Preparation method of polyimide/copper calcium titanate coated silver nanoparticle composite material

A nanoparticle and polyimide technology, applied in the field of electronic materials, can solve the problems of low dielectric constant, lower percolation threshold, high conductivity, etc., and achieve the goal of increasing dielectric constant, improving electric field distribution and reducing dielectric loss Effect

Inactive Publication Date: 2014-04-30
WUHAN UNIV
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Problems solved by technology

[0008] The present invention aims at the problems of poor two-phase compatibility, low dielectric constant and high dielectric loss of composite materials in the prior art, and provides a composite material with high dielectric constant Preparation method of polyimide / CCTOAg nanoparticle composite material with low dielectric loss
CCTOAg nanoparticles can effectively reduce the percolation threshold due to the high conductivity and low dielectric constant of silver particles on the surface, and solve the problems of poor compatibility and difficult intercalation of macromolecules when polymers and large-sized particles are combined. Improve the compatibility between polyimide and CCTOAg nanoparticles, promote the combination of polyimide macromolecules and CCTOAg nanoparticles, so as to obtain polyimide / CCTOAg nanoparticle composite materials with excellent performance

Method used

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  • Preparation method of polyimide/copper calcium titanate coated silver nanoparticle composite material
  • Preparation method of polyimide/copper calcium titanate coated silver nanoparticle composite material
  • Preparation method of polyimide/copper calcium titanate coated silver nanoparticle composite material

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Embodiment 0

[0040] Embodiment 0, preparation of CCTOAg nanoparticles with good dispersibility

[0041] First, the oxalic acid precursor reaction method is used to prepare nano-CCTO particles with good dispersion. The method specifically includes the following steps:

[0042] (1) Titanium tetrachloride (TiCl 4 ) (18.2093 g) was added to ice water (distilled water at 0°C) (1920 ml) for hydrolysis, and ammonia water (NH 4 OH) to adjust the pH to a certain value, that is, when the white flocculent precipitation in the solution is the most produced (when the pH is adjusted to about 8), it will generate titanium dioxychloride (TiOCl 2 ).

[0043] (2) Put the above mixture in a Buchner funnel for several times of washing and suction filtration to obtain a white floc precipitate.

[0044] (3) Transfer the white floc precipitate to a beaker, add an appropriate amount of oxalic acid dihydrate (C 2 h 2 o 4 .2H 2 O) (24.2054 g) mixed, fully stirred and reacted at 25°C to 45°C for several hou...

Embodiment 1

[0055] a) press figure 1 According to the procedure in , weigh 2.554 g of diaminodiphenyl ether (ODA) into a three-necked bottle containing 7.4 ml of N,N-dimethylacetamide (DMAC) solution.

[0056] b) Weigh 0.1955 g of CCTOAg nanoparticle powder (volume fraction 1.5 vol%) and add it into the above mixture, and perform magnetic stirring while adding.

[0057] c) Put the solution obtained in b) into an ultrasonic disperser for 2 hours to mix the solution evenly.

[0058] d) Weigh 2.835 grams of pyromellitic dianhydride (PMDA) and add it to the mixture, stir it magnetically while adding it, and then react at 30°C for 8 hours in a nitrogen-protected environment to obtain polyimide Stock solution of CCTOAg nanoparticle composites.

[0059] e) Pour the original solution of the composite material on the glass substrate, spread it flat, put it in a muffle furnace, anneal it in a vacuum environment, and keep it at 60°C, 100°C, 200°C and 300°C for 1 hour , and then cool down naturall...

Embodiment 2

[0068] a) press figure 1 According to the procedure in , weigh 2.554 g of diaminodiphenyl ether (ODA) into a three-necked bottle containing 74 ml of N,N-dimethylacetamide (DMAC) solution.

[0069] b) Weigh 0.393 g of the prepared CCTOAg nanoparticle powder (volume fraction 3 vol%) and add it into the above mixed solution, and perform magnetic stirring while adding.

[0070] c) Put the solution obtained in b) into an ultrasonic disperser for 2 hours to mix the solution evenly.

[0071] d) Weigh 2.835 grams of pyromellitic dianhydride (PMDA) and add it to the mixed solution, stir magnetically while adding, and then react at room temperature for 4 hours in a nitrogen-protected environment to obtain polyimide / Stock solution of CCTOAg nanoparticle composites.

[0072] e) Pour the original solution of the composite material on the glass substrate, spread it flat, put it in a muffle furnace, anneal it in a vacuum environment, and keep it at 60°C, 100°C, 200°C and 300°C for 1 hour ...

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Abstract

The invention discloses a preparation method of polyimide / CCTO@Ag nanoparticle composite material with high dielectric and low loss. According to the method, polyimide is used as matrix, the prepared CCTO@Ag nanoparticles are ultrasonically dispersed in absolute ethyl alcohol, then is blended with polyimide monomer in solvent, then in situ polymerization reaction is carried out on the monomer at room temperature to simultaneously realize copolymerization of polyimide and intercalation recombination with the CCTO@Ag nanoparticles, obtained stock solution is subjected to gradient annealing according to a coating method to finally obtain the polyimide / CCTO@Ag nanoparticle composite film. Compared with pure polyimide, the polyimide / CCTO@Ag nanoparticle composite material prepared according to the preparation method has the dielectric constant (103) increased by 30 times, also has low dielectric loss (0.006) and can be widely applied in fields of high energy storage capacitors, artificial organs, high speed integrated circuits, and the like.

Description

[0001] technical field [0002] The invention relates to a preparation method of a high-dielectric, low-loss polyimide / copper calcium titanate (CCTO)-coated silver (Ag) core-shell nanoparticle composite material, which belongs to the technical field of electronic materials. Background technique [0003] Polymers are widely used in capacitors, integrated circuits, and high-voltage insulation due to their excellent electrical, thermal, and ductile properties, but their low dielectric constant limits their further development. With the continuous development of device integration and miniaturization in today's electronic field, it is necessary to provide new materials with both high dielectric constant and low dielectric loss to meet the requirements. [0004] In order to obtain the required high-performance materials, the commonly used method is to modify polymer materials by doping. There are two commonly used doping methods. One is to prepare a polymer / ferroelectric ceramic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L79/08C08J5/18C08K9/10C08K3/24
Inventor 杨阳孙浩亮王自昱刘雍熊锐石兢雷清泉
Owner WUHAN UNIV
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