High-intensity high-temperature-resistant polymer-based dielectric thin film and preparation method thereof

A high-temperature-resistant polymer and dielectric film technology, which can be applied to flat products, other household appliances, household appliances, etc., can solve problems such as interfacial compatibility that is prone to agglomeration, high glass transition temperature, and poor heat resistance. Achieve the effect of improving mechanical strength and temperature resistance level, high dielectric constant and improving performance

Inactive Publication Date: 2017-12-15
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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Problems solved by technology

[0003] In summary, the existing problems in the prior art are: currently graphene has a very large specific surface area and high surface energy, and is prone to agglomeration in the polymer matrix and poor interfacial compatibility with the polymer matrix
The composite material prepared by this method can increase the dielectric constant, but still has a high dielectric loss
At the same time, the modification of graphene oxide with copper phthalocyanine is only an in-situ physical coating of graphene rather than chemical bonding, and the preparation method of this document still has the problem of local agglomeration and interface polarization, so the dielectric loss higher
In addition, the highest glass transition temperature of the composite material prepared by this method is 182 °C, and the heat resistance is still poor.

Method used

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  • High-intensity high-temperature-resistant polymer-based dielectric thin film and preparation method thereof
  • High-intensity high-temperature-resistant polymer-based dielectric thin film and preparation method thereof
  • High-intensity high-temperature-resistant polymer-based dielectric thin film and preparation method thereof

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preparation example Construction

[0029] Such as figure 1 As shown, the preparation method of the high-strength and high-temperature-resistant polymer-based dielectric film provided by the embodiment of the present invention includes the following steps:

[0030] S101: Grafting 4-aminophenoxyphthalonitrile (4-APN) onto the surface of graphene oxide (GO) by chemical modification;

[0031]S102: Use cyano-functionalized graphene (GN-CN) as a filler and cross-linkable polyarylether nitrile (PEN-ph) as a matrix to prepare a mixed solution, and use high-speed ball milling to obtain uniformly dispersed PEN-ph PEN-ph / GN-CN composite film with controllable thickness and size can be obtained by melting and pressing ultrafine powder of / GN-CN into film;

[0032] S103: A polymer-based dielectric composite film with comprehensive properties such as high temperature resistance, excellent mechanical and dielectric properties obtained through uniaxial thermal stretching and high-temperature crosslinking.

[0033] The prepar...

Embodiment 1

[0046] Preparation of cyano-functionalized graphene (GN-CN):

[0047] GO was put into thionyl chloride solution and stirred ultrasonically, and heated under reflux at 70°C for 24 h under the catalysis of N,N-dimethylformamide. After the reaction was completed, the thionyl chloride in the system was removed by refluxing toluene, and the obtained black reaction product was vacuum-dried to obtain acid-chlorinated graphene (GN-COCl). Then, excess 4-APN and GN-COCl were added to the toluene solvent, and the reaction was stirred and refluxed at 25°C for 72h. The reaction product obtains cyano-functionalized graphene (GN-CN) after repeated washing, centrifugation and vacuum drying, and the infrared spectrum and structural formula of GN-CN are as follows figure 2 shown.

[0048] Synthesis of crosslinkable polyarylene ether nitrile (PEN-ph):

[0049] (1) Add 34.4g of 2,6-dichlorobenzonitrile to 75mL of N-methylpyrrolidone to obtain a solution with a concentration of 0.229g / mL;

[...

Embodiment 2

[0065] Preparation of cyano-functionalized graphene (GN-CN):

[0066] The preparation of cyano-functionalized graphene (GN-CN) is consistent with the process in Example 1.

[0067] Preparation of PEN-ph / GN-CN Dielectric Film:

[0068] (1) Dissolve 4g of PEN-ph in 20mL of N-methylpyrrolidone (NMP) to obtain a PEN-ph solution with a concentration of 200mg / mL;

[0069] (2) Dissolve 80mg of GN-CN in 20mL of N-methylpyrrolidone (NMP), and stir in a water bath ultrasonically (60°C, 100W) to obtain a uniformly dispersed GN-CN solution with a concentration of 4mg / mL;

[0070] (3) Slowly add the GN-CN solution obtained in step (2) to the PEN-ph solution in step (1), and ultrasonically and mechanically stir at 60°C for 0.5-2 hours to obtain a concentration of 100 mg / mL dispersed Uniform PEN-ph / GN-CN solution, wherein the mass fraction of GN-CN in PEN-ph is 2%;

[0071] (4) Add 200mL of precipitation solution (precipitation solution is a mixture of deionized water and NMP, the volume ...

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Abstract

The invention belongs to the technical field of a macromolecular dielectric material, and discloses a high-intensity high-temperature-resistant polymer-based dielectric thin film and a preparation method thereof. Graphene oxide is subjected to chemical grafting by 4-aminophenoxyl-o-phthalonitrile; cyan functional graphene is obtained; the continuous ultrasonic and high-speed ball milling precipitation technology is used for obtaining the uniformly dispersed crosslinking poly (arylene ether nitrile) / cyan functional graphene ultrafine powder; a composite thin film with the controllable thickness and dimension is obtained in a fusion pressing film forming mode. The composite thin film provided by the invention has ultrahigh heat-resistant performance (Tg is higher than 360 DEG C), high mechanical strength (the stretch intensity is higher than 450 MPa, and the modulus is higher than 4.5GPa) and excellent toughness; the dielectric constant is 11 to 28.5; the dielectric loss is 0.02 to 0.045. The composite material belongs to a polymer-based composite dielectric material and can be applied to the technical field of dielectric energy storage as a dielectric thin film.

Description

technical field [0001] The invention belongs to the technical field of polymer dielectric materials, and in particular relates to a high-strength and high-temperature-resistant polymer-based dielectric film and a preparation method thereof. Background technique [0002] With the rapid development of communication equipment and electronics industry, lightweight, miniaturized and high-performance electronic equipment has attracted extensive attention and exploration of scientific researchers, especially electronic materials used in extreme environmental conditions such as high temperature environments. It has gradually become one of the research hotspots. In recent years, adding dielectric ceramic particles to polymers to prepare dielectric materials has been initially applied, but in order to obtain an ideal dielectric constant, it is necessary to add a large amount of dielectric ceramic particles (volume fraction greater than 50%), due to The interfacial compatibility betwe...

Claims

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Application Information

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IPC IPC(8): C08L71/10C08K9/04C08K3/04C08J5/18B29C69/02B29L7/00
CPCB29C69/02B29L2007/00C08J5/18C08J2371/10C08K3/04C08K9/04C08L71/00
Inventor 蒲泽军郑晓翼田雨涵侯洪波钟家春
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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