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CN-121975053-A - High-heat-resistance low-dielectric low-loss resin colloid and preparation method and application thereof

CN121975053ACN 121975053 ACN121975053 ACN 121975053ACN-121975053-A

Abstract

The invention discloses a high heat-resistant low-dielectric low-loss resin colloid and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing soluble polyfunctional vinyl aromatic copolymer and vinyl-containing cross-linked aromatic resin, adding solvent, filler and accelerator, heating and stirring to react. The high heat-resistant low-dielectric low-loss resin colloid prepared by the preparation method has a dielectric constant less than or equal to 3.0 at 10GHz, a dielectric loss less than or equal to 0.0007, a glass transition temperature more than or equal to 250 ℃, a linear thermal expansion coefficient less than 1.15 ppm/DEGC and a water absorption less than or equal to 0.033%. The invention also discloses application of the resin colloid in a copper-clad plate. The resin colloid obtained by the invention has high crosslinking density, ultralow dielectric constant and ultralow electrical loss at 10GHz, excellent dimensional stability, good resistance to damp-heat aging and thermal shock, good mechanical property, excellent moisture resistance, good long-term use stability and simple process.

Inventors

  • Huang Juji
  • WANG ZITONG

Assignees

  • 中城财宏新材料(江苏)有限公司

Dates

Publication Date
20260505
Application Date
20260228

Claims (10)

  1. 1. A process for preparing the high-heat-resistance low-dielectric low-loss resin colloid includes such steps as mixing the soluble multifunctional vinyl aromatic copolymer with vinyl-contained cross-linked aromatic resin, adding solvent, filler and promoter, and heating while stirring.
  2. 2. The method of claim 1, wherein the mass ratio of the soluble multifunctional vinyl aromatic copolymer, the vinyl-containing cross-linked aromatic resin, the solvent, the filler and the accelerator is 100:46.8-85.6:146.8-185.6:146.8-185.6:0.538.
  3. 3. The method for preparing a resin colloid having high heat resistance, low dielectric constant and low loss according to claim 1, wherein said soluble multifunctional vinyl aromatic copolymer is SQDB-X001 with the structural formula 。
  4. 4. The method for preparing a high heat-resistant low dielectric low-loss resin colloid according to claim 1, wherein said vinyl-containing cross-linked aromatic resin is one or more of a divinylbenzene resin and a divinylphenyl resin.
  5. 5. The method for preparing a resin colloid having high heat resistance and low dielectric constant and low loss according to claim 4, wherein said divinylbenzene resin is 1, 2-bis (4-vinylphenyl) ethane.
  6. 6. The method for preparing a resin colloid having high heat resistance and low dielectric constant and low loss according to claim 4, wherein said divinyl benzyl resin is 9, 9-bis (2-vinyl benzyl) -9H-fluorene or 9, 9-bis (4-vinyl benzyl) -9H-fluorene.
  7. 7. The method for preparing a high heat-resistant low dielectric low-loss resin colloid according to claim 1, wherein the solvent is butanone, the filler is spherical silica, and the accelerator is 1, 4-bis (tert-butylperoxyisopropyl) benzene.
  8. 8. The method for preparing the high heat-resistant low-dielectric low-loss resin colloid according to claim 1, wherein the temperature of the heating and stirring reaction is 75-85 ℃, and the time of the heating and stirring reaction is 2-2.5 hours.
  9. 9. The high heat-resistant low-dielectric low-loss resin colloid prepared by the preparation method according to any one of claims 1-8, wherein the high heat-resistant low-dielectric low-loss resin colloid has a dielectric constant of less than or equal to 3.0 at 10GHz, a dielectric loss of less than or equal to 0.0007, a glass transition temperature of more than or equal to 250 ℃, a linear thermal expansion coefficient of less than 1.15 ppm/DEGC and a water absorption of less than or equal to 0.033%.
  10. 10. The use of the high heat-resistant low dielectric low-loss resin colloid according to claim 9 in copper-clad plates.

Description

High-heat-resistance low-dielectric low-loss resin colloid and preparation method and application thereof Technical Field The invention belongs to a resin colloid and a preparation method and application thereof, in particular to a high heat-resistant low-dielectric low-loss resin colloid and a preparation method and application thereof. Background In the field of resin materials, with the increasing demand for high-performance materials for related applications, there is an urgent need for resin products meeting the M8, ultra-low dielectric performance standard in particular. The conventional resin materials on the market at present are difficult to meet the high standard requirements on specific performance indexes, and development of a novel preparation method is needed to obtain resin products meeting the requirements. Common resins in the existing high-speed high-frequency copper-clad plate comprise modified epoxy, PTFE, polyimide, bismaleic resin, polyphenylene oxide PPO, hydrocarbon resin and the like. The thermosetting crosslinking system formed by curing in the process of preparing the copper-clad plate by taking the single hydrocarbon resin as the matrix resin can greatly improve the glass transition temperature, heat resistance and strength of the material, but the cohesive force and toughness are poor, so that the application requirements of a 5G communication chip and the like can not be met. Hydrocarbon resins are used in combination with other types of resins, but high frequency stability, thermal reliability, dielectric properties are still to be further improved. Disclosure of Invention The invention aims to: in order to overcome the defects in the prior art, the invention aims to provide a preparation method of a high heat-resistant low-dielectric low-loss resin colloid with high crosslinking density, and another aim of the invention is to provide a high heat-resistant low-dielectric low-loss resin colloid with excellent dimensional stability, and further aims to provide an application of the high heat-resistant low-dielectric low-loss resin colloid in a copper-clad plate. The preparation method of the high heat-resistant low-dielectric low-loss resin colloid comprises the following steps of mixing a soluble polyfunctional vinyl aromatic copolymer and a vinyl-containing cross-linked aromatic resin, adding a solvent, a filler and an accelerator, and heating and stirring for reaction to obtain the high heat-resistant low-dielectric low-loss resin colloid. Further, the mass ratio of the soluble multifunctional vinyl aromatic copolymer to the vinyl-containing cross-linked aromatic resin to the solvent to the filler to the accelerator is 100:46.8-85.6:146.8-185.6:146.8-185.6:0.538. Further, the soluble multifunctional vinyl aromatic copolymer is SQDB-X001 with the structural formula 。 Further, the vinyl-containing cross-linked aromatic resin is one or more of a divinylbenzene resin and a divinylbenzene resin. Further, the divinylbenzene resin was 1, 2-bis (4-vinylphenyl) ethane (BVPE). The structural formula is as follows: 。 Further, the divinylbenzene-based resin was 9, 9-bis (2-vinylbenzyl) -9H-fluorene (oBVF) or 9, 9-bis (4-vinylbenzyl) -9H-fluorene (pBVF). OBVF has the structural formula: 。 pBVF has the structural formula: 。 further, the solvent is butanone, the filler is spherical silicon dioxide, and the accelerator is 1, 4-bis (tert-butylperoxyisopropyl) benzene. Further, the temperature of the heating and stirring reaction is 75-85 ℃, and the time of the heating and stirring reaction is 2-2.5 h. The high heat-resistant low-dielectric low-loss resin colloid prepared by the preparation method has a dielectric constant less than or equal to 3.0 at 10GHz, a dielectric loss less than or equal to 0.0007, a glass transition temperature more than or equal to 250 ℃, a linear thermal expansion coefficient less than 1.15 ppm/DEGC and a water absorption less than or equal to 0.033%. The invention relates to application of high heat-resistant low-dielectric low-loss resin in copper-clad plates. The method is characterized by comprising the steps of preparing a copper-clad plate, namely, a high-heat-resistance low-dielectric low-loss resin, and carrying out vacuum hot pressing on the copper-clad plate. Compared with the prior art, the invention has the following remarkable characteristics: 1. The obtained resin has no glycerol structure, high crosslinking density, ultralow dielectric constant and ultralow electrical loss at 10GHz, excellent dimensional stability, good resistance to damp and heat aging and thermal shock, good mechanical property, excellent moisture resistance and good long-term use stability; 2. The process is simple and easy to operate, can be widely applied to the high-frequency electronic fields of AI servers, high-speed switches and the like, and meets the performance requirements of ultra-low dielectric levels. Drawings FIG. 1 is a hydrogen spectrum of the product obtained in exa