CN104927733A - Underfill and preparing method thereof - Google Patents
Underfill and preparing method thereof Download PDFInfo
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- CN104927733A CN104927733A CN201510355328.XA CN201510355328A CN104927733A CN 104927733 A CN104927733 A CN 104927733A CN 201510355328 A CN201510355328 A CN 201510355328A CN 104927733 A CN104927733 A CN 104927733A
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Abstract
The invention discloses an underfill, comprising, 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 flexibilizer, 1 to 25 parts of diluent, 0.1 to 0.3 part of dispersant, 0.05 to 1 part of defoamer, 0.1 to 1 part of coupler and 0.1 to 0.5 part of pigment. The underfill comprises, by weight, 30 to 70 parts of the filler; the filler is in a core-shell structure, a core is made of SiO2 having low expansion coefficient, and a shell is made of at least one of Al2O3, AlN, BN, SiC and Si3N4, having thermal conductivity; the underfill comprising the filler is high in thermal conductivity and helps transmit and dissipate heat in a packaging structure. Compared with the traditional underfill, the underfill is lower in thermal expansion coefficient and better in thermal conductivity.
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
In electronic product use procedure, if the temperature of its chip is too high, injurious effects will be produced to the signal stabilization of electronic devices and components, reliability and work-ing life, as the node of too high temperature entail dangers to semi-conductor, the connection of damage circuit, increases the resistance of conductor and causes mechanical thermal stress damage.Therefore guarantee that the heat that heating electronic component produces can be discharged timely, oneself is through becoming an importance of microelectronic product system assembles, and for degree of integration and all higher portable type electronic product of packing density, heat radiation even becomes the technical bottleneck problem of whole product.
Underfill is the sizing agent that a class is filled between chip and substrate, mainly plays protection soldered ball, balances thermal expansivity between chip and substrate, have important effect to the raising of chip thermomechanical reliability.Simultaneously, because underfill is filled between chip and substrate, if having high thermal conductivity simultaneously, also the principal passage of chip thermodiffusion will be become, avoid the limitation that existing heat is only transmitted by soldered ball, improve the anti-fatigue ability of soldered ball and the thermomechanical reliability of packaging.
But the heat conductivility bottom traditional underfill is poor, thus constrain further developing of high-density systems level encapsulation technology.
Summary of the invention
Based on this, be necessary to provide a kind of heat conductivility good underfill.
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 the filler of nucleocapsid structure, and the material of the core of the filler of described nucleocapsid structure is SiO
2, the material of the shell of the filler of described nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one.
In one embodiment, the particle diameter of the core of the filler of described nucleocapsid structure is 0.05 μm ~ 10 μm, the thickness of the shell of the filler of described nucleocapsid structure is 10nm ~ 200nm, and the shell mass ratio of the core of the filler of described nucleocapsid structure and the filler of described nucleocapsid structure is 1:0.01 ~ 10.
In one embodiment, 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, 3, 4-epoxycyclohexyl-methyl 3, 4-epoxycyclohexyl manthanoate, 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 EPICLONHP7200, 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.
In one embodiment, described solidifying agent is selected from least one in alicyclic acid anhydride type curing agent, amine curing agent and phenolic solidifying agent.
In one embodiment, described alicyclic acid anhydride type curing agent is selected from least one in tetrahydrophthalic anhydride, HHPA, methyl tetrahydro phthalic anhydride and methyl hexahydrophthalic anhydride;
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 selected from least one in phenol formaldehyde resin and thio-alcohol solidifying agent.
In one embodiment, described catalyzer be selected from tertiary amine salt complex compound, imidazoles, imdazole derivatives, boron trifluoride complex, metal carboxylate promotor and microcapsule subsidence feed to ー kind less.
In one embodiment, described tertiary amine salt complex compound is selected from 2,4, three (2-ethyl acid) salt and 2 of 6-tri-(dimethylamino methyl) phenol (DMP-30), at least one in the carboxylate salt of 4,6-tri-(dimethylamino methyl) phenol (DMP-30);
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 boron trifluoride complex is selected from least one in boron triflouride-mono aminoethane complex compound, boron trifluoride ethyl ether complex and boron trifluoride-phenol complex;
Described metal carboxylate promotor is selected from least one in zinc naphthenate, cobalt naphthenate, manganese naphthenate, calcium naphthenate and zinc octoate;
Described microcapsule subsidence feed is selected from the production of Japanese Asahi Kasei Corporation
with
in at least one.
In one embodiment, described toughner is selected from least one in hydroxyl terminated butyl nitrile (HTBN) rubber, carboxyl end of the liquid acrylonitrile-butadiene rubber, thiorubber, liquid silastic and thermoplastic elastomer toughening agent.
In one embodiment, described liquid silastic is selected from least one in dimethyl silicone rubber, ethylene methacrylic silicon rubber and methyl phenyl vinyl silicon rubber;
Described thermoplastic elastomer toughening agent is selected from least one in styrene butadiene, polyethers, polysulfones, polyimide, core-shell copolymerized thing, segmented copolymer and hyperbranched polymer;
Described core-shell copolymerized thing 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 styrene-butadiene one styrene block copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate triblock copolymer, acrylonitrile-butadiene-styrene copolymer and polyurethane modified acrylic resin-organo-silicone rubber multipolymer;
Described hyperbranched polymer is selected from least one in the super-branched polyesteramide of benzene ring structure and response type epoxy toughening agent CYH-277.
In one embodiment, described thinner is selected from least one in single epoxide diluent and multi-epoxy thinner.
In one embodiment, described single epoxide diluent is selected from least one in phenyl glycidyl ether, neopentylglycol diglycidyl ether, propenyl glycidyl ether, n-butyl glycidyl ether and glycidyl methacrylate;
Described multi-epoxy thinner is selected from least one in diglycidylether, ethylene glycol diglycidylether and vinyl cyclohexene diepoxide.
In one embodiment, 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.
In one embodiment, described defoamer is selected from least one in polysiloxane defoamer and acryl-based antifoaming agent.
In one embodiment, 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 Bi Ke chemistry BYK-352, BYK-354, BYK-359 and BYK-392.
In one embodiment, described coupling agent is selected from least one in organo-silicon coupling agent, organotitanate coupling agent, organic aluminates coupling agent and organozirconates coupling agent.
In one embodiment, 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 the filler of nucleocapsid structure, the material of the core of the filler of described nucleocapsid structure is SiO
2, the material of the shell of the filler of described nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one.
In one embodiment, describedly 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 in the step of the first mixture, described in time of mixing be 5min ~ 30min;
Describedly 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 is added in described first mixture, mix, obtain in the step of the second mixture, described in time of mixing be 5min ~ 30min;
Describedly 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 in the step of described underfill, the described time mixed is 1min ~ 10min, and the time of described vacuum defoamation is 5min ~ 30min.
This underfill comprises the filler of 30 parts ~ 70 parts according to the mass fraction, and filler is the filler of nucleocapsid structure, and the material of the core of the filler of nucleocapsid structure is SiO
2, the material of the shell of the filler of nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one, this filler has high thermal conductivity and has nucleocapsid structure, and the material of core is SiO
2the material with low-expansion advantage and shell is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one there is thermal conduction characteristic, the underfill containing this filler, except having high thermal conductivity, is conducive to transmission and the dissipation of heat in encapsulating structure.Relative to traditional underfill; the thermal expansivity of this underfill is lower, heat conductivility is better; thus can meet in flip-chip the low-expansion requirement of underfill; play the packaging protection effect to flip-chip, and further developing of high-density systems level encapsulation technology can not be restricted.
Accompanying drawing explanation
Fig. 1 is the structural representation of the underfill of an embodiment;
Fig. 2 is the schema of the preparation method of underfill as shown in Figure 1.
Embodiment
Mainly in conjunction with the drawings and the specific embodiments underfill and preparation method thereof is described in further detail below.
The underfill of a kind of embodiment as shown in Figure 1, 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.
Filler is the filler of nucleocapsid structure, and the material of the core of the filler of nucleocapsid structure is SiO
2, the material of the shell of the filler of nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one.
In one preferably embodiment, the particle diameter of the core of the filler of nucleocapsid structure is 0.05 μm ~ 10 μm, and the thickness of the shell of the filler of nucleocapsid structure is 10nm ~ 200nm, and the shell mass ratio of the core of the filler of nucleocapsid structure and the filler of nucleocapsid structure is 1:0.01 ~ 10.
This underfill comprises the filler of 30 parts ~ 70 parts according to the mass fraction, and filler is the filler of nucleocapsid structure, and the material of the core of the filler of nucleocapsid structure is SiO
2, the material of the shell of the filler of nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one, this filler has high thermal conductivity and has nucleocapsid structure, and the material of core is SiO
2the material with low-expansion advantage and shell is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one there is thermal conduction characteristic, the underfill containing this filler, except having high thermal conductivity, is conducive to transmission and the dissipation of heat in encapsulating structure.Relative to traditional underfill; the thermal expansivity of this underfill is lower, heat conductivility is better; thus can meet in flip-chip the low-expansion requirement of underfill; play the packaging protection effect to flip-chip, and further developing of high-density systems level encapsulation technology can not be restricted.
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, 3, 4-epoxycyclohexyl-methyl 3, 4-epoxycyclohexyl manthanoate, 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 EPICLONHP7200, 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 tetrahydrophthalic anhydride, HHPA, methyl tetrahydro phthalic anhydride and methyl hexahydrophthalic anhydride.
Amine curing agent is selected from least one in aromatic amine, aromatic amine derivant, polymeric amide and Dyhard RU 100.
Phenolic solidifying agent is selected from least one in phenol formaldehyde resin and thio-alcohol solidifying agent.
Catalyzer be selected from tertiary amine salt complex compound, imidazoles, imdazole derivatives, boron trifluoride complex, metal carboxylate promotor and microcapsule subsidence feed to ー kind less.
Tertiary amine salt complex compound is selected from 2,4, at least one in three (2-ethyl acid) salt of 6-tri-(dimethylamino methyl) phenol (DMP-30) and the carboxylate salt of 2,4,6-tri-(dimethylamino methyl) phenol (DMP-30).
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.
Boron trifluoride complex is selected from least one in boron triflouride-mono aminoethane complex compound, boron trifluoride ethyl ether complex and boron trifluoride-phenol complex.
Metal carboxylate promotor is selected from least one in zinc naphthenate, cobalt naphthenate, manganese naphthenate, calcium naphthenate and zinc octoate.
Microcapsule subsidence feed is selected from the production of Japanese Asahi Kasei Corporation
with
in at least one.
Toughner is selected from least one in hydroxyl terminated butyl nitrile (HTBN) rubber, carboxyl end of the liquid acrylonitrile-butadiene rubber, thiorubber, liquid silastic and thermoplastic elastomer toughening agent.Use toughner can improve toughness and the impact resistance of underfill, improve the thermomechanical property of chip.
Liquid silastic is selected from least one in dimethyl silicone rubber, ethylene methacrylic silicon rubber and methyl phenyl vinyl silicon rubber.
Thermoplastic elastomer toughening agent is selected from least one in styrene butadiene, polyethers, polysulfones, polyimide, core-shell copolymerized thing, segmented copolymer and hyperbranched polymer.
Core-shell copolymerized thing 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.Segmented copolymer is selected from least one in styrene-butadiene one styrene block copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate triblock copolymer, acrylonitrile-butadiene-styrene copolymer and polyurethane modified acrylic resin-organo-silicone rubber multipolymer.Hyperbranched polymer is selected from least one in the super-branched polyesteramide (HBP) of benzene ring structure and response type epoxy toughening agent CYH-277.
Thinner is selected from least one in single epoxide diluent and multi-epoxy thinner.
Single epoxide diluent is selected from least one in phenyl glycidyl ether, neopentylglycol diglycidyl ether, propenyl glycidyl ether, n-butyl glycidyl ether and glycidyl methacrylate.
Multi-epoxy thinner is selected from least one in diglycidylether, ethylene glycol diglycidylether and vinyl cyclohexene diepoxide.
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 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.Polysiloxane defoamer is selected from least one in BYK-320, BYK-322 and BYK-323 of Bi Ke chemical production.Acryl-based antifoaming agent is selected from least one in Bi Ke chemistry BYK-352, BYK-354, BYK-359 and BYK-392.
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, graphite and glaucous organic pigment phthalocyanine pigment.
This underfill comprises the filler of 30 parts ~ 70 parts according to the mass fraction, and filler is the filler of nucleocapsid structure, and the material of core is SiO
2the material with low-expansion advantage and shell is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one there is thermal conduction characteristic, the underfill containing this filler, except having high thermal conductivity, is conducive to transmission and the dissipation of heat in encapsulating structure.Relative to traditional underfill; the thermal expansivity of this underfill is lower, heat conductivility is better; thus can meet in flip-chip the low-expansion requirement of underfill; play the packaging protection effect to flip-chip, and further developing of high-density systems level encapsulation technology can not be restricted.
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 the filler of nucleocapsid structure, and the material of the core of the filler of nucleocapsid structure is SiO
2, the material of the shell of the filler of nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one.
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.The filler occurred in embodiment is the condiment of nucleocapsid structure, SiO
2al
2o
3filler represents SiO
2for core, Al
2o
3for shell.In following embodiment.The thermal conductance thermal resistance tester test that the thermal conductivity of obtained underfill is produced by the scientific and technological LW-9389 of the auspicious neck of TaiWan, China obtains, 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 E5110g, tetrahydrophthalic anhydride 10g, hydroxyl terminated butyl nitrile (HTBN) rubber 1g mixes 5min in reactor, then add SiO
2al
2o
3filler 68.05g, dispersion agent 0.1g, defoamer 0.05g, silane coupling agent 0.2g, pigment 0.5g, drop in reactor and mix 5min.And then add Latence catalyst 0.1g, thinner phenyl glycidyl ether 10g, drop in reactor and mix 5min, vacuum defoamation 5mim, obtain required underfill.
The thermal conductivity recording the underfill that the present embodiment obtains is 1.5W/mK, thermal expansivity CTE1:40ppm/K, CTE2:110ppm/K.
Embodiment 2
Take bisphenol f type epoxy resin EPIKOTE 86220g, cycloaliphatic epoxy resin 3,4-epoxycyclohexyl-methyl 3,4-epoxycyclohexyl manthanoate 10g, diaminodiphenyl-methane 8g, nucleocapsid structure toughner 2g mix 10min in reactor, then add SiO
2bN filler 53.4g, dispersion agent 0.2g, defoamer 0.10g, silane coupling agent 0.2g, pigment 1g, drop in reactor and mix 10min.And then add imidazole catalyst 0.1g, ethylene glycol diglycidylether 5g, drop in reactor and mix 10min, vacuum defoamation 5min, obtain required underfill.
The thermal conductivity recording the present embodiment obtained is 1W/mK, thermal expansivity CTE1:50ppm/K, CTE2:120ppm/K.
Embodiment 3
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 HP470015g, biphenyl structural, polymeric amide 10g, block copolymer-toughened dose of 1.5g mix 20min in reactor, then add SiO
2siC filler 46.9g, dispersion agent 0.2g, defoamer 0.10g, silane coupling agent 0.2g, pigment 1g, drop in reactor and mix 20min.And then add catalyzer 2-ethyl-4-methylimidazole 0.1g, neopentylglycol diglycidyl ether 3g, drop in reactor and mix 20min, vacuum defoamation 5min, obtain required underfill.
Record the thermal conductivity 3W/mK that the present embodiment is obtained, thermal expansivity CTE1:60ppm/K, CTE2:120ppm/K.
Embodiment 4
Take bisphenol A type epoxy resin E4410g, phenol aldehyde type epoxy resin EPICLONHP720020g, phenolic mixes 25min as phenol formaldehyde resin 10g, liquid silastic 1.5g in reactor, then add SiO
2si
3n
4filler 52.1g, dispersion agent 0.1g, defoamer 0.1g, silane coupling agent 0.1g, pigment 1g, drop in reactor and mix 25min.And then add catalyst metal carboxylate salt 0.1g, glycidyl methacrylate 5g, drop in reactor and mix 25min, vacuum defoamation 5min, obtain required underfill.
The thermal conductivity recording the present embodiment obtained is 2.2W/mK, thermal expansivity CTE1:30ppm/K, CTE2:100ppm/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 the filler of nucleocapsid structure, and the material of the core of the filler of described nucleocapsid structure is SiO
2, the material of the shell of the filler of described nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one.
2. underfill according to claim 1, it is characterized in that, the particle diameter of the core of the filler of described nucleocapsid structure is 0.05 μm ~ 10 μm, the thickness of the shell of the filler of described nucleocapsid structure is 10nm ~ 200nm, and the shell mass ratio of the core of the filler of described nucleocapsid structure and the filler of described nucleocapsid structure is 1:0.01 ~ 10.
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, 3, 4-epoxycyclohexyl-methyl 3, 4-epoxycyclohexyl manthanoate, 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 EPICLONHP7200, 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.
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 tetrahydrophthalic anhydride, HHPA, methyl tetrahydro phthalic anhydride and methyl hexahydrophthalic anhydride;
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 selected from least one in phenol formaldehyde resin and thio-alcohol solidifying agent.
6. underfill according to claim 1, is characterized in that, described catalyzer be selected from tertiary amine salt complex compound, imidazoles, imdazole derivatives, boron trifluoride complex, metal carboxylate promotor and microcapsule subsidence feed to ー kind less.
7. underfill according to claim 6, it is characterized in that, described tertiary amine salt complex compound is selected from 2,4, three (2-ethyl acid) salt and 2 of 6-tri-(dimethylamino methyl) phenol (DMP-30), at least one in the carboxylate salt of 4,6-tri-(dimethylamino methyl) phenol (DMP-30);
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 boron trifluoride complex is selected from least one in boron triflouride-mono aminoethane complex compound, boron trifluoride ethyl ether complex and boron trifluoride-phenol complex;
Described metal carboxylate promotor is selected from least one in zinc naphthenate, cobalt naphthenate, manganese naphthenate, calcium naphthenate and zinc octoate;
Described microcapsule subsidence feed is selected from the production of Japanese Asahi Kasei Corporation
hX-3741,
hX-3088 and
at least one in HX-3792.
8. underfill according to claim 1, is characterized in that, described toughner is selected from least one in hydroxyl terminated butyl nitrile (HTBN) rubber, carboxyl end of the liquid acrylonitrile-butadiene rubber, thiorubber, liquid silastic and thermoplastic elastomer toughening agent.
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 thermoplastic elastomer toughening agent is selected from least one in styrene butadiene, polyethers, polysulfones, polyimide, core-shell copolymerized thing, segmented copolymer and hyperbranched polymer;
Described core-shell copolymerized thing 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 styrene-butadiene one styrene block copolymer, ethylene/n-butyl acrylate-glycidyl methacrylate triblock copolymer, acrylonitrile-butadiene-styrene copolymer and polyurethane modified acrylic resin-organo-silicone rubber multipolymer;
Described hyperbranched polymer is selected from least one in the super-branched polyesteramide of benzene ring structure and response type epoxy toughening agent CYH-277.
10. underfill according to claim 1, is characterized in that, described thinner is selected from least one in single epoxide diluent and multi-epoxy thinner.
11. underfills according to claim 10, it is characterized in that, described single epoxide diluent is selected from least one in phenyl glycidyl ether, neopentylglycol diglycidyl ether, propenyl glycidyl ether, n-butyl glycidyl ether and glycidyl methacrylate;
Described multi-epoxy thinner is selected from least one in diglycidylether, ethylene glycol diglycidylether and vinyl cyclohexene diepoxide.
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 Bi Ke chemistry BYK-352, BYK-354, BYK-359 and BYK-392.
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 the filler of nucleocapsid structure, the material of the core of the filler of described nucleocapsid structure is SiO
2, the material of the shell of the filler of described nucleocapsid structure is selected from Al
2o
3, AlN, BN, SiC and Si
3n
4in at least one.
The preparation method of 18. underfills according to claim 17, is characterized in that,
Describedly 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 in the step of the first mixture, described in time of mixing be 5min ~ 30min;
Describedly 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 is added in described first mixture, mix, obtain in the step of the second mixture, described in time of mixing be 5min ~ 30min;
Describedly 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 in the step of described underfill, the described time mixed is 1min ~ 10min, and the time of described vacuum defoamation is 5min ~ 30min.
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