfill according to claim 1 is characterized in that, described acrylate is a kind of or any several mixture in butyl acrylate, Isooctyl acrylate monomer, the lauryl methacrylate(LMA); Described polyvalent alcohol is a kind of or any several mixture in polyester polyol, polyether glycol, polycaprolactone polyol, the BDO; Described silane coupling agent is a kind of or any several mixture in β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-glycidoxypropyltrimewasxysilane, γ mercaptopropyitrimethoxy silane, the γ-aminopropyl triethoxysilane.
8. Double-solidification system fast-flowing underfill according to claim 1 is characterized in that, described cationic initiator is hexafluoro antimonate; Described radical initiator is a kind of or any several mixture in benzoyl peroxide, Diisopropyl azodicarboxylate, di-tert-butyl peroxide, the peroxidation-2-ethyl acid tert-butyl ester.
9. the preparation method of a Double-solidification system fast-flowing underfill, it is characterized in that, described method comprises: take by weighing Resins, epoxy 30～80% by following weight percent, cationic initiator 0.3～4%, it is dropped in the reactor, mixed 30 minutes at 30～35 ℃, make it dissolving and become uniform solution, and then take by weighing acrylic acid epoxy resin 10～50%, acrylate 5～30%, polyvalent alcohol 2～20%, silane coupling agent 1～20%, radical initiator 0.1～3% and carbon black 0.1～0.5%, add successively in the reactor, in 15～20 ℃ of temperature, vacuum tightness-0.08～-0.05MPa, 500～1000 rev/mins of rotating speeds, mix 1～2 hour, namely get product.
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| US9783713B2 (en) | 2011-11-06 | 2017-10-10 | Henkel Ag & Co. Kgaa | Dual-curable adhesive composition, use thereof, and process for bonding substrates |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9783713B2 (en) | 2011-11-06 | 2017-10-10 | Henkel Ag & Co. Kgaa | Dual-curable adhesive composition, use thereof, and process for bonding substrates |
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