CN117165236B - Insulating die bond adhesive for LED and preparation method thereof - Google Patents

Insulating die bond adhesive for LED and preparation method thereof Download PDF

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CN117165236B
CN117165236B CN202311415626.4A CN202311415626A CN117165236B CN 117165236 B CN117165236 B CN 117165236B CN 202311415626 A CN202311415626 A CN 202311415626A CN 117165236 B CN117165236 B CN 117165236B
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parts
epoxy resin
die bond
stirring
viscosity
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CN117165236A (en
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陈江聪
张淑娟
曹锋
徐远炬
彭兆平
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Kongjing Vision Intelligent Technology Co ltd
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Abstract

The invention relates to the field of adhesives, in particular to an insulating die bond adhesive for LEDs and a preparation method thereof. The insulating die bond adhesive for the LED comprises the following raw materials in parts by weight: 30-100 parts of matrix resin, 0.1-3 parts of photo-thermal initiator, 10-40 parts of filler, 0-2 parts of Lewis acid salt, 0.1-3 parts of coupling agent and 1-10 parts of auxiliary agent. The insulating die bond adhesive for the LED provided by the application is an epoxy insulating die bond adhesive which is cured by UV light and heat, has excellent adhesive property and other properties, is suitable for being used in various LED series products, and has excellent universality.

Description

Insulating die bond adhesive for LED and preparation method thereof
Technical Field
The invention relates to the field of adhesives, in particular to an insulating die bond adhesive for LEDs and a preparation method thereof.
Background
With the development of economy and the technological progress in the electronic field, the related industries have also entered a continuously updated stage in recent years. Along with the continuous upgrading and innovation of the LED packaging industry, the requirements of the market on products are more and more embodied and high-quality, particularly in the field of small-size chip packaging, the requirements of common epoxy die bonding glue are more and more raised, and the initial viscosity is changed into the high-viscosity, so that the performance is stable, the poisoning resistance is high, the curing speed is high, the thrust is high and the like.
The improvement of the insulating die bond for LEDs in the prior art is mainly focused on the modification of epoxy resin, and the blending physical modification of organosilicon and the grafting modification of organosilicon are generally adopted. However, the blending modification faces the problem of phase separation caused by poor compatibility of the organosilicon and the epoxy resin; the grafting modification of the organosilicon can effectively improve part of the performance of the die bond adhesive, but the modification operation is relatively complex, the steps are complicated, the process requirement is high, and the problems of stability, poisoning resistance and thrust are not further solved although the phase separation problem of physical blending is avoided. In the patent CN107974232B, the silicone resin is directly used as the main resin to prepare the die bond adhesive, and although the die bond adhesive prepared by the method is claimed to have excellent performance and good heat conduction and heat resistance, the technical problems are still not solved.
Therefore, in order to solve the problems, the application provides an insulating die bond adhesive for an LED and a preparation method thereof.
Disclosure of Invention
In order to solve the problems, the first aspect of the invention provides an insulating die bond adhesive for an LED, which comprises the following raw materials in parts by weight: 30-100 parts of matrix resin, 0.1-3 parts of photo-thermal initiator, 10-40 parts of filler, 0-2 parts of Lewis acid salt, 0.1-3 parts of coupling agent and 1-10 parts of auxiliary agent.
As a preferred embodiment, the matrix resin is an epoxy resin.
As a preferable embodiment, the epoxy resin is a mixture of an epoxy resin having a viscosity of 200 to 500 mPas/70 ℃ and an epoxy resin having a viscosity of 2000 to 3000 mPas/70 ℃.
As a preferable scheme, the mass ratio of the epoxy resin with the viscosity of 200-500 mPas/70 ℃ to the epoxy resin with the viscosity of 2000-3000 mPas/70 ℃ is 4-5.5:2-3.5.
As a preferable scheme, the mass ratio of the epoxy resin with the viscosity of 200-500 mPas/70 ℃ to the epoxy resin with the viscosity of 2000-3000 mPas/70 ℃ is 5.04:2.16.
As a preferred embodiment, the filler is spherical silica.
As a preferable embodiment, the average particle diameter of the spherical silica is2 to 4 μm.
As a preferred embodiment, the photo-thermal initiator is any one of cationic photoinitiators.
As a preferred scheme, the cationic photoinitiator IS any one of IS052, SS061, IS054 and SS 058.
As a preferred embodiment, the lewis acid salt is at least one of ammonium blocked lewis acid salts.
As a preferred embodiment, the Lewis acid salt is the ammonium blocked Lewis acid salt MLSB001.
As a preferred embodiment, the coupling agent is at least one of silane coupling agents.
As a preferable scheme, the silane coupling agent is any one of KH560 and KBM4803.
As a preferred embodiment, the silane coupling agent is KBM4803.
As a preferred embodiment, the auxiliary agents are antioxidants and anti-settling agents.
As a preferable scheme, the antioxidant is any one of phosphite antioxidants.
As a preferred embodiment, the anti-settling agent is anti-settling starch.
As a preferred scheme, the anti-sedimentation starch is anti-sedimentation powder DM30.
As a preferable scheme, the mass ratio of the epoxy resin to the anti-settling agent is 66.7-76.7: 2.9-5.8.
As a preferable scheme, the mass ratio of the matrix resin to the filler is 60-80: 10-30.
As a preferable scheme, the mass ratio of the matrix resin to the filler is 66-77: 15-27.
As a preferable scheme, the mass ratio of the matrix resin to the filler is 72:18.
in the application, the performance stability, the curing speed and the poisoning resistance of the prepared die bond adhesive can be effectively improved by adopting the compounding of epoxy resins with different viscosities. This is mainly because: when the mass ratio of the epoxy resin with the viscosity of 200-500 mPas/70 ℃ to the epoxy resin with the viscosity of 2000-3000 mPas/70 ℃ is 5.04:2.16, the mixing and coaction of the epoxy resin and the epoxy resin not only avoids the problem of resin compatibility, but also enables the interfacial kneading effect of different viscosity systems to form a compact linked network structure, the more compact structure can form a good bottom effect when external impurities enter, and a fixing groove is formed during curing to avoid the negative influence of the fixing groove on the bonding interface caused by the removal of the bonding interface, so that the product has excellent bonding stability and poisoning resistance.
The invention provides a preparation method of the insulating die bond adhesive for the LED, which comprises the following steps: (1) Weighing matrix resin and filler, adding the matrix resin and the filler into a stirring kettle, and stirring under pressure for 10-20 min to obtain a uniform mixture; (2) Adding an auxiliary agent and Lewis acid salt into the mixture, stirring at a temperature of 20-35 ℃ at a stirring speed of 1000-2000 r/min and a dispersing speed of 600-1000 r/min, and stirring for 1-2 hours to obtain a second mixture; (3) And (3) further adding a coupling agent and a photo-thermal initiator into the second mixture, stirring at a speed of 500-1000 r/min and a dispersion speed of 300-500 r/min, stirring for 0.5-2 h, and discharging to obtain the modified polyurethane foam.
The beneficial effects are that:
1. the insulating die bond adhesive for the LED provided by the application is an epoxy insulating die bond adhesive which is cured by UV light and heat, has excellent adhesive property and other properties, is suitable for being used in various LED series products, and has excellent universality.
2. The insulating die bonding adhesive for the LED has excellent surface drying performance, short curing time, high preparation initiation speed, small addition amount and high thrust performance at high temperature, and can realize the surface drying performance within 30 seconds.
3. The utility model provides an insulating solid brilliant glue for LED that this application provided, it can prevent effectively that the chip that collision or vibrations LED to in-process from sliding and tilting phenomenon in the support transportation after solid brilliant. The adhesive has excellent fixing and bonding properties, and can be effectively applied to transportation and transfer scenes.
4. The insulating die bond adhesive for the LED has excellent performance stability and poisoning resistance, can effectively avoid the influence on the bonding performance when sundries fall into the liquid die bond adhesive after die bonding, and keeps good bonding performance.
5. According to the insulating die bonding adhesive for the LED, the performance stability, the curing speed and the poisoning resistance of the prepared die bonding adhesive can be effectively improved by compounding epoxy resins with different viscosities, when the mass ratio of the epoxy resin with the viscosity of 200-500 mPas/70 ℃ to the epoxy resin with the viscosity of 2000-3000 mPas/70 ℃ is 5.04:2.16, the problem of resin compatibility is avoided by the mixing and coaction of the epoxy resin with the viscosity of 2000-3000 mPas/70 ℃, and the interface mixing effect of different viscosity systems can form a tight linked network structure.
Detailed Description
Example 1
Embodiment 1 provides an insulating die bond adhesive for an LED in a first aspect, which comprises the following raw materials in parts by weight: 66.7 parts of matrix resin, 1.34 parts of photo-thermal initiator, 26.7 parts of filler, 0 part of Lewis acid salt, 0.67 part of coupling agent and 4.67 parts of auxiliary agent.
Matrix resin: 46.7 parts of alicyclic epoxy resin CEL2021P, with average viscosity of 250 mPa.s/70 ℃; cycloaliphatic epoxy resin EHPE3150, 20 parts, average viscosity 2500 mPa.s/70 ℃.
The photo-thermal initiator was cationic initiator IS052, purchased from Hubei solid wetting technologies Co., ltd.
The filler was spherical silica having an average particle size of 2 μm and purchased from Jian City wood Lin Sen New Material technology Co., ltd.
The coupling agent is silane coupling agent KH560.
The auxiliary agent is an antioxidant and an anti-settling agent; the antioxidant is 168,1.34 parts of antioxidant; the anti-settling agent is anti-settling powder DM30,3.33 parts, purchased from Li yang Rui Cheng New Material Co.
The second aspect of the present embodiment provides a method for preparing the insulating die bond adhesive for an LED, including the following steps: (1) Weighing matrix resin and filler, adding into a stirring kettle, stirring under the pressure of-0.1 MPa for 10min to obtain a uniform mixture; (2) Adding an auxiliary agent and Lewis acid salt into the mixture, stirring at the temperature of 35 ℃ at the stirring speed of 1500r/min and the dispersing speed of 900r/min, and stirring for 1h to obtain a second mixture; (3) And (3) further adding a coupling agent and a photo-thermal initiator into the second mixture, stirring at a speed of 900r/min and a dispersion speed of 300r/min, stirring for 0.5h, and discharging to obtain the final product.
Example 2
The specific implementation of this example is the same as example 1, except that: the formula comprises the following components:
matrix resin: 46 parts of alicyclic epoxy resin CEL2021P, and the average viscosity is 250 mPa.s/70 ℃; 30.7 parts of cycloaliphatic epoxy resin EHPE3150 and having an average viscosity of 2500 mPa.s/70 ℃.
The photo-thermal initiator was cationic initiator IS052,1.54 parts, purchased from Hubei solid wetting technologies Co., ltd.
The filler was 15.4 parts of spherical silica having an average particle diameter of 2. Mu.m.
The coupling agent is 1.54 parts of silane coupling agent KBM4803.
The auxiliary agent is an antioxidant and an anti-settling agent; the antioxidant is 168,1.54 parts of antioxidant; the anti-settling agent is anti-settling powder DM30,5.8 parts, purchased from Li yang Rui Cheng New Material Co.
Example 3
The specific implementation of this example is the same as example 1, except that: the formula comprises the following components:
matrix resin: alicyclic epoxy resin CEL2021P,50.4 parts, average viscosity 250 mPa.s/70 ℃; cycloaliphatic epoxy resin EHPE3150, 21.6 parts, average viscosity 2500 mPa.s/70 ℃.
The photo-thermal initiator was cationic initiator SS061,1.44 parts, purchased from Hubei solid wet technologies Co., ltd.
The filler was spherical silica having an average particle diameter of 4. Mu.m, 18 parts.
The coupling agent is 1.44 parts of silane coupling agent KBM4803.
The auxiliary agent is an antioxidant and an anti-settling agent; the antioxidant is 168,2.16 parts of antioxidant; the anti-settling agent is anti-settling powder DM30,5.8 parts, purchased from Li yang Rui Cheng New Material Co.
Example 4
The specific implementation of this example is the same as example 1, except that: the formula comprises the following components:
matrix resin: 49.5 parts of alicyclic epoxy resin CEL2021P, and the average viscosity is 250 mPa.s/70 ℃; cycloaliphatic epoxy resin EHPE3150, 21 parts, average viscosity 2500 mPa.s/70 ℃.
The photo-thermal initiator was cationic initiator IS052,0.35 parts, purchased from Hubei solid wetting technologies Co., ltd.
The Lewis acid salt was ammonium blocked Lewis acid salt MLSB001,0.7 part, purchased from Ji Anshi wood Lin Sen New Material technologies Co., ltd.
The filler was spherical silica having an average particle diameter of 2. Mu.m, 21 parts.
The coupling agent is 1.44 parts of silane coupling agent KBM4803.
The auxiliary agent is an antioxidant and an anti-settling agent; the antioxidant is 168,2.1 parts of antioxidant; the anti-settling agent is anti-settling powder DM30,3.5 parts, purchased from Li yang Rui Cheng New Material Co.
Example 5
The specific implementation of this example is the same as example 1, except that: the formula comprises the following components:
matrix resin: 50 parts of alicyclic epoxy resin CEL2021P with average viscosity of 250 mPa.s/70 ℃; cycloaliphatic epoxy resin EHPE3150, 21.4 parts, average viscosity 2500 mPa.s/70 ℃.
The photo-thermal initiator was cationic initiator SS058,0.71 parts, purchased from hubei solid wet technologies inc.
The Lewis acid salt was ammonium blocked Lewis acid salt MLSB001,0.36 parts, purchased from Ji Anshi wood Lin Sen New Material technologies Co., ltd.
The filler was spherical silica having an average particle diameter of 2. Mu.m, 21 parts.
The coupling agent is silane coupling agent KH560,1.4 parts.
The auxiliary agent is an antioxidant and an anti-settling agent; the antioxidant is 168,1.78 parts of antioxidant; the anti-settling agent is anti-settling powder DM30,2.9 parts, purchased from Li yang Rui Cheng New Material Co.
Comparative example1
The specific embodiment of this comparative example is the same as example 1, except that: the formula comprises the following components:
matrix resin: 46.6 parts of alicyclic epoxy resin CEL2021P, with average viscosity of 250 mPa.s/70 ℃; cycloaliphatic epoxy resin EHPE3150, 20 parts, average viscosity 2500 mPa.s/70 ℃.
The photo-thermal initiator was cationic initiator IS054,1.33 parts, purchased from Hubei solid wetting technologies Co., ltd.
26.6 parts of spherical silica having an average particle diameter of 2. Mu.m.
The coupling agent is silane coupling agent KH560,0.341 parts.
The auxiliary agent is an antioxidant and an anti-settling agent; the antioxidant is 168,1.33 parts of antioxidant; the anti-settling agent is anti-settling powder DM30,2.67 parts, purchased from Li yang Rui Cheng New Material Co.
Comparative example 2
The specific embodiment of this comparative example is the same as example 1, except that: the formula comprises the following components:
matrix resin: 40 parts of alicyclic epoxy resin CEL2021P with average viscosity of 250 mPa.s/70 ℃; cycloaliphatic epoxy resin EHPE3150, 26.6 parts, average viscosity 2500 mPa.s/70 ℃.
The photo-thermal initiator was cationic initiator SS058,1.33 parts, purchased from hubei solid wet technologies inc.
The filler was spherical silica having an average particle diameter of 4. Mu.m, 26.7 parts.
The coupling agent is silane coupling agent KBM4803,1 part.
The auxiliary agent is an antioxidant and an anti-settling agent; the antioxidant is 168,1.67 parts of antioxidant; the anti-settling agent is anti-settling powder DM30,2.67 parts, purchased from Li yang Rui Cheng New Material Co.
Evaluation of Performance
Viscosity test: the viscosities Vis1 and Vis2 of the examples and comparative examples were measured using a Brookfield DV3T viscometer at 2r and 20r rates, where 2r and 20r represent the rotational speed of the viscometer, 2r is the 1 minute rotation of the viscometer spindle 2 turns, 20r represents the 1 minute rotation of the viscometer spindle 20 turns, vis1 and Vis2 represent the viscosity numbers at 2r and 20r, respectively, the thixotropic index is Vis 1/Vis 2, and the Vis2 results were taken as the product viscosity values, where viscosity @25 ℃ (5 # cps) represents the 25 ℃ test, 5# cps represents the use of a No. 5 spindle, and the results are reported in Table 1.
And (3) surface dry time test: the prepared glue solution is stored in a light-proof environment for standby, the glue solution is coated on a glass slide under the light-proof condition, the coating thickness is2 mu m, the glass slide is put into an ultraviolet curing machine for irradiation light curing under the same condition, after curing, the glass slide is lightly touched by fingers, the surface of the glue layer is free of viscosity or the glue layer is free of transfer, and the glue layer has certain strength, namely the surface dryness is achieved, and the curing time(s) required by the surface dryness of the glue layer is recorded.
Thrust testing: the die bond glue prepared in the above examples and comparative examples was cured on a 1515 surface silvered LED bare support using a full-automatic die bonder, the die bond was a sapphire chip size of 4 x 7mil, the post die bond support was cured by a UV curing oven (UV curing oven is a mercury lamp light source, wavelength 200-450 nm, peak wavelength 365nm, power density 35W/cm) for 10-30 s, and then transferred to a 170 ℃ oven for baking for 0.5h, and the thrust was tested at 25 ℃ and 160 ℃ using a Dage4000 push-pull machine, the results are reported in table 1.
Poisoning-resistant thrust: after the bracket is cured by a UV curing furnace according to the second normal die bonding operation, 150g of injection molding reclaimed material particles (such as reclaimed PPA particle master batch) are placed at the bottom of the material box, the material box is wrapped by tinfoil, the material box is placed in an oven for baking at 170 ℃ for 0.5h, and then the thrust at 160 ℃ is tested, so that the anti-poisoning performance of the die bonding adhesive is obtained, and the result is recorded in Table 1.
TABLE 1

Claims (4)

1. An insulating die bond adhesive for an LED, which is characterized in that: the raw materials comprise the following components in parts by weight: 66.7-76.7 parts of matrix resin, 0.1-3 parts of photo-thermal initiator, 10-40 parts of filler, 0-2 parts of Lewis acid salt, 1.54-3 parts of coupling agent and 1-10 parts of auxiliary agent;
the matrix resin is epoxy resin;
the epoxy resin is a mixture of epoxy resin with the viscosity of 200-500 mPas/70 ℃ and epoxy resin with the viscosity of 2000-3000 mPas/70 ℃;
the mass ratio of the epoxy resin with the viscosity of 200-500 mPas/70 ℃ to the epoxy resin with the viscosity of 2000-3000 mPas/70 ℃ is 5.04:2.16;
the filler is spherical silicon dioxide;
the average particle size of the spherical silicon dioxide is 2-4 mu m;
the mass ratio of the matrix resin to the filler is 72:18;
the photo-thermal initiator is any one of cationic photoinitiators; the cationic photoinitiator IS any one of IS052, SS061, IS054 and SS 058;
the auxiliary agent is an antioxidant and an anti-settling agent;
the anti-settling agent is anti-settling powder DM30;
the mass ratio of the epoxy resin to the anti-settling agent is 66.7-76.7: 3.33 to 5.8.
2. The insulating die bond paste for LEDs of claim 1, wherein: the Lewis acid salt is at least one of ammonium blocking Lewis acid salts.
3. The insulating die bond paste for LEDs as claimed in claim 2, wherein: the coupling agent is at least one of silane coupling agents.
4. A method for preparing the insulating die bond adhesive for LEDs according to any one of claims 1 to 3, which is characterized in that: the method comprises the following steps: (1) Weighing matrix resin and filler, adding the matrix resin and the filler into a stirring kettle, and stirring under pressure for 10-20 min to obtain a uniform mixture; (2) Adding an auxiliary agent and Lewis acid salt into the mixture, stirring at a temperature of 20-35 ℃ and a stirring speed of 1000-2000 r/min, and stirring for 1-2 hours to obtain a second mixture; (3) And (3) further adding a coupling agent and a photo-thermal initiator into the second mixture, stirring at the speed of 500-1000 r/min, stirring for 0.5-2 h, and discharging to obtain the final product.
CN202311415626.4A 2023-10-30 2023-10-30 Insulating die bond adhesive for LED and preparation method thereof Active CN117165236B (en)

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