CN108841353A - A kind of large size chip encapsulation preparation method of underfill - Google Patents
A kind of large size chip encapsulation preparation method of underfill Download PDFInfo
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- CN108841353A CN108841353A CN201810713231.5A CN201810713231A CN108841353A CN 108841353 A CN108841353 A CN 108841353A CN 201810713231 A CN201810713231 A CN 201810713231A CN 108841353 A CN108841353 A CN 108841353A
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- underfill
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- diglycidyl ether
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to a kind of preparation methods of large size chip encapsulation underfill, are made of following raw material：From 18~25 parts of synthetic resin, 10~15 parts of flexible-epoxy, 13~20 parts of diluent, 0.1~0.3 part of wetting dispersing agent, 0.1~0.3 part of defoaming agent, 13~40 parts of filler, 0.1~0.4 part of black pigment, 15~20 parts of curing agent, 3~6 parts of curing accelerator.Underfill prepared by the present invention has many advantages, such as that room temperature flowing velocity is fast, fillable area is big, low-temperature fast-curing, internal stress is small, flexibility is good, is suitable for large size chip and encapsulates.
Description
Technical field
The present invention relates to a kind of large size chip encapsulation underfills and preparation method thereof, belong to adhesive field.
Background technique
Nearly 2 years, Global Auto industry all was accelerating to change to intelligent, motorized direction, and new energy, intelligent network join vapour
The chip technology of vehicle critical component develops rapidly, as lithium battery management system chip, automated driving system module chip, digital-to-analogue are mixed
Close signal processing chip etc..Meanwhile chip encapsulation technology is also to high speed, size-enlargement, more number of pins and high-power
Trend development.Underfill is one of necessity material needed for chip package, protects, makes to chip and soldered ball node
Component has wider applicability and reliability.
The most of underfill used on the market all exist solidification temperature is high, slow, the fillable area of flowing velocity is small,
The problems such as internal stress is big, flexibility is poor much can not meet nowadays chip encapsulation technology and send out to new energy, intelligent network connection automobile
Performance requirement brought by exhibition.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of above-mentioned prior art, a kind of large size chip encapsulation underfill is provided
Glue and preparation method thereof, underfill prepared by the present invention have that fast, the fillable area of room temperature flowing velocity is big, low temperature is quick
Solidification, the advantages that internal stress is small, flexibility is good.
The technical solution that the present invention solves above-mentioned technical problem is as follows：A kind of large size chip encapsulation underfill
Preparation method is as follows：
A. 46~56 parts of amine terminated polyether and bisphenol-A -37~51 parts of diglycidyl ether of alkylene oxide addition product are added anti-
It answers in kettle, setting speed 40RPM, is quickly stirred and heated to 110 DEG C~115 DEG C, be added with stirring 2,4,6- tri-（Dimethylamino
Methyl）0.1~0.3 part of phenol, reacted 2~3 hours in the environment of nitrogen protection, be then added 1,6 hexylene glycols two shrink it is sweet
3~6 parts, setting speed 15RPM of oily ether, then react 1~2 hour, it is made from synthetic resin；
B. according to the mass fraction：From 18~25 parts of synthetic resin, 10~15 parts of flexible-epoxy, 13~20 parts of diluent, profit
0.1~0.3 part of hygroscopic water powder, 0.1~0.3 part of defoaming agent, 13~40 parts of filler, 0.1~0.4 part of black pigment, curing agent 15
~20 parts, 3~6 parts of curing accelerator are successively put into stirred tank, vacuumizing and defoaming, setting speed 30RPM, and stirring 3~4 is small
When, underfill of the invention is made.
The beneficial effects of the invention are as follows：Fast, the fillable area of underfill room temperature flowing velocity of the invention is big, prevents
Occurs the failure mode that can not be stuffed entirely in large size chip encapsulation process；It is low-temperature fast-curing, adapt to densification, more
The technique requirement of memberization encapsulation；Internal stress is small, flexibility is good, and the applicability of large size chip encapsulation and reliable is effectively guaranteed
Property.
Based on the above technical solution, the present invention has also carried out following improvement.
Further, described from the synthesis mechanism of synthetic resin is that the amido of amine terminated polyether and bisphenol-A-alkylene oxide add
Hydroxyl is generated at the epoxy group addition reaction of object diglycidyl ether, hydroxyl continues to be formed with the oxygen atom of unreacted epoxy group
Hydrogen bond, 2,4,6- tri-（Dimethylamino methyl）Further occurrence epoxy group under the catalytic action of phenol, amido and hydroxyl it is poly-
Close reaction.The epoxy group of 1,6 hexanediol diglycidyl ethers and unreacted amido carry out addition reaction.
Beneficial effect using above-mentioned further scheme is the epoxy that amine terminated polyether strand is grafted from synthetic resin
Group can participate in further solidifying crosslinking；The flexible group of strand grafting, has good toughening effect, can be improved
From the flexibility and shock resistance of synthetic resin.
Further, the amine terminated polyether be Tianjin Petrochemical Corp.'s third petrochemical plant production D400,
Any one in D2000, T403, T5000.
Further, the bisphenol-A-alkylene oxide addition product diglycidyl ether is raw for South Korea SHIN-A T & C company
The SE-4125P of production or ADEKA company of Japan production EP-4000 in any one.
Beneficial effect using above-mentioned further scheme is the bisphenol-A-alkylene oxide addition product 2-glycidyl
Ether has good toughening effect, can further increase the flexibility from synthetic resin.
Further, the catalyst 2,4,6- tri-（Dimethylamino methyl）Phenol, the preferably trade mark are that resin is easily contained in Jinan
The DMP-30 of Co., Ltd's production.
Further, 1,6 hexanediol diglycidyl ethers, the preferably trade mark are Japanese Nagase Industrial Co., Ltd.'s production
DENACOL EX-212P.
Beneficial effect using above-mentioned further scheme is, Japanese Nagase Industrial Co., Ltd. production
DENACOL EX-212P can reduce the viscosity from synthetic resin, make have good chemical reactivity and phase from synthetic resin
Capacitive.
Further, the flexible-epoxy is the EXA-4850 of DIC company of Japan production.
Beneficial effect using above-mentioned further scheme is the EXA-4850 molecule knot of the Japanese DIC company production
Structure such as following formula：A large amount of low polar group can be improved the wettability of system and substrate, flexible back bone tool in its molecular structure
There is good toughening effect, can be improved the toughness and shock resistance of system.
Further, the diluent is polypropylene glycol diglycidyl ether, and preferably the trade mark is the production of Huntsman Corporation of the U.S.
Arladite DY 3601 or Dow company production DER-732 in any one.
Beneficial effect using above-mentioned further scheme is, in the molecular structure of the polypropylene glycol diglycidyl ether
With flexible fatty long-chain, can rotate freely and high resilience, flexibility is good, greatly improves the impact resistance of system
Energy；System viscosity is greatly reduced simultaneously, meets the requirement of rapid flow velocities.
Further, the wetting dispersing agent is the Y-19268 of U.S. Mai Tu new material company production.
Beneficial effect using above-mentioned further scheme is the Y-19268 of Mai Tu new material company of the U.S. production
It is added so that system internal resin is uniformly dispersed with filler, performance is stablized.Improve system to the wettability of substrate, substantially simultaneously
Improve flowing velocity and filling area.
Further, the filler is maximum particle diameter less than 10 μm, 12~16m of specific surface area2The ball-shaped silicon micro powder of/g, it is excellent
Selecting the trade mark is the DQ1120A of Jiangsu Lian Rui new material limited liability company production.
Beneficial effect using above-mentioned further scheme is, the Jiangsu Lian Rui new material limited liability company production
Ball-shaped silicon micro powder DQ1120A is more advantageous to system than common silicon powder and keeps low viscosity and flow uniformity, improves the viscous of system
Connect intensity and reliability.
Further, the curing agent is any one in line style low molecular weight phenol aralkyl resin, and preferably the trade mark is
Japan is bright and is melted into the MEH-8000H of Co., Ltd.'s production.
Beneficial effect using above-mentioned further scheme is that the Japan is bright and is melted into the MEH- of Co., Ltd.'s production
8000H has many advantages, such as that water imbibition is low, adhesive strength is high, elasticity modulus is low, is imbued with obdurability and pliability.
Further, the curing accelerator is any one in Modified by Aromatic Amines imidazole adducts or derivatives thereof.It is excellent
Select EH-5001P, EH- of HX3088, HX3721 that the trade mark is Japanese Asahi Kasei Corporation's production or Japan ADEKA production
4331S。
Beneficial effect using above-mentioned further scheme is that the curing accelerator room temperature has latency and low temperature fast
Quick solidification, and there is good pliability.Effectively raise the curing performance of system.
Specific embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
A. by amine terminated polyether D2000 275g and bisphenol-A-alkylene oxide addition product diglycidyl ether SE-4125P 195g
It being added in reaction kettle, setting speed 40RPM is quickly stirred and heated to 110 DEG C, it is added with stirring catalyst DMP-30 1g,
It is reacted 2 hours in the environment of nitrogen protection, 1,6 hexanediol diglycidyl ether DENACOL EX-212P 29g is then added, if
Determine revolving speed 15RPM, then react 1 hour, is made from synthetic resin；
B. from synthetic resin 418g, flexible-epoxy EXA-4850 230g, diluent Arladite DY-3601 320g, profit
Hygroscopic water powder Y-19268 6g, defoaming agent BYK-052 4g, filler DQ1120A 590g, black pigment 2g, curing agent MEH-
8000H 340g, curing accelerator EH-5001P 90g are successively put into stirred tank, vacuumizing and defoaming, setting speed 30RPM,
Underfill is made in stirring 4 hours.
Embodiment 2
A. amine terminated polyether T5000 280g and bisphenol-A-alkylene oxide addition product diglycidyl ether E-4000 189g are added
Enter in reaction kettle, setting speed 40RPM is quickly stirred and heated to 110 DEG C, catalyst DMP-30 1g is added with stirring, in nitrogen
It is reacted 2 hours in the environment of gas shielded, 1,6 hexanediol diglycidyl ether DENACOL EX-212P 30g is then added, set
Revolving speed 15RPM, then react 1 hour, it is made from synthetic resin；
B. from synthetic resin 500g, flexible-epoxy EXA-4850 300g, diluent Arladite DY-3601 400g, profit
Hygroscopic water powder Y-19268 6g, defoaming agent BYK-A535 4g, filler DQ1120A 268g, black pigment 2g, curing agent MEH-
8000H 400g, curing accelerator HX3088 120g are successively put into stirred tank, and vacuumizing and defoaming, setting speed 30RPM is stirred
It mixes 4 hours, underfill is made.
Embodiment 3
A. amine terminated polyether T403 230g and bisphenol-A-alkylene oxide addition product diglycidyl ether E-4000 254g are added
Enter in reaction kettle, setting speed 40RPM is quickly stirred and heated to 110 DEG C, catalyst DMP-30 1g is added with stirring, in nitrogen
It is reacted 2 hours in the environment of gas shielded, 1,6 hexanediol diglycidyl ether DENACOL EX-212P 15g is then added, set
Revolving speed 15RPM, then react 1 hour, it is made from synthetic resin；
B. from synthetic resin 360g, flexible-epoxy EXA-4850 200g, diluent DER-732 268g, wetting dispersing agent
Y-19268 6g, defoaming agent BYK-066N 4g, filler DQ1120A 800g, black pigment 2g, curing agent MEH-8000H
300g, curing accelerator EH-4331S 60g are successively put into stirred tank, vacuumizing and defoaming, setting speed 30RPM, and stirring 4 is small
When, underfill is made.
Embodiment 4
A. by amine terminated polyether D2000 275g and bisphenol-A-alkylene oxide addition product diglycidyl ether SE-4125P 195g
It being added in reaction kettle, setting speed 40RPM is quickly stirred and heated to 110 DEG C, it is added with stirring catalyst DMP-30 1g,
It is reacted 2 hours in the environment of nitrogen protection, 1,6 hexanediol diglycidyl ether DENACOL EX-212P 29g is then added, if
Determine revolving speed 15RPM, then react 1 hour, is made from synthetic resin；
B. from synthetic resin 418g, flexible-epoxy EXA-4850 230g, diluent Arladite DY-3601 326g, disappear
Infusion BYK-052 4g, filler DQ1120A 590g, black pigment 2g, curing agent MEH-8000H 340g, curing accelerator EH-
5001P 90g is successively put into stirred tank, vacuumizing and defoaming, setting speed 30RPM, is stirred 4 hours, and underfill is made.
Comparative example 1
By amine terminated polyether D2000 230g of following weight percent, bisphenol-A-alkylene oxide addition product diglycidyl ether
SE-4125P 167g, 1,6 hexanediol diglycidyl ether DENACOL EX-212P 21g, flexible-epoxy EXA-4850
230g, diluent Arladite DY-3601 320g, wetting dispersing agent Y-19268 6g, defoaming agent BYK-052 4g, filler
DQ1120A 590g, black pigment 2g, curing agent MEH-8000H 340g, curing accelerator EH-5001P 90g, successively put into
In stirred tank, vacuumizing and defoaming, setting speed 30RPM is stirred 4 hours, and underfill is made.
Comparative example 2
Common bottom fills glue formula：By bisphenol A epoxide resin Epon828 418g, bisphenol F epoxy resin Epon862
230g, toughening agent C TBN 148g diluent H8 320g, silane coupling agent KH-560 6g, defoaming agent BYK-A535 4g, spherical shape
Silicon powder 590g, black pigment 2g, curing agent Japan aginomoto PN-23 282g successively put into stirred tank, vacuumize de-
Bubble, setting speed 30RPM stir 4 hours, common underfill are made.
Specific test example
By following test, the performance of the underfill of the above embodiment of the present invention 1-4 and comparative example 1,2 is tested.
Wherein, mobile performance and curing performance are characterized by flowing velocity and DSC cure speed respectively；Flexibility by anti-dropping capability Lai
Characterization；Internal stress, flexibility are characterized by storage modulus.
The test of 1 mobile performance of test example
100mm × 100mm test sample is made of coverslip, glass slide and spacer shims, and gap is 30 microns（Simulation encapsulation core
Piece）, 25 DEG C of test flowing velocities and fillable area.
The test of 2 curing performance of test example
Use DSC（Differential scanning calorimetry）Curing rate is tested, 60 DEG C/min of heating rate, 100 DEG C of constant temperature solidify, unit
Min。
The test of 3 storage modulus of test example
Use DMA（Dynamic Mechanical Analyzer）Test, 10 DEG C/min of heating rate, unit Mpa.
The test of 4 anti-dropping capability of test example
Using roller dropping testing machine, height 150cm is set, is fallen 300 times, tests electrical property.
Shown in the table 1 in test result is as follows face.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | |
| Flowing velocity（S） | 590 | 470 | 750 | 1600 | 490 | 1800 |
| Fillable area（—） | It fills up | It fills up | It fills up | It can not fill up | It fills up | It can not fill up |
| Curing rate (Min) | 9 | 15 | 13 | 9 | 12 | 37 |
| Storage modulus（Mpa） | 176 | 200 | 600 | 176 | 1600 | 2357 |
| Fall-down test（—） | OK | OK | OK | Fail | Fail | Fail |
The test performance contrast test result of sample made from 1 embodiment 1-4 of table and 1,2 sample of comparative example
From the data in watch 1 can be seen that underfill of the invention is fast with room temperature flowing velocity, fillable area is big,
Low-temperature fast-curing, the advantages that internal stress is small, flexibility is good, is suitable for large size chip and encapsulates.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. the preparation method that underfill is used in a kind of encapsulation of large size chip, which is characterized in that preparation step is：
A. 46~56 parts of amine terminated polyether and bisphenol-A -37~51 parts of diglycidyl ether of alkylene oxide addition product are added anti-
It answers in kettle, is quickly stirred and heated to 110 DEG C~115 DEG C, be added with stirring 2,4,6- tri-（Dimethylamino methyl）Phenol 0.1~
It 0.3 part, is reacted 2~3 hours in the environment of nitrogen protection, 3~6 parts of 1,6 hexanediol diglycidyl ether is then added, then instead
It answers 1~2 hour, is made from synthetic resin；
B. according to the mass fraction：From 18~25 parts of synthetic resin, 10~15 parts of flexible-epoxy, 13~20 parts of diluent, profit
0.1~0.3 part of hygroscopic water powder, 0.1~0.3 part of defoaming agent, 13~40 parts of filler, 0.1~0.4 part of black pigment, curing agent 15
~20 parts, 3~6 parts of curing accelerator are successively put into stirred tank, vacuumizing and defoaming, are stirred 3~4 hours, are made of the invention
Underfill.
2. preparation method according to claim 1, which is characterized in that the amine terminated polyether is Tianjin Petrochemical Corp.
Third petrochemical plant production D400, D2000, T403, T5000 in any one；The bisphenol-A-alkylene oxide adds
At the EP- of SE-4125P or the production of ADEKA company of Japan that object diglycidyl ether is the production of South Korea SHIN-A T & C company
Any one in 4000.
3. preparation method according to claim 1, which is characterized in that the flexible-epoxy is raw for DIC company of Japan
The EXA-4850 of production.
4. preparation method according to claim 1, which is characterized in that the diluent is polypropylene glycol diglycidyl
Ether, the wetting dispersing agent are the Y-19268 of U.S. Mai Tu new material company production, and the filler is maximum particle diameter less than 10 μ
M, 12~16m of specific surface area2The ball-shaped silicon micro powder of/g.
5. preparation method according to claim 1, which is characterized in that the curing agent is Japanese bright and chemical conversion Co., Ltd.
The MEH-8000H of production；The curing accelerator is HX3088, HX3721 or the Japan of Japanese Asahi Kasei Corporation's production
One of EH-5001P, EH-4331S of ADEKA production.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810713231.5A CN108841353A (en) | 2018-07-03 | 2018-07-03 | A kind of large size chip encapsulation preparation method of underfill |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810713231.5A CN108841353A (en) | 2018-07-03 | 2018-07-03 | A kind of large size chip encapsulation preparation method of underfill |
Publications (1)
| Publication Number | Publication Date |
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| CN108841353A true CN108841353A (en) | 2018-11-20 |
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ID=64199999
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810713231.5A Pending CN108841353A (en) | 2018-07-03 | 2018-07-03 | A kind of large size chip encapsulation preparation method of underfill |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114045137A (en) * | 2022-01-12 | 2022-02-15 | 武汉市三选科技有限公司 | Panel driving circuit bottom filling adhesive, preparation method thereof and chip packaging structure |
| WO2024066254A1 (en) * | 2022-09-27 | 2024-04-04 | 武汉市三选科技有限公司 | Low-modulus die attach film adhesive for vertically stacked package, preparation method therefor and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0885913A1 (en) * | 1996-12-09 | 1998-12-23 | Daiso Co., Ltd. | Copolyether and solid polymer electrolyte |
| CN105255423A (en) * | 2015-11-17 | 2016-01-20 | 烟台市九邦新材料科技有限公司 | Quick-flowing bottom filling adhesive stored at room temperature and preparing method of quick-flowing bottom filling adhesive |
| CN105295796A (en) * | 2015-11-27 | 2016-02-03 | 烟台德邦科技有限公司 | High-reliability epoxy bottom filling glue and preparation method thereof |
| CN107424964A (en) * | 2017-07-27 | 2017-12-01 | 武汉市三选科技有限公司 | Underfill constituent and its bottom filling method of use and Electronic Assemblies component |
-
2018
- 2018-07-03 CN CN201810713231.5A patent/CN108841353A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0885913A1 (en) * | 1996-12-09 | 1998-12-23 | Daiso Co., Ltd. | Copolyether and solid polymer electrolyte |
| CN105255423A (en) * | 2015-11-17 | 2016-01-20 | 烟台市九邦新材料科技有限公司 | Quick-flowing bottom filling adhesive stored at room temperature and preparing method of quick-flowing bottom filling adhesive |
| CN105295796A (en) * | 2015-11-27 | 2016-02-03 | 烟台德邦科技有限公司 | High-reliability epoxy bottom filling glue and preparation method thereof |
| CN107424964A (en) * | 2017-07-27 | 2017-12-01 | 武汉市三选科技有限公司 | Underfill constituent and its bottom filling method of use and Electronic Assemblies component |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114045137A (en) * | 2022-01-12 | 2022-02-15 | 武汉市三选科技有限公司 | Panel driving circuit bottom filling adhesive, preparation method thereof and chip packaging structure |
| WO2024066254A1 (en) * | 2022-09-27 | 2024-04-04 | 武汉市三选科技有限公司 | Low-modulus die attach film adhesive for vertically stacked package, preparation method therefor and application thereof |
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Address after: No.3-3, Kaifeng Road, Yantai Development Zone, Shandong Province 264006 Applicant after: Yantai Debang Technology Co.,Ltd. Address before: No.3-3, Kaifeng Road, Yantai Development Zone, Shandong Province 264006 Applicant before: DARBOND TECHNOLOGY Co.,Ltd. |
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Application publication date: 20181120 |