CN110724487A - Infrared chip packaging adhesive with excellent cold and hot shock resistance and preparation method thereof - Google Patents
Infrared chip packaging adhesive with excellent cold and hot shock resistance and preparation method thereof Download PDFInfo
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- CN110724487A CN110724487A CN201911014531.5A CN201911014531A CN110724487A CN 110724487 A CN110724487 A CN 110724487A CN 201911014531 A CN201911014531 A CN 201911014531A CN 110724487 A CN110724487 A CN 110724487A
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- anhydride
- packaging adhesive
- chip packaging
- infrared chip
- component
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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
- C09J11/06—Non-macromolecular additives organic
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses an infrared chip packaging adhesive with excellent cold and heat shock resistance, which comprises a component A and a component B in a mass ratio: 1: 0.9-1.05; the component A comprises the following components in percentage by mass: 75-95% of epoxy resin, 4-25% of reactive diluent and 0.5-4% of auxiliary agent; the component B comprises the following components in percentage by mass: 60-98% of acid anhydride, 1-15% of flexibilizer, 0.7-8% of accelerator, 0.03-3.0% of antioxidant and 0.03-3.0% of ultraviolet absorber. The infrared chip packaging adhesive provided by the invention has the advantages that the purpose that the cycle number is more than 300 under the cold and hot shock condition of-40-105 ℃ under the condition of not sacrificing light decay is realized by adding the modified anhydride with specific equivalent weight and viscosity into the system, and the infrared chip packaging adhesive is remarkably improved compared with the prior art.
Description
Technical Field
The invention belongs to the technical field of chemical materials, and particularly relates to an infrared chip packaging adhesive with excellent cold and heat shock resistance and a preparation method thereof.
Background
The infrared chip packaging adhesive is a protective adhesive applied to an LED infrared chip, can protect the LED chip from adverse effects of mechanical, high temperature, humidity and other external impacts, ensures normal contact between the LED chip and a next layer of circuit, and improves the working stability of the LED chip. Therefore, the qualified LED packaging adhesive must have excellent sealing property, light transmission property, adhesion property and mechanical property. The packaging adhesive commonly used on the LED chip at present is mainly epoxy resin packaging adhesive and organic silicon packaging adhesive. The packaging adhesive made of epoxy resin materials is suitable for low-power LED chips, and the packaging adhesive made of organic silicon is suitable for high-power LED chips. Compared with the packaging adhesive made of organic silicon materials, the epoxy resin packaging adhesive has the advantages of low cost, good adhesion and the like, but the defects of large light attenuation and high attenuation rate exist when most of the larger epoxy resin packaging adhesives are applied to infrared LED chip packaging.
In view of the above defects, chinese patent application CN107353858A proposes a packaging adhesive for an infrared LED chip, and a preparation method and an application thereof, in which epoxy resin and modified anhydride are reacted and crosslinked under the action of an accelerator to form a stable solid plastic, so as to achieve the effect of reducing the light attenuation and attenuation rate of the infrared LED. However, the packaging adhesive has poor thermal shock resistance, and does not have the characteristic of keeping the light intensity attenuation within a range and passing through 300 cycles under the condition of-40 ℃ to 105 ℃.
Therefore, it is necessary to provide a glue suitable for LED infrared chip packaging, which has excellent thermal shock resistance and low light attenuation.
Disclosure of Invention
The invention aims to provide the infrared chip packaging adhesive with excellent cold and heat shock resistance and the preparation method thereof, and the key progress is that the infrared chip packaging adhesive has excellent cold and heat shock resistance while keeping low light attenuation, and has obvious progress compared with the prior art.
In order to achieve the above object, the present invention provides the following solutions: an infrared chip packaging adhesive with excellent cold and hot shock resistance is prepared from a component A and a component B in a mass ratio: 1: 0.9-1.05;
the component A comprises the following components in percentage by mass: 75-95% of epoxy resin, 4-25% of reactive diluent and 0.5-4% of auxiliary agent;
the component B comprises the following components in percentage by mass: 75-98% of acid anhydride, 1-15% of flexibilizer, 0.7-8% of accelerator, 0.03-3.0% of antioxidant and 0.03-3.0% of ultraviolet absorber.
Further, the mass ratio of the component A to the component B is as follows: 1:1.
Further, the epoxy resin is at least one of bisphenol a type epoxy resin, bisphenol F type epoxy resin, alicyclic epoxy resin, and hydrogenated bisphenol a epoxy resin.
Further, the epoxy resin is composed of bisphenol A epoxy resin and bisphenol F epoxy resin according to the mass ratio of 1: 0.05-0.2.
Further, the reactive diluent is at least one of cyclohexanediol ether, phenyl glycidyl ether, cyclohexanediol diglycidyl ether, polypropylene glycol diglycidyl ether and cyclohexanediol diglycidyl ester;
further, the reactive diluent is phenyl glycidyl ether.
Further, the auxiliary agent is at least one of a defoaming agent, a leveling agent and a dispersing agent.
Still further, the defoaming agent is one commonly used in the art, including but not limited to at least one of BYK-141, BYK-A530, BYK-020, BYK-022, BYK-024, BYK-028, BYK-034, BYK-052, BYK-053, BYK-055, BYK-057, BYK-065, BYK-066N, BYK-072, BYK-088, and BYK-SPECIAL.
Still further, the leveling agent is one commonly used in the art, including, but not limited to, at least one of SLE-7350, BYK-300, BYK-306, BYK-307, BYK-310, BYK-315, BYK-320, BYK-323, BYK-325, BYK-331, BYK-333, BYK-335, BYK-337, BYK-344, BYK-346, BYK-354, BYK-356, BYK-358N, BYK-361N, BYK-370, BYK-371, BYK-390, BYK-410, and BYK-077.
Still further, the dispersant is one commonly used in the art, including, but not limited to, at least one of BYK-P104S, BYK-P104, BYK-101, BYK-103, BYK-107, BYK-108, BYK-110, BYK-111, BYK-161, BYK-163, BYK-164, BYK-166, BYK-170, BYK-180, BYK-181, BYK-182, BYK-190, and BYK-220S.
Further, the acid anhydride is tetrahydrophthalic anhydride and methyl tetrahydrophthalic anhydride, wherein the mass fraction of the tetrahydrophthalic anhydride in the acid anhydride is 20-35%.
Further, the toughening agent is modified anhydride, the modified anhydride is prepared by grafting and modifying methyl hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride or a mixture of the methyl hexahydrophthalic anhydride and the methyl tetrahydrophthalic anhydride, and the tail end of the modified anhydride has an anhydride functional group.
Further, the modified acid anhydride has an equivalent weight of 550 to 750g/mol and a viscosity of 40 to 50 cps.
Further, the modified anhydride is modified methyl tetrahydrophthalic anhydride, the equivalent weight is 550-750 g/mol, and the viscosity is 50 cps.
Further, the accelerator is at least one of DBU p-toluenesulfonate, DBU formate, DBU caprylate, DBN and benzyltriphenylphosphonium chloride.
Further, the antioxidant is at least one of a basf antioxidant 1010, an antioxidant 1098, and an antioxidant 168.
Further, the ultraviolet absorbent is a hydroxy triazine derivative and/or TINUVIN 622.
Still further, the chain extender is at least one of cyclohexanediol, hexanediol, benzyl alcohol and diethylene glycol ether.
The invention also aims to provide a method for preparing the infrared chip packaging adhesive, which comprises the following steps:
s1, preheating the epoxy resin, adding an active diluent and an auxiliary agent, and uniformly stirring to obtain a component A;
s2, adding the accelerant into the anhydride while stirring, adding the antioxidant and the ultraviolet absorbent, stirring and dissolving uniformly, adding the flexibilizer, stirring uniformly, and filtering to obtain the component B.
In order to improve the cold and heat shock resistance of an epoxy resin system, JH0610, JH-0611, JH-0612 and JH-0621 modified anhydrides are directly added into the epoxy resin to obtain expected high cold and heat shock resistance, but the general light decay is high, and the light decay is more than 50% after 48 hours. Therefore, the product packaged by the packaging adhesive does not have the performance of having the cycle times of more than 300 under the cold and hot shock condition of-40-105 ℃ while having low light attenuation (less than 5 percent). The inventor surprisingly finds that the cold and heat shock resistance of the modified anhydride can be remarkably improved without sacrificing the light attenuation condition by optimizing the type of the modified anhydride and controlling the equivalent weight and the viscosity of the modified anhydride within a certain range (550-750 g/mol, the viscosity of 40-50 cps), and particularly, when the anhydride is optimized to be the modified methyl tetrahydrophthalic anhydride, the equivalent weight of 550-750 g/mol and the viscosity of 50cps, the optimal effect is achieved.
Compared with the prior art, the invention has the following beneficial effects:
the infrared chip packaging adhesive provided by the invention has the advantages that the purpose of remarkably improving the cold and heat shock resistance of the infrared chip packaging adhesive is realized on the premise of not sacrificing the light decay condition by adding the modified anhydride with specific equivalent weight and specific viscosity into the system as the toughening agent, the light decay is less than 5%, the cycle frequency reaches more than 300 under the cold and heat shock condition of-40-105 ℃, and the infrared chip packaging adhesive is remarkably improved compared with the prior art.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments of examples. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1 Infrared chip Package adhesive with Excellent thermal shock resistance
Consists of a component A and a component B, wherein:
the preparation method of the packaging adhesive comprises the following steps:
s1, preheating epoxy resin, adding benzyl glycidyl ether, BYK-SPECIAL and BYK-320, and stirring uniformly to obtain a component A;
s2, adding DBU p-toluenesulfonate into the mixture of methyl tetrahydrophthalic anhydride and tetrahydrophthalic anhydride while stirring, adding Pasteur antioxidant 1010 and TINUVIN 622, stirring to dissolve uniformly, adding modified methyl tetrahydrophthalic anhydride, stirring uniformly, and filtering to obtain component B.
Example 2 Infrared chip Package adhesive with Excellent thermal shock resistance
Consists of a component A and a component B, wherein:
the preparation process is referred to example 1.
Example 3 Infrared chip Package adhesive with Excellent thermal shock resistance
Consists of a component A and a component B, wherein:
the preparation process is referred to example 1.
Comparative example 1 infrared chip packaging adhesive
Comparative example 1 is different from example 1 in that the content of methyl tetrahydrophthalic anhydride was increased to 68.5g and the content of tetrahydrophthalic anhydride was increased to 29.5g without adding modified methyl tetrahydrophthalic anhydride, and the remaining parameters were the same as in example 1.
Comparative example 2 infrared chip packaging adhesive
Comparative example 2 is different from example 1 in that the equivalent weight of the modified methyl tetrahydrophthalic anhydride is 400 to 450g/mol, the viscosity is 30cps, and the remaining parameters are the same as those of example 1.
Comparative example 3 infrared chip packaging adhesive
Comparative example 3 is different from example 1 in that the equivalent weight of the modified methyl tetrahydrophthalic anhydride is 800 to 850g/mol, the viscosity is 60cps, and the remaining parameters are the same as those of example 1.
Comparative example 4 and Chinese patent application CN107353858A Infrared LED chip packaging adhesive prepared in example 3
Test example I, Performance test
Testing the infrared chip packaging adhesive prepared in the embodiments 1-3 and the comparative examples 1-4, uniformly mixing the component A and the component B according to a corresponding proportion, pouring 850nm infrared LED chip lamp beads, pasting, baking and curing at 125 ℃/1hrs +135 ℃/8hrs, and performing light decay, reflow soldering and cold and heat shock resistance tests on the prepared product, wherein the test results are shown in the following table 1:
TABLE 1 test results
Note: the light attenuation test method comprises the following steps: taking a cured 850nm infrared LED chip lamp bead of 100pcs, illuminating for 1000 hours at 50mA/100mA, and recording the light attenuation condition; the reflow soldering resistant frequency test method comprises the following steps: testing a cured 850nm infrared LED chip bead of 100pcs at 260-275 ℃/15s, stopping the test when the product is dead, and recording the reflow soldering resistant times; and (3) testing the number of cold and heat shock resistant cycles: the test conditions are-40 ℃/20min, 105 ℃/20min, the test is stopped when the lamp is stopped, the cycle number is recorded, and the number of samples is 100 pcs.
As can be seen from the above table 1, the product is lighted for 1000H at 50mA/100mA after being packaged by the packaging adhesive, the light attenuation is less than 5%, and meanwhile, the cold and heat shock resistance (40-105 ℃, 300 cycles) is obviously improved compared with the comparative ratio of 4.
Test example two, toughener screening test
On the basis of the formula of the embodiment 1, different toughening agents are respectively added to prepare various groups of packaging adhesives, packaging is carried out according to a method of a test example, and the light attenuation condition and the cold and heat shock resistance of various groups of LED products are tested, and the test results are shown in the following table 2.
TABLE 2 test results
The equivalent weight of the modified anhydride is 550-750 g/mol, and the viscosity is 50 cps.
As can be seen from the above table, in the formulation of the embodiment 1 of the present invention, the lowest light decay can be obtained by adding the modified methyl tetrahydrophthalic anhydride with specific equivalent and viscosity for toughening, and the modified methyl tetrahydrophthalic anhydride has the characteristic of reaching 300 cycles at the temperature of 40 ℃ to 105 ℃, while the addition of other types of toughening agents has the capability of reaching 300 cycles at the temperature of 40 ℃/105 ℃, but the general light decay is higher, and the light decay exceeds 50% after individual samples are taken for 48 hours.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. An infrared chip packaging adhesive with excellent cold and hot shock resistance is characterized by comprising a component A and a component B in a mass ratio: 1: 0.9-1.05;
the component A comprises the following components in percentage by mass: 75-95% of epoxy resin, 4-25% of reactive diluent and 0.5-4% of auxiliary agent;
the component B comprises the following components in percentage by mass: 75-98% of acid anhydride, 1-15% of flexibilizer, 0.7-8% of accelerator, 0.03-3.0% of antioxidant and 0.03-3.0% of ultraviolet absorber.
2. The infrared chip packaging adhesive of claim 1, wherein the epoxy resin is at least one of bisphenol a epoxy resin, bisphenol F epoxy resin, cycloaliphatic epoxy resin, and hydrogenated bisphenol a epoxy resin.
3. The infrared chip packaging adhesive according to claim 1, wherein the reactive diluent is at least one of cyclohexanediol ether, phenyl glycidyl ether, cyclohexanediol diglycidyl ether, polypropylene glycol diglycidyl ether, and cyclohexanediol diglycidyl ester; the auxiliary agent is at least one of a defoaming agent, a leveling agent and a dispersing agent.
4. The infrared chip packaging adhesive according to claim 1, wherein the acid anhydride is tetrahydrophthalic anhydride and methyl tetrahydrophthalic anhydride, and the mass fraction of the tetrahydrophthalic anhydride in the acid anhydride is 20-35%.
5. The infrared chip packaging adhesive of claim 1, wherein the toughening agent is a modified anhydride, the modified anhydride is prepared by graft modification of methyl hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride or a mixture of the methyl hexahydrophthalic anhydride and the methyl tetrahydrophthalic anhydride, and the end of the modified anhydride has an anhydride functional group.
6. The infrared chip packaging adhesive according to claim 5, wherein the equivalent weight of the modified acid anhydride is 550 to 750g/mol, and the viscosity is 40 to 50 cps.
7. The infrared chip packaging adhesive according to claim 6, wherein the modified anhydride is modified methyl tetrahydrophthalic anhydride, the equivalent weight of the modified methyl tetrahydrophthalic anhydride is 550 to 750g/mol, and the viscosity is 50 cps.
8. The infrared chip packaging adhesive of claim 1, wherein the accelerator is at least one of DBU p-toluenesulfonate, DBU formate, DBU octanoate, DBN and benzyltriphenylphosphonium chloride.
9. The infrared chip packaging adhesive of claim 1, wherein the antioxidant is at least one of basf antioxidant 1010, antioxidant 1098, and antioxidant 168; the ultraviolet absorbent is hydroxyl triazine derivative and/or TINUVIN 622.
10. A method for preparing the infrared chip packaging adhesive as claimed in any one of claims 1 to 9, characterized by comprising the following steps:
s1, preheating the epoxy resin, adding an active diluent and an auxiliary agent, and uniformly stirring to obtain a component A;
s2, adding the accelerant into the anhydride while stirring, continuing to add the antioxidant and the ultraviolet absorbent, stirring and dissolving uniformly, adding the flexibilizer, stirring uniformly, and filtering to obtain the component B.
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| CN201911014531.5A CN110724487B (en) | 2019-10-23 | 2019-10-23 | Infrared chip packaging adhesive with excellent cold and hot shock resistance and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112086254A (en) * | 2020-08-12 | 2020-12-15 | 西安宏星电子浆料科技股份有限公司 | Environment-friendly thick-film resistor paste |
| CN116179131A (en) * | 2023-03-20 | 2023-05-30 | 广州聚合新材料科技股份有限公司 | Underfill as well as preparation method and application thereof |
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| CN107353858A (en) * | 2017-07-12 | 2017-11-17 | 广州惠利电子材料有限公司 | Infrared LED chip packaging plastic and its preparation method and application |
| CN108219727A (en) * | 2018-01-03 | 2018-06-29 | 郑州中原思蓝德高科股份有限公司 | A kind of modifying epoxy resin by organosilicon encapsulating material and LED packaging plastics |
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| JP2009155450A (en) * | 2007-12-26 | 2009-07-16 | Sekisui Chem Co Ltd | Adhesive for electronic component |
| CN107057623A (en) * | 2017-05-22 | 2017-08-18 | 重庆江川化工（集团）有限公司 | A kind of filling special epoxy pouring sealant of transformer large volume and preparation method and application |
| CN107353858A (en) * | 2017-07-12 | 2017-11-17 | 广州惠利电子材料有限公司 | Infrared LED chip packaging plastic and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116179131A (en) * | 2023-03-20 | 2023-05-30 | 广州聚合新材料科技股份有限公司 | Underfill as well as preparation method and application thereof |
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| CN110724487B (en) | 2021-08-06 |
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