Method for preparing composite dielectric film

A composite dielectric film and polymer technology, which is applied in the field of composite dielectric film preparation, can solve the problems of poor polymer compatibility, complex preparation method and high sintering temperature, and achieves low composite temperature, environmental friendliness and simple preparation process. Effect

Inactive Publication Date: 2012-07-18
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 1. Ordinary dielectric ceramic materials: such as copper calcium titanate (CCTO), which has a large capacitance and a dielectric constant of up to 10 4 -10 5 (Lin Zhang, et al., Ferroelectrics.2010, 405, 92.), but the material is sintered at a high temperature, brittle, and the machinability is affected
2. Polymer materials: such as polyvinylidene fluoride (PVDF) has high flexibility and low dielectric loss, but its own dielectric constant is too small (Baojin Chu, et al., science.2006, 313, 334.), severely limit its application
3. Polymer-based composite material with high dielectric properties: conductive titanium carbide (TiC) is used as an additive and filled into PVDF to form a composite material. The dielectric constant of the composite material can reach 540 at 100 Hz (Fajun Wang, et a., Phys .Status Solidi (RRL).2009, 3, 22.), but it is severely limited by the seepage threshold, and the dielectric loss will be greatly increased near the seepage threshold, and it is difficult to control the filling amount
[0004] However, the disadvantage of this method is that the preparation method of most ceramic additive materials is relatively complicated, and its compatibility with polymers is poor, and it is not easy to make thin films.
The ultra-high dielectric constant of most ceramic materials is quite different from that of polymer substrates. When subjected to an external electric field, an inhomogeneous electric field will be generated inside the composite material, which will greatly reduce the compressive strength of the composite material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] a. Preparation of mixed crystal nano-TiO by reflux method 2 , the reflux time is 6h, and the molar components of the two crystal forms are:

[0029] 45% for anatase and 55% for rutile;

[0030] This example is for the preparation of mixed crystal TiO2 nanoparticles. 100mL of deionized water and 10mL of hydrogen peroxide were used to make a mixed solvent, and 2.2g of butyl titanate was slowly added dropwise thereto, stirred at room temperature for 30min, and then refluxed at 98°C for 6h, the obtained precipitate was washed away, and dried at 80°C for 20h.

[0031] b. 0.0054g of the mixed crystal TiO prepared in step a 2 , After mixing 0.1000g vinylidene fluoride-trifluoroethylene copolymer [P(VDF-TrFE)] and 1.0005g solvent DMF, the ultrasonic stirring is uniformly dispersed to form a stable sol. The mass percentage of the ingredients is composed of: mixed crystal TiO 2 5% for polymer and 95% for polymer;

[0032] c. Cast the sol prepared in step b on a mold at 80°C t...

Embodiment 2

[0034] a. Preparation of mixed crystal nano-TiO by reflux method 2 , the reflux time is 6h, and the molar components of the two crystal forms are: 45% for anatase and 55% for rutile;

[0035] b. 0.0247g of the mixed crystal TiO prepared in step a 2 , 0.1000g vinylidene fluoride-trifluoroethylene copolymer [P(VDF-TrFE)] and 1.1313g solvent DMF are mixed, ultrasonically stirred and dispersed uniformly to form a stable sol. The mass percentage of the ingredients is composed of: mixed crystal TiO 2 20% for polymer and 80% for polymer;

[0036] c. Cast the sol prepared in step b on a mold at 80°C to form a film, dry for 18h; then cool naturally and anneal at 120°C for 8h to prepare TiO 2 / P(VDF-TrFE) composite dielectric film. The dielectric constant can reach 17.3.

Embodiment 3

[0038] a. Preparation of mixed crystal nano-TiO by reflux method 2 , the reflux time is 6h, and the molar components of the two crystal forms are: 45% for anatase and 55% for rutile;

[0039] b. 0.0667g of the mixed crystal TiO prepared in step a 2 , 0.1000g vinylidene fluoride-trifluoroethylene copolymer [P(VDF-TrFE)] and 1.2830g solvent DMF are mixed, ultrasonically stirred and dispersed uniformly to form a stable sol. The mass percentage of the ingredients is composed of: mixed crystal TiO 2 40% for polymer and 60% for polymer;

[0040]c. Cast the sol prepared in step b on a mold at 80°C to form a film, dry for 18h; then cool naturally and anneal at 120°C for 8h to prepare TiO 2 / P(VDF-TrFE) composite dielectric film. The dielectric constant can reach 23.9.

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Abstract

The invention discloses a method for preparing a composite dielectric film. According to the method, the film is prepared by mixing fluorine-containing polymer and mixed crystal nanometer TiO2 and casting, wherein the molar ratio of two crystal forms in the mixed crystal nanometer TiO2 can be controlled according to reaction time, anatase accounts for 36 to 45 percent, and rutile accounts for 55 to 64 percent; and the composite dielectric film consists of the following components in percentage by mass: 5 to 40 percent of mixed crystal nanometer TiO2 and 60 to 95 percent of fluorine-containingpolymer. The composite dielectric film is a novel dielectric material with a high dielectric constant and low dielectric loss; the composite dielectric film with the required dielectric constant can be prepared by controlling the addition amount of a filler and the ratio of the filler to the crystal forms; and the composite dielectric film is easy to prepare, low in composite temperature and environment-friendly and has a wide application prospect.

Description

technical field [0001] The invention belongs to the field of preparation of composite dielectric films, in particular to a preparation method of composite dielectric films. Background technique [0002] Polymer-based composite dielectric materials with high dielectric constant, low dielectric loss, and easy processability are functional materials with unique functions and wide applications due to their good flexibility, ability to store charges, and uniform electric field. It has a wide range of applications in the fields of hybrid locomotives, sensors, aerospace military and electric energy storage. Currently, there are three main types of dielectric materials: [0003] 1. Ordinary dielectric ceramic materials: such as copper calcium titanate (CCTO), which has a large capacitance and a dielectric constant of up to 10 4 -10 5 (Lin Zhang, et al., Ferroelectrics.2010, 405, 92.), but the material has a high sintering temperature and is brittle, which affects the machinabilit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L27/12C08L27/16C08K3/22
Inventor 朱红林爽匡锡文王芳辉
Owner BEIJING UNIV OF CHEM TECH
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