CN104962224A - Underfill adhesive and preparation method thereof - Google Patents
Underfill adhesive and preparation method thereof Download PDFInfo
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- CN104962224A CN104962224A CN201510392325.3A CN201510392325A CN104962224A CN 104962224 A CN104962224 A CN 104962224A CN 201510392325 A CN201510392325 A CN 201510392325A CN 104962224 A CN104962224 A CN 104962224A
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Abstract
The invention discloses underfill adhesive. The underfill adhesive comprises the following ingredients in parts by weight: 30 to 70 parts of filler, 10 to 50 parts of epoxy resin, 2 to 20 parts of curing agent, 0.1 to 0.5 part of catalyst, 1 to 15 parts of plasticizer, 1 to 25 parts of diluting agent, 0.1 to 3 parts of dispersing agent, 0.05 to 1 part of defoaming agent, 0.1 to 1 part of coupling agent and 0.1 to 0.5 part of pigment. Compared with traditional underfill adhesive, the underfill adhesive comprises 30 to 70 parts of filler, so that the thermal expansion coefficient is relatively low, the requirement of a flip chip on the low expansion coefficient of the underfill adhesive can be met, and an effect for protecting the flip chip can be realized. The invention also provides a preparation method of the underfill adhesive.
Description
Technical field
The present invention relates to sizing agent technical field, particularly relate to a kind of underfill and preparation method thereof.
Background technology
Flip-chip is a kind of chip interconnect and bonding technology, has been applied to high-end electronic device and high density integrated circuit encapsulation field at present.It effectively can shorten interconnection vias, increases I/O land counts and reduce chip size, realizes the frivolous microminiaturization of encapsulation, represents the final direction of chip encapsulation technology and high density packing.Underfill is as the critical material of Flip-Chip Using; can the highdensity soldered ball of available protecting; the stress of dispersed chip surface carrying; alleviate the internal stress that chip, solder and substrate three thermal expansivity do not mate generation simultaneously, increase the processibility of chip and packaging, reliability and work-ing life.
At present, the filler content of traditional underfill is all lower, to be difficult to meet in flip-chip the low-expansion requirement of underfill, not to have the packaging protection effect to flip-chip.
Summary of the invention
Based on this, be necessary the underfill providing a kind of thermal expansivity lower.
A kind of underfill, according to the mass fraction, comprises
The pigment of the filler of 30 parts ~ 70 parts, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts, the catalyzer of 0.1 part ~ 0.5 part, the toughner of 1 part ~ 15 parts, the thinner of 1 part ~ 25 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part;
Wherein, described filler is preparing spherical SiO 2, and the particle diameter of described filler is 50nm ~ 500nm.
Give in embodiment one, the finishing of described preparing spherical SiO 2 has at least one in amino, epoxy group(ing) and double bond.
Give in embodiment one, described epoxy resin is selected from hexanaphthene-1, 2-dicarboxylic acid 2-glycidyl ester, bisphenol A type epoxy resin E51, bisphenol A type epoxy resin E44, EPON 825 epoxy resin, bisphenol f type epoxy resin EPIKOTE 862, bisphenol-s epoxy resin, 3, 4-epoxycyclohexyl-methyl-3, 4-epoxycyclohexyl manthanoate, 3-Oxyranyle-7-oxabicyclo [4.1.0] heptane, two ((3, 4-epoxycyclohexyl) methyl) adipic acid ester, 3, 4-epoxycyclohexyl-methyl methacrylic ester, 4, 5-epoxy cyclohexane-1, 2-dioctyl phthalate 2-glycidyl ester, 1, 4-cyclohexanedimethanol two (3, 4-epoxy cyclohexane formic acid) ester, Ppolynuclear aromatic epoxy resin ICLON
@hP4700, Ppolynuclear aromatic epoxy resin ICLON
@hP4770, Ppolynuclear aromatic epoxy resin ICLON
@hP5000, Ppolynuclear aromatic epoxy resin ICLON
@hP4032 (D), phenol aldehyde type epoxy resin EPICLON@HP7200, novolac epoxy DEN 431, novolac epoxy DEN 438, novolac epoxy DEN 439 and 3,3, at least one in 5,5-tetramethyl biphenyl diphenol diglycidylether.
Give in embodiment one, described solidifying agent is selected from least one in alicyclic acid anhydride type curing agent, amine curing agent and phenolic solidifying agent.
Give in embodiment one, described alicyclic acid anhydride type curing agent is selected from least one in brown oil anhydride, tetrahydrophthalic anhydride, HHPA, methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride and Pyroglutaric acid;
Described amine curing agent is selected from least one in aromatic amine, aromatic amine derivant, polymeric amide and Dyhard RU 100;
Described phenolic solidifying agent is phenol formaldehyde resin.
Give in embodiment one, described catalyzer be selected from imidazoles, imdazole derivatives and microcapsule subsidence feed Zhi Shao ー kind.
7, underfill according to claim 6, it is characterized in that, described imdazole derivatives is selected from least one in 2-ethyl-4-methylimidazole, 2-undecyl imidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole and DMP-30;
Described microcapsule subsidence feed is selected from the production of Japanese Asahi Kasei Corporation
with
in at least one.
Give in embodiment one, described toughner is selected from phthalic acid dibutyl ester, dioctyl phthalate, liquid silastic, end is the paracril of hydroxyl, amino or carboxyl, end is the acrylonitrile butadiene rubber modified bisphenol A epoxide resin of hydroxyl, amino or carboxyl, end is the acrylonitrile butadiene rubber modified neopentylglycol diglycidyl ether epoxy resin diluent of hydroxyl, amino or carboxyl, thiorubber, polyamide resin, urethane, at least one in core-shell polymer and segmented copolymer.
Give in embodiment one, described liquid silastic is selected from least one in dimethyl silicone rubber, ethylene methacrylic silicon rubber and methyl phenyl vinyl silicon rubber;
Described core-shell polymer is selected from least one in the coated butyl polyacrylate of the coated butadiene-styrene copolymer of polymethylmethacrylate, polymethylmethacrylate and the coated polyhutadiene of Styrene-Acrylnitrile Copolymer;
Described segmented copolymer is selected from least one in methyl methacrylate one butyl acrylate monomethyl methyl acrylate segmented copolymer, styrene-butadiene one styrene block copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate segmented copolymer, acrylonitrile-butadiene-styrene copolymer and polyurethane modified acrylic resin-organo-silicone rubber multipolymer.
Give in embodiment one, described thinner is reactive thinner.
Give in embodiment one, described reactive thinner is selected from butylglycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, lauryl diglycidyl ether, p-cresol glycidyl ether, neopentylglycol diglycidyl ether, 1, at least one in 4-butanediol diglycidyl ether, ethylene glycol diglycidylether, polypropylene glycol diglycidyl ether, 1,6-hexanediol diglycidyl ether, glycidyl allyl ether and glycidyl methacrylate.
Give in embodiment one, described dispersion agent is selected from least one in BYK-9010, BYK-995, BYK-306, BYK-2008 and BYK-2009 of Bi Ke chemical production.
Give in embodiment one, described defoamer is selected from least one in polysiloxane defoamer and acryl-based antifoaming agent.
Give in embodiment one, described polysiloxane defoamer is selected from least one in BYK-320, BYK-322 and BYK-323 of Bi Ke chemical production;
Described acryl-based antifoaming agent is selected from least one in BYK-352, BYK-354, BYK-359 and BYK-392 of Bi Ke chemical production.
Give in embodiment one, described coupling agent is selected from least one in organo-silicon coupling agent, organotitanate coupling agent, organic aluminates coupling agent and organozirconates coupling agent.
Give in embodiment one, described organo-silicon coupling agent is selected from least one in γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-mercaptopropyl trimethoxysilane, octadecyl trimethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane and vinyltriethoxysilane;
Described organotitanate coupling agent is selected from least one in three Unimac 5680 isopropyl titanates, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, organic aluminates coupling agent aluminium isopropoxide, isopropoxy distearyl acid acyloxy Aluminate;
Described organic aluminates coupling agent is selected from least one in aluminium isopropoxide and isopropoxy distearyl acid acyloxy Aluminate;
Described organozirconates coupling agent is selected from least one in alkoxyl group three (vinyl-oxyethyl group) zirconate and alkoxyl group three (p-aminophenyl oxygen base) zirconate.
A preparation method for above-mentioned underfill, comprises the steps:
By mass fraction, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts and the toughner of 1 part ~ 15 parts are mixed, obtain the first mixture;
Add in described first mixture by the pigment of mass fraction by the filler of 30 parts ~ 70 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part, mix, obtain the second mixture; And
By mass fraction, the thinner of the catalyzer of 0.1 part ~ 0.5 part and 1 part ~ 25 parts is added in described second mixture, mix, vacuum defoamation, obtain described underfill, wherein, described underfill according to the mass fraction, comprise the filler of 30 parts ~ 70 parts, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts, the catalyzer of 0.1 part ~ 0.5 part, the toughner of 1 part ~ 15 parts, the thinner of 1 part ~ 25 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the pigment of the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part, described filler is preparing spherical SiO 2, the particle diameter of described filler is 50nm ~ 500nm.
Give in embodiment one, described epoxy resin, solidifying agent and toughner to be mixed, obtain in the step of the first mixture, described in time of mixing be 5min ~ 30min;
Described filler, dispersion agent, defoamer, coupling agent and pigment to be added in described first mixture, mix, obtain in the step of the second mixture, described in time of mixing be 5min ~ 30min;
Described catalyzer and thinner to be added in described second mixture, mix, vacuum defoamation, obtain in the step of described underfill, described in time of mixing be 1min ~ 10min, the time of described vacuum defoamation is 5min ~ 30min.
Compared with traditional underfill; containing the filler of 30 parts ~ 70 parts in this underfill; make the thermal expansivity of this underfill lower, thus can to meet in flip-chip the low-expansion requirement of underfill, play the packaging protection effect to flip-chip.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the underfill of an embodiment.
Embodiment
Mainly in conjunction with the drawings and the specific embodiments underfill and preparation method thereof is described in further detail below.
A kind of underfill of embodiment, according to the mass fraction, the pigment of the filler of 30 parts ~ 70 parts, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts, the catalyzer of 0.1 part ~ 0.5 part, the toughner of 1 part ~ 15 parts, the thinner of 1 part ~ 25 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part is comprised.
The preparing spherical SiO 2 of Fillers selection high-quality, preparing spherical SiO 2 is of a size of 50nm ~ 500nm, the foreign ion Na of preparing spherical SiO 2
+, Cl
-ion content is less than 0.1ppm, spherical silica particle smooth surface, soilless sticking.
Filler in this underfill is high-quality, undersized spherical silica, particle size is little, be conducive to the applying glue at high-density thin space flip-chip underfill, avoid particle size large, block at filling process and fill the appearance of hole, when especially the thin space of the flip-chip spacing in the semiconductor technology processing procedure of below 20nm below 25 μm being filled, there is irreplaceable advantage.Compared with traditional underfill; containing the filler of 30 parts ~ 70 parts in this underfill; the thermal expansivity of this underfill is lower, thus can to meet in flip-chip the low-expansion requirement of underfill, plays the packaging protection effect to flip-chip.
In addition, the impurity ion content in spherical silica particle is low, effectively can improve the work-ing life of institute's protection soldered ball.
Preferably, the finishing of preparing spherical SiO 2 has at least one in amino, epoxy group(ing) and double bond.The dispersiveness of silica dioxide granule in underfill and the mobility of raising glue-applying technique process then effectively can improve in the functional group such as amino, epoxy group(ing), double bond that the surface of preparing spherical SiO 2 is contained.
Finishing has the preparation process of the preparing spherical SiO 2 of at least one in amino, epoxy group(ing) and double bond to be: adopt silane coupling agent containing at least one in amino, epoxy group(ing) and double bond in alcohol-water mixed solvent organic solvents such as (or) toluene, through the surface of hydrolytic condensation chemical graft at preparing spherical SiO 2, thus prepare the preparing spherical SiO 2 that finishing has at least one in amino, epoxy group(ing) and double bond.
Epoxy resin is selected from hexanaphthene-1, 2-dicarboxylic acid 2-glycidyl ester, bisphenol A type epoxy resin E51, bisphenol A type epoxy resin E44, EPON 825 epoxy resin, bisphenol f type epoxy resin EPIKOTE 862, bisphenol-s epoxy resin (185S, U.S. Compton), 3, 4-epoxycyclohexyl-methyl-3, 4-epoxycyclohexyl manthanoate, 3-Oxyranyle-7-oxabicyclo [4.1.0] heptane, two ((3, 4-epoxycyclohexyl) methyl) adipic acid ester, 3, 4-epoxycyclohexyl-methyl methacrylic ester, 4, 5-epoxy cyclohexane-1, 2-dioctyl phthalate 2-glycidyl ester, 1, 4-cyclohexanedimethanol two (3, 4-epoxy cyclohexane formic acid) ester, Ppolynuclear aromatic epoxy resin ICLON
@hP4700, Ppolynuclear aromatic epoxy resin ICLON
@hP4770, Ppolynuclear aromatic epoxy resin ICLON
@hP5000, Ppolynuclear aromatic epoxy resin ICLON
@hP4032 (D), phenol aldehyde type epoxy resin EPICLON@HP7200, novolac epoxy DEN 431, novolac epoxy DEN 438, novolac epoxy DEN 439 and 3,3, at least one in 5,5-tetramethyl biphenyl diphenol diglycidylether.Use hybrid resin to be conducive to reducing the viscosity of resin matrix, farthest can improve loading level thus reduce thermal expansivity.Use the curing process and thermomechanical property and cohesive strength that underfill while of blending epoxy, can be improved in addition.
Solidifying agent is selected from least one in alicyclic acid anhydride type curing agent, amine curing agent and phenolic solidifying agent.
Alicyclic acid anhydride type curing agent is selected from least one in brown oil anhydride, tetrahydrophthalic anhydride, HHPA, methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride and Pyroglutaric acid.
Amine curing agent is selected from least one in aromatic amine, aromatic amine derivant, polymeric amide and Dyhard RU 100.
Phenolic solidifying agent is phenol formaldehyde resin.
Catalyzer be selected from imidazoles, imdazole derivatives and microcapsule subsidence feed Zhi Shao ー kind.
Imdazole derivatives is selected from least one in 2-ethyl-4-methylimidazole, 2-undecyl imidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole and DMP-30.
Microcapsule subsidence feed is selected from the production of Japanese Asahi Kasei Corporation
with
in at least one.The use of Latence catalyst effectively can slow down the growth of system viscosity, extends shelf lives and the working life of underfill, has greatly widened technological operation window.
Toughner is selected from phthalic acid dibutyl ester, dioctyl phthalate, liquid silastic, end is the paracril of hydroxyl, amino or carboxyl, and end is the acrylonitrile butadiene rubber modified bisphenol A epoxide resin of hydroxyl, amino or carboxyl, and end is the acrylonitrile butadiene rubber modified neopentylglycol diglycidyl ether epoxy resin diluent of hydroxyl, amino or carboxyl, thiorubber, polyamide resin, urethane, at least one in core-shell polymer and segmented copolymer.Use toughner effectively can improve the toughness of underfill, effectively can absorb the thermal and mechanical stress and extraneous additional mechanical shock stress that self produce, avoid cracking and the layering of underfill, improve the reliability of device.
Concrete, liquid silicon rubber can be selected from least one in dimethyl silicone rubber, ethylene methacrylic silicon rubber and methyl phenyl vinyl silicon rubber by glue; Core-shell polymer can be selected from least one in the coated butyl polyacrylate of the coated butadiene-styrene copolymer of polymethylmethacrylate, polymethylmethacrylate and the coated polyhutadiene of Styrene-Acrylnitrile Copolymer; Segmented copolymer can be selected from least one in methyl methacrylate one butyl acrylate monomethyl methyl acrylate segmented copolymer, styrene-butadiene one styrene block copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate segmented copolymer, acrylonitrile-butadiene-styrene copolymer and polyurethane modified acrylic resin-organo-silicone rubber multipolymer.
Thinner is reactive thinner.Concrete, reactive thinner is selected from butylglycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, lauryl diglycidyl ether, p-cresol glycidyl ether, neopentylglycol diglycidyl ether, 1, at least one in 4-butanediol diglycidyl ether, ethylene glycol diglycidylether, polypropylene glycol diglycidyl ether, 1,6-hexanediol diglycidyl ether, glycidyl allyl ether and glycidyl methacrylate.The use of reactive thinner not only effectively can reduce the viscosity of system, and they can participate in the curing reaction of epoxy resin directly, become a part for epoxy resin cured product cross-linked network structure, effectively improves the physical strength of cured product.
Dispersion agent is selected from least one in BYK-9010, BYK-995, BYK-306, BYK-2008 and BYK-2009 of Bi Ke chemical production.The use of dispersion agent effectively can improve the dispersiveness of described filler in resin matrix and reduces the reunion of filler thus reduce the viscosity of system, dispersion agent can improve the wetting and spreading of resin matrix at filling surface in addition, prevents filler from reassembling in system and sedimentation thus improve the stability of glue.
Defoamer is selected from least one in polysiloxane defoamer and acryl-based antifoaming agent.Defoamer effectively can reduce the probability producing bubble and cavity in glue preparation and use procedure, improves the reliability of device.
Concrete, polysiloxane defoamer can be selected from least one in BYK-320, BYK-322 and BYK-323 of Bi Ke chemical production; Acryl-based antifoaming agent can be selected from least one in BYK-352, BYK-354, BYK-359 and BYK-392 of Bi Ke chemical production.
Coupling agent is selected from least one in organo-silicon coupling agent, organotitanate coupling agent, organic aluminates coupling agent and organozirconates coupling agent.Have in coupling agent molecule simultaneously can and the chemically combined reactive group of inanimate matter material and with organic material (synthetic resins etc.) chemically combined reactive group, therefore their use not only can improve the dispersiveness of mineral filler in organic matrix and consistency, the viscosity of reduction system, can strengthen again glue cohesive strength on different substrates simultaneously.
Organo-silicon coupling agent is selected from least one in γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-mercaptopropyl trimethoxysilane, octadecyl trimethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane and vinyltriethoxysilane.
Organotitanate coupling agent is selected from least one in three Unimac 5680 isopropyl titanates, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, organic aluminates coupling agent aluminium isopropoxide, isopropoxy distearyl acid acyloxy Aluminate.
Organic aluminates coupling agent is selected from least one in aluminium isopropoxide and isopropoxy distearyl acid acyloxy Aluminate.
Organozirconates coupling agent is selected from least one in alkoxyl group three (vinyl-oxyethyl group) zirconate and alkoxyl group three (p-aminophenyl oxygen base) zirconate.
Pigment optimization is the mineral dye carbon black of black and glaucous organic pigment phthalocyanine pigment.
Compared with traditional underfill; containing the filler of 30 parts ~ 70 parts in this underfill; make the thermal expansivity of this underfill lower, thus can to meet in flip-chip the low-expansion requirement of underfill, play the packaging protection effect to flip-chip.
In addition, owing to have employed said components formula, compared with traditional underfill, this underfill has low viscosity, and low thermal coefficient of expansion, cohesive strength are high, and the shelf lives stablizes, can fast setting, advantage that heat-resisting impact resistance is good.
The preparation method of above-mentioned underfill as shown in Figure 1, comprises the steps:
S10, by mass fraction, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts and the toughner of 1 part ~ 15 parts to be mixed, obtain the first mixture.
By mass fraction the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts and the toughner of 1 part ~ 15 parts added in high speed shear mixing tank and mix, obtain the first mixture.
Preferably, the time mixed is 5min ~ 30min.
S20, by mass fraction the pigment of the filler of 30 parts ~ 70 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part to be added in the first mixture that S10 obtains, mix, obtain the second mixture.
The pigment of the filler of 30 parts ~ 70 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part dropped into during above-mentioned batch mixing fills with by mass fraction, mix, obtain the second mixture.
Preferably, the time mixed is 5min ~ 30min.
S30, by mass fraction the thinner of the catalyzer of 0.1 part ~ 0.5 part and 1 part ~ 25 parts to be added in the second mixture that S20 obtains, mix, vacuum defoamation, obtain underfill.
Drop in the filling of above-mentioned batch mixing by the thinner of mass fraction by the catalyzer of 0.1 part ~ 0.5 part and 1 part ~ 25 parts, mix, vacuum defoamation, obtain underfill.
The underfill obtained according to the mass fraction, comprises the pigment of the filler of 30 parts ~ 70 parts, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts, the catalyzer of 0.1 part ~ 0.5 part, the toughner of 1 part ~ 15 parts, the thinner of 1 part ~ 25 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part.
Wherein, filler is preparing spherical SiO 2, and the particle diameter of filler is 50nm ~ 500nm.
Preferably, the time mixed is 1min ~ 10min, and the time of vacuum defoamation is 5min ~ 30min.
The preparation method of above-mentioned underfill, technique is simple, can prepare the low and underfill that reliability is high of good heat conductivity, the coefficient of expansion.
Be specific embodiment below.In following embodiment, the viscosity of obtained underfill is obtained by Austrian Anton Paar MCR 302 test, modulus is for obtaining by U.S. TA dynamic thermomechanical analysis apparatus DMAQ800 test, and thermal expansivity is obtained by the resistance to Model of the speeding 402F1 thermomechanical analyzer test of Germany.
Embodiment 1
Take bisphenol A type epoxy resin E51 15g, methyl hexahydrophthalic anhydride 10g, methyl methacrylate one butyl acrylate monomethyl methyl acrylate segmented copolymer 1g mixes 10min in high speed shear reactor, then adding particle diameter is the spherical SiO that the finishing of 400nm has epoxy-functional
2filler 63.05g, BYK W9010 0.1g, defoamer BYK-320 0.05g, γ-aminopropyl triethoxysilane and each 0.1g of γ-methacryloxypropyl trimethoxy silane, pigment 0.5g, drop in reactor and mix 10min.And then Latence catalyst is added
0.1g, thinner butylglycidyl ether 10g, drop in reactor and mix, vacuum defoamation, obtains required underfill.
The viscosity recording the underfill that the present embodiment obtains is 25PaS, and modulus is 7Gpa, Tg is 130 DEG C, thermal expansivity CTE1:30ppm/K, CTE2:90ppm/K.
Embodiment 2
Take bisphenol A type epoxy resin E51 10g, tetrahydrophthalic anhydride 10g, phthalic acid dibutyl ester 1g mixes 10min in high speed shear reactor, then add the spherical SiO that particle diameter is 500nm
2filler 68.05g, BYK W9010 0.1g, defoamer BYK-322 0.05g, γ-aminopropyl triethoxysilane 0.2g, pigment 0.5g, drop in reactor and mix 10min.And then Latence catalyst is added
0.1g, thinner butylglycidyl ether 10g, drop in reactor and mix, vacuum defoamation, obtains required underfill.
The viscosity recording the underfill that the present embodiment obtains is 30PaS, and modulus is 7Gpa, Tg is 140 DEG C, thermal expansivity CTE1:35ppm/K, CTE2:95ppm/K.
Embodiment 3
Take bisphenol f type epoxy resin EPIKOTE 862 20g, cycloaliphatic epoxy resin 3,4-epoxycyclohexyl-methyl 3,4-epoxycyclohexyl manthanoate 10g, diaminodiphenyl-methane 8g, polyurethane modified acrylic resin-organo-silicone rubber multipolymer 2g mixes 15min in high speed shear reactor, then adds the spherical SiO that particle diameter is 200nm
2filler 53.4g, BYK 306 0.2g, defoamer BYK-323 0.10g, γ-methacryloxypropyl trimethoxy silane 0.2g, pigment 1g, drop in reactor and mix 10min.And then Latence catalyst is added
0.1g, ethylene glycol diglycidylether 5g, drop in reactor and mix, vacuum defoamation, obtains required underfill.
The viscosity recording the underfill that the present embodiment obtains is 20PaS, and modulus is 5.5Gpa, Tg is 150 DEG C, thermal expansivity CTE1:40ppm/K, CTE2:100ppm/K.
Embodiment 4
Take bisphenol A type epoxy resin E54 15g, Ppolynuclear aromatic epoxy resin ICLON
@hP470015g, Dyhard RU 100 8g, nucleocapsid structure toughner 1.2g mix 15min in high speed shear reactor, then add the spherical SiO that particle diameter is 300nm
2filler 56.25g, BYK-2009 0.2g, defoamer BYK-3520.05g, three Unimac 5680 isopropyl titanate 0.2g, pigment 1g, drop in reactor and mix 10min.And then add catalyzer 2-phenyl-4-methylimidazole 0.1g, glycidyl allyl ether 3g, drop in reactor and mix, vacuum defoamation, obtains required underfill.
The viscosity recording the underfill that the present embodiment obtains is 20PaS, and modulus is 5.5Gpa, Tg is 150 DEG C, thermal expansivity CTE1:40ppm/K, CTE2:100ppm/K.
Embodiment 5
Take bisphenol A type epoxy resin E5112g, Ppolynuclear aromatic epoxy resin ICLON
@epoxy resin 3,3,5, the 5-tetramethyl biphenyl diphenol diglycidylether 10g of HP477015g, biphenyl structural, polymeric amide 10g, nbr carboxyl terminal 1.5g mix 15min in high speed shear reactor, then add the spherical SiO that particle diameter is 50nm
2filler 46.9g, BYK-2009 0.2g, defoamer BYK-354 0.10g, organozirconates coupling agent alkoxyl group three (vinyl-oxyethyl group) zirconate 0.2g, pigment 1g, drop in reactor and mix 10min.And then add catalyzer 2-ethyl-4-methylimidazole 0.1g, BDDE 3g, drop in reactor and mix, vacuum defoamation, obtains required underfill.
The viscosity recording the underfill that the present embodiment obtains is 20PaS, and modulus is 5.0Gpa, Tg is 150 DEG C, thermal expansivity CTE1:45ppm/K, CTE2:110ppm/K.
Embodiment 6
Take bisphenol A type epoxy resin E44 10g, phenol aldehyde type epoxy resin EPICLON@HP7200 10g, phenol formaldehyde resin 20g, liquid silastic 1.5g mix 15min in high speed shear reactor, then add the spherical SiO that particle diameter is 500nm
2filler 52.1g, BYK-995 0.1g, defoamer BYK-359 0.1g, γ-glycidyl ether oxygen propyl trimethoxy silicane 0.1g, pigment 1g, drop in reactor and mix 10min.And then add catalyzer 2-ethyl-4-methylimidazole 0.1g, neopentylglycol diglycidyl ether 5g, drop in reactor and mix, vacuum defoamation, obtains required underfill.
The viscosity recording the underfill that the present embodiment obtains is 40PaS, and modulus is 5.0Gpa, Tg is 120 DEG C, thermal expansivity CTE1:35ppm/K, CTE2:90ppm/K.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (18)
1. a underfill, is characterized in that, according to the mass fraction, comprises
The pigment of the filler of 30 parts ~ 70 parts, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts, the catalyzer of 0.1 part ~ 0.5 part, the toughner of 1 part ~ 15 parts, the thinner of 1 part ~ 25 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part;
Wherein, described filler is preparing spherical SiO 2, and the particle diameter of described filler is 50nm ~ 500nm.
2. underfill according to claim 1, is characterized in that, the finishing of described preparing spherical SiO 2 has at least one in amino, epoxy group(ing) and double bond.
3. underfill according to claim 1, it is characterized in that, described epoxy resin is selected from hexanaphthene-1, 2-dicarboxylic acid 2-glycidyl ester, bisphenol A type epoxy resin E51, bisphenol A type epoxy resin E44, EPON 825 epoxy resin, bisphenol f type epoxy resin EPIKOTE 862, bisphenol-s epoxy resin, 3, 4-epoxycyclohexyl-methyl-3, 4-epoxycyclohexyl manthanoate, 3-Oxyranyle-7-oxabicyclo [4.1.0] heptane, two ((3, 4-epoxycyclohexyl) methyl) adipic acid ester, 3, 4-epoxycyclohexyl-methyl methacrylic ester, 4, 5-epoxy cyclohexane-1, 2-dioctyl phthalate 2-glycidyl ester, 1, 4-cyclohexanedimethanol two (3, 4-epoxy cyclohexane formic acid) ester, Ppolynuclear aromatic epoxy resin
ppolynuclear aromatic epoxy resin
ppolynuclear aromatic epoxy resin
ppolynuclear aromatic epoxy resin
at least one in phenol aldehyde type epoxy resin EPICLON@HP7200, novolac epoxy DEN 431, novolac epoxy DEN 438, novolac epoxy DEN 439 and 3,3,5,5-tetramethyl biphenyl diphenol diglycidylether.
4. underfill according to claim 1, is characterized in that, described solidifying agent is selected from least one in alicyclic acid anhydride type curing agent, amine curing agent and phenolic solidifying agent.
5. underfill according to claim 4, is characterized in that, described alicyclic acid anhydride type curing agent is selected from least one in brown oil anhydride, tetrahydrophthalic anhydride, HHPA, methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride and Pyroglutaric acid;
Described amine curing agent is selected from least one in aromatic amine, aromatic amine derivant, polymeric amide and Dyhard RU 100;
Described phenolic solidifying agent is phenol formaldehyde resin.
6. underfill according to claim 1, is characterized in that, described catalyzer be selected from imidazoles, imdazole derivatives and microcapsule subsidence feed Zhi Shao ー kind.
7. underfill according to claim 6, it is characterized in that, described imdazole derivatives is selected from least one in 2-ethyl-4-methylimidazole, 2-undecyl imidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole and DMP-30;
Described microcapsule subsidence feed is selected from the production of Japanese Asahi Kasei Corporation
with
in at least one.
8. underfill according to claim 1, it is characterized in that, described toughner is selected from phthalic acid dibutyl ester, dioctyl phthalate, liquid silastic, end is the paracril of hydroxyl, amino or carboxyl, end is the acrylonitrile butadiene rubber modified bisphenol A epoxide resin of hydroxyl, amino or carboxyl, end is the acrylonitrile butadiene rubber modified neopentylglycol diglycidyl ether epoxy resin diluent of hydroxyl, amino or carboxyl, thiorubber, polyamide resin, urethane, at least one in core-shell polymer and segmented copolymer.
9. underfill according to claim 8, is characterized in that, described liquid silastic is selected from least one in dimethyl silicone rubber, ethylene methacrylic silicon rubber and methyl phenyl vinyl silicon rubber;
Described core-shell polymer is selected from least one in the coated butyl polyacrylate of the coated butadiene-styrene copolymer of polymethylmethacrylate, polymethylmethacrylate and the coated polyhutadiene of Styrene-Acrylnitrile Copolymer;
Described segmented copolymer is selected from least one in methyl methacrylate one butyl acrylate monomethyl methyl acrylate segmented copolymer, styrene-butadiene one styrene block copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate segmented copolymer, acrylonitrile-butadiene-styrene copolymer and polyurethane modified acrylic resin-organo-silicone rubber multipolymer.
10. underfill according to claim 1, is characterized in that, described thinner is reactive thinner.
11. underfills according to claim 10, it is characterized in that, described reactive thinner is selected from butylglycidyl ether, phenyl glycidyl ether, benzyl glycidyl ether, lauryl diglycidyl ether, p-cresol glycidyl ether, neopentylglycol diglycidyl ether, 1, at least one in 4-butanediol diglycidyl ether, ethylene glycol diglycidylether, polypropylene glycol diglycidyl ether, 1,6-hexanediol diglycidyl ether, glycidyl allyl ether and glycidyl methacrylate.
12. underfills according to claim 1, is characterized in that, described dispersion agent is selected from least one in BYK-9010, BYK-995, BYK-306, BYK-2008 and BYK-2009 of Bi Ke chemical production.
13. underfills according to claim 1, is characterized in that, described defoamer is selected from least one in polysiloxane defoamer and acryl-based antifoaming agent.
14. underfills according to claim 13, is characterized in that, described polysiloxane defoamer is selected from least one in BYK-320, BYK-322 and BYK-323 of Bi Ke chemical production;
Described acryl-based antifoaming agent is selected from least one in BYK-352, BYK-354, BYK-359 and BYK-392 of Bi Ke chemical production.
15. underfills according to claim 1, is characterized in that, described coupling agent is selected from least one in organo-silicon coupling agent, organotitanate coupling agent, organic aluminates coupling agent and organozirconates coupling agent.
16. underfills according to claim 15, it is characterized in that, described organo-silicon coupling agent is selected from least one in γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, γ-mercaptopropyl trimethoxysilane, octadecyl trimethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane and vinyltriethoxysilane;
Described organotitanate coupling agent is selected from least one in three Unimac 5680 isopropyl titanates, sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, organic aluminates coupling agent aluminium isopropoxide, isopropoxy distearyl acid acyloxy Aluminate;
Described organic aluminates coupling agent is selected from least one in aluminium isopropoxide and isopropoxy distearyl acid acyloxy Aluminate;
Described organozirconates coupling agent is selected from least one in alkoxyl group three (vinyl-oxyethyl group) zirconate and alkoxyl group three (p-aminophenyl oxygen base) zirconate.
The preparation method of 17. 1 kinds of underfills according to any one of claim 1 ~ 16, is characterized in that, comprises the steps:
By mass fraction, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts and the toughner of 1 part ~ 15 parts are mixed, obtain the first mixture;
Add in described first mixture by the pigment of mass fraction by the filler of 30 parts ~ 70 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part, mix, obtain the second mixture; And
By mass fraction, the thinner of the catalyzer of 0.1 part ~ 0.5 part and 1 part ~ 25 parts is added in described second mixture, mix, vacuum defoamation, obtain described underfill, wherein, described underfill according to the mass fraction, comprise the filler of 30 parts ~ 70 parts, the epoxy resin of 10 parts ~ 50 parts, the solidifying agent of 2 parts ~ 20 parts, the catalyzer of 0.1 part ~ 0.5 part, the toughner of 1 part ~ 15 parts, the thinner of 1 part ~ 25 parts, the dispersion agent of 0.1 part ~ 3 parts, the defoamer of 0.05 part ~ 1 part, the pigment of the coupling agent of 0.1 part ~ 1 part and 0.1 part ~ 0.5 part, described filler is preparing spherical SiO 2, the particle diameter of described filler is 50nm ~ 500nm.
The preparation method of 18. underfills according to claim 17, is characterized in that,
Described epoxy resin, solidifying agent and toughner to be mixed, obtain in the step of the first mixture, described in time of mixing be 5min ~ 30min;
Described filler, dispersion agent, defoamer, coupling agent and pigment to be added in described first mixture, mix, obtain in the step of the second mixture, described in time of mixing be 5min ~ 30min;
Described catalyzer and thinner to be added in described second mixture, mix, vacuum defoamation, obtain in the step of described underfill, described in time of mixing be 1min ~ 10min, the time of described vacuum defoamation is 5min ~ 30min.
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