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Nano-copper-containing epoxide resin composite material and preparation method thereof

A technology of epoxy resin and composite materials, applied in the field of epoxy resin composite materials and its preparation, to achieve the effect of dielectric loss control and high dielectric constant

Active Publication Date: 2013-11-27
SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current general method of mechanically mixing fillers with the matrix under the action of ultrasound cannot truly achieve uniform dispersion of nanoparticles in the polymer matrix.

Method used

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  • Nano-copper-containing epoxide resin composite material and preparation method thereof
  • Nano-copper-containing epoxide resin composite material and preparation method thereof
  • Nano-copper-containing epoxide resin composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: Add 40g of bisphenol A epoxy resin (E51), 10g of copper hydroxide, 1g of polyvinyl alcohol, and 20mL of ethylene glycol to a 250mL flask in sequence, then raise the temperature to 200°C, and react for 2 hours to obtain brown-red Nano copper / epoxy composite paste. Weigh 5.0g of slurry, add methyl ethyl ketone to disperse, then add 0.4g of dicyandiamide and 0.13g of dimethyltetraethylimidazole, ultrasonically stir evenly, rod-type film, and cure it at 150°C for 2h, 180 After curing at ℃ for 2h, the nano-copper / epoxy composite film was obtained. By changing the quality of the precursor copper hydroxide, composite materials with different mass fractions of Cu can be obtained.

[0038] Specifically, such as figure 1 As shown, the mass fraction of nano-copper in the epoxy matrix can be controlled between 5% and 80%. In addition, according to the difference between the mass fraction of nano-copper during feeding and the thermal decomposition of the slurry, it als...

Embodiment 2

[0040] Example 2: Add 40g of bisphenol A epoxy resin (E44), 10g of copper oxide, 1g of polyvinylpyrrolidone, and 20mL of ethylene glycol to a 250mL flask in sequence, then raise the temperature to 200°C, and react for 2 hours to obtain brown-red nano Copper / epoxy composite paste. Weigh 1.0 g of the slurry, add acetone to disperse, then add 0.8 g of an acid anhydride curing agent, stir it evenly with ultrasonic waves, and coat it, and cure it at 150°C for 2 hours to obtain a nano-copper / epoxy composite film. By changing the quality of the precursor copper oxide, composite materials with different mass fractions of Cu can be obtained.

Embodiment 3

[0041] Example 3: Into a 250mL flask, add 20g of bisphenol A epoxy resin (E51), 10g of Cu(acac) in sequence 2 , 1g of tetraethyl orthosilicate, 10mL of glycerin, then heated up to 260°C, and reacted for 4h to obtain a brown-red nano-copper / epoxy composite slurry. Weigh 15.0g slurry, 51.2gBaTiO 3 , add absolute ethanol to disperse, then add 0.4g tetraethylenepentamine, stir it evenly with ultrasonic, and make a rod coating film, and then cure it at 150°C for 4h to obtain nano-Cu / BaTiO 3 / Epoxy resin composite film. Changing the precursor Cu(acac) 2 The mass of Cu / BaTiO with different mass fractions of Cu can be obtained 3 / Epoxy resin composite film material.

[0042] Specifically, such as image 3 As shown, the cured composite film only appears the characteristic diffraction peak of the face-centered cubic structure of pure copper, and does not appear Cu 2 The characteristic peaks of copper oxides such as O and CuO indicate that the nanoparticles in the prepared slurry...

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Abstract

The invention discloses a nano-copper-containing epoxide resin composite material and a preparation method thereof. The preparation method comprises the following steps: sequentially adding a copper precursor, a protective agent, polyalcohol and epoxide resin to a reaction flask, increasing temperature to reaction temperature, and carrying out an in-situ thermal reduction reaction to obtain nano-copper / epoxide composite slurry; and dispersing the nano-copper / epoxide composite slurry into a solvent, adding a solidifying agent, and then solidifying at solidifying temperature to obtain the nano-copper / epoxide resin composite material. Nano-copper granules obtained by utilizing the method are uniformly dispersed in an epoxy matrix, the sizes of the nano-copper granules can be controlled between 50 nanometers and 250 nanometers, the mass fraction of the nano-copper granules can be controlled between 5% and 80%; the prepared slurry is free of impurities in such a way that appropriate precursor, reducing agent and protective agent are selected, and meanwhile, the slurry has good dispersion stability and oxidation stability in the organic solvent. The preparation method disclosed by the invention is simple in process and low in production cost, can be applied to the field of electronic packaging as an embedded type capacitor dielectric material and is suitable for large-scale industrialized production.

Description

technical field [0001] The invention relates to an epoxy resin composite material containing nanometer copper and a preparation method thereof. Background technique [0002] Polymer-based composite materials used as embedded capacitors usually require high dielectric constant, low dielectric loss, and good processability. However, the dielectric constant of the polymer matrix is ​​usually very low, and the selection of functional fillers is the key to determine the dielectric properties of composites. At present, the fillers used in composite materials are mainly high-dielectric barium titanate ceramic materials, which can be combined with polymers to form two-phase composite materials, and composite dielectric materials with high dielectric constants can be prepared. However, it is difficult to further increase the dielectric constant of the composite material by this method. If the content of barium titanate component continues to increase, the flexibility and mechanical ...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08K3/08C08K3/24B22F9/24
Inventor 孙蓉李刚于淑会罗遂斌郭慧子张治军
Owner SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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