CN1687229A - Method for preparing composition of epoxy resin for packaging semiconductor - Google Patents
Method for preparing composition of epoxy resin for packaging semiconductor Download PDFInfo
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- CN1687229A CN1687229A CN 200510038942 CN200510038942A CN1687229A CN 1687229 A CN1687229 A CN 1687229A CN 200510038942 CN200510038942 CN 200510038942 CN 200510038942 A CN200510038942 A CN 200510038942A CN 1687229 A CN1687229 A CN 1687229A
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Abstract
The present invention relates to a preparation method of epoxy resin compound for semiconductor packaging process. Said epoxy resin compound has the advantages of low-viscosity, high-flowability, low water absorption and low porosity, etc. and can be used for packaging various integrated circuits and semiconductor devices.
Description
Technical field
The present invention relates to a kind of preparation method of composition epoxy resin, particularly a kind of preparation method who is used for the composition epoxy resin of semiconductor packages.
Background technology
Along with developing rapidly of semicon industry, the semiconductor packages industry has also obtained development fast.As a kind of epoxy resin composition for semiconductor encapsulation, with advantages such as its low cost, good reliabilitys and used widely, account for more than 95% of semiconductor sealing material.Under the variation trend that electronic technology is maked rapid progress, unicircuit just develops rapidly towards ultra-large, ultra-high speed, high-density, high-power, high precision, multi-functional direction, thereby the composition epoxy resin that unicircuit is encapsulated usefulness has also proposed more and more higher requirement.Viscosity is an important factor that influences the composition epoxy resin encapsulation performance always, in the process of plastic packaging, plastic cement directly has influence on the performance of unicircuit to the size of spun gold surging force, viscosity can cause the spun gold distortion when big and cause short circuit, thereby reduce yield rate.Yet, the preparation method of existing composition epoxy resin can not satisfy produce possess low-viscosity, the composition epoxy resin of the performance requriements in high workability, weak breath hole.Therefore, the new production technique of research is produced this kind composition epoxy resin and is just seemed particularly important.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, a kind of preparation method who is used for the composition epoxy resin of semiconductor packages is provided, composition epoxy resin with this method preparation has good flowability, and pore also seldom occurs when the semiconductor packages moulding.
Technical problem to be solved by this invention can realize by following technical scheme.The present invention is a kind of preparation method who is used for the composition epoxy resin of semiconductor packages, is characterized in, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 70-110 degree centigrade, and stir, after cooling, be crushed to particle diameter again and will account for 70% of Resins, epoxy and phenolic resin amount of the mixture at least less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 70-130 degree centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of preparation method who is used for the composition epoxy resin of semiconductor packages, be characterized in, described Resins, epoxy is biphenyl type epoxy resin, and described solidifying agent resol is the phenol lacquer resins, and described curing catalyst is phosphorous/tertiary amines curing catalyst.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of preparation method who is used for the composition epoxy resin of semiconductor packages, be characterized in, described compound inorganic stuffing is the mixture of being made up of the silica flour of A, B, three kinds of different-grain diameters of C, and wherein the median size of A part is 0.05-1 μ m, accounts for the 4-15% of filler total amount; The median size of B part is 1-20 μ m, accounts for the 45-70% of filler total amount; The median size of C part is 20-45 μ m, accounts for the 20-35% of filler total amount.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of preparation method who is used for the composition epoxy resin of semiconductor packages is characterized in, the median size of described compound inorganic stuffing is 5-40 μ m.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of preparation method who is used for the composition epoxy resin of semiconductor packages is characterized in that the loading level of described compound inorganic stuffing is the 80%-92% of composition epoxy resin gross weight.Like this, can guarantee that its flowability can significantly not descend, the water-intake rate of finished product is low, the yield rate height of encapsulating products.
Each raw material optimum weight of using in the inventive method is: the Resins, epoxy of 4-20 part, the solidifying agent resol of 2-15 part, 0.01-1 the curing catalyst of part, the compound inorganic stuffing of 60-92 part, 0.01-2 the releasing agent of part, 0.01-1 the tinting material of part, the fire retardant of 0.01-3 part, the coupling agent of 0.01-1 part.
Resins, epoxy used in the present invention can be biphenyl type epoxy resin, ortho-cresol linear epoxy resin, polyfunctional group type Resins, epoxy, dihydroxyphenyl propane-type Resins, epoxy, aliphatic epoxy resin, heterocyclic-type epoxy resin etc.The Resins, epoxy that wherein has can be used alone or as a mixture.Preferred biphenyl type epoxy resin, polyfunctional group type Resins, epoxy and heterocyclic-type epoxy resin.
Solidifying agent resol used in the present invention, can be the multipolymer etc. of condenses, phenol-ing fixed agent dicyclopentadiene and the phenol of polyfunctional group solidifying agent, phenol lacquer resins and its derivative, phenyl methylcarbamate lacquer resins, p-Xylol and phenol or naphthols, they can use separately also can mix use.
Curing catalyst used in the present invention, can be 2, glyoxaline compounds such as 4-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, triethylamine benzyldimethylamine, 1, tertiary amine compound such as 8-diazabicyclo (5,4,0) undecylene-7 grade, organic phosphine compounds such as triphenylphosphine, three (p-methylphenyl) phosphine, they can use separately also can mix use.
Compared with prior art, use the prepared composition epoxy resin of the inventive method to have advantages such as low-viscosity, high workability, low water absorption, weak breath hole, that its performance can satisfy is ultra-large, the demand of ultra-high speed, high-density, high-power, high precision, multifunctional integrated circuit encapsulation; The composition epoxy resin of using the inventive method preparation carries out the encapsulation of various unicircuit and semiconducter device, can significantly reduce bad phenomenon such as dashing silk, layering, pore, improve the encapsulation yield rate of various unicircuit and semiconducter device, thereby reduce cost.The prepared composition epoxy resin of the inventive method is applicable to various unicircuit of encapsulation and semiconducter device.
Embodiment
Embodiment 1.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 80 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 70% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 100 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
Embodiment 2.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 110 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 80% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 130 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
The compound inorganic stuffing of present embodiment is the mixture of being made up of the silica flour of A, B, three kinds of different-grain diameters of C, and wherein the median size of A part is 1 μ m, accounts for 15% of filler total amount; The median size of B part is 10 μ m, accounts for 60% of filler total amount; The median size of C part is 30 μ m, accounts for 25% of filler total amount, and the loading level of described compound inorganic stuffing is 80% of a composition epoxy resin gross weight.
Embodiment 3.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 90 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 75% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 120 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
The compound inorganic stuffing of present embodiment is the mixture of being made up of the silica flour of A, B, three kinds of different-grain diameters of C, and wherein the median size of A part is 0.05 μ m, accounts for 4% of filler total amount; The median size of B part is 1 μ m, accounts for 70% of filler total amount; The median size of C part is 20 μ m, accounts for 26% of filler total amount, and the loading level of described compound inorganic stuffing is 87% of a composition epoxy resin gross weight.
Embodiment 4.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 70 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 85% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 70 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
The compound inorganic stuffing of present embodiment is the mixture of being made up of the silica flour of A, B, three kinds of different-grain diameters of C, and wherein the median size of A part is 0.5 μ m, accounts for 10% of filler total amount; The median size of B part is 20 μ m, accounts for 55% of filler total amount; The median size of C part is 45 μ m, accounts for 35% of filler total amount, and the loading level of described compound inorganic stuffing is 92% of a composition epoxy resin gross weight.
Embodiment 5.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 100 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 90% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 110 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
The compound inorganic stuffing of present embodiment is the mixture of being made up of the silica flour of A, B, three kinds of different-grain diameters of C, and wherein the median size of A part is 0.1 μ m, accounts for 15% of filler total amount; The median size of B part is 15 μ m, accounts for 50% of filler total amount; The median size of C part is 40 μ m, accounts for 35% of filler total amount, and the loading level of described compound inorganic stuffing is 89% of a composition epoxy resin gross weight.
Embodiment 6.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 85 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 78% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 95 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
The median size of the compound inorganic stuffing of present embodiment is 5 μ m.The loading level of described compound inorganic stuffing is 80% of a composition epoxy resin gross weight.
Embodiment 7.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 105 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 72% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 115 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
The median size of the compound inorganic stuffing of present embodiment is 40 μ m.The loading level of described compound inorganic stuffing is 82% of a composition epoxy resin gross weight.
Embodiment 8.A kind of preparation method who is used for the composition epoxy resin of semiconductor packages, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 75 degrees centigrade, and stir, after cooling, be crushed to particle diameter again and account for 82% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 85 degrees centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
The median size of the compound inorganic stuffing of present embodiment is 20 μ m.The loading level of described compound inorganic stuffing is 90% of a composition epoxy resin gross weight.
Embodiment 9.Be detection and the result thereof that the contriver does the finished product that adopts the inventive method to produce below.
The finished product preparation.Select 1. Resins, epoxy for use: 60 grams; 2. resol: 52 grams; 3. phosphorous curing catalyst/tertiary amines curing catalyst: 1.5/1.0 gram; 4. compound inorganic stuffing: A part 78 grams, B part 532 grams, C part 358 grams; 5. carbon black: 4 grams; 6. carnauba wax: 4 grams; 7. coupling agent: 5mL; 8. fire retardant: 3 grams.This kind composition epoxy resin is made in accordance with the following methods: at first, with 1. load weighted and 2., under 100 degrees centigrade, carry out heat and melt and mix, through cooling, be crushed to particle diameter and account for 70% of Resins, epoxy and phenolic resin amount of the mixture less than the amount of the powder of 250um.Secondly, with 4. load weighted and 7. carry out pre-treatment, and stir.At last, with above handle well 1.+2. and 4.+7., and 3. 5. 6. 8. carry out pre-mixing, high-speed stirring, mix, under 130 degrees centigrade condition, carry out melting mixing, again through calendering, cooling, meal, fine powder (granularity is below the 0.5mm), after mix, beat series of process flow processs such as cake, packing, get final product finished product.
Test with following method:
1, gelation time GT: get the sample (powder) of about 1 ~ 2 gram, be placed on the electric heating plate (175 ± 2 ℃) and test.
2, helicoidal flow length SF: taking by weighing the sample (powder) of 15 grams, is that (175 ± 2 ℃), injection pressure are 3.5Mpa (35Kg/cm in mobile die temperature
2), mold pressure is 21Mpa (210Kg/cm
2), injection moulding speed is under the condition of 6cm/sec, in die for molding, solidify and recorded in 2 ~ 3 minutes.
3, water-absorbent: sample is made the disk of Φ 100 * 2 (mm), and under the condition of 100 ℃/24h, carry out after fixing, then successively: oven dry-drying-weighing m according to GB1034-86
1-boil-the dried surface of sassafras-weighing m
2The calculating of water-intake rate: Wp=(m
2-m
1)/m
1* 100%,
4, viscosity: the CFT heightization instrument that flows, sample is made Φ 100 * 2g, under 150 ℃/10kg condition, test obtaining.
5, pore: powerful microscope and infrared scan.Test result (seeing the following form):
| Index parameter | ? ????GT(sec) | ? ????21 |
| ????SF(cm) | ????124 | |
| Viscosity (Pa.s) | ????21.5 | |
| Water-intake rate | ????0.11 | |
| Pore | No |
Claims (5)
1, a kind of preparation method who is used for the composition epoxy resin of semiconductor packages is characterized in that, its step is as follows,
(1) with load weighted Resins, epoxy and solidifying agent resol, in reactor, carry out heat and melt mixing with 70-110 degree centigrade, and stir, after cooling, be crushed to particle diameter again and will account for 70% of Resins, epoxy and phenolic resin amount of the mixture at least less than the amount of the powder of 250um;
(2), in homogenizer, carry out surface treatment, and stir with silane coupling agent with load weighted compound inorganic stuffing;
(3) with above Resins, epoxy and solidifying agent resol mixed powder, the compound inorganic stuffing of anticipating, and minor component curing catalyst, tinting material, releasing agent, coupling agent and fire retardant carry out high-speed stirring in mixing machine, mixes;
(4) mixture with step (3) carries out melting mixing through the through-hole type twin screw extruder, its melting temperature is set in 70-130 degree centigrade, being broken to granularity through calendering, cooling, coarse reduction, fine powder again is that 0.5mm is following, the back is mixed, beaten cake, packaging process, promptly.
2, a kind of preparation method who is used for the composition epoxy resin of semiconductor packages according to claim 1, it is characterized in that, described Resins, epoxy is biphenyl type epoxy resin, described solidifying agent resol is the phenol lacquer resins, and described curing catalyst is phosphorous/tertiary amines curing catalyst.
3, a kind of preparation method who is used for the composition epoxy resin of semiconductor packages according to claim 1, it is characterized in that, described compound inorganic stuffing is the mixture of being made up of the silica flour of A, B, three kinds of different-grain diameters of C, wherein the median size of A part is 0.05-1 μ m, accounts for the 4-15% of filler total amount; The median size of B part is 1-20 μ m, accounts for the 45-70% of filler total amount; The median size of C part is 20-45 μ m, accounts for the 20-35% of filler total amount.
4, a kind of preparation method who is used for the composition epoxy resin of semiconductor packages according to claim 1 is characterized in that, the median size of described compound inorganic stuffing is 5-40 μ m.
5, a kind of preparation method who is used for the composition epoxy resin of semiconductor packages according to claim 1 is characterized in that, the loading level of described compound inorganic stuffing is the 80%-92% of composition epoxy resin gross weight.
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| CNB200510038942XA CN100335541C (en) | 2005-04-15 | 2005-04-15 | Method for preparing composition of epoxy resin for packaging semiconductor |
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|---|---|---|---|
| CNB200510038942XA CN100335541C (en) | 2005-04-15 | 2005-04-15 | Method for preparing composition of epoxy resin for packaging semiconductor |
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| CN1687229A true CN1687229A (en) | 2005-10-26 |
| CN100335541C CN100335541C (en) | 2007-09-05 |
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| CN110642998A (en) * | 2019-08-27 | 2020-01-03 | 中山精合电子材料有限公司 | Epoxy resin composition, curable dry film, cured product and printed circuit board |
| CN111978678A (en) * | 2020-08-31 | 2020-11-24 | 江苏华海诚科新材料股份有限公司 | Epoxy resin composition and preparation method thereof |
| CN111978678B (en) * | 2020-08-31 | 2023-09-19 | 江苏华海诚科新材料股份有限公司 | Epoxy resin composition and preparation method thereof |
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| CN100335541C (en) | 2007-09-05 |
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