CN105368003A - Preparation method of epoxy resin composition for semiconductor packaging - Google Patents
Preparation method of epoxy resin composition for semiconductor packaging Download PDFInfo
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- CN105368003A CN105368003A CN201510922548.6A CN201510922548A CN105368003A CN 105368003 A CN105368003 A CN 105368003A CN 201510922548 A CN201510922548 A CN 201510922548A CN 105368003 A CN105368003 A CN 105368003A
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- epoxy resin
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Abstract
The invention relates to a preparation method of an epoxy resin composition for semiconductor packaging. The preparation method comprises the following steps: Step 1, a curing accelerator is reserved, and the curing accelerator is made into a solution if the curing accelerator is solid; Step 2, various materials of the epoxy resin composition except the curing accelerator are uniformly mixed through a high-speed mixer, and the mixture is conveyed to the next step; Step 3, materials obtained from the Step 2 undergo hot-melt extrusion by a single screw extruder or a twin-screw extruder, and the hot-melt extrusion product is conveyed to the next step; Step 4, the curing accelerator or a solution containing the curing accelerator is dropwise added to a feed zone of an open mill, and the materials are uniformly mixed through the open mill; and Step 5, the materials undergo blanking, tabletting, cooling, crushing and sieving to make small granules, and the small granules are then mixed and uniformly dispersed so as to obtain the epoxy resin composition with performance uniformity. The prepared epoxy resin composition has excellent mechanical properties and packaging outline yield, and also has good fluidity, formability, flame resistance and reliability.
Description
Technical field
The present invention relates to a kind of preparation method of epoxy resin composition for semiconductor encapsulation, be related specifically to a kind of preparation method that can improve epoxy resin composition for semiconductor encapsulation mechanical property and packaging appearance yield.
Background technology
The component of epoxy resin composition for semiconductor encapsulation generally comprises epoxy resin, solidifying agent, curing catalyst, filler, fire retardant, releasing agent, coupling agent, tinting material, mechanics properties-correcting agent etc.Wherein, curing catalyst component accelerates the speed of response of epoxy resin and solidifying agent under can be implemented in hot conditions.
The preparation method of epoxy resin composition for semiconductor encapsulation generally includes starting material mixing, it is mixing to extrude, compressing tablet cooling, pulverizing, rear mixing, the process such as shaping.At starting material mixing step, all components of composition epoxy resin has added all.And at follow-up compounding procedure of extruding, each component of composition epoxy resin needs to realize sufficient Homogeneous phase mixing, need to realize the abundant dispersion of filler particles and resin especially to the abundant infiltration of filler particles and coated; Need the epoxy composite avoiding the formation of over-curing simultaneously, to cause when semiconductor packages large particulate matter in due to epoxy composite too much to block mould gum-injecting port, form encapsulation defect.For realizing the requirement avoiding the formation of over-curing, usually melting temperature and the material extruded velocity of extruding compounding procedure will be controlled, therefore certain to the abundant mixing formation of material restriction, and then with encapsulation yield, negative restriction is caused to the mechanical property of composition epoxy resin.
Summary of the invention
The technical problem to be solved in the present invention overcomes above-mentioned deficiency, provides a kind of preparation method of epoxy resin composition for semiconductor encapsulation, can improve epoxy resin composition for semiconductor encapsulation mechanical property and packaging appearance yield.
The preparation method of epoxy resin composition for semiconductor encapsulation of the present invention, its raw material comprises epoxy resin, solidifying agent, curing catalyst, filler, fire retardant, releasing agent, coupling agent and tinting material, and preparation method comprises the steps:
The first step: reserved curing catalyst, if curing catalyst is that solid can be mixed with solution;
Second step: by homogenizer, each for the composition epoxy resin except curing catalyst component materials is mixed, and be sent to next step;
3rd step: by singe screw or twin screw extruder by the material hot-melt extruded of second step gained, and be sent to next step;
4th step: drip curing catalyst or the solution containing curing catalyst in mill intake zone, and by mill, material is evenly mixing;
5th step: material makes molecule through blanking, compressing tablet, cooling, pulverizing, sub-sieve, after through after blending dispersion evenly obtain the consistent composition epoxy resin of performance;
In the 3rd described step, extruded material speed 200 ~ 600kg/h; Described singe screw or twin screw extruder extrusion temperature of charge are 90-150 DEG C;
In the 4th described step, drip the rate of addition 0.04 ~ 3kg/h of curing catalyst or the solution containing curing catalyst in mill intake zone;
In the 5th described step, be ground into the particle size range 0.2-2mm of molecule, rear mixing time 20 ~ 60min.
In the present invention:
Epoxy resin weight percentage is in the composition 12-14%; Solidifying agent weight percentage is in the composition 6-7%; Curing catalyst weight percentage is in the composition 0.02-0.5%; Filler weight percentage is in the composition 74.3-78.5%; Fire retardant weight percentage is in the composition 1.7-2.5%; Releasing agent weight percentage is in the composition 0.4-0.6%; Coupling agent weight percentage is in the composition 0.6-0.68%; Tinting material weight percentage is in the composition 0.5-0.7%.
Epoxy resin is o-cresol formaldehyde epoxy resin; Solidifying agent is phenol linear phenolic resin; Curing catalyst is one or both in the 10wt% aqueous solution of diazabicylo and glyoxal ethyline; Fine silica powder elected as by filler; Fire retardant is brominated epoxy resin and antimonous oxide; Releasing agent is carnauba wax; Coupling agent is γ-epoxypropyl propyl ether Trimethoxy silane; Tinting material is carbon black.
In technique scheme, by reserved curing catalyst, make each component materials of the composition epoxy resin except curing catalyst can obtain larger process window in hot-melt extruded operation, realize higher melting temperature and mixing intensity, realize the abundant dispersion of filler particles and resin to the full extent to the abundant infiltration of filler particles and coated, for solving, composition epoxy resin is evenly mixing plays crucial improvement result.After this curing catalyst is achieved evenly mixing by dripping mode on a mill until, and rear mixed processes ensures that material molecule fully mixes, finally to obtain the consistent composition epoxy resin of performance.
Composition epoxy resin prepared by the present invention possesses excellent mechanical property and packaging appearance yield, also possesses good mobility, formability, flame retardant resistance and reliability simultaneously.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but this is only citing, is not limitation of the present invention.
Be each composition of relating to and code name below:
Filler: fine silica powder D1 (d50 is 25 μm)
Filler: fine silica powder D2 (d50 is 10 μm)
Filler: fine silica powder D3 (d50 is 5 μm)
Fire retardant: brominated epoxy resin Z1
Fire retardant: antimonous oxide Z2
Tinting material: carbon black T
Coupling agent: γ-epoxypropyl propyl ether Trimethoxy silane G
Epoxy resin: o-cresol formaldehyde epoxy resin A
Solidifying agent: phenol linear phenolic resin B
Curing catalyst: diazabicylo C1
Curing catalyst: the 10wt% aqueous solution C2 of glyoxal ethyline.
Releasing agent: carnauba wax W
Embodiment 1-5 prepares epoxy resin composition for semiconductor encapsulation
In embodiment 1-5, raw material, preparation process, process parameter and evaluation result are as shown in table 1:
Table 1
The preparation process of embodiment 1 ~ 5 composition is as follows:
The first step: diazabicylo C1 is reserved out.
Second step: fine silica powder D1, fine silica powder D2, fine silica powder D3 and carbon black T are stirred by homogenizer, and carry out surface treatment with γ-epoxypropyl propyl ether Trimethoxy silane G; Add o-cresol formaldehyde epoxy resin A, phenol linear phenolic resin B, brominated epoxy resin Z1, antimonous oxide Z2 and carnauba wax W afterwards, continue to mix, be then sent to next step.
3rd step: second step is obtained material and is melt extruded by single screw extrusion machine, is controlled extruded material speed and extrusion temperature of charge, and extruded material serialization is sent to next step;
4th step: drip diazabicylo C1 in mill intake zone, and control rate of addition, make it evenly mixing on a mill until with the 3rd step supplied materials;
5th step: material in mill discharging area through dise knife serialization cutting stock, cooling, pulverizer pulverizing, vibratory screening apparatus sub-sieve is being transmitted through rolling press compressing tablet, steel band, obtain the molecule of granularity 0.2 ~ 2mm, mix after mixing machine after using after whole material production completes, obtain the composition epoxy resin that performance is consistent.
The evaluation method of the composition that embodiment 1 ~ 5 is obtained is as follows, and evaluation result is in table 1.
Flexural strength and modulus in flexure: (Shanghai Shen mechanical means company limited produces to use low pressure Transfer molding machine, SY-250T) it is 175 DEG C in die temperature, injection pressure is 9.8MPa, set time is under 120s condition, the composition epoxy resin formed material of gained is shaped to the test batten of 150*12*10mm, subsequently after fixing 8 hours at 175 DEG C of temperature.
According to the prescriptive procedure of GB/T1449-2005, span 100mm, speed 3mm/min, carry out flexural strength and modulus test.
Encapsulation yield: use low pressure Transfer molding machine to be 175 DEG C in die temperature, injection pressure is 5MPa, and set time is under 120s condition, and gained composition epoxy resin formed material is shaped to triode TO220, every mould 240, continuously encapsulation 40 moulds.After this whether outward appearance test package sample surface exists defect or pin hole, and adds up fraction defective.
Reference examples 1-5 prepares epoxy resin composition for semiconductor encapsulation
Reference examples 1-5 raw material, preparation process, process parameter and evaluation result are as table 2:
Table 2
The preparation process of reference examples 1 ~ 5 composition is as follows:
The first step: fine silica powder D1, fine silica powder D2, fine silica powder D3 and carbon black T are stirred by homogenizer, and carry out surface treatment with γ-epoxypropyl propyl ether Trimethoxy silane G; Add o-cresol formaldehyde epoxy resin A, phenol linear phenolic resin B, diazabicylo C1, brominated epoxy resin Z1, antimonous oxide Z2 and carnauba wax W afterwards, continue to mix, be then sent to next step;
Second step: the first step is obtained material and is melt extruded by single screw extrusion machine, is controlled extruded material speed and extrusion temperature of charge, and extruded material serialization is sent to next step;
3rd step: in mill by evenly mixing for second step supplied materials;
4th step: material in mill discharging area through dise knife serialization cutting stock, cooling, pulverizer pulverizing, vibratory screening apparatus sub-sieve is being transmitted through rolling press compressing tablet, steel band, obtain the molecule of granularity 0.2 ~ 2mm, mix after mixing machine after using after whole material production completes, obtain the composition epoxy resin that performance is consistent.
The evaluation method of the composition that reference examples 1 ~ 5 is obtained is with embodiment 1, and evaluation result is in table 2.
Can be found out by above-described embodiment and comparative example, by reserved curing catalyst, composition epoxy resin extrude operation realize mixing more fully, curing catalyst is added again in subsequent handling, finally be fully mixed to get to obtain the consistent composition epoxy resin of performance, said composition possesses good mechanical property and packaging appearance yield.
Claims (1)
1. a preparation method for epoxy resin composition for semiconductor encapsulation, its raw material comprises epoxy resin, solidifying agent, curing catalyst, filler, fire retardant, releasing agent, coupling agent and tinting material, it is characterized in that, described preparation method comprises the steps:
The first step: reserved curing catalyst, if curing catalyst is that solid is then mixed with solution;
Second step: by homogenizer, each for the composition epoxy resin except curing catalyst component materials is mixed, and be sent to next step;
3rd step: by singe screw or twin screw extruder by the material hot-melt extruded of second step gained, and be sent to next step;
4th step: drip curing catalyst or the solution containing curing catalyst in mill intake zone, and by mill, material is evenly mixing;
5th step: material makes molecule through blanking, compressing tablet, cooling, pulverizing, sub-sieve, after through after blending dispersion evenly obtain the consistent composition epoxy resin of performance;
In the 3rd described step, extruded material speed 200 ~ 600kg/h; Described singe screw or twin screw extruder extrusion temperature of charge are 90-150 DEG C;
In the 4th described step, drip the rate of addition 0.04 ~ 3kg/h of curing catalyst or the solution containing curing catalyst in mill intake zone;
In the 5th described step, be ground into the particle size range 0.2-2mm of molecule, rear mixing time 20 ~ 60min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510922548.6A CN105368003A (en) | 2015-12-14 | 2015-12-14 | Preparation method of epoxy resin composition for semiconductor packaging |
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| CN201510922548.6A CN105368003A (en) | 2015-12-14 | 2015-12-14 | Preparation method of epoxy resin composition for semiconductor packaging |
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| CN105368003A true CN105368003A (en) | 2016-03-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113798037A (en) * | 2021-09-13 | 2021-12-17 | 苏州锐朗新材料有限公司 | Raw material pretreatment process suitable for chip packaging materials with different attributes |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150597A (en) * | 1996-04-29 | 1997-05-28 | 无锡市化工研究设计院 | Method for preparing reinforced epoxy moulding compound for packaging electric equipment |
| JP2002069203A (en) * | 2000-08-25 | 2002-03-08 | Shin Etsu Chem Co Ltd | Method for manufacturing epoxy resin composition for sealing semiconductor |
| CN1687229A (en) * | 2005-04-15 | 2005-10-26 | 江苏中电华威电子股份有限公司 | Method for preparing composition of epoxy resin for packaging semiconductor |
| CN102504493A (en) * | 2011-11-18 | 2012-06-20 | 江苏华海诚科新材料有限公司 | Epoxy resin composition applicable to pre-encapsulation of inner interconnection framework system |
-
2015
- 2015-12-14 CN CN201510922548.6A patent/CN105368003A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150597A (en) * | 1996-04-29 | 1997-05-28 | 无锡市化工研究设计院 | Method for preparing reinforced epoxy moulding compound for packaging electric equipment |
| JP2002069203A (en) * | 2000-08-25 | 2002-03-08 | Shin Etsu Chem Co Ltd | Method for manufacturing epoxy resin composition for sealing semiconductor |
| CN1687229A (en) * | 2005-04-15 | 2005-10-26 | 江苏中电华威电子股份有限公司 | Method for preparing composition of epoxy resin for packaging semiconductor |
| CN102504493A (en) * | 2011-11-18 | 2012-06-20 | 江苏华海诚科新材料有限公司 | Epoxy resin composition applicable to pre-encapsulation of inner interconnection framework system |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113798037A (en) * | 2021-09-13 | 2021-12-17 | 苏州锐朗新材料有限公司 | Raw material pretreatment process suitable for chip packaging materials with different attributes |
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