CN114806473A - Cold-heat-resistant low-moisture-absorption epoxy underfill adhesive and preparation method thereof - Google Patents
Cold-heat-resistant low-moisture-absorption epoxy underfill adhesive and preparation method thereof Download PDFInfo
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- CN114806473A CN114806473A CN202210426550.4A CN202210426550A CN114806473A CN 114806473 A CN114806473 A CN 114806473A CN 202210426550 A CN202210426550 A CN 202210426550A CN 114806473 A CN114806473 A CN 114806473A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention belongs to the technical field of filling adhesives, and particularly relates to a cold and heat resistant low moisture absorption epoxy bottom filling adhesive and a preparation method thereof, wherein the cold and heat resistant low moisture absorption epoxy bottom filling adhesive comprises the following raw materials in percentage by mass: 65-80% of epoxy resin, 15-20% of curing agent, 0.75-3% of accelerating agent, 0.5-5% of filler, 2-8% of diluent, 0.5-3% of coupling agent and 0.1-0.4% of defoaming agent. The cold and heat resistant low moisture absorption epoxy underfill has the following characteristics: 1. has low temperature resistance; 2. has high temperature resistance; 3. has good cold and heat impact resistance; 4. has extremely low water absorption and moisture absorption.
Description
Technical Field
The invention belongs to the technical field of filling adhesives, and particularly relates to a cold-heat resistant low-moisture-absorption epoxy bottom filling adhesive and a preparation method thereof.
Background
Flip chip (Flip chip) is a leadless structure. The flip Chip is connected with three main types C4(Controlled Collapse Chip Connection), DCA (direct Chip attach), and FCAA (Flip Chip additive attachment). FCAA connections exist in a variety of forms and are currently still in the early stages of development. The connection between the silicon chip and the substrate is not made by solder, but by glue.
Nowadays, with the development of scientific technology and new materials, the technical requirements of flip chips are increased more and more, and in continuous change and development, in order to further enhance the quality of the flip chips, the performance reliability and application durability of the filling material become critical, and most of the underfill adhesives have good adhesion and insulation properties.
Disclosure of Invention
The invention aims to provide a cold and heat resistant low-moisture-absorption epoxy underfill adhesive and a preparation method thereof, and aims to solve the technical problems of the cold and heat resistant low-moisture-absorption epoxy underfill adhesive and the preparation method thereof in the prior art.
In order to achieve the above purpose, an epoxy underfill adhesive with cold and hot resistance and low moisture absorption provided by the embodiments of the present invention includes the following raw materials by mass: 65-80% of epoxy resin, 15-20% of curing agent, 0.75-3% of accelerating agent, 0.5-5% of filler, 2-8% of diluent, 0.5-3% of coupling agent and 0.1-0.4% of defoaming agent.
Optionally, the epoxy resin viscosity is 2000-.
Optionally, the coupling agent is selected from any one of a silane coupling agent, a titanate coupling agent and a zirconium aluminum ester coupling agent or a mixture of at least two of them.
Optionally, the filler is selected from any one of reinforcing powder, flame-retardant powder and heat-conducting powder or a mixture of at least two of them.
Optionally, the filler is selected from any one of fumed silica, boron nitride and alumina or a mixture of at least two thereof.
Optionally, the curing agent is a latent curing agent selected from any one of or a mixture of at least two of dicyandiamide curing agent, SHD curing agent and ketimine curing agent.
Optionally, the accelerator is a fatty amine accelerator or an imidazole accelerator, or a mixture of both.
Optionally, the epoxy resin is selected from any one of bisphenol a type epoxy resin, bisphenol F type epoxy resin or glycidyl ether type epoxy resin or a mixture of at least two of the above.
Optionally, the diluent is selected from any one or a mixture of at least two of allyl glycidyl ether, n-butanol or acetone.
In order to achieve the above object, the preparation method of the cold and hot resistant low moisture absorption epoxy underfill provided by the embodiment of the present invention comprises the following steps:
1) weighing epoxy resin and filler according to a ratio, putting the epoxy resin and the filler into a stirring barrel, quickly stirring for 0.8-1.2 hours in vacuum at 80-100 ℃, and cooling to 45-55 ℃;
2) then adding a coupling agent with a proportional amount, continuously stirring for 0.4-0.6 h in vacuum, and decompressing and cooling to room temperature;
3) and continuously adding the curing agent, the accelerator, the diluent and the defoaming agent in proportion, and stirring for 0.4-0.6 hour in vacuum to prepare the cold-resistant and low-moisture-absorption epoxy underfill adhesive.
The technical scheme or schemes in the cold and hot resistant low moisture absorption epoxy underfill adhesive and the preparation method thereof provided by the embodiment of the invention at least have one of the following technical effects: the cold and heat resistant low moisture absorption epoxy underfill has the following characteristics: 1. has low temperature resistance; 2. has high temperature resistance; 3. has good cold and heat impact resistance; 4. has extremely low water absorption and moisture absorption.
Detailed Description
The present invention will be further described with reference to the following examples, but the embodiments of the present invention are not limited thereto.
In an embodiment of the invention, a cold and hot resistant low moisture absorption epoxy underfill is provided, which comprises the following raw materials by mass percent: 65-80% of epoxy resin, 15-20% of curing agent, 0.75-3% of accelerating agent, 0.5-5% of filler, 2-8% of diluent, 0.5-3% of coupling agent and 0.1-0.4% of defoaming agent.
The proportioning coupling agent in the raw materials improves the interface state after curing, prevents media from permeating into colloid, such as moisture and steam, and ensures lower hygroscopicity.
In some preferred embodiments of the present invention, the viscosity of the epoxy resin in the cold and hot resistant low moisture absorption epoxy underfill is 2000-5000cps, which is used to adjust the fluidity during application.
In some preferred embodiments of the present invention, the coupling agent in the cold-hot resistant low moisture absorption epoxy underfill is selected from any one of a silane coupling agent, a titanate coupling agent, and a zirconium aluminum ester coupling agent, or a mixture of at least two thereof.
In some preferred embodiments of the present invention, the filler in the cold-hot resistant low moisture absorption epoxy underfill is selected from any one or a mixture of at least two of reinforcing powder, flame retardant powder and heat conductive powder. The reinforcing powder mainly has the functions of improving the strength of the polymer, improving the toughness and the ductility of the polymer and improving the high and low temperature resistance. The flame retardant powder provides flame retardant properties and the heat conducting powder provides heat conducting effects.
In some preferred embodiments of the present invention, the filler in the cold and hot resistant low moisture absorption epoxy underfill is selected from any one or a mixture of at least two of fumed silica, boron nitride and alumina.
In some preferred embodiments of the present invention, the curing agent in the cold-hot resistant low moisture absorption epoxy underfill is a latent curing agent, and the latent curing agent is selected from any one or a mixture of at least two of dicyandiamide curing agent, SHD curing agent and ketimine curing agent, and has good storage stability.
In some preferred embodiments of the present invention, the accelerator in the cold and hot resistant low moisture absorption epoxy underfill is an aliphatic amine accelerator or an imidazole accelerator, or a mixture of both. The accelerator has the function of enabling the curing reaction of the epoxy resin and the curing agent to be carried out at lower temperature in the process of producing the high molecular polymer.
In some preferred embodiments of the present invention, the epoxy resin in the cold and hot resistant low moisture absorption epoxy underfill is selected from any one of bisphenol a type epoxy resin, bisphenol F type epoxy resin or glycidyl ether type epoxy resin or a mixture of at least two thereof.
In some preferred embodiments of the present invention, the diluent in the cold and hot resistant low moisture absorption epoxy underfill is selected from any one or a mixture of at least two of allyl glycidyl ether, n-butanol, or acetone.
In an embodiment of the present invention, a method for preparing the cold and hot resistant low moisture absorption epoxy underfill is also provided, which comprises the following steps:
1) weighing epoxy resin and filler according to a ratio, putting the epoxy resin and the filler into a stirring barrel, quickly stirring for 0.8-1.2 hours in vacuum at 80-100 ℃, and cooling to 45-55 ℃;
2) then adding a coupling agent with a proportional amount, continuously stirring for 0.4-0.6 h in vacuum, and decompressing and cooling to room temperature;
3) and continuously adding the curing agent, the accelerator, the diluent and the defoaming agent in proportion, and stirring for 0.4-0.6 hour in vacuum to prepare the cold-resistant and low-moisture-absorption epoxy underfill adhesive.
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The amounts of the respective raw materials in examples 1 to 6 are shown in Table 1
TABLE 1
| Raw materials | Example 1 | Example 2 | Example 3 | Example 4 |
| Epoxy resin (%) | 65 | 70 | 75 | 80 |
| Curing agent (%) | 20 | 18 | 16 | 15 |
| Accelerator (%) | 3 | 2 | 1 | 0.75 |
| Filler (%) | 0.6 | 5 | 3 | 0.5 |
| Diluent (%) | 8 | 2 | 2.5 | 3 |
| Coupling agent (%) | 3 | 2.9 | 2.3 | 0.5 |
| Antifoaming agent (%) | 0.4 | 0.1 | 0.2 | 0.25 |
Examples 1 to 6
The preparation method of the cold and heat resistant low moisture absorption epoxy underfill comprises the following steps:
1) weighing epoxy resin and filler according to a ratio, putting the epoxy resin and the filler into a stirring barrel, quickly stirring for 1 hour in vacuum at 90 ℃, and cooling to 50 ℃;
2) then adding a coupling agent with a proportional amount, continuously stirring for 0.5 hour in vacuum, and decompressing and cooling to room temperature;
3) and continuously adding the curing agent, the accelerator, the diluent and the defoaming agent in proportion, and stirring for 0.5 hour in vacuum to prepare the cold-resistant and low-moisture-absorption epoxy underfill adhesive.
Example 7
This example tests the cold and heat resistant, low moisture absorption epoxy underfill made in examples 1-6 for cold and heat resistance, high temperature resistance, cold and heat shock resistance, and moisture absorption.
Wherein:
the cold and hot impact method comprises the following steps: 50 ℃/1 hour, normal temperature 5 minutes, 150 ℃/1 hour, 2 hours one cycle; and (4) judging the standard: the colloid has no cracking, no foaming and no color change; and (3) testing equipment: a cold and hot impact test chamber;
water absorption was tested according to ASTM D570-98;
the high temperature resistance is tested according to GB/T2423.2-2008; the test temperature is 150 ℃;
the low temperature resistance is tested according to GB/T2423.1-2008; the test temperature was-50 ℃.
The test results are shown in Table 2.
TABLE 2
The cold-heat-resistant low-moisture-absorption epoxy underfill has good performances of long-term low temperature resistance of-50 ℃ and high temperature resistance of 180 ℃, can be quickly recycled for more than 1000 hours at the temperature of-50 ℃ and 150 ℃, has extremely low water absorption rate, cannot cause performance reduction when applied to environments with large moisture and humidity, and integrally improves the applicability of the underfill to high-requirement environments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The cold-heat-resistant low-moisture-absorption epoxy underfill is characterized by comprising the following raw materials in percentage by mass: 65-80% of epoxy resin, 15-20% of curing agent, 0.75-3% of accelerator, 0.5-5% of filler, 2-8% of diluent, 0.5-3% of coupling agent and 0.1-0.4% of defoaming agent.
2. The cold-heat resistant low-moisture absorption epoxy underfill as set forth in claim 1, wherein the epoxy resin has a viscosity of 2000-5000 cps.
3. The cold and hot resistant low moisture absorption epoxy underfill according to claim 1, wherein said coupling agent is selected from any one of a silane coupling agent, a titanate coupling agent and a zirconium aluminum ester coupling agent or a mixture of at least two thereof.
4. The cold-hot resistant low moisture absorption epoxy underfill according to claim 1, wherein the filler is selected from any one of reinforcing powder, flame retardant powder and heat conducting powder or a mixture of at least two thereof.
5. The cold and hot resistant low moisture absorption epoxy underfill of claim 1, wherein said filler is selected from any one of fumed silica, boron nitride and alumina or a mixture of at least two thereof.
6. The cold and hot resistant low moisture absorption epoxy underfill according to claim 1, wherein said curing agent is a latent curing agent selected from any one or a mixture of at least two of dicyandiamide curing agent, SHD curing agent and ketimine curing agent.
7. The cold-hot resistant low moisture absorption epoxy underfill according to claim 1, wherein said accelerator is a fatty amine accelerator or an imidazole accelerator, or a mixture of both.
8. The cold and hot resistant low moisture absorbing epoxy underfill according to any one of claims 1 to 7, wherein said epoxy resin is selected from any one of bisphenol A type epoxy resin, bisphenol F type epoxy resin or glycidyl ether type epoxy resin or a mixture of at least two thereof.
9. Cold heat resistant low moisture absorption epoxy underfill according to any one of claims 1 to 7 wherein said diluent is selected from the group consisting of allyl glycidyl ether, n-butanol or acetone or a mixture of at least two thereof.
10. The method of making a cold and hot resistant low moisture absorption epoxy underfill according to any one of claims 1 to 9, comprising the steps of:
1) weighing epoxy resin and filler according to a ratio, putting the epoxy resin and the filler into a stirring barrel, quickly stirring for 0.8-1.2 hours in vacuum at 80-100 ℃, and cooling to 45-55 ℃;
2) then adding a coupling agent with a proportional amount, continuously stirring for 0.4-0.6 h in vacuum, and decompressing and cooling to room temperature;
3) and continuously adding the curing agent, the accelerator, the diluent and the defoaming agent in proportion, and stirring for 0.4-0.6 hour in vacuum to prepare the cold-resistant and low-moisture-absorption epoxy underfill adhesive.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210426550.4A CN114806473A (en) | 2022-04-21 | 2022-04-21 | Cold-heat-resistant low-moisture-absorption epoxy underfill adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210426550.4A CN114806473A (en) | 2022-04-21 | 2022-04-21 | Cold-heat-resistant low-moisture-absorption epoxy underfill adhesive and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709983A (en) * | 2013-12-23 | 2014-04-09 | 东莞市亚聚电子材料有限公司 | High temperature resisting bottom filler glue and preparation method thereof |
| JP2014125631A (en) * | 2012-12-27 | 2014-07-07 | Namics Corp | Liquid epoxy resin composition |
| CN104910845A (en) * | 2015-06-12 | 2015-09-16 | 深圳先进技术研究院 | Underfill adhesive and preparation method thereof |
| JP2019151839A (en) * | 2018-03-05 | 2019-09-12 | 日産化学株式会社 | Epoxy resin composition |
| CN111303382A (en) * | 2020-03-03 | 2020-06-19 | 深圳市勇泰运科技有限公司 | Rigid-flexible integrated epoxy resin and reworkable underfill |
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2022
- 2022-04-21 CN CN202210426550.4A patent/CN114806473A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014125631A (en) * | 2012-12-27 | 2014-07-07 | Namics Corp | Liquid epoxy resin composition |
| CN103709983A (en) * | 2013-12-23 | 2014-04-09 | 东莞市亚聚电子材料有限公司 | High temperature resisting bottom filler glue and preparation method thereof |
| CN104910845A (en) * | 2015-06-12 | 2015-09-16 | 深圳先进技术研究院 | Underfill adhesive and preparation method thereof |
| JP2019151839A (en) * | 2018-03-05 | 2019-09-12 | 日産化学株式会社 | Epoxy resin composition |
| CN111303382A (en) * | 2020-03-03 | 2020-06-19 | 深圳市勇泰运科技有限公司 | Rigid-flexible integrated epoxy resin and reworkable underfill |
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