CN105778411B - A kind of secondary mixing method of the composition epoxy resin of semiconductor-sealing-purpose - Google Patents
A kind of secondary mixing method of the composition epoxy resin of semiconductor-sealing-purpose Download PDFInfo
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- CN105778411B CN105778411B CN201410799095.8A CN201410799095A CN105778411B CN 105778411 B CN105778411 B CN 105778411B CN 201410799095 A CN201410799095 A CN 201410799095A CN 105778411 B CN105778411 B CN 105778411B
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Abstract
The present invention relates to the secondary mixing method of the composition epoxy resin of semiconductor-sealing-purpose.The present invention be by the composition epoxy resin for preparing semiconductor-sealing-purpose epoxy resin, phenolic resin curing agent, inorganic filler, releasing agent, low stress modified dose, colorant, fire retardant, silane coupling agent and inorganic ion scavenger be put into homogenizer, after stirring evenly, in temperature for 70~100 DEG C of progress melting mixings, tabletting after mixing cools down, is ground into powder；Then it is 70~100 DEG C of progress second melting mixings in temperature, tabletting, cooling, crushing after mixing obtain the composition epoxy resin of semiconductor-sealing-purpose after stirring evenly obtained powder and curing accelerator in homogenizer.The present invention uses secondary mixing method, can obtain with good mobility, and insolubles content is low, excellent encapsulated moulding, and leakage envelope ratio reduces, the composition epoxy resin of semiconductor-sealing-purpose that die sinking hardness improves.
Description
Technical field
The present invention relates to the preparation methods of the composition epoxy resin of semiconductor-sealing-purpose, can more particularly to improve epoxy
The secondary mixing method of the composition epoxy resin of the semiconductor-sealing-purpose of resin combination mobility and encapsulated moulding and
The composition epoxy resin of semiconductor-sealing-purpose.
Background technology
With the rapid development of semicon industry, semiconductor packaging industry is also developed rapidly；In recent years, semiconductor
Device develops, and develop to ultra-large direction to miniaturization, slimming and surface mounting technique direction, it is desirable that semiconductor packages
Material has good filling capacity, high mobility, fast curing properties.But traditional processing method being once kneaded is simultaneously
It does not improve on a large scale, the mixing method of composition epoxy resin relatively lags behind, and traditional one time melting mixing pattern is easy
Lead to the poor fluidity of composition epoxy resin, insoluble matter is more, and die sinking hardness is low.The size and number of insoluble matter directly affects half
The filling capacity of conductor encapsulation, because the impurity in composition epoxy resin is excessive or can excessively block encapsulation runner, causes sealing
Leakage envelope during dress, seriously affects the yield rate of encapsulation process, and poor fluidity is also easy to cause leakage envelope in end in encapsulation process
Phenomenon, die sinking lower hardness can cause the formation problems such as sticking to mould, disconnected muscle.
Bibliography：CN 201310272431.9
Invention content
It is an object of the present invention to by using second melting mixing method, to solve obtained by current preparation method
The problem of poor fluidity, the insoluble matter of the composition epoxy resin arrived are more, die sinking hardness is low a kind of prepare insoluble matter so as to provide
Content is low, mobility is high, the secondary mixing method of the composition epoxy resin of die sinking semiconductor-sealing-purpose with high hardness.
The second object of the present invention is to provide the semiconductor-sealing-purpose of second melting mixing method for use in the present invention
Composition epoxy resin.
The present invention epoxy resin composition for semiconductor encapsulation secondary mixing method through the following steps that realize：
(1) by the epoxy resin, phenolic resin curing agent, inorganic in the composition epoxy resin for preparing semiconductor-sealing-purpose
Filler, releasing agent, low stress modified dose, colorant, fire retardant, silane coupling agent and inorganic ion scavenger are put into high-speed stirring
It mixes in machine, after stirring evenly, in temperature for 70~100 DEG C of progress melting mixings, tabletting after mixing cools down, is ground into powder；
(2) curing in the powder for obtaining step (1) and the composition epoxy resin for preparing semiconductor-sealing-purpose promotes
After agent stirs evenly in homogenizer, in temperature for 70~100 DEG C of progress second melting mixings, tabletting after mixing, cooling,
It crushes, obtains the composition epoxy resin of semiconductor-sealing-purpose.
Equipment used in the melting mixing is included in double roll mill, single screw rod kneading machine, twin screw compounder
It is one or more of.When carrying out melting mixing using double roll mill, the time of melting mixing can be 4~8 minutes；It is using
When single screw rod kneading machine or twin screw compounder carry out melting mixing, the time of melting mixing is to add in single screw rod from raw material to mix
To extrusion in mill or twin screw compounder.The rotating speed of single screw rod kneading machine or twin screw compounder is usually 100~150 turns/
Minute.
The present invention also provides the epoxy resin of the semiconductor-sealing-purpose of second melting mixing method for use in the present invention
Composition, the component and content of the composition epoxy resin of the semiconductor-sealing-purpose are：
The epoxy resin is the monomer, oligomer or polymer for having in 1 epoxy molecule 2 or more epoxy groups,
Its molecular weight and molecular structure are not particularly limited.The epoxy resin can be selected from o-cresol formaldehyde epoxy resin, bisphenol-A type ring
Oxygen resin, bisphenol f type epoxy resin, linear phenolic epoxy resin, biphenyl type epoxy resin, dicyclopentadiene type epoxy resin,
One or more of open chain aliphatic epoxy resin, cycloaliphatic epoxy resin, heterocyclic-type epoxy resin etc..
The phenolic resin curing agent has the monomer, oligomer or polymerization of 2 or more hydroxyls for 1 phenolic aldehyde intramolecular
Object, molecular weight and molecular structure are not particularly limited.The phenolic resin can be selected from phenol linear phenolic resin and its spread out
Biology, phenyl methylcarbamate linear phenolic resin and its derivative, monohydroxy or dihydroxy naphthlene phenolic resin and its derivative, paraxylene
One or more of with the copolymer of the condensation product of phenol or naphthols, dicyclopentadiene and phenol etc..
The inorganic filler is not particularly limited.It is micro- that the inorganic filler can be selected from fine silica powder, aluminium oxide
One or more of powder, titanium oxide fine powder, silicon nitride powder, aluminium nitride micro mist etc..Fine silica powder can be crystal type
Fine silica powder or fusion fine silica powder；The fusion fine silica powder can be angular micro mist or ball-type
Micro mist.Wherein, it is preferable to use the fusion fine silica powder of ball-type.Above-mentioned powdered quartz micro mist and fusion dioxy
SiClx micro mist may be used alone or in combination.In addition, the surface of the fine silica powder can use it is silane coupled
Agent is surface-treated (high-speed stirred mixing).
The curing accelerator as long as can promote the curing reaction of epoxy group and phenolic hydroxyl group, is not particularly limited.Institute
The content of the curing accelerator stated generally in the composition is 0.16~0.8wt%；Imidazolium compounds, tertiary amine chemical combination can be selected from
One or more of object and organic phosphine compound etc..
The imidazolium compounds is selected from 2-methylimidazole, 2,4- methylimidazoles, 2-ethyl-4-methylimidazole, 2- benzene
One or more of base imidazoles, 2- phenyl -4-methylimidazole and 2- (heptadecyl) imidazoles etc..
The tertiary amine compound is selected from triethylamine benzyl group dimethylamine, Alpha-Methyl benzyl group dimethylamine, 2- (dimethylamino first
Base) one kind in -7 grade of phenol, (dimethylamino methyl) phenol of 2,4,6- tri- and 1,8- diazabicyclos (5,4,0) endecatylene
It is or several.
The organic phosphine compound is selected from triphenylphosphine, trimethyl-phosphine, triethyl phosphine, tributylphosphine, three (to methylbenzene
One or more of base) phosphine and three (nonyl phenyl) phosphines etc..
The content of the releasing agent generally in the composition is 0.3~0.5wt%；Brazil wax can be selected from, closed
Into one or more of wax and mineral matter wax.
The general content in the composition of described low stress modified dose is 0.7~0.9wt%；Such as liquid silicone oil, silicon rubber
Rubber powder end or their mixture etc..
The content of the colorant generally in the composition is 0.4~0.6wt%；Such as carbon black.
The content of the fire retardant generally in the composition is 0.5~10wt%；The fire retardant is selected from bromo ring
One or more of oxygen, antimony oxide, zinc molybdate, zinc borate, magnesium hydroxide and aluminium hydroxide.
The range of the grain size d50 of zinc molybdate, zinc borate, magnesium hydroxide and aluminium hydroxide etc. in the fire retardant is all
0.1~10 μm, ranging from 0.2~2.0 μm of preferable particle size d50.
The content of the silane coupling agent generally in the composition is 0.4~0.6wt%；γ-epoxy third can be selected from
Base propyl ether trimethoxy silane, γ aminopropyltriethoxy silane, γ mercaptopropyitrimethoxy silane and γ-ammonia third
One or more of base trimethoxy silane.
One in compound of the inorganic ion scavenger selected from hydrated metal oxide, acid metal salt and magnalium
Kind is several；
The hydrated metal oxide is Bi2O3·3H2O；The acid metal salt is Zr (HPO4)2·H2O；Institute
The compound for the magnalium stated is Mg6Al2(CO3)(OH)16·4H2O。
Various raw materials involved by the composition epoxy resin of the semiconductor-sealing-purpose of the present invention are commercially
It obtains.The secondary mixing method of epoxy resin composition for semiconductor encapsulation provided by the present invention, can obtain with good
Mobility, insolubles content is low, excellent encapsulated moulding, and leakage envelope ratio reduces, the semiconductor-sealing-purpose that die sinking hardness improves
Composition epoxy resin.Temperature of the traditional melting mixing pattern in melting mixing is higher, is easy to cause gained ring
Insolubles content in epoxy resin composition is more, and the present invention is temperature during each melting mixing using secondary mixing method
It is all relatively low, make the insolubles content in gained composition epoxy resin low or do not have substantially, uniformity is good, and the performance of composition is more
Add excellent.Partly leading for composition epoxy resin mobility and encapsulated moulding is improved using what the method for the present invention was prepared
The composition epoxy resin of body encapsulation carries out semiconductor devices and integrated antenna package, can improve the finished product in encapsulation process
Rate reduces leakage envelope ratio, promotes curing characteristics.
The present invention is further illustrated with reference to embodiments, but they do not form limitation of the invention, right
In those skilled in the art, some the nonessential variations and adjustment done according to the present invention are accordingly to be regarded as falling the present invention's
In protection domain.
Specific embodiment
Embodiment 1
The component and content prepared in the composition epoxy resin of semiconductor-sealing-purpose be：
O-cresol formaldehyde epoxy resin A1 (Japanese DIC Corporation systems " N-665 ") 15wt%
Phenol linear phenolic resin B1 (Japanese DIC Corporation systems " TD-2131 ") 7wt%
2-methylimidazole C1 0.15wt%
1,8- diazabicyclos (5,4,0) endecatylene -7C2 0.45wt%
Fine silica powder D (d50 is 25 μm) 67wt%
Fire retardant (mixture of zinc borate, magnesium hydroxide and aluminium hydroxide, wherein zinc borate：Magnesium hydroxide：Aluminium hydroxide
Weight ratio be 8：2：1；The range of grain size d50 is all 0.1~10 μm) E 8wt%
Brazil wax F 0.4wt%
γ-glycidyl propyl ether trimethoxy silane G 0.5wt%
Inorganic ion scavenger H 0.2wt% (Japanese TOAGOSEI Co., Ltd IXE500 (Bi2O3·3H2O))
Carbon black I 0.5wt%
Liquid silicone oil J 0.3wt%
Silicone rubber powder K 0.5wt% (d50 is 1 μm)
(1) according to said ratio, by A1, B1 in the load weighted composition epoxy resin for preparing semiconductor-sealing-purpose,
D, E, F, G, H, I, J, K are put into homogenizer, after stirring evenly, (are turned in the twin screw compounder that temperature is 70~100 DEG C
Speed is 100~150 revs/min) in carry out melting mixing, tabletting after mixing extrusion cools down, is ground into powder；
(2) after the powder for obtaining step (1) is stirred evenly with above-mentioned load weighted C1 and C2 in homogenizer,
Second melting mixing is carried out in the twin screw compounder (rotating speed is 100~150 revs/min) that temperature is 70~100 DEG C, is kneaded and squeezes
Go out rear tabletting, cool down, be ground into powder, then be pre-formed as biscuit, obtain the composition epoxy resin molding of semiconductor-sealing-purpose
Material is evaluated, the results are shown in Table 1 using the following method.
Spiral flow：Measured on transfer modling press by helical flow metal die, briquetting pressure for 70 ±
2Kgf/cm2Mold temperature takes above-mentioned 20 ± 5g of composition epoxy resin to be tested at 175 ± 2 DEG C.
Insolubles content：It weighs above-mentioned 300 grams of composition epoxy resin to be placed in beaker, adds in suitable acetone, carry out
Stirring 30 minutes by the liquid after stirring by the sieve of 60 mesh, will be collected, dries and be claimed not over the insoluble matter of sieve
Amount, will be as insoluble not by the quality of the insoluble matter of sieve divided by the quality of the composition epoxy resin weighed, ratio
Object content.
Leak envelope ratio：After above-mentioned composition epoxy resin, SOT-23 is encapsulated, envelope shared by the number abnormal by there is filling
The ratio of dress quantity is defined as leakage envelope ratio.
Mold hardness：It is measured on transfer modling press by flash mold, molds 60s, briquetting pressure is 70 ± 2Kgf/
cm2, mold temperature at 175 ± 2 DEG C, die sinking 11s~15s in using Shao ASKER D hardometers test test semiconductor-sealing-purpose
Epoxy resin composition is molded the hardness of rear surface.
Embodiment 2~10
The composition and content of the composition epoxy resin of semiconductor-sealing-purpose are shown in Table 1, and the preparation method is the same as that of Example 1, evaluation
Method is with embodiment 1, and evaluation results are shown in Table 1.
Comparative example 1~10
The same Examples 1 to 10 of composition of the composition epoxy resin of semiconductor-sealing-purpose, preparation method are traditional primary
Melting mixing method, for evaluation method with embodiment 1, evaluation result is shown in Table 2.
Embodiment 2~10,2~10 semiconductor-sealing-purpose of comparative example composition epoxy resin in use in embodiment 1
Ingredient in addition is as follows.
Biphenyl type epoxy resin A2 (Japan Epoxy Resins Co., Ltd. systems " YX-4000H ")
Dicyclopentadiene type epoxy Resin A 3 (Japanese DIC Corporation systems " HP-7200 ")
Phenol alkyl phenolic resin (phenol linear phenolic resin derivative) B2 (Mitsui Chemicals, Inc. systems
“XLC-4L”)
Triphenylphosphine C3
Table 1：The composition and content and evaluation result of the composition epoxy resin of the semiconductor-sealing-purpose of Examples 1 to 10
(by weight percentage)
Table 2：The evaluation result of the composition epoxy resin of the semiconductor-sealing-purpose of comparative example 1~10
It can be seen that by the results of property of above-described embodiment and comparative example, half obtained using the secondary mixing method of the present invention
The composition epoxy resin of conductor encapsulation, with the semiconductor-sealing-purpose epoxy resin as obtained by a traditional mixing method
Composition compares, and makes that the composition epoxy resin mobility being obtained by the present invention is more preferable, and insolubles content is lower, into
Envelope ratio is leaked during type to be reduced, and die sinking hardness improves.
Claims (9)
1. a kind of secondary mixing method of the composition epoxy resin of semiconductor-sealing-purpose, it is characterized in that：
(1) by the composition epoxy resin for preparing semiconductor-sealing-purpose epoxy resin, phenolic resin curing agent, inorganic fill out
Material, releasing agent, low stress modified dose, colorant, fire retardant, silane coupling agent and inorganic ion scavenger are put into blender,
After stirring evenly, in temperature for 70~100 DEG C of progress melting mixings, tabletting after mixing cools down, is ground into powder；
(2) curing accelerator in the powder for obtaining step (1) and the composition epoxy resin for preparing semiconductor-sealing-purpose exists
It is 70~100 DEG C of progress second melting mixings in temperature, tabletting, cooling, crushing, obtain after mixing after being stirred evenly in blender
To the composition epoxy resin of semiconductor-sealing-purpose；
The component and content of the composition epoxy resin of the semiconductor-sealing-purpose be：
2. secondary mixing method according to claim 1, it is characterized in that：The epoxy resin is selected from o-cresol formaldehyde epoxy
Resin, bisphenol A type epoxy resin, bisphenol f type epoxy resin, linear phenolic epoxy resin, biphenyl type epoxy resin, bicyclic penta 2
One or more of ene-type epoxy resin, open chain aliphatic epoxy resin, cycloaliphatic epoxy resin, heterocyclic-type epoxy resin.
3. secondary mixing method according to claim 1, it is characterized in that：The phenolic resin is selected from phenol novolac
Resin and its derivative, phenyl methylcarbamate linear phenolic resin and its derivative, monohydroxy or dihydroxy naphthlene phenolic resin and its derivative
One or more of object.
4. secondary mixing method according to claim 1, it is characterized in that：It is micro- that the inorganic filler is selected from silica
One or more of powder, alumina powder, titanium oxide fine powder, silicon nitride powder, aluminium nitride micro mist；
The fine silica powder is selected from powdered quartz micro mist, fusion fine silica powder or their mixing
Object；
The fusion fine silica powder is angular micro mist or ball-type micro mist.
5. secondary mixing method according to claim 1, it is characterized in that：The curing accelerator is selected from imidazoles chemical combination
One or more of object, tertiary amine compound and organic phosphine compound；
The imidazolium compounds is selected from 2-methylimidazole, 2,4- methylimidazoles, 2-ethyl-4-methylimidazole, 2- phenyl miaows
One or more of azoles, 2- phenyl -4-methylimidazole and 2- (heptadecyl) imidazoles；
The tertiary amine compound is selected from triethylamine, benzyl group dimethylamine, 2- (dimethylamino methyl) phenol, tri- (diformazans of 2,4,6-
Aminomethyl) one or more of phenol and 1,8- diazabicyclos (5,4,0) endecatylene -7；
The organic phosphine compound is selected from triphenylphosphine, trimethyl-phosphine, triethyl phosphine, tributylphosphine, three (p-methylphenyls)
One or more of phosphine and three (nonyl phenyl) phosphines.
6. secondary mixing method according to claim 1, it is characterized in that：The releasing agent is selected from Brazil wax, closes
Into one or more of wax and mineral matter wax；
Described low stress modified dose is liquid silicone oil, silicone rubber powder or their mixture；
The colorant is carbon black；
The fire retardant is in Brominated Epoxy, antimony oxide, zinc molybdate, zinc borate, magnesium hydroxide and aluminium hydroxide
It is one or more of；
The silane coupling agent be selected from γ aminopropyltriethoxy silane, γ mercaptopropyitrimethoxy silane and γ-
One or more of aminopropyl trimethoxysilane.
7. secondary mixing method according to claim 6, it is characterized in that：The zinc molybdate, zinc borate, magnesium hydroxide and
The range of the grain size d50 of aluminium hydroxide is all 0.1~10 μm.
8. secondary mixing method according to claim 1, it is characterized in that：The inorganic ion scavenger is selected from hydration gold
Belong to one or more of compound of oxide, acid metal salt and magnalium；
The hydrated metal oxide is Bi2O3·3H2O；The acid metal salt is Zr (HPO4)2·H2O；The aluminium
The compound of magnesium is Mg6Al2(CO3)(OH)16·4H2O。
9. secondary mixing method according to claim 1, it is characterized in that：Equipment used in the melting mixing includes double
One or more of roller kneading machine, single screw rod kneading machine, twin screw compounder.
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| CN108070213A (en) * | 2016-11-16 | 2018-05-25 | 北京科化新材料科技有限公司 | A kind of composition epoxy resin and its application |
| CN107353546A (en) * | 2017-09-02 | 2017-11-17 | 苏建 | A kind of epoxy resin composition for semiconductor encapsulation |
| CN109517336B (en) * | 2018-10-31 | 2021-05-28 | 江苏科化新材料科技有限公司 | Preparation method of super-heat-resistant high-thermal-conductivity epoxy plastic packaging material for semiconductor packaging |
| CN111899954B (en) * | 2020-07-28 | 2023-03-24 | 江苏中科科化新材料股份有限公司 | Thermosetting epoxy resin composition for packaging inductor and preparation method thereof |
| CN112625398B (en) * | 2020-12-02 | 2022-10-25 | 北京科化新材料科技有限公司 | Reflecting material, preparation method thereof and application of reflecting material to LED reflecting support |
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| CN100335541C (en) * | 2005-04-15 | 2007-09-05 | 江苏中电华威电子股份有限公司 | Method for preparing composition of epoxy resin for packaging semiconductor |
| CN102382422B (en) * | 2010-09-01 | 2013-01-02 | 北京科化新材料科技有限公司 | Epoxy resin composition with hydrated alumina |
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