CN117700929A - Underfill material for protecting 5G communication chip - Google Patents

Underfill material for protecting 5G communication chip Download PDF

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Publication number
CN117700929A
CN117700929A CN202311631793.2A CN202311631793A CN117700929A CN 117700929 A CN117700929 A CN 117700929A CN 202311631793 A CN202311631793 A CN 202311631793A CN 117700929 A CN117700929 A CN 117700929A
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parts
epoxy resin
underfill material
stirring
communication chip
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闫善涛
王建斌
陈田安
解海华
徐友志
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Yantai Darbond Technology Co Ltd
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Yantai Darbond Technology Co Ltd
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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
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • C08G59/4207—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
    • C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • 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
    • 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
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • 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
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/18—Spheres
    • C08L2205/20—Hollow spheres

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention relates to an underfill material for protecting a 5G communication chip, which is prepared by blending and modifying self-synthesized biphenol type epoxy resin and naphthol type epoxy resin, sequentially adding epoxy modified silicone oil, mixed filler, dodecenyl succinic anhydride and 1-cyanoethyl-2-ethyl-4-methylimidazole, uniformly mixing, and carrying out vacuum defoaming treatment. The invention introduces biphenyl structure and binaphthyl structure, which can obviously reduce the dielectric constant of the bottom filling material. The mixed filler of the spherical aluminum nitride and the hollow polystyrene microbeads can greatly improve the heat conduction performance and the dielectric performance of the bottom filling material. The underfill material prepared by the invention has the advantages of low dielectric property, high heat conduction property, good heat resistance, good high and low temperature resistance and the like, and is suitable for packaging and protecting various high-speed and high-frequency band 5G mobile communication chips.

Description

Underfill material for protecting 5G communication chip
Technical Field
The invention relates to an underfill material for protecting a 5G communication chip, and belongs to the field of adhesives.
Background
With the rapid development of the internet, the explosive growth of mobile data traffic makes it difficult for the 4G communication technology to meet the requirements of mobile data traffic explosion. The high-frequency and high-speed 5G communication technology is becoming a key technology for supporting the economic and social intelligence digitization. The 5G communication technology adopts millimeter wave band transmission, has the characteristics of high power, high frequency band, high speed, low time delay and the like, but the millimeter wave has large heat release and large attenuation in the transmission process. Based on the above, the 5G communication technology requires that the dielectric material used has a large thermal conductivity and a small dielectric constant and dielectric loss. Delay and loss are reduced while high-speed transmission of signals is ensured.
The protection of the 5G communication chip needs to adopt an underfill material with high heat conduction and low dielectric, and the conventional underfill material cannot meet the transmission requirements of high frequency and high speed of the 5G communication technology at present. Chinese patent CN113122172a discloses an underfill for 5G device chip packaging, which reduces dielectric constant and improves thermal conductivity by using low molecular weight naphthol modified epoxy resin and adding thermal conductive filler. However, high thermal conductivity is not characterized. Chinese patent CN111440575a discloses a special low dielectric high thermal conductivity underfill for chip package, which adopts low molecular weight fluorine-containing polyphenolic structural epoxy resin and thermal conductive filler to improve thermal conductivity. But low dielectric properties are not characterized.
Therefore, new material technology is needed for 5G communication chip protection, and a chip protection underfill material with high heat conduction, low dielectric property and high reliability is prepared.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an underfill material for protecting a 5G communication chip, and the underfill material prepared by the invention has the advantages of low dielectric property, high heat conduction property, heat resistance, high and low temperature resistance and the like.
The technical scheme for solving the technical problems is as follows: the preparation method of the underfill material for protecting the 5G communication chip comprises the following steps:
a. the weight portions are as follows: sequentially adding 30-33 parts of diphenol, 1-2 parts of 2-chloroethyl trimethyl ammonium chloride and 65-69 parts of epoxy chloropropane into a 500ml three-neck flask, installing a condensing tube, heating to 50-60 ℃, setting the rotating speed to 20RPM, mechanically stirring for 2-3 hours, and cooling to room temperature; under the stirring condition of 20RPM (rotational speed), 5-7 parts of sodium hydroxide solution with the concentration of 9.5mol/L are added dropwise at 1 drop/second, the temperature is heated to 60-70 ℃, 35RPM of rotational speed is set, the mechanical stirring is carried out for 5-6 hours, the temperature is cooled to room temperature, deionized water is washed to be neutral, and the pressure is reduced, so that the self-synthesized biphenol epoxy resin is prepared; the reaction formula is as follows:
b. the weight portions are as follows: adding 80 parts of spherical silicon nitride and 20 parts of hollow polystyrene microspheres into a V-shaped mixer for uniform dispersion to prepare mixed filler;
c. the weight portions are as follows: 15-24 parts of self-synthesized biphenol type epoxy resin, 14-20 parts of naphthol type epoxy resin, 1-5 parts of epoxy modified silicone oil, 20-25 parts of dodecenyl succinic anhydride, 1-2 parts of 1-cyanoethyl-2-ethyl-4-methylimidazole and 34-39 parts of mixed filler are sequentially put into a stirring kettle, and the stirring kettle is subjected to stirring for 3-4 hours under the condition of vacuum pumping at a rotating speed of 40 RPM.
On the basis of the technical scheme, the invention also improves as follows.
Further, the synthetic mechanism of the self-synthesized biphenol epoxy resin is that epoxy groups in epoxy chloropropane are subjected to etherification reaction with hydroxyl groups in biphenol under the catalysis of 2-chloroethyl trimethyl ammonium chloride, and then polycondensation reaction is carried out under the condition of sodium hydroxide alkali.
The self-synthesized biphenol epoxy resin has the advantages of unique biphenyl structure and excellent low dielectric property and heat resistance.
Further, the mixed filler is TA-S30 manufactured by Yaan Bai Toku Gao New Material Co., ltd. And the hollow polystyrene microbeads are NM HT200 manufactured by Suzhou Nami micro technology Co., ltd.
The adoption of the further scheme has the beneficial effects that the spherical aluminum nitride in the mixed filler has the characteristics of high thermal conductivity and low thermal expansion coefficient, and on the premise of meeting the chip filling requirement, the average particle diameter is selected to be 35-45 mu m, so that the optimization of the thermal conductivity is facilitated; the hollow polystyrene microbeads have the characteristics of low dielectric property and low thermal expansion coefficient, and the average particle diameter of 15-25 mu m is selected to be favorable for optimizing the low dielectric property and increasing the filling property of the bottom filling material. The mass ratio of the mixed filler is 4:1, providing the best high thermal conductivity and low dielectric properties.
The naphthol type epoxy resin is XY676 produced by Anhui New and remote technology and technology Co., ltd, and has the specific structural formula:
the further scheme has the beneficial effects that the naphthol type epoxy resin has a unique binaphthyl structure and shows excellent low dielectric property and heat resistance.
Further, the epoxy modified silicone oil is HR163EP-2 manufactured by Shanghai Yangzhi Co., ltd, and has the specific structural formula:
the further scheme has the beneficial effects that the epoxy modified silicone oil is low-viscosity liquid at room temperature, and has the characteristics of good dilution performance, good flexibility and good high-low temperature resistance.
Further, the dodecenyl succinic anhydride is DDSA produced by Vertellus company, and the specific structural formula is as follows:
the dodecenyl succinic anhydride has the advantages of maleic anhydride and branched chain olefin isomer structures, and has the characteristics of quick solidification at medium and low temperatures, good flexibility and good high and low temperature resistance.
Further, the 1-cyanoethyl-2-ethyl-4-methylimidazole is 2E4MZ-CN manufactured by Kagaku Kogyo Co., ltd., and has the specific structural formula:
the adoption of the further scheme has the beneficial effects that the room temperature of the 1-cyanoethyl-2-ethyl-4-methylimidazole is liquid, and the method has the characteristics of good compatibility with epoxy resin, quick acceleration of curing at medium and low temperature and good heat resistance of a cured product.
The beneficial effects of the invention are as follows: the underfill material of the invention has low dielectric property, and effectively reduces delay and loss of high-speed signal transmission. High heat-conducting property, and effectively ensures the heat radiation function requirement of high-power signal transmission. The solder ball for the 5G mobile chip is effectively protected by the solder ball, so that the solder ball has high reliability.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
a. The weight portions are as follows: 90g of biphenol, 3g of 2-chloroethyl trimethyl ammonium chloride and 207g of epoxy chloropropane are sequentially added into a 500ml three-neck flask, a condensing tube is arranged, the mixture is heated to 55 ℃, the rotating speed is set to 20RPM, and the mixture is mechanically stirred for 2 hours and cooled to room temperature; under the stirring condition of 20RPM, 21g of sodium hydroxide solution with the concentration of 9.5mol/L is added dropwise at the speed of 1 drop/second, the temperature is heated to 65 ℃, the RPM is set at 35RPM, the mechanical stirring is carried out for 6 hours, the temperature is cooled to the room temperature, the deionized water is washed to be neutral, and the pressure is reduced for rotary evaporation, thus obtaining the synthetic biphenol epoxy resin;
b. the weight portions are as follows: adding spherical aluminum nitride TA-S30400g and hollow polystyrene microsphere NMHT200100g into a V-shaped mixer to uniformly disperse to prepare mixed filler;
c. the weight portions are as follows: 240g of self-synthesized biphenol type epoxy resin, 676140g of naphthol type epoxy resin, 163EP-210g of epoxy modified silicone oil HR, 250g of dodecenyl succinic anhydride DDSA, 20g of 1-cyanoethyl-2-ethyl-4-methylimidazole 2E4MZ-CN and 340g of mixed filler are sequentially put into a stirring kettle, the rotating speed is set to 40RPM under the vacuumizing condition, and stirring is carried out for 3 hours, so that the underfill material is prepared.
Example 2
a. The weight portions are as follows: 96g of biphenol, 6g of 2-chloroethyl trimethyl ammonium chloride and 198g of epoxy chloropropane are sequentially added into a 500ml three-neck flask, a condensing tube is arranged, the mixture is heated to 55 ℃, the rotating speed is set to 20RPM, and the mixture is mechanically stirred for 3 hours and cooled to room temperature; under the stirring condition of 20RPM, 18g of sodium hydroxide solution with the concentration of 9.5mol/L is added dropwise at the speed of 1 drop/second, the temperature is heated to 65 ℃, the RPM is set at 35RPM, the mechanical stirring is carried out for 6 hours, the temperature is cooled to the room temperature, the deionized water is washed to be neutral, and the pressure is reduced for rotary evaporation, thus obtaining the synthetic biphenol epoxy resin;
b. the weight portions are as follows: adding spherical aluminum nitride TA-S30400g and hollow polystyrene microsphere NMHT200100g into a V-shaped mixer to uniformly disperse to prepare mixed filler;
c. the weight portions are as follows: 200g of self-synthesized biphenol type epoxy resin, 676160g of naphthol type epoxy resin, HR163EP-230g of epoxy modified silicone oil, DDSA 220g of dodecenyl succinic anhydride, 15g of 1-cyanoethyl-2-ethyl-4-methylimidazole 2E4MZ-CN and 375g of mixed filler are sequentially put into a stirring kettle, the rotating speed is set at 40RPM under the vacuumizing condition, and the stirring is carried out for 3 hours, so that the underfill material is prepared.
Example 3
a. The weight portions are as follows: 99g of biphenol, 6g of 2-chloroethyl trimethyl ammonium chloride and 195g of epoxy chloropropane are sequentially added into a 500ml three-neck flask, a condensing tube is arranged, the mixture is heated to 55 ℃, the rotating speed is set to 20RPM, and the mixture is mechanically stirred for 3 hours and cooled to room temperature; under the stirring condition of 20RPM, 15g of sodium hydroxide solution with the concentration of 9.5mol/L is added dropwise at the speed of 1 drop/second, the temperature is heated to 65 ℃, the RPM is set at 35RPM, the mechanical stirring is carried out for 5 hours, the temperature is cooled to the room temperature, the deionized water is washed to be neutral, and the pressure is reduced for rotary evaporation, thus obtaining the synthetic biphenol epoxy resin;
b. the weight portions are as follows: adding spherical aluminum nitride TA-S30400g and hollow polystyrene microsphere NMHT200100g into a V-shaped mixer to uniformly disperse to prepare mixed filler;
c. the weight portions are as follows: 150g of self-synthesized biphenol type epoxy resin, 676200g of naphthol type epoxy resin, 163EP-250g of epoxy modified silicone oil HR, 200g of dodecenyl succinic anhydride DDSA, 10g of 1-cyanoethyl-2-ethyl-4-methylimidazole 2E4MZ-CN and 390g of mixed filler are sequentially put into a stirring kettle, the rotating speed is set at 40RPM under the vacuumizing condition, and the stirring is carried out for 4 hours, thus obtaining the underfill material.
Comparative example 1
a. The weight portions are as follows: adding spherical aluminum nitride TA-S30400g and hollow polystyrene microsphere NMHT200100g into a V-shaped mixer to uniformly disperse to prepare mixed filler;
b. the weight portions are as follows: 150g of bisphenol F type epoxy resin EXA-830CRP, 676200g of naphthol type epoxy resin XY, 163EP-250g of epoxy modified silicone oil HR, 200g of dodecenyl succinic anhydride DDSA, 10g of 1-cyanoethyl-2-ethyl-4-methylimidazole 2E4MZ-CN and 390g of mixed filler are sequentially put into a stirring kettle, the rotating speed is set at 40RPM under the vacuumizing condition, and the stirring is carried out for 4 hours, thus obtaining the underfill material.
Comparative example 2
a. The weight portions are as follows: 90g of biphenol, 3g of 2-chloroethyl trimethyl ammonium chloride and 207g of epoxy chloropropane are sequentially added into a 500ml three-neck flask, a condensing tube is arranged, the mixture is heated to 55 ℃, the rotating speed is set to 20RPM, and the mixture is mechanically stirred for 2 hours and cooled to room temperature; under the stirring condition of 20RPM, 21g of sodium hydroxide solution with the concentration of 9.5mol/L is added dropwise at the speed of 1 drop/second, the temperature is heated to 65 ℃, the RPM is set at 35RPM, the mechanical stirring is carried out for 6 hours, the temperature is cooled to the room temperature, the deionized water is washed to be neutral, and the pressure is reduced for rotary evaporation, thus obtaining the synthetic biphenol epoxy resin;
b. the weight portions are as follows: adding spherical aluminum nitride TA-S30400g and hollow polystyrene microsphere NMHT200100g into a V-shaped mixer to uniformly disperse to prepare mixed filler;
c. the weight portions are as follows: 240g of self-synthesized biphenol type epoxy resin, 140g of bisphenol F type epoxy resin EXA-830CRP, 140g of epoxy modified silicone oil HR163EP-210g, 250g of dodecenyl succinic anhydride DDSA, 20g of 1-cyanoethyl-2-ethyl-4-methylimidazole 2E4MZ-CN and 340g of mixed filler are sequentially put into a stirring kettle, the rotating speed is set to 40RPM under the vacuumizing condition, and the stirring is carried out for 3 hours, thus obtaining the underfill material.
Comparative example 3
a. The weight portions are as follows: 96g of biphenol, 6g of 2-chloroethyl trimethyl ammonium chloride and 198g of epoxy chloropropane are sequentially added into a 500ml three-neck flask, a condensing tube is arranged, the mixture is heated to 55 ℃, the rotating speed is set to 20RPM, and the mixture is mechanically stirred for 3 hours and cooled to room temperature; under the stirring condition of 20RPM, 18g of sodium hydroxide solution with the concentration of 9.5mol/L is added dropwise at the speed of 1 drop/second, the temperature is heated to 65 ℃, the RPM is set at 35RPM, the mechanical stirring is carried out for 6 hours, the temperature is cooled to the room temperature, the deionized water is washed to be neutral, and the pressure is reduced for rotary evaporation, thus obtaining the synthetic biphenol epoxy resin;
b. the weight portions are as follows: adding spherical aluminum nitride TA-S30390g and hollow polystyrene microsphere NMHT200110g into a V-shaped mixer to uniformly disperse to prepare mixed filler;
c. the weight portions are as follows: 200g of self-synthesized biphenol type epoxy resin, 676160g of naphthol type epoxy resin, HR163EP-230g of epoxy modified silicone oil, DDSA 220g of dodecenyl succinic anhydride, 15g of 1-cyanoethyl-2-ethyl-4-methylimidazole 2E4MZ-CN and 375g of mixed filler are sequentially put into a stirring kettle, the rotating speed is set at 40RPM under the vacuumizing condition, and the stirring is carried out for 3 hours, so that the underfill material is prepared.
Comparative example 4
a. The weight portions are as follows: 96g of biphenol, 6g of 2-chloroethyl trimethyl ammonium chloride and 198g of epoxy chloropropane are sequentially added into a 500ml three-neck flask, a condensing tube is arranged, the mixture is heated to 55 ℃, the rotating speed is set to 20RPM, and the mixture is mechanically stirred for 3 hours and cooled to room temperature; under the stirring condition of 20RPM, 18g of sodium hydroxide solution with the concentration of 9.5mol/L is added dropwise at the speed of 1 drop/second, the temperature is heated to 65 ℃, the RPM is set at 35RPM, the mechanical stirring is carried out for 6 hours, the temperature is cooled to the room temperature, the deionized water is washed to be neutral, and the pressure is reduced for rotary evaporation, thus obtaining the synthetic biphenol epoxy resin;
b. the weight portions are as follows: adding spherical aluminum nitride TA-S30410g and hollow polystyrene microsphere NMHT20090g into a V-shaped mixer to uniformly disperse to prepare mixed filler;
c. the weight portions are as follows: 200g of self-synthesized biphenol type epoxy resin, 676160g of naphthol type epoxy resin, HR163EP-230g of epoxy modified silicone oil, DDSA 220g of dodecenyl succinic anhydride, 15g of 1-cyanoethyl-2-ethyl-4-methylimidazole 2E4MZ-CN and 375g of mixed filler are sequentially put into a stirring kettle, the rotating speed is set at 40RPM under the vacuumizing condition, and the stirring is carried out for 3 hours, so that the underfill material is prepared.
Comparative example 5
a. The weight portions are as follows: 90g of naphthol, 9g of benzyl triethyl ammonium chloride and 201g of epoxy chloropropane are sequentially added into a 500ml three-neck flask, a condensing tube is arranged, the mixture is heated to 50 ℃, the rotating speed is set to 20RPM, and the mixture is mechanically stirred for 2 hours and cooled to room temperature; under the stirring condition of 20RPM (rotational speed), 15g of sodium hydroxide solution with the concentration of 9.5mol/L is added dropwise at 1 drop/second, the temperature is heated to 50 ℃, the rotational speed is set at 35RPM, the mechanical stirring is carried out for 4 hours, the temperature is cooled to room temperature, deionized water is washed to be neutral, and the pressure is reduced for rotary evaporation, so that the low molecular weight naphthol modified epoxy resin is prepared;
b. the weight portions are as follows: 200g of spherical graphite and 200g of hollow glass microspheres are added into a V-shaped mixer to be uniformly dispersed, so as to prepare a mixed heat conducting filler;
c. the weight portions are as follows: 70g of low molecular weight naphthol modified epoxy resin, 630g of bisphenol A epoxy resin, 50g of cyclohexylamine curing agent, 240g of heat conducting mixed filler, 10g of phenyl glycidyl ether and 1g of silane coupling agent are sequentially put into a stirring kettle, and the stirring is carried out for 3 hours under the condition of vacuum pumping at a set rotating speed of 40RPM, so as to obtain the underfill material.
Comparative example 6
a. The weight portions are as follows: 100g of 2, 6-difluoronaphthol acrylate, 50g of 2, 6-dimethylphenol acrylate, 50g of glycidyl methacrylate, 2000g of xylene-soluble epoxy resin, 20g of diisobutyryl peroxide serving as an initiator, and sequentially adding the materials into a reaction kettle, heating to 80 ℃, setting the rotating speed to 20RPM, mechanically stirring for 5 hours, cooling to room temperature, and purifying to obtain the low-molecular-weight fluorine-containing polyphenyl phenol structural epoxy resin;
b. the weight portions are as follows: 100g of low molecular weight fluorine-containing polyphenyl phenol structural epoxy resin, 50g of bisphenol F epoxy resin, 100g of trimethylolpropane triglycidyl ether, 200g of core-shell modified epoxy flexibilizer, 50g of methyl nadic anhydride curing agent, 50g of imidazole compound accelerator, 1g of silane coupling agent, 200g of spherical alumina and 3g of organosilicon defoamer are sequentially put into a stirring kettle, and the stirring kettle is subjected to stirring for 4 hours at a set rotating speed of 40RPM under the vacuumizing condition, so that the underfill material is prepared.
Specific test examples
The performance of the underfill materials of the above examples 1 to 3 and comparative examples 1 to 6 of the present invention was tested by the following test. Wherein the low dielectric property is characterized by a dielectric constant and a dielectric loss, the smaller the value, the better the low dielectric property is characterized; the high heat conduction performance is characterized by a heat conduction coefficient, and the larger the numerical value is, the better the heat conduction performance is characterized; the heat resistance is characterized by the number of times of lead-free reflow soldering, and the more the number of times is, the better the heat resistance is. The high and low temperature resistance is characterized by the number of cold and hot impact cycles, and the higher the number is, the better the high and low temperature resistance is.
Test example 1 dielectric constant test
The dielectric constant in ε is measured according to GB/T1409-2006 test standard using a radio frequency impedance material analyzer at a test frequency of 60 Hz.
Test example 2 dielectric loss tangent test
Testing frequency 10 using a radio frequency impedance material analyzer 6 Hz, dielectric loss tangent, unit tan delta, was measured according to GB/T1409-2006 test standard.
Test example 3 thermal conductivity test
The thermal conductivity coefficient is measured according to GB/T10294-2008 test standard by using a thermal conductivity coefficient measuring instrument, and the unit W/(m.K)
Test example 4 lead-free reflow test
And (3) using an SMT lead-free reflow soldering machine, and according to a semiconductor industry standard J-STD-030 test method, placing the packaging chip of the underfill material after curing, and testing the electrical property of the chip in a single unit.
Test example 5 Cold and Hot impact test
Setting parameters of-40-100 ℃ by using a cold and hot impact box, and keeping the program for 30min according to IEC60068-2-14Na:2009 testing standard, the packaging chip of the bottom filling material is put in after being solidified, and the electrical property of the chip is tested in unit time.
The test results are shown in table 1 below.
Table 1 test results of samples prepared in examples 1 to 3 and comparative examples 1 to 6
As can be seen from the data in Table 1, the underfill material prepared by the invention has the advantages of low dielectric property, high heat conduction property, good heat resistance, good high and low temperature resistance and the like, and is suitable for packaging and protecting various high-speed and high-frequency band 5G mobile communication chips.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (6)

1. A method for preparing an underfill material for 5G communication chip protection, comprising the steps of:
a. the weight portions are as follows: sequentially adding 30-33 parts of diphenol, 1-2 parts of 2-chloroethyl trimethyl ammonium chloride and 65-69 parts of epoxy chloropropane into a 500ml three-neck flask, installing a condensing tube, heating to 50-60 ℃, setting the rotating speed to 20RPM, mechanically stirring for 2-3 hours, and cooling to room temperature; under the stirring condition of 20RPM (rotational speed), 5-7 parts of sodium hydroxide solution with the concentration of 9.5mol/L are added dropwise at 1 drop/second, the temperature is heated to 60-70 ℃, 35RPM of rotational speed is set, the mechanical stirring is carried out for 5-6 hours, the temperature is cooled to room temperature, deionized water is washed to be neutral, and the pressure is reduced, so that the self-synthesized biphenol epoxy resin is prepared; the reaction is as follows：b. The weight portions are as follows: adding 80 parts of spherical aluminum nitride and 20 parts of hollow polystyrene microspheres into a V-shaped mixer to uniformly disperse, so as to prepare a mixed filler;
c. the weight portions are as follows: 15-24 parts of self-synthesized biphenol type epoxy resin, 14-20 parts of naphthol type epoxy resin, 1-5 parts of epoxy modified silicone oil, 20-25 parts of dodecenyl succinic anhydride, 1-2 parts of 1-cyanoethyl-2-ethyl-4-methylimidazole and 34-39 parts of mixed filler are sequentially put into a stirring kettle, and the stirring kettle is subjected to stirring for 3-4 hours under the condition of vacuum pumping at a rotating speed of 40 RPM.
2. The method for preparing the underfill material for 5G communication chip protection according to claim 1, wherein the mixed filler is spherical aluminum nitride with an average particle diameter of 35-45 μm and hollow polystyrene microbeads with an average particle diameter of 15-25 μm according to a mass ratio of 4: 1.
3. The method for preparing the underfill material for 5G communication chip protection according to claim 1, wherein the naphthol type epoxy resin is naphthol type epoxy resin with a softening point of 85-98 ℃, a high-temperature viscosity of 300-800 mPa.s at 150 ℃ and an epoxy equivalent of 155-170G/eq.
4. The method for preparing the underfill material for 5G communication chip protection according to claim 1, wherein the epoxy modified silicone oil is an organosilicon modified epoxy resin with a viscosity of 20-40 mPa.s at 25 ℃, an epoxy equivalent of 505-545G/eq and a molecular weight of 1000.
5. The method for preparing an underfill material for 5G communication chip protection according to claim 1, wherein the dodecenyl succinic anhydride has a viscosity of 400-600 mPa.s at 20 ℃, an acid value of 395-432 and a molecular weight of 266.4.
6. The method for preparing the underfill material for protecting the 5G communication chip according to claim 1, wherein the purity of the 1-cyanoethyl-2-ethyl-4-methylimidazole is more than or equal to 99%, the molecular weight is 163.22, and the melting point is 61-66 ℃.
CN202311631793.2A 2023-12-01 2023-12-01 Underfill material for protecting 5G communication chip Pending CN117700929A (en)

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