CN115678476B - Low-thermal-expansion high-temperature-resistance chip underfill adhesive and preparation method thereof - Google Patents
Low-thermal-expansion high-temperature-resistance chip underfill adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of adhesives, and mainly relates to a low-thermal-expansion high-temperature-resistance chip underfill adhesive and a preparation method thereof. The low-thermal-expansion high-temperature-resistance chip underfill disclosed by the invention is mainly prepared from the following raw materials in parts by weight: 10-30 parts of epoxy resin; 15-35 parts of a curing agent; 0.5-2 parts of a coupling agent; 0.1-5 parts of an accelerator; 2-20 parts of a diluent; 0.1-1 part of a dispersant; 0.5-5 parts of pigment; 40-70 parts of a filler; 0.5-10 parts of expanded particle resin; the expanded particle resin is prepared by mixing particles consisting of a metal shell and a high-molecular expanded core material with resin and then performing two-dimensional treatment. The invention has the advantages of simple synthesis and good stability, and the prepared underfill has the characteristics of no shrinkage, low thermal expansion coefficient, high dimensional stability, drop resistance, impact resistance, high temperature resistance and quick flow.
Description
Technical Field
The invention relates to a low-thermal expansion high-temperature resistance chip bottom filling adhesive and a preparation method thereof, belonging to the technical field of adhesives.
Background
With the development of electronic products towards miniaturization, lightness, thinness and performance, IC packages also tend to be miniaturized and highly integrated. The underfill is used to disperse the stress of the chip, reduce the influence of the solder ball under the external force of impact, bending and the like, prevent the solder part from breaking, and improve the reliability of the whole product, so the underfill becomes a necessary process for improving the reliability of the electronic product. Underfill technology is becoming increasingly important. The underfill process is to dot coat the epoxy resin on the chip edge, fill the resin to cover the device by capillary effect, complete the underfill process, and cure the epoxy resin by heating. The underfill can solve many problems of the precise electronic element, such as the underfill can greatly improve the shock resistance, improve the failure of the solder ball caused by thermal stress generated by inconsistent thermal expansion coefficients, and effectively improve the thermal stress resistance.
Along with the development of vehicle mounting, components face a more severe working environment, and how to further solve the stress problem of underfill and chips is the key of industry development. The prior art generally adopts a method of increasing the content of the filler to reduce the volume shrinkage rate and the thermal expansion coefficient, but causes the problems of viscosity increase, fluidity reduction, poor filling and poor falling caused by overhigh modulus.
Therefore, how to reduce the volume shrinkage and the thermal expansion coefficient on the premise of not influencing the permeability and the dropping performance is an urgent problem to be solved in the industry.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a low-thermal-expansion high-temperature-resistance chip underfill adhesive and a preparation method thereof.
The technical scheme for solving the technical problems is as follows:
the invention aims to provide a low-thermal-expansion high-temperature-resistance chip underfill which is mainly prepared from the following raw materials in parts by weight:
10-30 parts of epoxy resin;
15-35 parts of a curing agent;
0.5-2 parts of a coupling agent;
0.1-5 parts of an accelerator;
2-20 parts of a diluent;
0.1-1 part of a dispersant;
0.5-5 parts of pigment;
40-70 parts of a filler;
0.5-10 parts of expanded particle resin;
the expanded particle resin is prepared by mixing particles consisting of a metal shell and a high-molecular expanded core material with resin and then performing two-dimensional treatment.
On the basis of the technical scheme, the invention can also make the following improvements:
further, the preparation of the expanded particle resin mainly comprises the following steps:
(1) Adding the polymer expanded microspheres into concentrated acid, ultrasonically dispersing uniformly, heating in a water bath at 70-90 ℃ for reaction, washing with deionized water, and filtering to neutrality;
(2) Adding the particles treated in the step (1) into a heavy metal salt solution, heating and stirring in a water bath at 40-60 ℃, and filtering for later use;
(3) Dropwise adding the heated acidic solution into the particles filtered in the step (2), stirring for 20-50min, washing with deionized water, and filtering to neutrality;
(4) Adding the particles treated in the step (3) into the prepared heavy metal plating solution, adjusting the pH value to 6-8, heating in a water bath at 40-50 ℃, stirring for 100-150min, washing with deionized water, and filtering to neutrality;
(5) And (3) mixing the particles prepared in the step (4) with alicyclic epoxy resin according to the proportion of 1.5-2, and rolling once by using a roller press to prepare the expanded particle resin.
Further, the roller press is a ceramic three-roller press, and the gap is set to be 2-3 μm.
The beneficial effect of adopting the further technical scheme is that after directional extrusion, the expanded particles form a sheet structure, and after heating, the particles expand to recover a three-dimensional spherical structure, so that the curing shrinkage of the epoxy resin can be counteracted.
Further, the polymer expanded microsphere is one or a combination of any several of Expancel 461 DU 20, 461 DU 40, 920 DU 20 and 920 DU 40.
Furthermore, the expansion temperature of the high polymer expanded microsphere is 100-150 ℃, the particle size is 5-15 μm, and the expansion rate is 0-400%.
Further, the heavy metal salt solution is 10g/L SnCl 2 A hydrochloric acid solution; the acid solution is 2g/L PdCl 2 An acidic solution; the heavy metal plating solution is a nickel plating solution。
Further, the epoxy resin is one or a combination of any more of bisphenol A type epoxy resin, bisphenol F type epoxy resin, novolac epoxy resin, biphenyl epoxy resin, naphthalene ring epoxy resin, dicyclopentadiene epoxy resin and alicyclic epoxy resin.
Further, the curing agent is one or the combination of any several of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride, 2,3-naphthalic anhydride, dodecenyl succinic anhydride, bisphenol A diether dianhydride, 4,4' -oxydiphthalic anhydride and cyclobutane tetracarboxylic dianhydride.
Further, the coupling agent is one or the combination of any more of 3-glycidoxypropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyltrimethoxysilane and 3-mercaptopropyltrimethoxysilane.
Further, the accelerator is one or any combination of imidazole, tertiary amine, quaternary ammonium salt, phosphorus salt and modified amine.
Further, the filler is one or the combination of any several of spherical alumina, spherical silicon micropowder, aluminum hydroxide and calcium carbonate.
Further, the pigment is carbon black or titanium dioxide.
Further, the diluent is one or the combination of any several of butyl glycidyl ether, o-tolyl glycidyl ether, p-tert-butylphenyl glycidyl ether, 1,4-cyclohexanedimethanol diglycidyl ether, resorcinol diglycidyl ether and triglycidyl-p-aminophenol.
Further, the dispersing agent is one or the combination of any more of BYK-9076, W903, W907, W966, W9010 and DISPERBYK-111.
The invention also aims to provide a preparation method of the underfill adhesive for the low-thermal-expansion high-temperature-resistance chip, which comprises the following steps of:
adding epoxy resin, curing agent, diluent, coupling agent, pigment and dispersing agent into a vacuum double-planet stirring kettle, and stirring for 50-70min; adding filler, and stirring for 50-70min; adding the expanded particle resin, and stirring for 20-50min; adding accelerator, and stirring for 20-50min to obtain the underfill.
The invention has the beneficial effects that:
according to the invention, the tough metal is wrapped outside the expansion particles, and after two-dimensional flattening treatment is carried out, the expansion particles inside the expansion particles expand in the heating process, so that the volume of the expansion particles is increased, and the expansion rate of the expansion particles can be effectively controlled due to the wrapping of the metal shell; compared with the conventional expansion particles, the expansion particles have lower thermal expansion coefficient and higher dimensional stability during temperature impact and thermal cycle, cannot generate stress difference due to excessive expansion, and can realize no shrinkage of glue; the expanded particle resin has the advantages of simple synthesis and good stability, and the prepared underfill has the characteristics of no shrinkage, low thermal expansion coefficient, high dimensional stability, drop resistance, impact resistance, high temperature resistance and quick flow.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The expanded particle resin of the present invention is carried out according to the following steps:
(1) Adding 20 10g of polymer expanded microsphere Expancel 461 DU into 200ml of concentrated sulfuric acid (98%), performing ultrasonic dispersion uniformly, heating in a water bath at 80 ℃ for 40min for reaction, washing with deionized water, and filtering to neutrality;
(2) Adding the particles treated in the step (1) into 10g/L SnCl 2 Heating in hydrochloric acid solution at 50 deg.C in water bath, stirring for 20min, and washing with deionized water to neutrality;
(3) Heating to 60 ℃ 2g/L PdCl 2 Dropwise adding the acidic solution into the particles treated in the step (2), stirring for 30min, washing with deionized water, and filtering to neutrality;
(4) Adding the particles treated in the step (3) into a nickel plating solution, adjusting the pH =6, heating in a water bath at 45 ℃, stirring for 120min, washing with deionized water, filtering, and drying in vacuum to obtain expanded particles;
(5) The expanded particles thus obtained and an alicyclic epoxy resin were mixed in accordance with 1:1, and a two-dimensional expanded particle resin was obtained by passing the mixture through a ceramic three-roll mill with a gap of 2 μm.
Example 1:
adding 7 parts of bisphenol F epoxy resin, 15 parts of novolac epoxy resin, 22 parts of methyl tetrahydrophthalic anhydride, 2.3 parts of p-tert-butylphenyl glycidyl ether, 0.5 part of 3-glycidyl ether oxypropyl trimethoxy silane, 0.5 part of carbon black and 5363 parts of BYK-90760.2 into a vacuum double-planet stirring kettle, and stirring for 60min under the conditions of the autorotation stirring speed of 1000r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15-0.098 MPa and the temperature of 25 +/-5 ℃; adding 50 parts of silicon micro powder, and stirring for 60min under the conditions that the autorotation stirring speed is 1000r/min +/-50 r/min, the revolution stirring speed is 20r/min +/-2 r/min, the pressure is-0.15 to-0.098 MPa, and the temperature is 25 ℃ +/-5 ℃; adding 2 parts of the self-made expanded particle resin, and stirring for 30min at the conditions of a rotation stirring speed of 500r/min +/-50 r/min, a revolution stirring speed of 20r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃; adding 0.5 part of imidazole accelerator, and stirring for 30min under the conditions of a rotation stirring speed of 500r/min +/-50 r/min, a revolution stirring speed of 18r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃ to obtain the underfill.
Example 2:
adding 6 parts of bisphenol F epoxy resin, 15 parts of novolac epoxy resin, 20 parts of methyl tetrahydrophthalic anhydride, 2.3 parts of p-tert-butylphenyl glycidyl ether, 0.5 part of 3-glycidyl ether oxypropyl trimethoxy silane, 0.5 part of carbon black and 5363 parts of BYK-90760.2 into a vacuum double-planet stirring kettle, and stirring for 60min under the conditions of the autorotation stirring speed of 1000r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15-0.098 MPa and the temperature of 25 +/-5 ℃; adding 50 parts of silicon micro powder, and stirring for 60min under the conditions that the autorotation stirring speed is 1000r/min +/-50 r/min, the revolution stirring speed is 20r/min +/-2 r/min, the pressure is-0.15 to-0.098 MPa, and the temperature is 25 ℃ +/-5 ℃; adding 5 parts of the self-made expanded particle resin, and stirring for 30min at the conditions of the autorotation stirring speed of 500r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15 to-0.098 MPa and the temperature of 25 ℃ +/-5 ℃; adding 0.5 part of imidazole accelerator, and stirring for 30min under the conditions of a rotation stirring speed of 500r/min +/-50 r/min, a revolution stirring speed of 18r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃ to obtain the underfill.
Example 3:
adding 6 parts of bisphenol F epoxy resin, 15 parts of dicyclopentadiene epoxy resin, 20 parts of methyl nadic anhydride, 2.3 parts of triglycidyl p-aminophenol, 0.5 part of 3-mercaptopropyl trimethoxy silane, 0.5 part of carbon black and 0.2 part of BYK-W903 into a vacuum double-planet stirring kettle, and stirring for 60min under the conditions of the autorotation stirring speed of 1000r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15 to-0.098 MPa and the temperature of 25 ℃ +/-5 ℃; adding 50 parts of silicon micro powder, and stirring for 60min under the conditions that the autorotation stirring speed is 1000r/min +/-50 r/min, the revolution stirring speed is 20r/min +/-2 r/min, the pressure is-0.15 to-0.098 MPa, and the temperature is 25 ℃ +/-5 ℃; adding 5 parts of the self-made expanded particle resin, and stirring for 30min at the conditions of the autorotation stirring speed of 500r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15 to-0.098 MPa and the temperature of 25 ℃ +/-5 ℃; adding 0.5 part of a phosphonium salt accelerator, and stirring for 30min under the conditions of a rotation stirring speed of 500r/min +/-50 r/min, a revolution stirring speed of 18r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃ to obtain the underfill.
Example 4:
adding 5 parts of bisphenol F epoxy resin, 14 parts of dicyclopentadiene epoxy resin, 19 parts of methyl nadic anhydride, 2.3 parts of triglycidyl p-aminophenol, 0.5 part of 3-mercaptopropyl trimethoxy silane, 0.5 part of carbon black and 0.2 part of BYK-9076 into a vacuum double-planet stirring kettle, and stirring for 60min under the conditions of the autorotation stirring speed of 1000r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15 to-0.098 MPa and the temperature of 25 ℃ +/-5 ℃; adding 50 parts of silicon micro powder, and stirring for 60min under the conditions that the autorotation stirring speed is 1000r/min +/-50 r/min, the revolution stirring speed is 20r/min +/-2 r/min, the pressure is-0.15 to-0.098 MPa, and the temperature is 25 ℃ +/-5 ℃; adding 8 parts of the self-made expanded particle resin, and stirring for 30min at the conditions of a rotation stirring speed of 500r/min +/-50 r/min, a revolution stirring speed of 20r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃; adding 0.5 part of a phosphonium salt accelerator, and stirring for 30min under the conditions of a rotation stirring speed of 500r/min +/-50 r/min, a revolution stirring speed of 18r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃ to obtain the underfill.
Comparative example 1:
adding 8 parts of bisphenol F epoxy resin, 15 parts of novolac epoxy resin, 23 parts of methyl tetrahydrophthalic anhydride, 2.3 parts of p-tert-butylphenyl glycidyl ether, 0.5 part of 3-glycidyl ether oxypropyl trimethoxy silane, 0.5 part of carbon black and 5363 parts of BYK-90760.2 into a vacuum double-planet stirring kettle, and stirring for 60min under the conditions of the autorotation stirring speed of 1000r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15-0.098 MPa and the temperature of 25 +/-5 ℃; adding 50 parts of silicon micro powder, and stirring for 60min under the conditions that the autorotation stirring speed is 1000r/min +/-50 r/min, the revolution stirring speed is 20r/min +/-2 r/min, the pressure is-0.15 to-0.098 MPa, and the temperature is 25 ℃ +/-5 ℃; adding 0.5 part of imidazole accelerator, and stirring for 30min under the conditions of autorotation stirring speed of 500r/min +/-50 r/min, revolution stirring speed of 18r/min +/-2 r/min, pressure of-0.15 to-0.098 MPa and temperature of 25 ℃ +/-5 ℃ to obtain the conventional underfill adhesive.
Comparative example 2:
adding 8 parts of bisphenol F epoxy resin, 15 parts of dicyclopentadiene epoxy resin, 23 parts of methyl nadic anhydride, 2.3 parts of triglycidyl p-aminophenol, 0.5 part of 3-mercaptopropyl trimethoxy silane, 0.5 part of carbon black and 0.2 part of BYK-W903 into a vacuum double-planet stirring kettle, and stirring for 60min under the conditions of the rotation stirring speed of 1000r/min +/-50 r/min, the revolution stirring speed of 20r/min +/-2 r/min, the pressure of-0.15 to-0.098 MPa and the temperature of 25 ℃ +/-5 ℃; adding 50 parts of silicon micro powder, and stirring for 60min under the conditions of a rotation stirring speed of 1000r/min +/-50 r/min, a revolution stirring speed of 20r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃; adding 2 parts of conventional expanded particles, and stirring for 30min under the conditions of a rotation stirring speed of 500r/min +/-50 r/min, a revolution stirring speed of 20r/min +/-2 r/min, a pressure of-0.15 to-0.098 MPa and a temperature of 25 ℃ +/-5 ℃; adding 0.5 part of a phosphate accelerator, and stirring for 30min under the conditions that the autorotation stirring speed is 500r/min +/-50 r/min, the revolution stirring speed is 18r/min +/-2 r/min, the pressure is-0.15 to-0.098 MPa, and the temperature is 25 ℃ +/-5 ℃ to obtain the conventional underfill.
The following performance tests were performed on the underfill prepared in examples 1 to 4 and the conventional underfill prepared in comparative examples 1 to 2, respectively, and the results of the measured performance data are shown in table 1 below.
TABLE 1 results of Performance data for examples 1-4 and comparative examples 1-2
It can be seen from the performance data results in table 1 that, when a certain proportion of self-made expanded particle resin is added, the glue can realize the effect of no shrinkage, the CTE (coefficient of thermal expansion) is reduced on the premise of not influencing TG (glass transition temperature), permeation speed and strength, the strength retention of cold and hot impact and thermal cycle is improved compared with the conventional system, thereby greatly improving the reliability and the service life of the chip, the volume expansion rate is difficult to control when conventional expanded particles are added, cavities are easily generated inside, the CTE is increased, the strength is reduced, and the thermal cycle performance is greatly reduced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (8)
1. The low-thermal-expansion high-temperature-resistance chip underfill is characterized by being mainly prepared from the following raw materials in parts by weight:
10-30 parts of epoxy resin;
15-35 parts of a curing agent;
0.5-2 parts of a coupling agent;
0.1-5 parts of an accelerator;
2-20 parts of a diluent;
0.1-1 part of a dispersant;
0.5-5 parts of pigment;
40-70 parts of a filler;
0.5-10 parts of expanded particle resin;
the expanded particle resin is prepared by mixing particles consisting of a metal shell and a high-molecular expanded core material with resin and then performing two-dimensional treatment;
the preparation of the expanded particle resin mainly comprises the following steps:
(1) Adding the polymer expanded microspheres into concentrated acid, ultrasonically dispersing uniformly, heating in a water bath at 70-90 ℃ for reaction, washing with deionized water, and filtering to neutrality;
(2) Adding the particles treated in the step (1) into a heavy metal salt solution, heating and stirring in a water bath at 40-60 ℃, and filtering for later use;
(3) Dropwise adding the heated acidic solution into the particles filtered in the step (2), stirring for 20-50min, washing with deionized water, and filtering to neutrality;
(4) Adding the particles treated in the step (3) into the prepared heavy metal plating solution, adjusting the pH to 6-8, heating in a water bath at 40-50 ℃, stirring for 100-150min, washing with deionized water, and filtering to neutrality;
(5) Mixing the particles prepared in the step (4) with alicyclic epoxy resin according to the proportion of 1.5-2, and rolling once by using a roller press to prepare expanded particle resin;
the heavy metal salt solution is 10g/L SnCl 2 A hydrochloric acid solution; the acid solution is 2g/L PdCl 2 An acidic solution; the heavy metal plating solution is a nickel plating solution.
2. The low-thermal-expansion high-temperature-resistance chip underfill according to claim 1, wherein the expansion temperature of the polymer expanded microspheres is 100-150 ℃, the particle size is 5-15 μm, and the expansion rate is 0-400%.
3. The underfill adhesive for low thermal expansion high temperature resistance chips according to claim 1, wherein the epoxy resin is one or a combination of any of bisphenol a epoxy resin, bisphenol F epoxy resin, novolac epoxy resin, biphenyl epoxy resin, naphthalene ring epoxy resin, dicyclopentadiene epoxy resin, and alicyclic epoxy resin.
4. The underfill for low thermal expansion high temperature resistance chips according to claim 1, wherein the curing agent is one or a combination of several of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride, 2,3-naphthalic anhydride, dodecenyl succinic anhydride, bisphenol A diether dianhydride, 4,4' -oxydiphthalic anhydride and cyclobutane tetracarboxylic dianhydride.
5. The low-thermal-expansion high-temperature-resistance chip underfill according to claim 1, wherein the coupling agent is one or a combination of any of 3-glycidoxypropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyltrimethoxysilane and 3-mercaptopropyltrimethoxysilane.
6. The low-thermal-expansion high-temperature-resistance chip underfill according to claim 1, wherein the accelerator is one or any combination of imidazole, tertiary amine, quaternary ammonium salt, phosphonium salt and modified amine; the filler is one or the combination of any more of spherical alumina, spherical silica micropowder, aluminum hydroxide and calcium carbonate.
7. The low-thermal-expansion high-temperature-resistance chip underfill according to claim 1, wherein the diluent is one or a combination of any of butyl glycidyl ether, o-tolyl glycidyl ether, p-tert-butylphenyl glycidyl ether, 1,4-cyclohexanedimethanol diglycidyl ether, resorcinol diglycidyl ether, and triglycidyl-p-aminophenol.
8. The preparation method of the low-thermal-expansion high-temperature-resistance chip underfill according to any one of claims 1 to 7, comprising the following steps:
adding epoxy resin, curing agent, diluent, coupling agent, pigment and dispersing agent into a vacuum double-planet stirring kettle, and stirring for 50-70min; adding filler, and stirring for 50-70min; adding the expanded particle resin, and stirring for 20-50min; adding accelerator, and stirring for 20-50min to obtain the underfill.
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