CN105778409A - Epoxy resin composition for semiconductor packaging, and preparation method thereof - Google Patents
Epoxy resin composition for semiconductor packaging, and preparation method thereof Download PDFInfo
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- CN105778409A CN105778409A CN201410795874.0A CN201410795874A CN105778409A CN 105778409 A CN105778409 A CN 105778409A CN 201410795874 A CN201410795874 A CN 201410795874A CN 105778409 A CN105778409 A CN 105778409A
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Abstract
The invention relates to an epoxy resin composition for semiconductor packaging, and a preparation method thereof. The preparation method comprises the following steps: adding a curing agent phenolic resin, a curing accelerator, a mold lubricant, a fire retardant and a low stress modifier to a reaction kettle, carrying out hot melting mixing at 120-180DEG C, stirring until uniformity, cooling the obtained mixture to room temperature, crushing the cooled mixture, carrying out ball milling, and sieving the ball-milled mixture by a sieve; uniformly stirring the above obtained powder, epoxy resin, an inorganic filler, a coloring agent and a silane coupling agent in a high speed stirrer; and mixing and extruding the above obtained mixture in a double screw extruder, cooing the extruded mixture, and crushing the cooled mixture to obtain the epoxy resin composition for semiconductor packaging. The epoxy resin composition for semiconductor packaging has the advantages of increase of the yield in the packaging process, good mold release performance, great increase of the packaging frequency, and reduction of the incidence rate of pores in packaged bodies in packaging of semiconductor devices and integrated circuits.
Description
Technical field
The present invention relates to the composition epoxy resin of semiconductor-sealing-purpose, be related specifically to the composition epoxy resin of semiconductor-sealing-purpose that can improve composition epoxy resin encapsulated moulding and preparation method thereof.
Background technology
In recent years, semicon industry develops rapidly, and the composition epoxy resin of semiconductor-sealing-purpose be it is also proposed higher requirement: improve the mouldability of encapsulation process, good release property, longer clear mould cycle, the fillibility that package interior is higher;Traditional processing mode, owing to component is too much, homogenizer and twin screw extrusion cannot ensure the uniformity of mixing, final product also easily occurs that release property is poor, the clear mould cycle is short, package interior has the problems such as pore, and studying the new processing mode of this composition epoxy resin to improve these problems is one of currently the most important ones direction.
List of references: CN1700973A, CN1654538A, CN201310272431.9.
Summary of the invention
An object of the present invention is to provide has excellent encapsulated moulding, good release property, and in the longer clear mould cycle, package interior has the composition epoxy resin of the semiconductor-sealing-purpose of higher fillibility.
The two of the purpose of the present invention are the modes by processing technology, composition epoxy resin product stripping to solve current semiconductor-sealing-purpose is poor, the clear mould cycle is short, package interior has the problems such as pore, thus the method that the composition epoxy resin of a kind of semiconductor-sealing-purpose preparing purpose one is provided.
The component of the composition epoxy resin of the semiconductor-sealing-purpose of the present invention and content is:
The preparation method of the composition epoxy resin of the semiconductor-sealing-purpose of the present invention is through the following steps that realize:
(1) it is 3.5~15wt% according to the content of the composition epoxy resin epoxy resin of semiconductor-sealing-purpose, the content of firming agent phenolic resin is 3.1~10wt%, the content of inorganic filler is 70~90wt%, the content of curing accelerator is 0.16~0.8wt%, the content of releasing agent is 0.3~0.5wt%, the content of low stress modified dose is 0.7~0.9wt%, the content of coloring agent is 0.4~0.6wt%, the content of fire retardant is the content of 0.5~3wt% and silane coupler is that 0.4~0.6wt% weighs above-mentioned raw materials;
(2) the good firming agent phenolic resin that step (1) weighed, curing accelerator, releasing agent, fire retardant and low stress modified dose are put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, room temperature it is cooled to after stirring, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, crosses screen cloth (screen cloth of preferred mistake 70 order);Then epoxy resin, inorganic filler, coloring agent and silane coupler that the powder obtained and step (1) weigh are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose can be shaped further.
Described epoxy resin is have the monomer of more than 2 epoxide groups, oligomer or polymer in 1 epoxy molecule, and its molecular weight and molecular structure are not particularly limited.Described epoxy resin can be selected from one or more in o-cresol formaldehyde epoxy resin, bisphenol A type epoxy resin, bisphenol f type epoxy resin, linear phenolic epoxy resin, biphenyl type epoxy resin, dicyclopentadiene type epoxy resin, open chain aliphatic epoxy resin, cycloaliphatic epoxy resin, heterocyclic-type epoxy resin etc..
Described firming agent phenolic resin is have the monomer of more than 2 hydroxyls, oligomer or polymer in 1 phenolic aldehyde molecule, and its molecular weight and molecular structure are not particularly limited.Described phenolic resin can be selected from one or more in the copolymer of phenol linear phenolic resin and derivant, phenyl methylcarbamate linear phenolic resin and derivant, monohydroxy or dihydroxy naphthlene phenolic resin and derivant, xylol and phenol or the condensation substance of naphthols, dicyclopentadiene and phenol etc..
Described inorganic filler is not particularly limited.Described inorganic filler can be selected from one or more in fine silica powder, alumina powder, titanium oxide fine powder, silicon nitride powder, aluminium nitride micropowder etc..Fine silica powder can be powdered quartz micropowder or fusion fine silica powder;Described fusion fine silica powder can be dihedral micropowder or ball-type micropowder.Wherein, it is preferred to use the fusion fine silica powder of ball-type.Above-mentioned powdered quartz micropowder and fusion fine silica powder can be used alone or mix use.Additionally, the surface of described fine silica powder can use silane coupler to carry out surface treatment (high-speed stirred mixing).
Described curing accelerator, as long as the curing reaction of epoxy radicals and phenolic hydroxyl group can be promoted, is not particularly limited.The general content in the composition of described curing accelerator is 0.16~0.8wt%;One or more in imidazolium compounds, tertiary amine compound and organic phosphine compound etc. can be selected from.
One or more in 2-methylimidazole, 2,4-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole and 2-(heptadecyl) imidazoles etc. of described imidazolium compounds.
Described tertiary amine compound selected from triethylamine benzyl group dimethylamine, Alpha-Methyl benzyl group dimethylamine, 2-(dimethylamino methyl) phenol, 2,4,6-tri-(dimethylamino methyl) phenol and 1,8-diazabicyclo (5,4,0) one or more in endecatylene-7 grade.
One or more in triphenylphosphine, trimethyl-phosphine, triethyl phosphine, tributylphosphine, three (p-methylphenyl) phosphines and three (nonyl phenyl) phosphine etc. of described organic phosphine compound.
The general content in the composition of described releasing agent is 0.3~0.5wt%;One or more in Brazil wax, synthetic wax and mineral wax can be selected from.
The general content in the composition of described low stress modified dose is 0.7~0.9wt%;Such as liquid silicone oil, silicone rubber powder or their mixture etc..
The general content in the composition of described coloring agent is 0.4~0.6wt%;Such as white carbon black.
The general content in the composition of described fire retardant is 0.5~3wt%, and including the mixture of brominated epoxy resin and antimony oxide, wherein brominated epoxy resin is 5:1 with the mass ratio of antimony oxide.
The general content in the composition of described silane coupler is 0.4~0.6wt%;One or more in γ-glycidyl propyl ether trimethoxy silane, γ aminopropyltriethoxy silane, γ mercaptopropyitrimethoxy silane and γ-aminopropyltrimethoxysilane can be selected from.
Various raw materials involved in the composition epoxy resin of the semiconductor-sealing-purpose of the present invention all commercially obtain.The preparation method of the composition epoxy resin of semiconductor-sealing-purpose provided by the present invention, can obtain and there is excellent encapsulated moulding, good release property, the longer clear mould cycle, package interior has the composition epoxy resin of the semiconductor-sealing-purpose of higher fillibility, and the performance of compositions is more stable.Use this can improve the composition epoxy resin of the semiconductor-sealing-purpose of composition epoxy resin encapsulated moulding and carry out semiconductor device and integrated antenna package, the yield rate in encapsulation process can be improved, demolding performace is good and Encapsulation Moulds time is significantly increased, and reduces the incidence rate of package interior pore.
Below in conjunction with embodiment, the present invention is further illustrated, but they are not intended that limitation of the invention, for those skilled in the art, according to some nonessential change and adjustment that the present invention does, is accordingly to be regarded as and is within the scope of the present invention.
Detailed description of the invention
Composition in embodiment is as follows:
O-cresol formaldehyde epoxy resin A1 (Japan's DICCorporation system " N-665 ")
Phenol linear phenolic resin B1 (Japan's DICCorporation system " TD-2131 ")
2-methylimidazole C1
1,8-diazabicyclo (5,4,0) endecatylene-7C2
Fine silica powder D (d50 is 25 μm)
Brazil wax E
γ-glycidyl propyl ether trimethoxy silane F
White carbon black G
Liquid silicone oil H1
Silicone rubber powder H2
Mixture (mass ratio the is 5:1) I of brominated epoxy resin and antimony oxide
Biphenyl type epoxy resin A2 (JapanEpoxyResinsCo., Ltd. system " YX-4000H ")
Dicyclopentadiene type epoxy Resin A 3 (Japan's DICCorporation system " HP-7200 ")
Phenol alkyl phenolic resin (phenol linear phenolic resin derivant) B2 (MitsuiChemicals, Inc. system " XLC-4L ")
Triphenylphosphine C3
Embodiment 1
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B1, C2 and C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A1, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-22O.
Embodiment 2
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B2, C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A2, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 3
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B1, C1 and C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A3, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 4
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B2, C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A1, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 5
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B2, C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A3, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 6
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B1 and B2, C3, E, H1 and H2, I raw material are put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A1, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 7
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B1, C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A2 and A3, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 8
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B2, C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A1, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 9
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B1, C3, E, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A1, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Embodiment 10
Above-mentioned various raw materials are weighed according to the content proportioning in table 1, and load weighted B1, C1 and C2, H1 and H2, I raw material is put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, after stirring, cooling down is to room temperature, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, and crosses the screen cloth of 70 orders;The powder obtained and load weighted A1 and A3, D, F and G raw material are stirred in homogenizer;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.The composition epoxy resin of gained semiconductor-sealing-purpose is shaped further, carries out the result of performance evaluation in Table 1 after the composition epoxy resin of molding is encapsulated TO-220.
Comparative example 1~10
The composition of compositions is with embodiment 1~10, and preparation method uses the method that traditional each component melt extrudes after directly mixing, and the same above-described embodiment of method of evaluating performance, Evaluation results is in Table 2.
Table 1: the composition of the composition epoxy resin of embodiment 1~10 and content and Evaluation results (by weight percentage)
Table 2: the Evaluation results of comparative example
Be can be seen that by the Evaluation results of above-described embodiment and comparative example, the composition epoxy resin of the semiconductor-sealing-purpose that the preparation method of the use present invention obtains, compared with the composition epoxy resin using conventional extrusion techniques to prepare, the clear mould cycle of the composition epoxy resin that the method for the use present invention obtains is improved, and reduces the incidence rate of pore.
Claims (11)
1. a composition epoxy resin for semiconductor-sealing-purpose, is characterized in that: the key component of described composition epoxy resin and content is:
2. the composition epoxy resin of semiconductor-sealing-purpose according to claim 1, is characterized in that: one or more in o-cresol formaldehyde epoxy resin, bisphenol A type epoxy resin, bisphenol f type epoxy resin, linear phenolic epoxy resin, biphenyl type epoxy resin, dicyclopentadiene type epoxy resin, open chain aliphatic epoxy resin, cycloaliphatic epoxy resin, heterocyclic-type epoxy resin of described epoxy resin.
3. the composition epoxy resin of semiconductor-sealing-purpose according to claim 1, is characterized in that: one or more in the copolymer of phenol linear phenolic resin and derivant, phenyl methylcarbamate linear phenolic resin and derivant, monohydroxy or dihydroxy naphthlene phenolic resin and derivant, xylol and phenol or the condensation substance of naphthols, dicyclopentadiene and phenol of described phenolic resin.
4. the composition epoxy resin of semiconductor-sealing-purpose according to claim 1, is characterized in that: one or more in fine silica powder, alumina powder, titanium oxide fine powder, silicon nitride powder, aluminium nitride micropowder of described inorganic filler.
5. the composition epoxy resin of semiconductor-sealing-purpose according to claim 4, is characterized in that: described fine silica powder is selected from powdered quartz micropowder, fusion fine silica powder or their mixture;
Described fusion fine silica powder is dihedral micropowder or ball-type micropowder.
6. the composition epoxy resin of semiconductor-sealing-purpose according to claim 1, is characterized in that: one or more in imidazolium compounds, tertiary amine compound and organic phosphine compound of described curing accelerator.
7. the composition epoxy resin of semiconductor-sealing-purpose according to claim 6, it is characterized in that: one or more in 2-methylimidazole, 2,4-methylimidazoles, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole and 2-(heptadecyl) imidazoles of described imidazolium compounds;
Described tertiary amine compound selected from triethylamine benzyl group dimethylamine, Alpha-Methyl benzyl group dimethylamine, 2-(dimethylamino methyl) phenol, 2,4,6-tri-(dimethylamino methyl) phenol and 1,8-diazabicyclo (5,4,0) one or more in endecatylene-7;
One or more in triphenylphosphine, trimethyl-phosphine, triethyl phosphine, tributylphosphine, three (p-methylphenyl) phosphines and three (nonyl phenyl) phosphine of described organic phosphine compound.
8. the composition epoxy resin of semiconductor-sealing-purpose according to claim 1, is characterized in that: one or more in Brazil wax, synthetic wax and mineral wax of described releasing agent.
9. the composition epoxy resin of semiconductor-sealing-purpose according to claim 1, is characterized in that: described low stress modified dose is liquid silicone oil, silicone rubber powder or their mixture.
10. the composition epoxy resin of semiconductor-sealing-purpose according to claim 1, is characterized in that: described coloring agent is white carbon black;
Described fire retardant is the mixture of brominated epoxy resin and antimony oxide, and wherein brominated epoxy resin is 5:1 with the mass ratio of antimony oxide;
One or more in γ-glycidyl propyl ether trimethoxy silane, γ aminopropyltriethoxy silane, γ mercaptopropyitrimethoxy silane and γ-aminopropyltrimethoxysilane of described silane coupler.
11. a preparation method for the composition epoxy resin of the semiconductor-sealing-purpose described in claim 1~10 any one, it is characterized in that:
(1) it is 3.5~15wt% according to the content of the composition epoxy resin epoxy resin of semiconductor-sealing-purpose, the content of firming agent phenolic resin is 3.1~10wt%, the content of inorganic filler is 70~90wt%, the content of curing accelerator is 0.16~0.8wt%, the content of releasing agent is 0.3~0.5wt%, the content of low stress modified dose is 0.7~0.9wt%, the content of coloring agent is 0.4~0.6wt%, the content of fire retardant is the content of 0.5~3wt% and silane coupler is that 0.4~0.6wt% weighs above-mentioned raw materials;
(2) the good firming agent phenolic resin that step (1) weighed, curing accelerator, releasing agent, fire retardant and low stress modified dose are put in reactor, it is 120~180 DEG C in temperature to carry out heat and melt mixing, room temperature it is cooled to after stirring, heat is melted mixture pulverizing that is rear and that be cooled to room temperature, ball milling, crosses screen cloth;Then epoxy resin, inorganic filler, coloring agent and silane coupler that the powder obtained and step (1) weigh are stirred in blender;The mixture that will stir is melting mixing extrusion in double screw extruder, cooling, pulverizing, obtains the composition epoxy resin of semiconductor-sealing-purpose.
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