CN-116769281-B - Preparation method of multi-load epoxy resin composite material

Abstract

The application provides a preparation method of a multi-load epoxy resin composite material, and belongs to the technical field of compositions containing epoxy resins. And (3) placing the artemisia annua and the bentonite in ethanol for uniform mixing, cooling, centrifugally separating and drying to obtain a product I, uniformly mixing the epoxy resin, the curing agent, the accelerator and the product I, and carrying out vacuum defoaming, so that the obtained mixture is cured to obtain the finished composite material. The composite material prepared by the scheme is used for high-end microelectronic packaging, aerospace, printing, biochemistry and sensors, and has the advantages of low nitriding rate, low water vapor permeability, excellent antibacterial property and the like.

Inventors

• QI RONGRONG
• ZAI JIANTAO
• QIAN XUEFENG

Assignees

• 上海交通大学绍兴新能源与分子工程研究院

Dates

Publication Date

20260505

Application Date

20230621

Claims (7)

1. 1. The preparation method of the multi-load epoxy resin composite material is characterized by comprising the following steps of: (1) Uniformly mixing 40-70 parts by mass of artemisia annua and 30-60 parts by mass of bentonite in ethanol, reacting for 6-24 hours at the temperature of 80-130 ℃, cooling, centrifugally separating, and vacuum drying at the temperature of 60 ℃ to obtain a product I; (2) Taking 50-70 parts by mass of epoxy resin, 0.5-40 parts by mass of curing agent and 0.1-3 parts by mass of accelerator, adding the first product obtained in the step (1), stirring until the mixture is uniformly mixed, carrying out vacuum defoaming, and curing the obtained mixture at 25-180 ℃ for 1-24 hours to obtain a finished composite material, wherein the addition amount of the first product is 3-15% of the total mass of the epoxy resin, the curing agent and the accelerator; The artemisia annua refers to roots, stems, leaves or a mixture of the roots, stems and leaves of the artemisia annua, the particle size of bentonite is 5 nanometers-200 microns, and the epoxy resin is hydroxymethyl bisphenol A epoxy resin, alicyclic epoxy resin, phenolic epoxy resin, bisphenol A epoxy resin, bisphenol F epoxy resin or glycidol amine epoxy resin; The multi-load epoxy resin composite material prepared by the method is used in the field of high-end microelectronic packaging, and is used for aerospace, printing, biochemistry and sensors.
2. 2. The method of claim 1, wherein in the step (1), the ethanol is ethanol with a purity of 95% or higher.
3. 3. The method of claim 1, wherein in the step (2), the curing agent is an amine curing agent, an acid anhydride curing agent or an imidazole curing agent.
4. 4. The method of claim 3, wherein the imidazole curing agent comprises any one of imidazole, 2-methylimidazole, 2-ethyl-4-methylimidazole, diphenylimidazole, or a mixture thereof.
5. 5. The method of claim 3 wherein the amine curing agent is one or more of polyamides, aliphatic amines, aromatic amines, alicyclic amines, polyether amines, dicyandiamide and mixtures thereof.
6. 6. The method of producing a multi-supported epoxy resin composite according to claim 3, wherein the acid anhydride curing agent is any one of an aromatic acid anhydride, an alicyclic acid anhydride, a long-chain aliphatic acid anhydride, a halogenated acid anhydride, an acid anhydride adduct, or a mixture thereof.
7. 7. The method of claim 1, wherein in the step (2), the accelerator is a tertiary amine accelerator, a quaternary ammonium salt accelerator, an aliphatic amine accelerator, 2,4, 6-tris (dimethylaminomethyl) phenol, N-p-chlorophenyl-N, N' -dimethylurea or thiourea.

Description

Preparation method of multi-load epoxy resin composite material Technical Field The application relates to a preparation method of a multi-load epoxy resin composite material, and belongs to the technical field of compositions containing epoxy resins. Background Microelectronic technology, one of the fastest growing and most important technologies in the industry information society today, is the "heart" of the electronic information industry. And the important mark of microelectronic technology is the rapid progress and development of semiconductor integrated circuit technology. Integrated circuit technology mainly comprises a plurality of technical systems of circuit design, manufacturing process and package inspection, and with the deep development of the integrated circuit industry, the manufacturing and package technology has become an important support of the microelectronic industry. The electronic packaging material is used for bearing electronic components and interconnection lines thereof, is used as a sealing body and a matrix material of an integrated circuit, is one of key factors for determining an electronic packaging technology, plays roles of mechanical support, environmental protection, heat dissipation of electronic components and the like, and is required to have good electrical insulation. The epoxy resin has excellent mechanical property, electrical property, processability, adhesive force, weather resistance, water resistance and thermal stability, and has the advantages of excellent cost performance, lower cost, small density, flexible packaging process and the like, and the epoxy resin accounts for more than 90 percent of the polymer-based packaging material. However, due to the inherent macromolecular structure of epoxy resin, the epoxy resin has higher hygroscopicity, so that the epoxy resin is sensitive to moisture, moisture invasion is an important factor causing device failure, and reliability loss problems such as corrosion failure, popcorn failure and the like are caused, so that the non-airtight packaging of the epoxy resin becomes the most main defect when the epoxy resin is used as packaging materials, and the application of the epoxy resin in some high-reliability occasions is limited. Meanwhile, the poor antibacterial property of the epoxy resin leads to the breeding of bacteria, often shortens the service life of the epoxy resin, and limits the use of the epoxy resin in occasions with high requirements on sterility, such as the fields of hospitals, food sanitation and the like. In order to improve the water-blocking and oxygen-blocking properties of epoxy resins, CN105131534A, CN110055021A, CN103602300a and the like have been used for compounding and modifying epoxy resins, and although the above studies have all improved the barrier properties of epoxy resins, the compound has poor heat resistance, and in particular, the low helium permeability required for high-end packaging epoxy resins has no limitation in use. The antibacterial aspect of epoxy resin is usually improved by adding antibacterial agents, the common antibacterial agents are generally classified into three types, namely inorganic antibacterial agents, organic antibacterial agents and natural antibacterial agents, wherein inorganic nano antibacterial agents (such as CN106065162A and the like) are used due to high specific surface energy and long-term stability, such as silver, zinc oxide, cuprous oxide and the like, but are limited in medicine due to the fact that heavy metal ions are introduced into the nano antibacterial agents, the organic antibacterial agents (such as CN105647453A and the like) mainly contain functional groups such as quaternary ammonium salts, phenolic hydroxyl groups or halogens, but are not resistant to high temperature, small molecules are difficult to graft-copolymerize with polymers, have certain toxicity and the like, and the application aspect is limited, and the natural antibacterial agents (such as CN104927538A, CN105368364A, CN 106065162A) are derived from natural plant components, are environment-friendly and can be developed continuously, but are not related to improving the air tightness of epoxy resin and reducing helium permeability, so the epoxy resin has limitations. Disclosure of Invention In view of the above, the application provides a preparation method of a multi-load epoxy resin composite material, which not only realizes the reduction of nitriding rate and water vapor permeability, but also endows the composite material with antibacterial property. Specifically, the application is realized by the following scheme: A preparation method of a multi-load epoxy resin composite material comprises the following steps: (1) Placing 40-70 parts by mass of artemisia annua and 30-60 parts by mass of bentonite in ethanol, uniformly mixing, placing in a high-pressure reaction kettle, reacting for 6-24 hours at the temperature of 80-130 ℃, taking out, cooling, centrifugally