A preparation method of high dielectric polyimide/copper calcium titanate nanowire composite material

A technology of calcium copper titanate and polyimide is applied in the field of preparation of high-dielectric polyimide/calcium copper titanate (CCTO) nanowire composite materials, which can solve the difficulty of macromolecular intercalation and reduce percolation. The problem of high threshold and aspect ratio can reduce the percolation threshold, save manpower, and improve the dielectric properties.

Inactive Publication Date: 2015-09-16
武汉一海数字医疗科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The aspect ratio of CCTO nanowires is high, which can effectively reduce the percolation threshold, solve the problems of poor compatibility and difficult intercalation of macromolecules when polymers and large-size particles (macro or micro) are combined, and improve the performance of polyimide. Compatibility with CCTO nanowires can promote the combination of polyimide macromolecules and CCTO nanowires, so as to obtain polyimide / CCTO nanowire composites with excellent performance

Method used

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  • A preparation method of high dielectric polyimide/copper calcium titanate nanowire composite material
  • A preparation method of high dielectric polyimide/copper calcium titanate nanowire composite material
  • A preparation method of high dielectric polyimide/copper calcium titanate nanowire composite material

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Experimental program
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Embodiment 1

[0040] 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.

[0041] b) Weigh 0.048 g of CCTO nanowire powder (mass fraction: 1%) and add it into the above mixture, and perform magnetic stirring while adding.

[0042] c) Put the solution obtained in b) into an ultrasonic disperser for 2 hours to mix the solution evenly.

[0043] 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 CCTO nanowire composites.

[0044] 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 naturally, wi...

Embodiment 2

[0050] 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.

[0051] b) Weigh 0.154 g of the prepared CCTO nanowire powder (mass fraction is 3%) and add it into the above mixture, and perform magnetic stirring while adding.

[0052] c) Put the solution obtained in b) into an ultrasonic disperser for 2 hours to mix the solution evenly.

[0053] d) Weigh 2.835 grams of pyromellitic dianhydride (PMDA) and add it to the mixture, stir it magnetically while adding, and then react at room temperature for 12 hours in a nitrogen-protected environment to obtain polyimide / Stock solution of CCTO nanowire composites.

[0054] 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 na...

Embodiment 3

[0060] 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.

[0061] b) Weigh 0.499 g of the prepared CCTO nanowire powder (mass fraction is 8%) and add it into the above mixture, and perform magnetic stirring while adding.

[0062] c) Put the solution obtained in b) into an ultrasonic disperser for 2 hours to mix the solution evenly.

[0063] d) Weigh 2.835 grams of pyromellitic acid dianhydride (PMDA) and add it to the mixed solution, stir magnetically while adding, and then react at room temperature for 8 hours in a nitrogen-protected environment to obtain polyimide / Stock solution of CCTO nanowire composites.

[0064] 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...

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Abstract

The invention discloses a preparation method of a high-dielectric polyimide / calcium copper titanate nanowire composite material. The composite material is prepared by using polymer as a substrate. The method comprises the following steps: carrying out ultrasonic dispersion on calcium copper titanate nanowires in anhydrous ethanol, blending with a polyimide monomer in a solvent, and carrying out in-situ polymerization reaction on the monomer at room temperature while implementing copolymerization of polyimide and intercalation compounding with calcium copper titanate nanowires; and carrying out gradient annealing on the stock solution by a coating process to obtain the polyimide / CCTO nanowire composite film. Compared with pure polyimide, the dielectric constant of the polyimide / calcium copper titanate nanowire composite material is enhanced by 25 times, the dielectric loss is lower (0.015), and thus, the polyimide / calcium copper titanate nanowire composite material has wide application prospects in the fields of high energy storage capacitors, artificial organs, high speed integrated circuits and the like.

Description

technical field [0001] The invention relates to a preparation method of a high-dielectric polyimide / copper calcium titanate (CCTO) nanowire composite material, which belongs to the field of electronic materials. Background technique [0002] 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. [0003] 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 composite material by combining ferroelectric ceramic particle...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08K7/08C08K3/24C08J5/18C08L79/08
Inventor 杨阳熊锐刘雍石兢石彬牛牧林晶
Owner 武汉一海数字医疗科技股份有限公司
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