CN-122011684-A - Low-conductivity resin composition and preparation method thereof

Abstract

The invention discloses a low-conductivity resin composition and a preparation method thereof, and in particular relates to the technical field of polymer composite materials, wherein the composition comprises 100 parts of liquid crystal epoxy resin, 5-15 parts of cage polysilsesquioxane, 20-40 parts of flaky boron nitride, 10-20 parts of spherical alumina and 30-50 parts of maleimide-allyl bisphenol A copolymer curing agent. The preparation method comprises the steps of S1, prepolymer preparation, S2, filler hybridization, S3 and solidification molding. According to the invention, the octaaminopropyl POSS is used for constructing the nano-pores in the matrix to effectively reduce the dielectric constant, and the oriented arrangement of the flaky boron nitride is used for forming the heat conduction path, so that the technical problem that the low dielectric property and the high heat conduction of the resin material are difficult to be compatible is cooperatively solved, and meanwhile, the octaaminopropyl POSS has high heat resistance, and is particularly suitable for the fields of 5G communication, semiconductor packaging and the like.

Inventors

• Che Dongjiang
• REN XIAODONG
• CHENG JINGJING

Assignees

• 山西兴安新材料有限公司

Dates

Publication Date

20260512

Application Date

20260410

Claims (9)

1. 1. The low-conductivity resin composition is characterized by comprising the following components in parts by mass: 100 parts of liquid crystal epoxy resin, 5-15 parts of cage polysilsesquioxane, 20-40 parts of flaky boron nitride, 10-20 parts of spherical alumina and 30-50 parts of maleimide-allyl bisphenol A copolymer curing agent; Wherein, the cage polysilsesquioxane is octaaminopropyl POSS, which is uniformly dispersed in the liquid crystal epoxy resin through chemical bonding to form a crosslinked network structure with nano pores; the flaky boron nitride is directionally arranged in the composition to form an anisotropic heat conduction path.
2. 2. The low-conductivity resin composition according to claim 1, wherein the liquid crystal epoxy resin is a liquid crystal compound comprising biphenyl mesogenic groups and epoxy groups, and has an epoxy value ranging from 0.5 to 0.8eq/100g.
3. 3. The low conductivity resin composition according to claim 2, wherein the plate-like boron nitride has a thickness of 10 to 50nm, a ratio of diameter to thickness of more than 50, and a surface thereof is modified by a silane coupling agent which is gamma-aminopropyl triethoxysilane having a benzene ring.
4. 4. The low-conductivity resin composition according to claim 3, wherein the spherical alumina has a particle diameter of 0.5 to 2. Mu.m, and is used for filling gaps between heat conduction paths made of the plate-like boron nitride.
5. 5. A process for producing the low-conductivity resin composition according to claim 4, comprising the steps of: S1, preparing a prepolymer, namely reacting cage-type polysilsesquioxane with liquid crystal epoxy resin for 1-3 hours at the temperature of 70-90 ℃ under the protection of inert gas to obtain a cage-type polysilsesquioxane-liquid crystal epoxy prepolymer; S2, filler hybridization, namely adding the flaky boron nitride and spherical alumina subjected to surface modification into a cage polysilsesquioxane-liquid crystal epoxy prepolymer, and uniformly dispersing under the synergistic effect of ultrasonic power 400-600W and shear rate 800-1200S -1 to obtain a resin mixture; S3, curing and molding, namely adding a maleimide-allyl bisphenol A copolymer curing agent into the resin mixture, uniformly mixing, and sequentially carrying out step heating and curing treatment.
6. 6. The method of claim 5, wherein in step S1, the inert gas is nitrogen or argon, the reaction temperature is 80 ℃, and the reaction time is 2 hours.
7. 7. The method according to claim 6, wherein the step-heating curing process in step S3 is specifically: The first stage, pre-curing for 1-2h at 110-130 ℃; a second stage of curing at 170-190 ℃ for 1-3 hours to form an ordered structure; and in the third stage, post-curing is carried out at 210-230 ℃ for 0.5-1.5h, and the final crosslinking is completed.
8. 8. The method according to claim 7, wherein the optimal conditions for the step-heating curing process are 120℃C/1h, 180℃C/2h, 220℃C/1h.
9. 9. The method according to claim 8, wherein in step S2, the flaky boron nitride and the spherical alumina are dry-mixed in a high-speed mixer for 5-15min at 80-100 ℃ before being added to form a homogeneous composite filler.

Description

Low-conductivity resin composition and preparation method thereof Technical Field The invention relates to the technical field of polymer composite materials, in particular to a low-conductivity resin composition and a preparation method thereof. Background With the rapid development of 5G communication, artificial intelligence and high performance computing technologies, electronic components are evolving towards high frequency, high speed, high power density and miniaturization, which has not only required to have extremely low dielectric constant and dielectric loss factor to reduce signal transmission delay and loss, but also excellent thermal conductivity to ensure timely dissipation of heat generated by core components such as chips, and meanwhile, high enough heat resistance is required to ensure reliability in high temperature process and service environment. In order to reduce the dielectric constant of the resin material, the following approaches are mainly adopted in the prior art: 1. Fluorine atoms are introduced, for example, fluorinated epoxy resin or cyanate resin is adopted, and although the method can effectively reduce the dielectric constant, the method has the defects of high material cost, often reduced heat resistance, possibility of precipitating corrosive hydrogen fluoride under certain conditions and the like; 2. introducing a porous structure, namely, pore forming in a resin matrix by adding a pore-forming agent or using a template method, however, the method generally faces the problems that the pore distribution and the size are difficult to control accurately, the mechanical strength of the material is remarkably deteriorated due to the introduction of excessive pores, the hygroscopicity is increased, and the high-frequency dielectric performance is possibly deteriorated; 3. Low polar polymers such as polyphenylene oxide and polyimide are used, and although the materials have excellent dielectric properties, the materials have poor compatibility with common matrixes such as epoxy resin and the like, are difficult to process and have high cost. In addition, in terms of improving thermal conductivity, it is common practice to add a high thermal conductive filler such as alumina, aluminum nitride or boron nitride to a resin matrix, however, to achieve a higher thermal conductive path, it is often necessary to fill a large amount of filler, which directly causes a sharp rise in material viscosity, deterioration in workability, and, since the filler itself contains a higher dielectric constant, it is inevitable to raise the overall dielectric constant of the composite material, contrary to the original intention of achieving low dielectric. In recent years, liquid crystal epoxy resins have been attracting attention because of the fact that the molecular chains thereof can spontaneously orient during curing to form an ordered structure, thereby imparting an intrinsic, anisotropic, high thermal conduction path to the material, however, simple liquid crystal epoxy resins have limited space for further lowering of the dielectric constant, and stability of the dielectric loss at high frequencies has yet to be improved. Accordingly, the present invention provides a low conductivity resin composition and a method for preparing the same. Disclosure of Invention In order to overcome the above-mentioned drawbacks of the prior art, the present invention provides a low-conductivity resin composition and a preparation method thereof, which solve the above-mentioned problems of the prior art. In order to achieve the purpose, the invention provides the following technical scheme that the low-conductivity resin composition comprises the following components in parts by mass: 100 parts of liquid crystal epoxy resin, 5-15 parts of cage polysilsesquioxane, 20-40 parts of flaky boron nitride, 10-20 parts of spherical alumina and 30-50 parts of maleimide-allyl bisphenol A copolymer curing agent; Wherein, the cage polysilsesquioxane is octaaminopropyl POSS, which is uniformly dispersed in the liquid crystal epoxy resin through chemical bonding to form a crosslinked network structure with nano pores; the flaky boron nitride is directionally arranged in the composition to form an anisotropic heat conduction path. Preferably, the liquid crystal epoxy resin is a liquid crystal compound containing biphenyl mesogenic groups and epoxy groups, and the epoxy value thereof ranges from 0.5 to 0.8eq/100g. Preferably, the thickness of the flaky boron nitride is 10-50nm, the diameter-thickness ratio is more than 50, and the surface of the flaky boron nitride is modified by a silane coupling agent, wherein the silane coupling agent is gamma-aminopropyl triethoxysilane containing benzene rings. Preferably, the particle size of the spherical alumina is 0.5-2 μm, and the spherical alumina is used for filling gaps among the heat conduction paths formed by the platy boron nitride. The invention also provides a preparation me