CN102807757A - Organic silica gel used for packaging IGBT (insulated gate bipolar translator) module, and preparation method of organic silica gel - Google Patents
Organic silica gel used for packaging IGBT (insulated gate bipolar translator) module, and preparation method of organic silica gel Download PDFInfo
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- CN102807757A CN102807757A CN2012102693655A CN201210269365A CN102807757A CN 102807757 A CN102807757 A CN 102807757A CN 2012102693655 A CN2012102693655 A CN 2012102693655A CN 201210269365 A CN201210269365 A CN 201210269365A CN 102807757 A CN102807757 A CN 102807757A
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- TYNQIKSJQXDLNA-UHFFFAOYSA-N C[SiH]1O[Si+](C)(CC=C)O[Si](C)(C)O1 Chemical compound C[SiH]1O[Si+](C)(CC=C)O[Si](C)(C)O1 TYNQIKSJQXDLNA-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- H01L2224/48091—Arched
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- 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
- H01L2224/481—Disposition
- H01L2224/48135—Connecting between different semiconductor or solid-state bodies, i.e. chip-to-chip
- H01L2224/48137—Connecting between different semiconductor or solid-state bodies, i.e. chip-to-chip the bodies being arranged next to each other, e.g. on a common substrate
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- 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
- H01L2224/73—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/10—Details of semiconductor or other solid state devices to be connected
- H01L2924/11—Device type
- H01L2924/13—Discrete devices, e.g. 3 terminal devices
- H01L2924/1304—Transistor
- H01L2924/1305—Bipolar Junction Transistor [BJT]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/10—Details of semiconductor or other solid state devices to be connected
- H01L2924/11—Device type
- H01L2924/13—Discrete devices, e.g. 3 terminal devices
- H01L2924/1304—Transistor
- H01L2924/1305—Bipolar Junction Transistor [BJT]
- H01L2924/13055—Insulated gate bipolar transistor [IGBT]
Abstract
The invention relates to an organic silica gel used for packaging an IGBT (insulated gate bipolar translator) module and a preparation method of the organic silica gel. The organic silica gel comprises a component A and a component B according to the weight proportion of 1:1, wherein the component A comprises the following raw materials by weight part: 94 to 99.89 parts of base material, 0.01 to 5 parts of silane coupling agent, and 0.1 to 1 part of catalyst; the component B comprises the following raw materials by weight part: 79 to 95 parts of base material, 5 to 15 parts of crosslinking agent, 0.01 to 5 parts of fire retardant and 0.1 to 1 part of inhibitor. The organic silica gel used for packaging the IGBT module has excellent optical property, high strength, low oil leakage, and fire resistance, is transparent, is solidified fast at high temperature, is capable of satisfying the long-term operating requirements under high and/or low temperature environments, and is mainly beneficial to sealing and encapsulation protection of the IGBT modules.
Description
Technical field
The present invention relates to silicon gel that a kind of IGBT module package uses and preparation method thereof, belong to the Embedding Material technical field.
Background technology
At present, the sealing of medium-high frequency IGBT module, embedding is defensive is high lead solder, and the used solder containing pb of IGBT accounts for 90% of the leaded application of used IC.Solder containing pb contains the deleterious element of the mankind plumbous, and European Union and RoHS prohibite use, replace it so need choose some lead-free solders.
The kind of the packaged material of IGBT module has a lot, the three major types that mainly contains commonly used: epoxy resin, organosilicon and urethane.
Epoxy resin is good to the mechanically resistant material bonding force, and hardness is high, and insulating property and heat resistance are good, and technology is simple, but it can't reach snappiness after solidifying, and has certain internal stress, and reparation property is poor, generally all can't realize large quantities of volume productions.
The cementability of urethane is between epoxy and organosilicon, and temperature tolerance is not high, generally is no more than 100 ℃.Its intensity is good, and resistance to low temperature is good, and price is also low relatively.But the toxicity of the preparation technology that it is complicated and and being restricted itself.
Silicon gel is a kind of environment-friendly solvent-free type material, can not emit low molecule when carrying out embedding, and unstressed contraction has certain elasticity, can absorb shockwave, will avoid chip to be damaged like this.It has no corrosion, can deep layer vulcanization, be transparent after the sulfuration, and be convenient to observe the components and parts of encapsulation like this, carry out the detection and the reparation of element.Its high and low temperature resistance is good, and cost is also relatively low.Can play protection against the tide, dustproof, protection against corrosion, shockproof effect.The ubiquitous problem of existing silicon gel is an oil impregnate, goes rancid, and can't accomplish the requirement of transparent flame-retarding, and cementability sticking power also relatively poor and body material is less etc.
Summary of the invention
Technical problem to be solved by this invention provides silicon gel that a kind of IGBT module package uses and preparation method thereof; The silicon gel that IGBT module package of the present invention is used is a kind of flame retardant resistance silicon gel that has the good optical performance and can satisfy the HS that life-time service requires under the high and low temperature environment, transparent, low oil impregnate, high temperature rapid curing, is mainly used in sealing, the embedding protection of IGBT module.
The technical scheme that the present invention solves the problems of the technologies described above is following: the silicon gel that a kind of IGBT module package is used is that A component and the B component of 1:1 formed by weight proportion, wherein
Said A component is made up of the raw material of following weight part: 94～99.89 parts of base-materials, 0.01～5 part of silane coupling agent, 0.1～1 part of catalyzer;
Said B component is made up of the raw material of following weight part: 79～95 parts of base-materials, 5～15 parts of linking agents, 0.01～5 part of fire retardant, 0.1～1 part in suppressor factor;
Wherein, said base-material is that the organopolysiloxane that contains alkenyl and the mixture or the said base-material that contain the liquid MQ resin of vinyl are the mixture that contains the organopolysiloxane of alkenyl and contain the liquid MT resin of vinyl.
The invention has the beneficial effects as follows: the silicon gel that IGBT module package of the present invention is used is the room temperature of no coupling product after a kind of environment-friendly solvent-free, odorlessness, the curing or the transparent embedding silicon gel that heats quick-setting add-on type; The A component provides vinyl in reaction, the B component provides linking agent.
The viscosity of the silicon gel that IGBT module package of the present invention is used is lower and controlled, has excellent flame-retardant performance, and the wettability that flows is easy to perfusion, can solidifies in the deep.It is very soft, can isolate moisture and other pollutent, alleviates the mechanical stress that machinery, thermal shocking and vibrations cause, holding circuit, and continuous plug still keeps auto repair capacity to IGBT module embedding member.
The silicon gel that IGBT module package of the present invention is used has the ideal mechanical property: gel hardness (g) reaches 90～140, cone penetration 35～65, tensile strength 0.01～0.3MPa; Do not produce xanthochromia under 150 ℃; Have ideal dielectric insulation performance: dielectric strength is 10～20Kv/mm, and volume specific resistance is 6.5*10
15～9.5*10
15Ω/cm, flame retardant properties is good, and cold-resistant thermal shocking property is good, can be ideally suited in the IGBT embedding that optical property and mechanical property is had harsh requirement.
The present invention is applicable to sealing, the embedding of components and parts such as medium-high frequency IGBT module, silicon rectifier module, silicon controlled module, special chip, air filter, is that a broad-spectrum industrial electronic is used type material, and is as shown in Figure 1.
On the basis of technique scheme, the present invention can also do following improvement.
Further, said silane coupling agent is γ-(2, the 3-glycidoxy) propyl trimethoxy silicane; γ-(methacryloxy) propyl trimethoxy silicane; γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, vinyltriethoxysilane; Vinyltrimethoxy silane, any one in vinyl three ('beta '-methoxy-oxyethyl group) silane;
Adopt the beneficial effect of above-mentioned further scheme to be: adopt silane coupling agent can eliminate internal stress, avoid solidifying the demixing phenomenon of back silicon gel, increase the silicon gel viscosity and with the adhesiveproperties at interface, and improve the weather resistance of silicon gel.
Further, said catalyzer is a noble metal catalyst;
Further, said noble metal catalyst is a kind of or any several kinds of mixing in rhodium system, iridium system, ruthenium system, palladium system, the platinum group catalyst, is preferably platinum group catalyst;
Further, said platinum group catalyst is any one in the Platinic chloride, THF coordinate platinum catalyst, diethyl phthalate coordinate platinum catalyst, platinum-olefin(e)complex of Platinic chloride, pure modification, is preferably platinum-vinyl siloxane complex;
Adopt the beneficial effect of above-mentioned further scheme to be: catalyzer adds the addition reaction that can promote silicon hydrogen, shortens set time, thereby quickens to solidify, and improves flame retardant properties.
Further, said platinum-vinyl siloxane complex content is 1000～10000ppm;
Adopt the beneficial effect of above-mentioned further scheme to be: the add-on of platinum-vinyl siloxane complex only need be enough to effectively get final product as hydrosilylation reaction catalyst; This amount can change according to required solidification rate; If this amount is excessive, it is uneconomical that this reaction will become;
Further, said fire retardant is phosphoric acid ester material or phosphorous acid esters material;
Further, said phosphoric acid ester material is a tritolyl phosphate, triaryl phosphate, triphenylphosphate; Triethyl phosphate, tri-2-ethylhexyl phosphate, three (2-chloroethyl) SULPHOSUCCINIC ACID ESTER; Three (1,3-two chloro-2-propyl group) SULPHOSUCCINIC ACID ESTER, isopropylation triphen SULPHOSUCCINIC ACID ESTER; In the dihydroxyphenyl propane-two (diphenyl phosphoester) any one, said phosphorous acid esters material is a triphenyl phosphite, effect is aryl phosphoric acids Ester or aromatic yl phosphite class material preferably;
The beneficial effect that adopts above-mentioned further scheme is that fire retardant is nontoxic, stable, and non-volatile, its adding not only can improve the flame retardant properties of silicon gel; And can guarantee the water white requirement of silicon gel, it also has toughness reinforcing, and is wear-resisting; Weather-proof, anlistatig function.
Further, said suppressor factor is alkynol class material, contains alkylene annular siloxane oligopolymer, benzotriazole that any one in the triphenylphosphine is preferably alkynol class material;
Further, said alkynol class material is 3-methyl isophthalic acid-butine-3-alcohol, the 1-ethynylcyclohexanol, and 3-propyl group-ethyl acetylene-3-alcohol, any one in 3-octyl group-ethyl acetylene-3-alcohol is preferably the 1-ethynylcyclohexanol;
The beneficial effect that adopts above-mentioned further scheme is the working hour that the adding of suppressor factor has prolonged silicon gel of the present invention, has improved the package stability of silicon gel;
Further, the said liquid MQ resin that contains vinyl is other raw material of refining level, and viscosity is 1000～10000 centipoises, and the content of vinyl is 0.01～5wt%, and molecular formula is following:
(Me
3SiO
0.5)
a(ViMe
2SiO
0.5)
b(SiO
2) (molecular formula 1)
Wherein, a+b=1.3～1.5, a=0～1.5, b=0～1.5;
Adopt the beneficial effect of above-mentioned further scheme to be: the liquid MQ resin that contains vinyl can be regulated cross-linking density, as mechanical property, the flame retardant properties of supporting material with raising silicon gel;
Further, the said liquid MT resin that contains vinyl is other raw material of refining level, and viscosity is 1000～10000 centipoises, and the content of vinyl is 0.01～5wt%, and molecular formula is following:
(Me
3SiO
0.5)
a(ViMe
2SiO
0.5)
b(MeSiO
1.5) (molecular formula 2)
Wherein, (a+b)/c=1.3～1.5, a=0～1.5, b=0～1.5.
Adopt the beneficial effect of above-mentioned further scheme to be: the adding that contains the liquid MT resin of vinyl can increase cross-linking density, thereby has improved the intensity of silicon gel;
Further, said organopolysiloxane is that alkenyl is bonded in silicone oil molecule chain end, silicone oil molecular chain side chain or is bonded in the silicone oil molecule chain end and silicone oil molecular chain side chain.
Further, said alkenyl is a kind of in vinyl, allyl group, crotonyl, pentenyl, hexenyl, the heptenyl or any several kinds.
Further, when said alkenyl was vinyl, vinyl silicone oil was for contain organopolysiloxane or its mixture of two vinyl at least.
Adopt the beneficial effect of above-mentioned further scheme to be: the organopolysiloxane that contains vinyl can have straight chain; The straight chain of part branching; Side chain, ring-type or network molecular structure, or the mixture of these structures; The content of regulating vinyl effectively regulates the gel hardness of silicon gel, intensity and cone penetration etc.;
Further, said vinyl silicone oil is other raw material of refining level for being the organopolysiloxane of vinyl at silicone oil molecular chain two ends, and viscosity is 100～10000 centipoises, and the content of vinyl is 0.1～5wt%, and structural formula is following:
Adopt the beneficial effect of above-mentioned further scheme to be: through adjustment, can adjust the viscosity of system, thereby realize controlled to the convenience of viscosity to matrix silicon oil viscosity, consumption.
Further, said vinyl silicone oil is other raw material of refining level on silicone oil molecular chain two ends, side group, all to contain vinyl, and viscosity is 100～2000 centipoises, and the content of vinyl is 0.1～10wt%, and structural formula is following:
Adopt the beneficial effect of above-mentioned further scheme to be: the ZGK 5 that all contains vinyl at molecular chain-end and side group has than high reaction activity, and its introducing can be regulated cross-linking density, improves the intensity of silicon gel;
Further, said vinyl silicone oil is the vinyl ring body, and viscosity is 10～100 centipoises, and the content of vinyl is 25～35wt%, and structural formula is exemplified below:
(structural formula 3) (structural formula 4) (structural formula 5).
Adopt the beneficial effect of above-mentioned further scheme to be: to add the vinyl ring body and can increase substantially the intensity of silicon gel, and have the suppressor factor effect, can be used for adjusting set time and shelf lives, have anti-xanthochromia characteristic;
Further, said linking agent is to contain the organic hydrogen polysiloxanes that is bonded to the Wasserstoffatoms on the Siliciumatom in the containing hydrogen silicone oil molecule more than 3 or 3, and the content of Si-H key is 0.05%～5%wt, and wherein, said containing hydrogen silicone oil is other raw material of refining level;
Further, said linking agent is the organic hydrogen polysiloxanes that contains pendant hydrogen, and structural formula is following:
Adopt the beneficial effect of above-mentioned further scheme to be: this containing hydrogen silicone oil can provide the massfraction of the active hydrogen that can control; The massfraction of active hydrogen is high more, and the active site that can participate in crosslinking reaction in the system is just many more, and reactive behavior is just big more; Cross-linking density is just high more; Thereby effectively regulate the hardness of silicon gel, modulus, vulcanization rate.
Further, said linking agent is the organic hydrogen polysiloxanes that contains terminal hydrogen, and its structural formula is following:
Adopt the beneficial effect of above-mentioned further scheme to be: the end capped organic hydrogen polysiloxanes of active hydrogen has higher activity, and can be used as chainextender and use, intensity and the toughness that can regulate the silicon gel through the consumption of regulating it, thus optimize mechanical performance of products.
Further, said linking agent is the organic hydrogen polysiloxanes that contains terminal hydrogen, pendant hydrogen, and its structural formula is following:
Adopt the beneficial effect of above-mentioned further scheme to be: the cross-linking density of this linking agent is high, and cross-linking set is many, can effectively shorten set time, raises the efficiency;
Further, said linking agent is hydrogeneous ring body, and viscosity is 10～100 centipoises, and the content of its Si-H key is 0.05%～5%wt, and structural formula is following for example:
(structural formula 9) (structural formula 10) (structural formula 11)
The present invention also provides the preparation method of the silicon gel that a kind of IGBT module package uses, and comprising:
The preparation of A component: at normal temperatures, be 94～99.89 parts base-material with parts by weight, 0.01～5 part silane coupling agent, 0.1～1 part catalyzer adds in the stirrer successively, mixes, and promptly gets said A component;
The preparation of B component: at normal temperatures, be 79～95 parts base-material with parts by weight, 5～15 parts linking agent, 0.01～5 fire retardant, 0.1～1 part suppressor factor adds in the stirrer successively, mixes, and promptly gets said B component;
At normal temperatures; The weight proportion that said A component and B component are pressed 1:1 mixes, and the sizing material that mixes is placed deaeration under the vacuum, is poured into the sizing material that has taken off bubble and accomplishes the embedding operation in the component; The part room temperature that embedding is intact leaves standstill curing or is heating and curing, and gets final product.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the condition of said vacuum is 0.06～-0.1MPa, be preferably 0.09MPa;
Further, the said deaeration time is 10～30 minutes, is preferably 20 minutes;
Further, the said condition that is heating and curing is for heating 0.5～4 hour at 70～110 ℃; Perhaps 90～130 ℃ of heating 0.5～2 hour; Perhaps 130～200 ℃ were heated 0.5～1.5 hour.
The preparing method's of silicon gel of the present invention beneficial effect is: the preparation method of silicon gel of the present invention is simple to operate, process stabilizing, and operable time is long; It is fast to be heating and curing; Antistatic effect is good, keeps stable machinery and electric property at-50～200 ℃, low oil impregnate; Transmittance reaches 98.2～99.5%, and excellent storage stability.
The present invention will contain the liquid MQ resin of vinyl, the liquid MT resin that contains vinyl, containing hydrogen silicone oil, vinyl silicone oil (not comprising the vinyl ring body) and put into Rotary Evaporators; Resin and silicone oil are carried out underpressure distillation; Temperature is 120 ℃, refines about 3h, promptly gets other raw material of refining level.The material purity of the refining level that the present invention adopts is higher; Can avoid that low-boiling-point substance and silicone oil are micromolecular to ooze out; Through regulating silicon hydrogen and vinyl ratio; Making the unsaturated mole number and the ratio of Si-H mole number is 0.6～1.0, avoids remaining too much vinyl, can significantly reduce and avoids oil impregnate and the phenomenon of going rancid through said process.
Description of drawings
The application synoptic diagram of the silicon gel that Fig. 1 uses for IGBT module package of the present invention;
In the accompanying drawing, the list of parts of each label representative is following:
1, scatterer, 2, heat-conducting silicone grease, 3, the base plate weld tabs, 4, igbt chip; 5, first bonding wire, 6, diode, 7, second bonding wire, 8, the silicon gel; 9, main electrode, 10, internal electrode, 11, the bond lead-in wire, 12, bonding; 13, first copper film, 14, pottery, 15, second copper film, 16, base plate.
Embodiment
Below principle of the present invention and characteristic are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
Embodiment 1
The preparation of A component: taking by weighing viscosity is the both-end vinyl ZGK 5 (contents of ethylene 0.3wt%) of 500cps, like structural formula 1, and 86.7g, viscosity is that the end, side vinyldimethicone (contents of ethylene 6wt%) of 100cps is like structural formula 2; 6.0g ethylene liquid MQ resin is like molecular formula 1 (contents of ethylene 1.3wt%; A=1.28, b=0.02), 4.0g; γ-(methacryloxy) propyl trimethoxy silicane 3.0g, platinum-vinyl siloxane complex catalyzer 0.3g, content 7000ppm; Add successively in the stirrer, mixing and stirring promptly gets said A component;
The preparation of B component: taking by weighing viscosity is the both-end vinyl ZGK 5 (contents of ethylene 0.7wt%) of 100cps, like structural formula 1, and 83.47g, ethylene liquid MQ resin; As molecular formula 1 (contents of ethylene=1.3wt%, a=1.28, b=0.02), 6.0g; Polymethyl hydrogen siloxane, like structural formula 6,10.0g, triaryl phosphate 0.5g; 1-ethynylcyclohexanol 0.3g adds in the stirrer successively, and mixing and stirring promptly gets said B component;
The resin of A and B component and silicone oil are other raw material of refining level.
During use, with A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating 150 ℃ of heating 0.5 hour, get final product on to be packaged.
Embodiment 2
The preparation of A component: the both-end vinyl ZGK 5 (contents of ethylene 0.42wt%) that takes by weighing viscosity and be 500cps is like structural formula 1,83.6g, and vinyl ring body (contents of ethylene 30wt%) is like structural formula 4; 8.0g ethylene liquid MQ resin is like molecular formula 1 (contents of ethylene 3wt%, a=1.25; B=0.05), 3.0g, γ-(2; The 3-glycidoxy) propyl trimethoxy silicane 2.0g, platinum-vinyl siloxane complex catalyzer 0.4g, content 5000ppm; Add successively in the stirrer, mixing and stirring promptly gets said A component;
The preparation of B component: taking by weighing viscosity is the both-end vinyl ZGK 5 (contents of ethylene 0.12wt%) of 500cps, like structural formula 1, and 79.9g, ethylene liquid MQ resin such as molecular formula 1 (contents of ethylene 3wt%; A=1.25, b=0.05), 4.0g, end, side group polymethyl hydrogen siloxane; Like structural formula 8,15.0g, triphenylphosphate 1.0g, ethynylcyclohexanol 0.1g; Add successively in the stirrer, mixing and stirring promptly gets said B component;
The resin of A and B component and silicone oil are other raw material of refining level.
During use, with A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 15 minutes, some glue or encapsulating 125 ℃ of heating 1.25 hours, get final product on to be packaged.
Embodiment 3
The preparation of A component: the both-end vinyl ZGK 5 (contents of ethylene 0.1wt%) that takes by weighing viscosity and be 10000cps is like structural formula 1,83g, and viscosity is that the end, side vinyldimethicone (contents of ethylene 0.5wt%) of 2000cps is like structural formula 2,5.0g; Vinyl ring body (contents of ethylene 30wt%) is like structural formula 5,7.0g, ethylene liquid MT resin such as molecular formula 2 (contents of ethylene 3.6wt%; A=1.23, b=0.07), 3.0g; Vinyltriethoxysilane 1.0g, the complex compound catalyst 1.0g of Platinic chloride and divinyl tetramethyl disiloxane, content 2000ppm; Add successively in the stirrer, mixing and stirring promptly gets said A component;
The preparation of B component: the both-end vinyl ZGK 5 (contents of ethylene 1.2wt%) that takes by weighing viscosity and be 450cps is like structural formula 1,85.98g, ethylene liquid MT resin such as molecular formula 2 (contents of ethylene 3.6wt%, a=1.23; B=0.07), 5.0g, polymethyl hydrogen siloxane; Like structural formula 6 and structural formula 7 each 4.0g, isopropylation triphen SULPHOSUCCINIC ACID ESTER 1.0g, the pure 0.2g of 3-phenyl-ethyl acetylene-3; Add successively in the stirrer, mixing and stirring promptly gets said B component;
The resin of A and B component and silicone oil are other raw material of refining level.
During use, with said A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating 100 ℃ of heating 3.5 hours, get final product on to be packaged.
Comparative Examples 1
The preparation of A component: taking by weighing viscosity is the both-end vinyl ZGK 5 (contents of ethylene 0.3wt%) of 500cps, like structural formula 1, and 86.7g, viscosity is that the end, side vinyldimethicone (contents of ethylene 6wt%) of 500cps is like structural formula 2; 6.0g ethylene liquid MQ resin is like molecular formula 1 (contents of ethylene=1.3wt%; A=1.28, b=0.02), 4.0g; γ-(methacryloxy) propyl trimethoxy silicane 3.0g, platinum-vinyl siloxane complex 0.3g, content 7000ppm; Add successively in the stirrer, mixing and stirring promptly gets said A component;
The preparation of B component: the both-end vinyl ZGK 5 (contents of ethylene 0.7wt%) that takes by weighing viscosity and be 200cps is like structural formula 1,86.97g, ethylene liquid MQ resin such as molecular formula 1 (contents of ethylene=1.3wt%; A=1.28, b=0.02), 3.0g; Polymethyl hydrogen siloxane is like structural formula 6 and structural formula 7 each 5.0g, ethynylcyclohexanol 0.3g; Add successively in the stirrer, mixing and stirring promptly gets said B component;
The resin of A and B component and silicone oil are the raw material of common grade.
During use, with said A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating 150 ℃ of heating 0.5 hour, get final product on to be packaged.
Comparative Examples 2
The preparation of A component: the both-end vinyl ZGK 5 (contents of ethylene 0.42wt%) that takes by weighing viscosity and be 500cps is like structural formula 1,97.6g, γ-(2; The 3-glycidoxy) propyl trimethoxy silicane 2.0g; Platinum-vinyl siloxane complex catalyzer 0.4g, content 5000ppm adds in the stirrer successively; Mixing and stirring promptly gets said A component;
The preparation of B component: taking by weighing viscosity is the both-end vinyl ZGK 5 (contents of ethylene 0.12wt%) of 500cps, like structural formula 1,83.9g; End, side group polymethyl hydrogen siloxane are like structural formula 8,15.0g; Triaryl phosphate 1.0g, ethynylcyclohexanol 0.1g adds in the stirrer successively; Mixing and stirring promptly gets said B component;
The resin of A and B component and silicone oil are the raw material of common grade.
During use, with said A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 15 minutes, some glue or encapsulating 125 ℃ of heating 1.25 hours, get final product on to be packaged.
Comparative Examples 3
The preparation of A component: the both-end vinyl ZGK 5 (contents of ethylene 0.15wt%) that takes by weighing viscosity and be 1500cps is like structural formula 1,90g, and vinyl ring body (contents of ethylene 30wt%) is like structural formula 4; 8.0g, vinyltriethoxysilane 1.0g, the complex compound catalyst 1.0g of Platinic chloride and divinyl tetramethyl disiloxane; Content 2000ppm; Add successively in the stirrer, mixing and stirring promptly gets said A component;
The preparation of B component: the both-end vinyl ZGK 5 (contents of ethylene 1.2wt%) that takes by weighing viscosity and be 450cps is like structural formula 1,89.98g, polymethyl hydrogen siloxane; Like structural formula 8,8.0g, three (1; 3-two chloro-2-propyl group) SULPHOSUCCINIC ACID ESTER, 1.0g, 3-phenyl-ethyl acetylene-3 alcohol is 0.2g; Add successively in the stirrer, mixing and stirring promptly gets said B component;
The resin of A and B component and silicone oil are the raw material of common grade.
During use, with said A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating 100 ℃ of heating 3.5 hours, get final product on to be packaged.
The present invention has investigated the various performances of silicon gel; Physicals (outward appearance, kinematic viscosity, density); Mechanical property (cone penetration, gel hardness, tensile strength), optical property (transmittance, specific refractory power), electric property (specific inductivity, volume specific resistance); Flame retardant properties (oxygen index), weathering resistance (cold-resistant thermal shocking property).
The present invention is the A that makes among each embodiment, the B component, and 1:1 mixes by mass ratio, 125 ℃ of solidification values, time 75min, the standard of each test event is undertaken by following:
Adopt the UV, visible light spectrophotometer to press GB/T2410-80 and measure transmittance;
Adopt rubber tensile test machine to press the test of GB/T528-1988 tensile strength;
Adopt oxygen index instrument to press GB/T10707-1989 test oxygen index;
Adopt the cone penetration tester to press GB/T269-91 test cone penetration;
Adopt matter structure appearance to press ISO9665 test gel hardness;
Adopt YH-8200 numeral insulation resistance to press GBT1410-2006 test resistance rate;
Adopt dielectrometer to test specific inductivity according to GB-T1694-1981;
Select the silicon gel sample after 10g solidifies to make extraction test at apparatus,Soxhlet's, adopt normal hexane as solvent, the extraction time is 4 hours, and the mass loss of extraction back test silicon gel sample is as shown in table 1.
Table 1 performance index
Can find out that from table 1 embodiment 1～3 can realize that through changing the viscosity of component silicone oil the viscosity of silicon gel is controlled; Embodiment and Comparative Examples 1 and Comparative Examples 2, the adding of fire retardant has improved the flame retardant properties of this silicon gel; The adding of resin has improved the physical strength of silicon gel, adds to contain intensity and the toughness that the silicone oil of holding hydrogen can improve the silicon gel, chooses the phenomenon that the raw material of refining level can avoid oil impregnate to go rancid; And specific refractory power is all more than 1.40, and transmittance is all above 98%.
The present invention is applied in above the IGBT module package, and concrete diagram sees Fig. 1 for details, and the IGBT module package generally includes the parts of following key: scatterer 1, heat-conducting silicone grease 2, base plate weld tabs 3; Igbt chip 4, the first bonding wires 5, diode 6, the second bonding wires 7; Silicon gel 8, main electrode 9, internal electrode 10, the bond lead-in wire 11; Bonding 12, the first copper films 13, pottery 14, the second copper films 15; Base plate 16, the silicon gel normally is encapsulated between chip and the shell, plays protection interconnection and moistureproof, dustproof and shockproof effect.
The above is merely preferred embodiment of the present invention, and is in order to restriction the present invention, not all within spirit of the present invention and principle, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the silicon gel that the IGBT module package is used is characterized in that, is that A component and the B component of 1:1 formed by weight proportion, wherein
Said A component is made up of the raw material of following weight part: 94～99.89 parts of base-materials, 0.01～5 part of silane coupling agent, 0.1～1 part of catalyzer;
Said B component is made up of the raw material of following weight part: 79～95 parts of base-materials, 5～15 parts of linking agents, 0.01～5 part of fire retardant, 0.1～1 part in suppressor factor;
Wherein, said base-material is that the organopolysiloxane that contains alkenyl and the mixture or the said base-material that contain the liquid MQ resin of vinyl are the mixture that contains the organopolysiloxane of alkenyl and contain the liquid MT resin of vinyl.
2. silicon gel according to claim 1 is characterized in that, said silane coupling agent is γ-(2; The 3-glycidoxy) propyl trimethoxy silicane, γ-(methacryloxy) propyl trimethoxy silicane, γ-mercaptopropyl trimethoxysilane; Gamma-mercaptopropyltriethoxysilane; Vinyltriethoxysilane, vinyltrimethoxy silane, any one in vinyl three ('beta '-methoxy-oxyethyl group) silane;
Said catalyzer is a kind of or any several kinds of mixing in rhodium system, iridium system, ruthenium system, palladium system, the platinum group catalyst;
Said fire retardant is phosphoric acid ester material or phosphorous acid esters material;
Said suppressor factor is alkynol class material, contain alkylene annular siloxane oligopolymer, benzotriazole, any one in the triphenylphosphine.
3. silicon gel according to claim 2; It is characterized in that said platinum group catalyst is any one in the Platinic chloride, THF coordinate platinum catalyst, diethyl phthalate coordinate platinum catalyst, platinum-olefin(e)complex of Platinic chloride, pure modification;
Said phosphoric acid ester material is a tritolyl phosphate, triaryl phosphate, triphenylphosphate; Triethyl phosphate, tri-2-ethylhexyl phosphate, three (2-chloroethyl) SULPHOSUCCINIC ACID ESTER; Three (1,3-two chloro-2-propyl group) SULPHOSUCCINIC ACID ESTER, isopropylation triphen SULPHOSUCCINIC ACID ESTER; In the dihydroxyphenyl propane-two (diphenyl phosphoester) any one, said phosphorous acid esters material is a triphenyl phosphite;
Said alkynol class material is 3-methyl isophthalic acid-butine-3-alcohol, 1-ethynylcyclohexanol, 3-propyl group-ethyl acetylene-3-alcohol, any one in 3-octyl group-ethyl acetylene-3-alcohol.
4. silicon gel according to claim 1 is characterized in that, the said liquid MQ resin that contains vinyl is other raw material of refining level, and viscosity is 1000～10000 centipoises, and the content of vinyl is 0.01～5wt%, and molecular formula is following:
(Me
3SiO
0.5)
a(ViMe
2SiO
0.5)
b(SiO
2) (molecular formula 1)
Wherein, a+b=1.3～1.5, a=0～1.5, b=0～1.5;
The said liquid MT resin that contains vinyl is other raw material of refining level, and viscosity is 1000～10000 centipoises, and the content of vinyl is 0.01～5wt%, and molecular formula is following:
(Me
3SiO
0.5)
a(ViMe
2SiO
0.5)
b(MeSiO
1.5) (molecular formula 2)
Wherein, (a+b)/c=1.3～1.5, a=0～1.5, b=0～1.5.
5. silicon gel according to claim 1; It is characterized in that; Said organopolysiloxane is that alkenyl is bonded in silicone oil molecule chain end, silicone oil molecular chain side chain or is bonded in the silicone oil molecule chain end and silicone oil molecular chain side chain; When said alkenyl was vinyl, vinyl silicone oil was for contain organopolysiloxane or its mixture of two vinyl at least.
6. silicon gel according to claim 5 is characterized in that, said vinyl silicone oil is for being the organopolysiloxane of vinyl at silicone oil molecular chain two ends; Be other raw material of refining level; Viscosity is 100～10000 centipoises, and the content of vinyl is 0.1～5wt%, and structural formula is following:
(structural formula 1)
Perhaps
Said vinyl silicone oil is other raw material of refining level on silicone oil molecular chain two ends, side group, all to contain vinyl, and viscosity is 100～2000 centipoises, and the content of vinyl is 0.1～10wt%, and structural formula is following:
Perhaps
Said vinyl silicone oil is the vinyl ring body, and viscosity is 10～100 centipoises, and the content of vinyl is 25～35wt%, and structural formula is following:
(structural formula 3) (structural formula 4) (structural formula 5).
7. silicon gel according to claim 1 is characterized in that, said linking agent is to contain the organic hydrogen polysiloxanes that is bonded to the Wasserstoffatoms on the Siliciumatom in the containing hydrogen silicone oil molecule more than 3 or 3, and the content of Si-H key is 0.05%～5%wt,
Wherein, said containing hydrogen silicone oil is other raw material of refining level.
8. silicon gel according to claim 7 is characterized in that said linking agent is the organic hydrogen polysiloxanes that contains pendant hydrogen, and structural formula is following:
Perhaps
Said linking agent is the organic hydrogen polysiloxanes that contains terminal hydrogen, and structural formula is following:
Perhaps
Said linking agent is the organic hydrogen polysiloxanes that contains terminal hydrogen, pendant hydrogen, and structural formula is following:
Perhaps
Said linking agent is hydrogeneous ring body, and viscosity is 10～100 centipoises, and the content of its Si-H key is 0.05%～5%wt, and structural formula is following:
(structural formula 9) (structural formula 10) (structural formula 11)
9. the preparation method of the silicon gel used of an IGBT module package is characterized in that, comprising:
The preparation of A component: at normal temperatures, be 94～99.89 parts base-material with parts by weight, 0.01～5 part silane coupling agent, 0.1～1 part catalyzer adds in the stirrer successively, mixes, and promptly gets said A component;
The preparation of B component: at normal temperatures, be 79～95 parts base-material with parts by weight, 5～15 parts linking agent, 0.01～5 fire retardant, 0.1～1 part suppressor factor adds in the stirrer successively, mixes, and promptly gets said B component;
At normal temperatures, said A component and B component are pressed the weight proportion mixing of 1:1, and the sizing material that mixes is placed deaeration under the vacuum, are poured into the sizing material that has taken off bubble and accomplish the embedding operation in the component, and the part room temperature that embedding is intact leaves standstill curing or is heating and curing, and gets final product.
10. the preparation method of silicon gel according to claim 9 is characterized in that, the condition of said vacuum is 0.06～-0.1MPa, the deaeration time is 10～30 minutes; The said condition that is heating and curing is for heating 0.5～4 hour at 70～110 ℃; Perhaps 90～130 ℃ of heating 0.5～2 hour; Perhaps 130～200 ℃ were heated 0.5～1.5 hour.
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Application publication date: 20121205 |