CN107001769A - The optical semiconductor device of the die bond material that heat-curing type silica composition, said composition are constituted and the solidfied material with the die bond material - Google Patents

The optical semiconductor device of the die bond material that heat-curing type silica composition, said composition are constituted and the solidfied material with the die bond material Download PDF

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CN107001769A
CN107001769A CN201580065668.7A CN201580065668A CN107001769A CN 107001769 A CN107001769 A CN 107001769A CN 201580065668 A CN201580065668 A CN 201580065668A CN 107001769 A CN107001769 A CN 107001769A
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composition
heat
mass parts
curing type
type silicon
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CN107001769B (en
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小内谕
小材利之
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Shin Etsu Chemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
    • C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
    • C08F290/06—Polymers provided for in subclass C08G
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
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    • C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
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    • H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
    • H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
    • H01L2224/321—Disposition
    • H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/32245—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/4805—Shape
    • H01L2224/4809—Loop shape
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    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/481—Disposition
    • H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/48221—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/48245—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
    • H01L2224/48247—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic connecting the wire to a bond pad of the item
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    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/481—Disposition
    • H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/48221—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/48245—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
    • H01L2224/48257—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic connecting the wire to a die pad of the item
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    • H01L2224/73—Means for bonding being of different types provided for in two or more of groups H01L2224/10, H01L2224/18, H01L2224/26, H01L2224/34, H01L2224/42, H01L2224/50, H01L2224/63, H01L2224/71
    • H01L2224/732—Location after the connecting process
    • H01L2224/73251—Location after the connecting process on different surfaces
    • H01L2224/73265—Layer and wire connectors
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    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
    • H01L2924/181—Encapsulation

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  • Chemical & Material Sciences (AREA)
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  • Computer Hardware Design (AREA)
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  • Led Device Packages (AREA)
  • Die Bonding (AREA)
  • Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
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Abstract

The present invention is a kind of heat-curing type silicon-ketone composition, and it contains following component：(A) organopolysiloxane of the structure represented in the molecule with least one by following formulas (1)：100 mass parts；(B) comprising more than a kind of the organic peroxide in diacyl peroxide, peroxy esters：The mass parts of total amount 100 relative to foregoing (A) composition are 0.1~20 mass parts；And, the silane compound of (C) containing epoxy radicals or the silicone compounds containing epoxy radicals：The mass parts of total amount 100 relative to foregoing (A) composition are 0.1~20 mass parts.Accordingly, a kind of heat-curing type silicon-ketone composition can be provided, its transparency is high, bonding strength and operability are excellent, and can obtains the solidfied material with heat resistance, light resistance and crumpling resistance,

Description

Die bond material and consolidated with this that heat-curing type silica composition, said composition are constituted The optical semiconductor device of the solidfied material of brilliant material
Technical field
The die bond material and use constituted the present invention relates to a kind of heat-curing type silica composition, by said composition should The optical semiconductor device of the solidfied material of die bond material.
Background technology
Because the optical semiconductors such as light emitting diode (Light Emitting Diode, LED) have power consumption On few such excellent specific property, the outer lighting use in room or mobile applications, gradually increase use luminescent semiconductor device (device).This The luminescent semiconductor device of sample, is usually to be sent the photosemiconductor light-emitting component for sending blue light, near ultraviolet ray or ultraviolet Light, carry out wavelength conversion by the way that wavelength shifter is fluorophor, and obtain the light-emitting device of similar white light.Such light In semiconductor devices, optical semiconductor is bonded with framework using die bond material, fixed.
In the past, used comprising tool excellent adhesiveness and machine mostly as optical semiconductor die bond material compositions The bisphenol A type epoxy resin of tool intensity, the epoxy resin that ultraviolet is not absorbed, the composition of curing agent and curing catalysts, its In, the epoxy resin that ultraviolet (UV) is not absorbed is such as bisphenol-A epoxy resin or alicyclic epoxy resin.However, Uprised with the brightness and output of LED element, because of the ultraviolet produced by LED element, heat etc., can trigger adhesive layer discoloration and The problem of fragmentation.
As the material for solving these problems, known is a kind of resin that epoxy radicals is imported in silicone resin, And the resin can provide do not absorb ultraviolet and with can be flexible solidfied material, for example, being proposed in report：One kind has 1 The cyclic ethers such as glycidyl, epoxycyclohexyl above contain the silicone resin (patent document 1) of base；One kind has intramolecular The glycidyl that silicone copolymer resin that the ester ring type epoxy of more than 1 contains base, intramolecular have more than 1 contains base Resin (patent document 2) obtained by 2 function silicone resins and use；Further, by the epoxide modified silicone resin of ester ring type and alicyclic ring Resin (patent document 3) etc. obtained by formula epoxy resin and use.However, these resins are come using acid anhydrides or amine compound As curing agent, in general, during using this curing agent, it is necessary to coordinate epoxide equivalent to add the allotment number of curing agent. Therefore, as a result cause in resin cured matter, become to have remained many organic functionals from cross-linked structure and with light absorption Base, because long-time is under the light of LED element more efficient than ever, heat, causes chipping or discoloration etc., at this These resins of aspect simultaneously can not meet required, it is desirable to be improved.
Prior art literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2008-45088 publications；
Patent document 2：Japanese Unexamined Patent Publication 2008-202036 publications；
Patent document 3：No. 2011-109058 report of Japanese Unexamined Patent Publication.
The content of the invention
Invent problem to be solved
The present invention considers above-described problem and completed that its object is to provide a kind of heat-curing type silicone combination Thing, its transparency is high, bonding strength and operability are excellent, and can obtain consolidating with heat resistance, light resistance and crumpling resistance Compound.In addition, other objects of the present invention are to provide a kind of die bond material being made up of said composition.Further, it is of the invention Another object be to provide a kind of optical semiconductor device, it is that optical semiconductor is carried out into die bond using the die bond material.
The technical scheme solved the problems, such as
In order to reach above-mentioned purpose, the present invention provides a kind of heat-curing type silicon-ketone composition, it is characterised in that containing with Lower composition：
(A) organopolysiloxane of the structure represented in the molecule with least one by following formulas (1)：100 mass Part；
In formula (1), m is any one in 0,1,2, R1It is hydrogen atom, phenyl or halogenated phenyl, R2It is hydrogen atom or methyl, R3It is through substituteding or unsubstituted and can be with 1 valency organic group of identical or different carbon number 1~12, Z1It is-R4-、-R4- O-、-R4(CH3)2Any of Si-O-, Z2It is oxygen atom or through substituteding or unsubstituted and can be with identical or different Carbon number 1~10 divalent organic group, wherein, R4Be through substituted or unsubstituted and can with identical or different carbon number 1~ 10 divalent organic group；
(B) comprising more than a kind of the organic peroxide in diacyl peroxide, peroxy esters：Relative to foregoing (A) mass parts of total amount 100 of composition are 0.1~20 mass parts；And,
(C) silane compound containing epoxy radicals or the silicone compounds containing epoxy radicals：Relative to foregoing (A) composition The mass parts of total amount 100 be 0.1~20 mass parts.
If this heat-curing type silicon-ketone composition, its transparency is high, bonding strength and operability are excellent, and can be with Obtain heat resistance, light resistance and the excellent solidfied material of crumpling resistance.
Furthermore it is preferred that being, the Z of the organopolysiloxane of foregoing (A) composition1It is-R4-, foregoing Z2It is oxygen atom.
Furthermore it is preferred that being, the Z of the organopolysiloxane of foregoing (A) composition1It is-R4- O- or-R4(CH3)2Si-O-, it is foregoing Z2It is through substituteding or unsubstituted and can be with the divalent organic group of identical or different carbon number 1~10.
If this heat-curing type silicon-ketone composition, then free radical produced during (B) ingredient breakdown and (A) composition Can effectively it be reacted, thus bonding strength and operability are excellent, and it is excellent to obtain heat resistance, light resistance and crumpling resistance Different solidfied material.
Furthermore it is preferred that being, the organopolysiloxane of foregoing (A) composition, in the molecule with least one by following formulas (2) structure represented：
In formula (2), m, R1、R2、R3、R4It is same as described above.
If this heat-curing type silicon-ketone composition, then free radical produced during (B) ingredient breakdown and (A) composition Reaction can be more effectively carried out, thus bonding strength and operability are excellent, and heat resistance, light resistance and crumpling resistance can be obtained Excellent solidfied material.
Furthermore it is preferred that be, in the organopolysiloxane of foregoing (A) composition, (the SiO with more than 0.1mol%2) single Member.
If this heat-curing type silicon-ketone composition, then free radical produced during (B) ingredient breakdown and (A) composition Can effectively further it be reacted, further, the epoxy radicals of the organic acid produced by (B) composition and (C) composition can be effective Ground is reacted, thus bonding strength and operability are excellent, and can obtain heat resistance, light resistance and crumpling resistance is excellent consolidates Compound.
Furthermore it is preferred that be, by foregoing heat-curing type silicon-ketone composition solidified obtained by thickness 2mm solidfied material, Its full light transmittance is more than 80%, and haze value is less than 20%.
If this heat-curing type silicon-ketone composition, the transparency of the solidfied material of said composition can change height.
Further, the present invention provides a kind of die bond material, it is characterised in that be the heat-curing type by the invention described above Silicon-ketone composition is constituted.
If this die bond material, can be suitable as the die bond material for LED chip being equipped on wiring board Material.
Further, the present invention provides a kind of optical semiconductor device, it is characterised in that with by the die bond of the invention described above Material solidified obtained by solidfied material.
The heat-curing type silicon-ketone composition of the present invention, its transparency is high, bonding strength and operability are excellent, and can obtain Obtain heat resistance, light resistance and the excellent solidfied material of crumpling resistance.Therefore, optical semiconductor device of the invention is used die bond material Solidfied material obtained by being solidified, and the die bond material is made up of the heat-curing type silicon-ketone composition, thus the present invention Optical semiconductor device become with heat resistance, light resistance and crumpling resistance.
Invention effect
The heat-curing type silicon-ketone composition of the present invention, results in a kind of solidfied material (transparent cured thing), the solidification The transparency of thing, bonding strength and operability are excellent, and with heat resistance, light resistance, crumpling resistance and discoloration-resistant.Therefore, By the die bond material that constitutes of heat-curing type silicon-ketone composition of the present invention, it can be suitably used for as by LED chip It is carried on the die bond material on wiring board.In addition, partly being led using the light of solidfied material obtained by the die bond material is solidified Body device, then become with heat resistance, light resistance and crumpling resistance.
Brief description of the drawings
Fig. 1 is the profile for an example for representing the optical semiconductor device of the present invention, wherein, the optical semiconductor device Used by die bond material solidified obtained by solidfied material, the die bond material be by the present invention heat-curing type silicone group Compound is constituted.
Embodiment
Hereinafter, the present invention is described in more detail.
As described above, it is necessary to which a kind of heat-curing type silicon-ketone composition, its transparency is high, bonding strength and operability are excellent It is different, and the solidfied material with heat resistance, light resistance and crumpling resistance can be obtained.
The present inventor is attentively studied to reach above-mentioned purpose.As a result, finding a kind of heat-curing type silicone Composition, its transparency is high, bonding strength and operability are excellent, and it is excellent to obtain heat resistance, light resistance and crumpling resistance Solidfied material, and can provide reliability high optical semiconductor device, so as to complete the present invention, wherein, the heat-curing type Silicon-ketone composition is characterised by, contains following component：
(A) organopolysiloxane of the structure represented in the molecule with least one by following formulas (1)：100 mass Part；
In formula (1), m is 0,1, any of 2, R1It is hydrogen atom, phenyl or halogenated phenyl, R2It is hydrogen atom or methyl, R3It is through substituteding or unsubstituted and can be with 1 valency organic group of identical or different carbon number 1~12, Z1It is-R4-、-R4- O-、-R4(CH3)2Si-O-(R4It is through substituteding or unsubstituted and can be with the divalent organic group of identical or different carbon number 1~10 Any of group), Z2It is oxygen atom or through substituteding or unsubstituted and can be with the 2 of identical or different carbon number 1~10 Valency organic group；
(B) comprising more than a kind of the organic peroxide in diacyl peroxide, peroxy esters：Relative to foregoing (A) mass parts of total amount 100 of composition are 0.1~20 mass parts；And,
(C) silane compound containing epoxy radicals or the silicone compounds containing epoxy radicals：Relative to foregoing (A) composition The mass parts of total amount 100 be 0.1~20 mass parts.
Hereinafter, the present invention is further illustrated, but the present invention is not limited to this.
[(A) organopolysiloxane]
(A) organopolysiloxane of composition, is to have the structure that at least one is represented by following formulas (1) in the molecule Organopolysiloxane.
In formula (1), m is any one in 0,1,2, R1It is hydrogen atom, phenyl or halogenated phenyl, R2It is hydrogen atom or methyl, R3It is through substituteding or unsubstituted and can be with 1 valency organic group of identical or different carbon number 1~12, Z1It is-R4-、-R4- O-、-R4(CH3)2Si-O-(R4It is through substituteding or unsubstituted and can be with the divalent organic group of identical or different carbon number 1~10 Any of group), Z2It is oxygen atom or through substituteding or unsubstituted and can be with the 2 of identical or different carbon number 1~10 Valency organic group.
(A) in the organopolysiloxane of composition, it is used as Z1With Z2Combination, be preferably, Z1It is-R4-、Z2It is the group of oxygen atom Close, or Z1It is-R4- O- or-R4(CH3)2Si-O-、Z2It is through substituteding or unsubstituted and can be with identical or different carbon number 1 The combination of~10 divalent organic group.If including the heat-curing type silicon-ketone composition of this (A) composition, then (B) composition Produced free radical can effectively be reacted with (A) composition during decomposition, thus bonding strength and operability are excellent, and can be with Obtain heat resistance, light resistance and the excellent solidfied material of crumpling resistance.
In addition, in the organopolysiloxane of (A) composition, being preferably, (the SiO with more than 0.1mol%2) unit.If The heat-curing type silicon-ketone composition for including this (A) composition, then free radical produced during (B) ingredient breakdown and (A) into Branch is effectively further reacted, further, and the epoxy radicals of the organic acid and (C) composition that are produced by (B) composition has Effect ground is reacted, thus bonding strength and operability are excellent, and it is excellent to obtain heat resistance, light resistance and crumpling resistance Solidfied material.
Further, the organopolysiloxane of (A) composition, be preferably, in the molecule with least one by following formulas (2) structure represented.If including the heat-curing type silicon-ketone composition of this (A) composition, then produced during (B) ingredient breakdown Raw free radical is more effectively carried out reaction with (A) into branch, thus bonding strength and operability are excellent, and can obtain heat-resisting Property, light resistance and the excellent solidfied material of crumpling resistance.
In formula (2), m, R1、R2、R3、R4It is same as described above.
Furthermore it is preferred that be, by the heat-curing type silicon-ketone composition of the present invention solidified obtained by thickness 2mm solidification Thing, its full light transmittance is more than 80%, and haze value is less than 20%.If such heat-curing type silicone combination Thing, the transparency of the solidfied material of said composition can change height.In addition, haze value is to define in the following manner：(haze value (%))=(diffusion light transmittance)/(full light transmittance) × 100.
(A) organopolysiloxane of composition, is preferably that viscosity at 25 DEG C is more than 10mPas liquid or solid Branched or space network organopolysiloxane.
In above-mentioned formula (1), as by R3It is represented be incorporated on silicon atom through substituteding or unsubstituted and can With 1 identical or different valency organic group, the alkyl that carbon number is 1~12 can be generally enumerated, is preferably, carbon number 1~8 or so Alkyl, specifically, can be enumerated：Methyl, ethyl, propyl group, isopropyl, butyl, isobutyl group, the tert-butyl group, amyl group, neopentyl, The alkyl such as hexyl, cyclohexyl, octyl group, nonyl, decyl；The aryl such as phenyl, tolyl, xylyl, naphthyl；Benzyl, benzene second The aralkyl such as base, phenylpropyl；Vinyl, pi-allyl, acrylic, isopropenyl, cyclobutenyl, hexenyl, cyclohexenyl group, octenyl Deng alkenyl；And, some or all of hydrogen atom of these groups is replaced and obtained by the halogen atoms such as fluorine, bromine, chlorine, cyano group etc. Group, halogen-substituted alkyl and cyanoethyl etc. such as chloromethyl, chloropropyl, bromoethyl, trifluoro propyl.
In above-mentioned formula (1), as by R4It is represented through substituteding or unsubstituted and can be with identical or different divalent Organic group, specifically, can be enumerated, and the carbon number such as methylene, ethylidene, propylidene, butylidene is 1~10 alkylene The divalent alkyls such as base；Preferably, carbon number is 1~3 alkylidene.
The example of the organopolysiloxane of (A) composition described below (in following formula, Me represents methyl).The composition can be Single component, can also be used in combination with other compositions.In addition, in following formula, equivalent to the R in above-mentioned formula (1)3Group, be with The situation of methyl is used as example, but it is also possible to be altered to other groups (through substituted or unsubstituted and can with identical or 1 valency organic group of different carbon numbers 1~12).
Organopolysiloxane represented by following formula, is with MA：M：Q=1：4：6 ratio come include MA units, M units, Q unit, and molecular weight is 5000, the molecular weight is the weight average molecular weight converted with polystyrene.
Organic polysiloxane represented by following formula, is with MA-D：D：T=2：6：7 ratio includes MA-D units, D Unit, T unit, and molecular weight is 3500, and the molecular weight is the weight average molecular weight converted with polystyrene.
(A) in composition, in order to adjust the purpose such as the viscosity of composition or the hardness of solidfied material, it can add following represented The reactive diluent comprising silicone or the reactive diluent without silicone.
As the specific example of the reactive diluent comprising silicone, it can enumerate by having that following formula (3)~(7) are represented Machine polysiloxanes (in following formula, Me represents methyl).The composition can be single component, can also be used in combination with other compositions.
In formula (5), p is that 18, q is 180.
In formula (6), p ' is that 20, q is 180.
In formula (7), p is that 18, q is 180.
As the synthetic method of this (A) composition, as long as example in the presence of chloroplatinic acid catalyst, making following compound With having comprising unsaturated group of aliphatic series (for example, ethene unsaturated group and acetylene unsaturated group) Machine polysiloxanes carries out hydrosilylation (hydrosilylation) reaction：Organohydrogensilicon alkane represented by following formula,
In above-mentioned formula, m, R1、R2、R3、Z1It is same as described above；
Preferably, the compound represented by following formula,
In above-mentioned formula, m, R1、R2、R3、Z1、Z2It is same as described above；
More particularly, (3- methacryloxypropyls) -1,1,3,3- tetramethyl disiloxane, its be by by 1, Double (3- methacryloxypropyls) tetramethyl disiloxanes of 3- and 1,1,3,3- tetramethyl disiloxane, in acid catalyst In the presence of being balanced reaction obtained；The compound for being suitable for the present invention can be produced using this method, but is not limited In foregoing synthetic method.In addition, the organopolysiloxane comprising unsaturated group of aliphatic series, it is possible to use comprising with fat Method known to (common) hydrolytic condensation of the alkoxy silane of the organopolysiloxane of race's unsaturated group etc. is manufactured, can also Use commercially available product.
As the reactive diluent without silicone, just like H2C=CGCO2R5Represented (methyl) esters of acrylic acid, on State in formula, G is any of hydrogen, halogen, the alkyl of carbon number 1~4, R5It is to be selected from the alkane with 1~16 carbon atom Any of base, cycloalkyl, alkenyl, cycloalkenyl group, alkaryl, aralkyl, aryl.Any of these groups, Ke Yigen According to needs, with silicon, oxygen, halogen, carbonyl, hydroxyl, ester, carboxylic acid, urea, urethane, carbamate, amine, acid amides, sulphur, sulphonic acid ester, Sulfo group etc. replaces.
As particularly preferred (methyl) esters of acrylic acid in reactive diluent, have for example with the following acrylic acid being consistent Ester：Polyethylene glycol two (methyl) acrylate, as ethoxylated bisphenol A (methyl) acrylate (" EBIPA " or " EBIPMA ") this Bisphenol-A two (methyl) acrylate, tetrahydrofuran (methyl) acrylate and two (methyl) acrylate, the acrylic acid of sample are fragrant Thatch ester and methacrylic acid citronellyl acrylate, (methyl) hydroxypropyl acrylate, hexylene glycol two (methyl) acrylate (" HDDA " or " HDDMA "), trimethylolpropane tris (methyl) acrylate, (methyl) acrylic acid tetrahydrochysene bicyclopentadiene ester, the hydroxyl of ethoxyquin three Propane tri (" ETTA "), triethylene glycol diacrylate and TEGDMA (" TRIEGMA "), isobornyl acrylate and isobornyl methacrylate.Certainly, the group of these (methyl) esters of acrylic acids Conjunction can also be used as reactive diluent.
The scope of addition, preferably 0.01~30 mass % during addition reactive diluent, more preferably 0.05~ 10 mass % scope.
The heat-curing type silicon-ketone composition of the present invention, under specific purposes, can also change containing other compositions Desired solidification or uncured characteristic.For example, can include as (methyl) acryloxypropyl trimethoxy silane, different three Adhesion promotor as paracyanogen acid three alkyl esters or fulminuric acid triallyl, vinyl front three oxosilane etc., be preferably, bag Containing the amount to about 20 mass %.Other any conditions, can enumerate non-(methyl) acrylic acid silicone diluent or plasticizer (plasticizer), it is preferably, includes the amount to about 30 mass %.As non-(methyl) silicon Acrylote ketone, tool can be enumerated There are the trimethylsilyl end carburetion and silicone rubber of 100~500mPas viscosity.Non- (methyl) silicon Acrylote ketone, can To include the co-curing base as vinyl.
[(B) organic peroxide]
(B) composition comprising more than a kind of organic peroxide in diacyl peroxide, peroxy esters, be for After the heat-curing type silicon-ketone composition of the present invention is configured into desired shape, heated and by crosslinking instead The silicon-ketone composition should be made to solidify blended composition, and it is possible to according to the connection temperature of purpose, Connection Time, use Time limit etc. properly selects.
Organic peroxide, for the viewpoint for having high response and long life concurrently, is preferably that half-life period is 10 small When temperature be more than 40 DEG C, and half-life period is less than 200 DEG C for the temperature of 1 minute, and more preferably, half-life period is 10 hours Temperature is more than 60 DEG C, and half-life period is less than 180 DEG C for the temperature of 1 minute.
Now, by the free radical produced by the thermal decomposition of the organic peroxide because of (B) composition, above-mentioned (A) can be caused Produced between the alkenyls such as vinyl, pi-allyl between the alkyl being bonded on silicon atom in composition or in above-mentioned (A) composition Bonding reaction, and crosslinking curing thing is made.Further, as (B) composition decomposition product a part, can produce has The organic acid of carboxyl, therefore the organic acid plays a role as the crosslinking agent with the epoxy reaction of (C) composition described later, energy It is enough to form firmer cross-linked structure.
As diacyl peroxide, for example, isobutyl peroxide, 2,4- dichloro-benzoyl base peroxidating Thing, 3,5,5- trimethyl acetyl bases peroxide, sim peroxides, dodecane acyl peroxide, stearyl peroxide Compound, succinic peroxide compound (succinic peroxide), benzoylperoxy toluene and benzoyl peroxide.
As peroxy esters, for example, the withered ester of peroxide neodecanoic acid, the tetramethyl butyl ester of peroxide neodecanoic acid 1,1,3,3-, Peroxide neodecanoic acid 1- cyclohexyl -1- Methylethyls, the tertiary own ester of peroxide neodecanoic acid, the peroxide trimethylace tonitric tert-butyl ester, peroxide -2- second Base caproic acid -1,1,3,3- tetramethyls butyl ester, 2,5- dimethyl -2,5- double (2- ethylhexanoylperoxies) hexane, peroxide -2- second Base caproic acid -1- cyclohexyl -1- Methylethyls, the tertiary own ester of peroxide -2 ethyl hexanoic acid, the peroxide -2 ethyl hexanoic acid tert-butyl ester, peroxide are different Tert-butyl acetate, 1,1-bis(t-butylperoxy)cyclohexane, the tertiary own ester of peroxy isopropyl base single carbon acid, peroxide -3,5,5- front threes Base hecanoic acid t-butyl ester, the peroxide lauric acid/dodecanoic acid tert-butyl ester, 2,5- dimethyl -2,5- double (a toluyl groups peroxy) hexane, peroxides Isopropyl single carbon tert-butyl acrylate, peroxide -2- ethylhexyl single carbons tert-butyl acrylate, the tertiary own ester of benzoper acid, Peracetic acid uncle Butyl ester and bis(t-butylperoxy) hexahydro terephthalic acid ester.These peroxy esters can be used alone a kind, can also combine 2 kinds with On use.
As other organic peroxides, for example, dialkyl peroxide, peroxydicarbonate, peroxide Ketal, hydroperoxides, silyl peroxides etc..Also these organic peroxides can namely be wrapped with above-mentioned (B) composition It is applied in combination containing more than a kind of the organic peroxide in diacyl peroxide, peroxy esters.
As dialkyl peroxide, for example, α, α ' it is-bis(t-butylperoxy) diisopropyl benzene, two withered Base peroxide, 2,5- dimethyl -2,5- bis(t-butylperoxy)s hexane and tert-butyl cumyl peroxide.
As peroxydicarbonate, for example, the carbonic acid di-n-propyl ester of peroxide two, diisopropyl peroxydicarbonate, The carbonic acid of peroxide two double (4- tert-butylcyclohexyls) ester, -2- ethyoxyls methoxyethoxy ester of two carbonic acid of peroxide two, double (2- ethylhexyl peroxides Base) two carbonic esters, the carbonic acid dimethoxy butyl ester of peroxide two and double (3- methyl -3- methoxybutyls peroxies) two carbonic esters.
As peroxy ketal, for example, 1,1- double (tertiary hexyl peroxies) -3,3,5- trimethyl-cyclohexanes, 1, 1- double (tertiary hexyl peroxy) hexamethylene, 1,1- bis(t-butylperoxy) -3,3,5- trimethyl-cyclohexanes, the 1,1- (tert-butyl groups Peroxy) cyclododecane and 2,2- bis(t-butylperoxy) decane.
As hydroperoxides, for example, diisopropyl benzene hydroperoxides and cumene hydroperoxide.
As silyl peroxides, for example, tert-butyl group trimethylsilyl peroxide, two (tert-butyl groups) Dimethylsilyl peroxide, tert-butyl group trivinyl silyl peroxides, two (tert-butyl group) divinyl silylation mistakes Oxide, three (tert-butyl group) vinyl silanes base peroxide, tert-butyl group triallyl silyl peroxides, two (tert-butyl groups) Diallylsilane base peroxide and three (tert-butyl group) allyl silicane base peroxide.
Relative to the mass parts of organopolysiloxane total amount 100 of (A) composition, the addition of (B) composition is 0.1~20 matter Measure part, preferably 0.5~10 mass parts.(B) when the addition of composition is less than 0.1 mass parts, it can cause reaction can not be fully Carry out, be possible to that hardness can not be obtained as the solidfied material of purpose.(B) when the addition of composition is more than 20 mass parts, except having Possibly the physical property after desired solidification can not be obtained, be possible to that sufficient heat resistance, light resistance, crumpling resistance can not be obtained Outside, it is also possible to colour, the full light transmittance as solidfied material is low, discoloration the reason for.
[silane compound of (C) containing epoxy radicals or the silicone compounds containing epoxy radicals]
The heat-curing type silicon-ketone composition of the present invention, contains the silane compound containing epoxy radicals as (C) composition Or the silicone compounds containing epoxy radicals.These compounds, as long as containing the epoxy radicals of more than 1 in intramolecular.This In specification, refer to containing epoxy radicals, epoxy radicals is included at least one of group, for example, alkyl, alkane can be contained The others functional group such as ether and epoxy radicals.
In the present invention, as mentioned earlier, as a part for the decomposition product of (B) composition, can produce having with carboxyl Machine is sour, therefore the purpose of addition (C) composition is, the crosslinking that the organic acid can be reacted as the epoxy radicals with (C) composition Agent plays a role, and forms further firm cross-linked structure, thus (C) composition be important component.
(C) in composition, it is not particularly limited as epoxy radicals, for example, glycidyl, epoxycyclohexyl etc.. More particularly, for example, 2,3- glycidyl, 3,4- epoxybutyls, 4,5- epoxypentyls, 2- glycidoxy second Base, 3- glycidoxypropyl groups, 4- glycidoxy butyl etc..
As (C) composition, as long as intramolecular has the silane compound or siliconization that the epoxy of more than 1 contains base Compound, then be not particularly limited.For example, containing the silane coupling agent of epoxy radicals or its hydrolytic condensate etc..As containing epoxy radicals Silane coupling agent or its hydrolytic condensate, for example, glycidoxypropyltrime,hoxysilane, glycidoxy The silane compounds such as propyl-triethoxysilicane or its hydrolytic condensate etc..
(C) in composition, as the silicone compounds containing epoxy radicals, following shown silicone compounds can be enumerated Thing, but can be not limited to use these silicone compounds.
A, r are 0~50 integers, and b, s, t are 1~50 integers.
By the way that containing (C) composition, heat-curing type silicon-ketone composition of the invention, the penetrability after solidification is high, for light The heating of semiconductor element or luminous heat resistance and excellent in light-resistance, and remain to acquisition by force even for thermal shock repeatedly Tough characteristic, i.e. crumpling resistance.
Relative to the mass parts of total amount 100 of foregoing (A) composition, the addition of (C) composition is 0.1~20 mass parts, excellent Elect 0.5~15 mass parts as.(C) when the addition of composition is less than 0.1 mass parts, it is possible to can not obtain after desired solidification Physical property, be possible to that sufficient heat resistance, light resistance, crumpling resistance can not be obtained.(C) addition of composition is more than 20 mass Part when, reaction can not be carried out fully, and unreacted epoxy radicals is remained in solidfied material, it is therefore possible to as discoloration the reason for.
[(D) other compositions]
In order to further maintain the transparency of composition, suppress to produce coloring, oxidative degradation of solidfied material etc., can by 2, The known antioxidants such as 6- di-t-butyl -4- sylvans are blended in the heat-curing type silicon-ketone composition of the present invention. In addition, in order to assign the repellence to light deterioration, the light stabilizers such as amine system stabilizer that be obstructed can also be blended in the present invention's In heat-curing type silicon-ketone composition.
In order to improve the intensity, adjustment viscosity, imparting thixotropy of heat-curing type silicon-ketone composition of the invention (thixotropy) etc., it is further possible to which it is inorganic to blend aerosil (fumed silica), nano aluminium oxide etc. Matter filler.As needed, in heat-curing type silicon-ketone composition of the invention, dyestuff, pigment, fire retardant etc. can also be blended.
In addition, the purpose in order to improve operability, can also be added using solvent etc..The species of solvent has no special limit System, can use can it is dissolving cured before heat-curing type silicon-ketone composition, aforementioned inorganic matter filler etc. is divided well Dissipate, and the solvent of uniform die bond material or adhesive etc. can be provided.As long as the blending ratio of the solvent is according to use die bond material Operating condition, environment, use time etc. of material etc. is suitably adjusted.Solvent of more than two kinds and can also be used.Make For this solvent, it can enumerate, fourth carbitol acetate, carbitol acetate, methyl ethyl ketone, α-abienol and cellosolve Acetic acid esters etc..
In addition, the heat-curing type silicon-ketone composition of the present invention, can also contain the bonding to improve its cohesive and assign Give agent.As the bonding imparting agent, such as silane coupling agent or its hydrolytic condensate beyond above-mentioned (C) composition.It is used as (C) Silane coupling agent beyond composition, such as silane coupling agent containing (methyl) acryloyl group, the silane containing isocyanate group are even Mixture, the silane coupling agent containing fulminuric acid base, the silane coupling agent containing amino, silane coupling agent containing sulfydryl etc. Known silane coupling agent, relative to the mass parts of total amount 100 of foregoing (A) composition, can be preferably used 0.1~20 mass Part, 0.3~10 mass parts can be more preferably preferably used.
The heat-curing type silicon-ketone composition of the present invention, can be by by mentioned component, using known mixed method, example Such as mixed to manufacture using mixer, roller.In addition, the heat-curing type silicon-ketone composition of the present invention, using rotary Viscosimeter, such as E type viscosimeters, measured viscosity is 10~1000000mPas in the state of 23 DEG C, especially, preferably For 100~1000000mPas.
The heat-curing type silicon-ketone composition of the present invention, can pass through known solidification side under known condition of cure Method is solidified.Specifically, be typically with 80~200 DEG C, be preferably heated with 100~160 DEG C, thus, this can be made Composition solidifies.Heat time is 0.5 minute~5 hours or so, especially, preferably 1 minute~3 hours or so.Can be by grasping Make the balance between condition, productivity, light-emitting component and framework heat resistance suitably to select condition of cure.
The heat-curing type silicon-ketone composition of the present invention, can suitably use and LED chip is fixed on packaging body. In addition it is also possible to suitably be used in organic electroluminescent device (organic EL), laser diode and light emitting diode matrix The others such as (LED array) optical semiconductor.
Further, the present invention provides a kind of die bond material, and it is the heat-curing type silicone combination by the invention described above Thing is constituted, and can be used for semiconductor element being connected to wiring board.
The heat-curing type silicon-ketone composition of the present invention, its transparency is high, bonding strength and operability are excellent, and can obtain Obtain heat resistance, light resistance and the excellent solidfied material of crumpling resistance.Therefore, if by above-mentioned heat-curing type silicon-ketone composition The die bond material of composition, can suitably be used as the die bond material LED chip to be carried on to wiring board.
There is no particular restriction for the method for coating die bond material, and for example, rotary coating, printing and compression molding Deng.The thickness of die bond material, as long as properly selecting, typically 5~50 μm, especially 10~30 μm.Divide for example, using Dispensing device, temperature be 23 DEG C, pressure be 0.5~5kgf/cm2Under conditions of sent out, thus, it is possible to be applied easily Cloth.In addition, by using punching press (stamping) device, can also be easily by the die bond material transferring of defined amount to base Plate.
There is no particular restriction for the bearing method of semiconductor element, and for example, bonder.Determine die bond material thickness Key factor, in addition to the viscosity of foregoing die bond material, can enumerate, when the crimping loading of optical semiconductor, crimping Between, crimping temperature.These conditions, as long as the outer shape according to optical semiconductor, the die bond material thickness as purpose Properly select.In general crimp loading is more than 1gf and below 1kgf.Preferably more than 10gf and below 100gf. If more than 1gf crimping loading, then die bond material can fully be crimped.If in addition, using below 1kgf crimping Loading, then will not cause damage to the luminescent layer on optical semiconductor surface.As long as the crimping time is according to the productivity with step Between balance properly select, be in general more than 0 millisecond and less than 1 second.Preferably more than 1 millisecond and 30 millis Below second.If less than 1 second, in productive viewpoint preferably.Crimping temperature is not particularly limited, as long as according to die bond material The temperature in use scope of material, but in general, it is preferred to be more than 15 DEG C and less than 100 DEG C.If the crimping stations of bonder On when there is no warming-up device, as long as the use within the temperature range of room temperature.If more than 15 DEG C, die bond material Viscosity will not become too high, therefore can fully crimp.If less than 100 DEG C, die bond material will not start solidification, therefore, The thickness for the die bond material that can be achieved the goal.
Further, the present invention provides a kind of optical semiconductor device, and there is the above-mentioned die bond material by the present invention to carry out for it Solidfied material obtained by solidification.
The optical semiconductor device of the present invention, it has the die bond that will be made up of the heat-curing type silicon-ketone composition of the present invention Material solidified obtained by solidfied material, therefore with heat resistance, light resistance and crumpling resistance.
The optical semiconductor device of the present invention, can be manufactured in the following manner：Adding by the present invention is coated with substrate After the die bond material that thermohardening type silicon-ketone composition is constituted, according to conventional known method, optical semiconductor is subjected to die bond.
Hereinafter, for one of embodiment of optical semiconductor device of the invention, illustrated with reference to diagram.Fig. 1 It is the profile for an example for representing the optical semiconductor device of the present invention, wherein, the optical semiconductor device has will be by this The die bond material that the heat-curing type silicon-ketone composition of invention is constituted solidified obtained by solidfied material.Light shown in Fig. 1 is partly led Body device is on the 1st lead electrode 3 of the framework 1 of package substrate, with by by the heat-curing type silicone combination of the present invention The die bond material 5 that thing is constituted solidified obtained by solidfied material, and the bearing semiconductor element 2 on the solidfied material.The light is partly led The electrode of volume elements part 2, is to be electrically connected by gold thread 6 with the 1st lead electrode 3.In addition, the electricity of the optical semiconductor 2 Pole, is to be electrically connected by gold thread 7 with the 2nd lead electrode 4.In addition, the optical semiconductor 2, is to utilize sealing resin 8 To be sealed.
As the manufacture method of Fig. 1 optical semiconductor device, following methods can be exemplified as.
First, on the 1st lead electrode 3 of the framework 1 of package substrate, quantitative transfer is by heat-curing type silicon of the invention The die bond material 5 that one compositions are constituted, and the carrying optical semiconductor 2 on the die bond material 5.Next, to die bond material Material 5 is heating and curing.Next, the electrode of optical semiconductor 2 is electrically connected with the 1st lead electrode 3 using gold thread 6 Connect, the electrode of semiconductor element 2 is electrically connected with the 2nd lead electrode 4 using gold thread 7, photosemiconductor is carried to obtain The package substrate of element 2.Then, sealing resin 8 is quantitatively coated with, by the sealing resin being coated with known condition of cure, Solidified according to known curing, thus, it is possible to be sealed to package substrate.As with by the present invention die bond Material solidified obtained by solidfied material luminescent semiconductor device, for example, LED, semiconductor laser, optical diode, Photistor (phototransistor), solar cell, charge coupling device (charge coupled device, CCD) etc..
[embodiment]
Hereinafter, embodiment and comparative example are provided, the present invention is specifically described, but the present invention is not limited to following examples. (in following formula, Me represents methyl.)
[preparation example]
(preparation example 1~3)
Following component is stirred and mixed, the silicon-ketone composition of the composition shown in table 1 is prepared.
[(A) composition]
(A-1)
Organopolysiloxane represented by following formula, is with MA：M：Q=1：4：6 ratio come include MA units, M units, Q units, and molecular weight is 5000, the molecular weight is the weight average molecular weight converted with polystyrene.
(A-2)
Organopolysiloxane represented by following formula.(in following formula, Me represents methyl.)
(A-3)
Organopolysiloxane represented by following formula, is with MA-D：D：T=2：6：7 ratio includes MA-D units, D Unit, T unit, and molecular weight is 3500, the molecular weight is the weight average molecular weight converted with polystyrene.(in following formula, Me Represent methyl.)
The blended amount of (A) composition of preparation example 1~3, as shown in table 1.
[table 1]
Preparation example 1 Preparation example 2 Preparation example 3
(A-1) 80 70
(A-2) 20 30 40
(A-3) 60
[(B) composition]
(B-1)
As diacyl peroxide, two (3- methyl benzoyls) peroxide (Di- (3- can be directly used Methylbenzoyl) peroxide), benzoyl (3- methyl benzoyls) peroxide (Benzoyl- (3- Methylbenzoyl) peroxide) and dibenzoyl peroxide (Dibenzol peroxide) (trade name：Niper BMT-K40, Japanese grease limited company manufacture).
(B-2)
As peroxy esters, the peroxide -2 ethyl hexanoic acid tert-butyl ester (t-Butyl peroxy-2- can be directly used Ethylhexanoate) (trade name：Perbutyl O, Japanese grease limited company manufacture).
(B-3)
As dialkyl peroxide, tert-butyl cumyl peroxide (t-Butyl cumyl can be directly used Peroxide) (trade name：Perbutyl C, Japanese grease limited company manufacture).
[(C) composition]
(C-1)
Reactive silicone oil (the trade name that side chain contains epoxy radicals can be used directly for：X-22-343, SHIN-ETSU HANTOTAI's chemical industry Limited company manufactures).
(C-2)
As the silane compound containing epoxy radicals, glycidoxypropyltrime,hoxysilane (business can be directly used The name of an article：KBM-403, Shin-Estu Chemical Co., Ltd's manufacture).
(C-3)
, can be directly using 2,4,6,8- tetramethyls represented by following formula as the silicone compounds containing epoxy radicals Base -2,4,6,8- four [β-(3,4- expoxycyclohexyls) ethyl] cyclotetrasiloxane (trade name：X-40-2670, SHIN-ETSU HANTOTAI's chemistry work Industry limited company manufactures).
(C-4)
As the silane compound for not containing epoxy radicals, 3- methacryloxypropyl trimethoxies can be directly used Silane (trade name：KBM-503, Shin-Estu Chemical Co., Ltd's manufacture).
[embodiment 1~6]
(embodiment 1)
Mass parts of silicon-ketone composition 100 that preparation example 1 as (A) composition is obtained, (B-1) as (B) composition 10 mass parts, (C-1) 4 mass parts as (C) composition, the mass parts (product of aerosol silica 7 as supporting material Name：REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, And carry out decompression de-bubble to manufacture resin combination.
(embodiment 2)
Mass parts of silicon-ketone composition 100 that preparation example 2 as (A) composition is obtained, (B-1) as (B) composition 10 mass parts, (C-1) 4 mass parts as (C) composition, the mass parts (product of aerosol silica 7 as supporting material Name：REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, And carry out decompression de-bubble to manufacture resin combination.
(embodiment 3)
Mass parts of silicon-ketone composition 100 that preparation example 3 as (A) composition is obtained, (B-1) as (B) composition 10 mass parts, (C-1) 4 mass parts as (C) composition, the mass parts (product of aerosol silica 7 as supporting material Name：REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, And carry out decompression de-bubble to manufacture resin combination.
(embodiment 4)
Mass parts of silicon-ketone composition 100 that preparation example 1 as (A) composition is obtained, (B-2) 5 as (B) composition Mass parts, (C-1) 4 mass parts as (C) composition, the mass parts (ProductName of aerosol silica 7 as supporting material： REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, is gone forward side by side Row depressurizes de-bubble to manufacture resin combination.
(embodiment 5)
Mass parts of silicon-ketone composition 100 that preparation example 1 as (A) composition is obtained, (B-2) 5 as (B) composition Mass parts, (C-2) 4 mass parts as (C) composition, the mass parts (ProductName of aerosol silica 7 as supporting material： REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, is gone forward side by side Row depressurizes de-bubble to manufacture resin combination.
(embodiment 6)
Mass parts of silicon-ketone composition 100 that preparation example 1 as (A) composition is obtained, (B-1) as (B) composition 10 mass parts, (C-3) 5 mass parts as (C) composition, the mass parts (product of aerosol silica 7 as supporting material Name：REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, And carry out decompression de-bubble to manufacture resin combination.
[comparative example 1~4]
(comparative example 1)
Mass parts of silicon-ketone composition 100 that preparation example 1 as (A) composition is obtained, (B-3) 5 as (B) composition Mass parts, (C-1) 4 mass parts as (C) composition, the mass parts (ProductName of aerosol silica 7 as supporting material： REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, is gone forward side by side Row depressurizes de-bubble to manufacture resin combination.
(comparative example 2)
Mass parts of silicon-ketone composition 100 that preparation example 1 as (A) composition is obtained, (B-1) 5 as (B) composition Mass parts, (C-4) 4 mass parts as (C) composition, the mass parts (ProductName of aerosol silica 7 as supporting material： REOLOSIL DM-30S, TOKUYAMA limited companies manufacture) mixing, kneading processing further is carried out with three rollers, is gone forward side by side Row depressurizes de-bubble to manufacture resin combination.
(comparative example 3)
Mass parts of silicon-ketone composition 100 that preparation example 1 as (A) composition is obtained, (B-1) 5 as (B) composition Mass parts, without (C) composition, be used as the mass parts (ProductName of aerosol silica 7 of supporting material：REOLOSIL DM- 30S, TOKUYAMA limited company manufacture) mixing, kneading processing is further carried out with three rollers, and carries out decompression de-bubble to come Manufacture resin combination.
(comparative example 4)
Following component is mixed：
The mass parts of silicone oil 35, its average composition formula is MViD300MVi；
The mass parts of silicone resin 65, it is by M units, MViUnit and Q units are constituted, and relative to MViUnit, M units Mol ratio be 6.25, relative to Q units, M units and MViTotal mol ratio of unit is 0.8；
The mass parts of methyl hydrogen siloxane 8, its average formula is by MDH 80M is represented；
The mass parts of toluene solution 0.06 containing chloroplatinic acid/1,3- divinyl tetramethyl disiloxane complex compound, and institute The pt atom content for stating toluene solution is 1 mass %；
Acetylene basic ring mass parts of alcohol 0.05；
The mass parts of γ-glycidoxypropyltrime,hoxysilane 3；And,
It is used as the mass parts (ProductName of aerosol silica 7 of supporting material：REOLOSIL DM-30S, TOKUYAMA strand Part Co., Ltd manufacture)；
Kneading processing is further carried out with three rollers, and carries out decompression de-bubble to prepare silicone die bond material.
In addition, in above-mentioned silicone die bond material, to represent that the mark of average composition of each composition is represented with lower unit.
M：(CH3)3SiO1/2
MVi：(CH2=CH) (CH3)2SiO1/2
DH：(CH3)HSiO2/2
D：(CH3)2SiO2/2
Q：SiO4/2
For embodiment, the composition of comparative example, following various characteristics are measured.It the results are shown in Table 2.
[measurement of haze measurement and full light transmittance]
Mist degree and full light are carried out using the haze meter NDH-5000SP of Japanese electricity Se Industries, Incs manufacture The measurement of penetrance.Mixed sample will be carried out with above-mentioned condition, and the thick sample cells (cell) of 2mm be poured into, with defined bar Part (embodiment 1~6, comparative example 2~4 are 150 DEG C, 4 hours, and comparative example 1 is 170 DEG C, 1 hour) is heating and curing, and is obtained The solidfied material that surface is clean and 2mm is thick is obtained, the solidfied material is installed on measurement portion to measure.Measurement 3 times, tries to achieve mist degree Value, the average value of full light transmittance.
[making of optical semiconductor package]
Package substrate [SMD5050 (the I-CHIUN of the LED with recess as LED package substrates are prepared respectively PRECISION limited companies manufacture, and resin portion is polyphthalamide (PPA；Polyphthalamide))], make The BXCD33 manufactured for the Bridgelux limited companies of optical semiconductor, wherein the recess is for loading light half Conductor element, and it is provided with silver-plated the 1st lead electrode and the 2nd lead electrode in the bottom of the recess.
Using bonder (ASM limited companies manufacture, AD-830), by the various die bonds shown in embodiment and comparative example Material, by way of punching press, is quantitatively needed on the 1st silver-plated lead electrode of package substrate, and in the die bond material Upper carrying optical semiconductor.The carrying condition of optical semiconductor now is 13 milliseconds of crimping time, crimps loading 60gf, Carried out without using heating apparatus and in the environment of 25 DEG C of room temperature.Next, package substrate is put into baking oven, make various die bonds Material is heating and curing (embodiment 1~6, comparative example 2~4 are 150 DEG C, 4 hours, and comparative example 1 is 170 DEG C, 1 hour).Next, Using gold thread (Tanaka's electronics industry limited company manufacture, 25 μm of line footpath (FA)) by the electrode of optical semiconductor and the 1st Lead electrode is electrically connected, and will partly be led using gold thread (Tanaka's electronics industry limited company manufactures, 25 μm of line footpath (FA)) The electrode of volume elements part is electrically connected with the 2nd lead electrode.Thus, each a piece of LED for carrying optical semiconductor is obtained to use Package substrate (so as to encapsulate for number be 120).
Then, above-mentioned the obtained LED package substrates for carrying photosemiconductor of half are taken (with for encapsulating number It is 60), using dispenser (Musashi high-tech limited company manufactures, Super Σ CM II), quantitatively it is coated with silicone close Closure material (ProductName：KER2500, Shin-Estu Chemical Co., Ltd's manufacture), and entered with 150 DEG C, 4 hours of condition Row encapsulant is heating and curing.
Manner described above, makes the different optical semiconductor package of die bond material, and use it for tests below.
[temperature cycling test]
By obtained using the above method be filled with the optical semiconductor package of encapsulant 10, for temperature Cyclic test (- 40 DEG C~125 DEG C, each 20 minutes, carry out 1000 circulations), utilizes the photosemiconductor after microscope viewing test The jointing material portion of packaging body whether there is fragmentation, and calculates the quantity of chipping optical semiconductor package.
[high temperature dot lantern test]
By obtained using the above method be filled with the optical semiconductor package of encapsulant 10, at high temperature After (85 DEG C), energization 150mA, lighting 1000 hours, micro- sem observation optical semiconductor and carrying optical semiconductor are utilized Recess bottom between whether there is the situation of Poor cohesion such as peel off, whether there is fragmentation occur and optical semiconductor around it is viscous Close layer whether there is discoloration, and calculate the quantity for the optical semiconductor package for occurring abnormal appearance.
[chip shear test (Die shear test)]
10 in the unfilled optical semiconductor package for having an encapsulant that will be obtained using the above method, at 25 DEG C Interior, carry out core using measurer for pulling force (bond tester) (Dage limited companies manufacture, Series 4000) The measurement of piece shear strength, and the average value of the measured value obtained is represented with MPa.
The result of acquisition is shown in table 2.
[table 2]
As shown in table 2, embodiment 1~6 is to use the heat-curing type silicon-ketone composition for meeting the scope of the invention as solid Brilliant material, wherein, from the result of full light transmittance, mist degree, the embodiment 1~6 can obtain consolidating for high transparency Compound, will not be chipping after temperature cycling test, and whole packaging bodies can carry out lighting.Even if in addition, carrying out High temperature dot lantern test, composition is in appearance and unchanged, and whole packaging bodies can carry out lighting.Further, by The result of Die shear measurement is understood, can manufacture bonding force height and the high luminescent semiconductor device of reliability.
On the other hand, comparative example 1 is the silicone resin component for using (B) composition not meet the scope of the invention, wherein, by Full light transmittance, the result of mist degree understand that its transparency is good, but in the heat-curing step of die bond material and can not It is sufficiently carried out solidification, it is impossible to obtain good solidfied material.Therefore, there is generation in temperature cycling test, high temperature dot lantern test The situation of fragmentation, in Die shear measurement experiment, can not also obtain sufficient bonding strength.
Comparative example 2 is the silicone resin component for using (C) composition not meet the scope of the invention, wherein, worn by full light Saturating rate, the result of mist degree understand that its transparency is good, but can not be entered in the heat-curing step of die bond material and fully Row solidification, it is impossible to obtain good solidfied material.Therefore, there are chipping feelings in temperature cycling test, high temperature dot lantern test Condition, in Die shear measurement experiment, can not also obtain sufficient bonding strength.
The formula of comparative example 3 is not added with (C) composition, wherein, from the result of full light transmittance, mist degree, its is transparent Property be good, in the heat-curing step of die bond material, although be sufficiently carried out solidification, but easily it is chipping, therefore, In temperature cycling test, high temperature dot lantern test, there is very low probability chipping, and in Die shear measurement experiment, Sufficient bonding strength can not be obtained.
Comparative example 4 is to use general silicone resin as die bond material, can by the result of full light transmittance, mist degree Know, can not be the solidfied material of high transparency.Not chipping after temperature cycling test, whole packaging bodies can be carried out Lighting, even if in addition, carrying out high temperature dot lantern test, resin combination is in appearance and unchanged, and whole packaging bodies can Enough carry out lighting.On the other hand, the result of Die shear measurement, is compared to the thing of the present invention, the bonding force of comparative example 4 compared with It is low.
In addition, the present invention is not limited to above-mentioned embodiment.Above-mentioned embodiment is example, as long as have and this hair The substantially identical composition of technological thought described in bright claims and the technical scheme for playing same action effect, all In the technical scope for being included in the present invention.

Claims (8)

1. a kind of heat-curing type silicon-ketone composition, it is characterised in that contain following component：
(A) organopolysiloxane of the structure represented in the molecule with least one by following formulas (1)：100 mass parts；
In formula (1), m is any one in 0,1,2, R1It is hydrogen atom, phenyl or halogenated phenyl, R2It is hydrogen atom or methyl, R3It is Through substituteding or unsubstituted and can be with 1 valency organic group of identical or different carbon number 1~12, Z1It is-R4-、-R4-O-、-R4 (CH3)2Any of Si-O-, Z2It is oxygen atom or through substituteding or unsubstituted and can be with identical or different carbon number 1 ~10 divalent organic group, wherein, R4It is through substituteding or unsubstituted and can be with the divalent of identical or different carbon number 1~10 Organic group；
(B) comprising more than a kind of the organic peroxide in diacyl peroxide, peroxy esters：Relative to foregoing (A) into The mass parts of total amount 100 divided are 0.1~20 mass parts；And,
(C) silane compound containing epoxy radicals or the silicone compounds containing epoxy radicals：Relative to the conjunction of foregoing (A) composition It is 0.1~20 mass parts to measure 100 mass parts.
2. heat-curing type silicon-ketone composition as claimed in claim 1, wherein, the Z of the organopolysiloxane of foregoing (A) composition1 It is-R4-, foregoing Z2It is oxygen atom.
3. heat-curing type silicon-ketone composition as claimed in claim 1, wherein, the Z of the organopolysiloxane of foregoing (A) composition1 It is-R4- O- or-R4(CH3)2Si-O-, foregoing Z2It is through substituteding or unsubstituted and can be with identical or different carbon number 1~10 Divalent organic group.
4. heat-curing type silicon-ketone composition as claimed any one in claims 1 to 3, wherein, foregoing (A) composition it is organic Polysiloxanes, the structure represented in the molecule with least one by following formulas (2)：
In formula (2), m, R1、R2、R3、R4It is same as described above.
5. the heat-curing type silicon-ketone composition as any one of Claims 1-4, wherein, in having for foregoing (A) composition In machine polysiloxanes, (the SiO with more than 0.1mol%2) unit.
6. the heat-curing type silicon-ketone composition as any one of claim 1 to 5, wherein, by foregoing heat-curing type Silicon-ketone composition solidified obtained by thickness 2mm solidfied material, its full light transmittance is more than 80%, and haze value is Less than 20%.
7. a kind of die bond material, it is characterised in that be as the heat-curing type silicone group any one of claim 1 to 6 Compound is constituted.
8. a kind of optical semiconductor device, it is characterised in that obtained by the die bond material described in claim 7 is solidified Solidfied material.
CN201580065668.7A 2014-12-08 2015-10-19 The optical semiconductor device of heat-curing type silicon oxygen composition, the die bond material that the composition is constituted and the solidfied material with the die bond material Active CN107001769B (en)

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