CN110551305A - preparation method of silver/potassium tantalate niobate/barium titanate composite polymer dielectric material - Google Patents

preparation method of silver/potassium tantalate niobate/barium titanate composite polymer dielectric material Download PDF

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CN110551305A
CN110551305A CN201910970526.5A CN201910970526A CN110551305A CN 110551305 A CN110551305 A CN 110551305A CN 201910970526 A CN201910970526 A CN 201910970526A CN 110551305 A CN110551305 A CN 110551305A
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barium titanate
silver
potassium
tantalate
niobate
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张启龙
张钊
杨辉
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Zhejiang University ZJU
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Abstract

The invention relates to the technical field of nano composite materials, and aims to provide a preparation method of a silver/potassium tantalate niobate/barium titanate composite polymer dielectric material. The method comprises the following steps: adding polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene into N, N-dimethylformamide, mixing and stirring at room temperature until the mixture is clear; dispersing the silver-loaded potassium niobate tantalate/barium titanate composite powder serving as a filler in a clear solution to obtain a uniform suspension; and (4) drop-coating and forming the suspension, drying, preserving heat and then carrying out quenching treatment to obtain the film-shaped composite polymer dielectric material. The composite dielectric material constructed by the invention can increase interaction areas among inorganic particles and between inorganic particle/polymer interfaces, realize the enhancement of the interface polarization effect, improve the dielectric constant of the composite material and reduce the dielectric loss. The preparation method is simple in preparation process, high in operability and repeatability, capable of being applied to manufacturing of energy storage capacitors, flexible electronic devices and the like, and wide in application prospect.

Description

preparation method of silver/potassium tantalate niobate/barium titanate composite polymer dielectric material
Technical Field
The invention belongs to the technical field of nano composite materials, and particularly relates to a silver/potassium tantalate niobate/barium titanate composite polymer dielectric material and a preparation method thereof.
Background
With the rapid development of sustainable energy production technology and electronic technology, energy storage capacitors have a wide application in the fields of energy storage devices and electronic devices due to their high dielectric constant, large energy storage density and the possibility of being embedded in the plates of integrated circuits. Dielectric materials are used as a very critical part of energy storage capacitors and play an important role in their performance.
The conventional dielectric materials mainly comprise two main types, namely ceramics and polymers, and the problems exist at present, the ceramics such as barium titanate (BaTiO 3) and the like have high dielectric constant and polarization strength, but the breakdown strength is very low, the weight is heavy, the processability is poor and the like, so that the ceramics cannot meet the current requirements on the dielectric materials, and the polymers have high breakdown strength, light weight, good processability and the like, but the dielectric constant of most polymers is low (<10), so that the dielectric materials which have good dielectric property and excellent flexibility are prepared and are the key for improving the energy storage capacitor.
The polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene is a terpolymer of the polyvinylidene fluoride, has higher dielectric constant (Tg & gt 30), good flexibility, is easy to form and is suitable for large-scale production. However, the dielectric properties such as dielectric constant are still insufficient, and the application of the material in the fields of energy storage capacitors, flexible electronic devices and the like is limited.
Disclosure of Invention
The invention aims to solve the problem of overcoming the defects in the prior art and provides a preparation method of a silver/potassium tantalate niobate/barium titanate composite polymer dielectric material with a high dielectric constant and low dielectric loss.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows:
the preparation method of the silver/potassium tantalate niobate/barium titanate composite polymer dielectric material comprises the following steps:
(1) Adding polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene into N, N-dimethylformamide according to the volume ratio of 1: 80, mixing at room temperature, and stirring until the mixture is clear; dispersing the silver-loaded potassium niobate tantalate/barium titanate composite powder serving as a filler in a clear solution to obtain a uniform suspension;
(2) Forming the suspension by drop coating, drying in a vacuum oven at 60 ℃ for 24 hours, and continuing to perform vacuum heat preservation at 150-170 ℃ for 10 minutes; taking out, placing in ice water for quenching treatment to obtain a film-shaped composite polymer dielectric material;
In the step (1), the mol ratio of silver, potassium tantalate niobate and barium titanate in the filler is 3: 25; the amount of the filler is controlled to be 5 to 20% of the total volume of the composite polymer dielectric material in the form of a film.
In the present invention, the dispersion in the step (1) means: after 1h of ultrasonic dispersion, the mixture was stirred at room temperature for 5h, and this operation was repeated once.
In the invention, the polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene in the step (1) is a terpolymer, and the molar ratios of the three components are respectively as follows: 64.2 mol% of polyvinylidene fluoride, 27.1 mol% of polytrifluoroethylene and 8.7 mol% of polytrifluorochloroethylene.
in the invention, the filler is prepared by the following method:
(1) Dissolving 28g of potassium hydroxide in 50ml of deionized water in a stainless steel reaction kettle with a polytetrafluoroethylene inner container, and stirring at room temperature until the solution is clear; taking powdery niobium pentoxide, tantalum pentoxide and barium titanate according to the mol ratio of 1: 4: 10, dispersing the powdery niobium pentoxide, tantalum pentoxide and barium titanate in a clear solution, and reacting at 180-200 ℃ for 22-26 h; the mass ratio of the potassium hydroxide to the niobium pentoxide is 28: 1.06;
(2) After the reaction is finished, naturally cooling to room temperature; centrifuging the solid product and washing with deionized water until the pH approaches 7; then drying for 24 hours at 60 ℃ to obtain potassium niobate tantalate/barium titanate composite powder;
(3) Dispersing the potassium niobate tantalate/barium titanate composite powder in deionized water according to the ratio of 0.2g of composite powder to 50ml of deionized water, then adding 0.1g of AgNO 3 particles, stirring for 1h at normal temperature in the dark place, placing the mixed solution under a 300W xenon lamp for irradiation reaction for 90-180 min, sequentially washing the powder by using deionized water and ethanol in a centrifugal mode, and drying for 12h at 60 ℃ to obtain the silver-loaded potassium niobate tantalate/barium titanate composite powder.
Description of the inventive principles:
Compared with the prior art, the silver/potassium tantalate niobate/barium titanate composite powder has the advantages that the silver/potassium tantalate niobate/barium titanate composite powder does not have great pollution to the environment caused by lead, the Curie temperature is higher, the interaction of interfaces among inorganic particles can be increased, the interface polarization effect is enhanced, the dielectric constant of the composite material is improved, and simultaneously the coulomb blockage effect and the quantum size effect of silver nanoparticles can reduce the dielectric loss. And the prior art mainly considers introducing the inorganic filler with high dielectric constant rather than improving the dielectric property of a polymer substrate when improving the dielectric property of the composite material, so the invention also replaces the traditional polymer with polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene (PVDF terpolymer) which has higher dielectric constant, flexibility and easy molding compared with PVDF from the aspect of improving the polymer. Therefore, the silver/potassium tantalate niobate/polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene composite dielectric material has wide application prospect, and has no pollution, high Curie temperature and high dielectric property.
Compared with the prior art, the invention has the advantages that:
1. The potassium niobate tantalate/barium titanate composite powder with uniform appearance and size is prepared by a hydrothermal method, nitrate is reduced by illumination, and nano silver particles are loaded on the surface of the nitrate. The silver-loaded potassium niobate tantalate/barium titanate composite polymer dielectric film is prepared by solution blending and drop coating molding. The composite dielectric material constructed can increase interaction areas between inorganic particles and between inorganic particle/polymer interfaces, realize the enhancement of interface polarization effect, improve the dielectric constant of the composite material, and simultaneously reduce the dielectric loss by the coulomb blockage effect and the quantum size effect of the silver nanoparticles.
2. The preparation method is simple in preparation process, high in operability and repeatability, capable of being applied to manufacturing of energy storage capacitors, flexible electronic devices and the like, and wide in application prospect.
Drawings
FIG. 1 is an electron micrograph of silver/potassium tantalate niobate/barium titanate.
Wherein, the picture (a) is a Transmission Electron Microscope (TEM) picture of silver/potassium tantalate niobate/barium titanate prepared in the examples, and the picture (b) is a High Resolution Transmission Electron Microscope (HRTEM) picture of silver/potassium tantalate niobate/barium titanate.
FIG. 2 is an XRD spectrum of potassium tantalate niobate/barium titanate and silver-loaded potassium tantalate/barium titanate.
Detailed Description
The present invention is further described below with reference to examples and comparative examples, which allow a person skilled in the art to more fully understand the present invention, but do not limit the present invention in any way.
In the present invention, the preparation method of polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene (terpolymer, abbreviated as P (VDF-TrFE-CTFE)) is the prior art, and the preparation can be realized by those skilled in the art according to the mastery skill thereof, so that the detailed description thereof is omitted. In the following examples of the present invention, the terpolymer employs three components in molar ratios, respectively: the preferable embodiment is 64.2 mol% of polyvinylidene fluoride, 27.1 mol% of polytrifluoroethylene and 8.7 mol% of polytrifluorochloroethylene. Of course, the purpose of the invention can be achieved by adopting the components in other proportioning relations, and only the product performance of the final product is slightly different.
The addition amount of the filler (silver-loaded potassium tantalate niobate/barium titanate composite powder) is controlled to be 5-20% of the total volume of the film composite dielectric material. The volume fraction rather than the mass fraction is mainly used because the dispersibility of the inorganic particles in the polymer is an important factor influencing the performance of the composite dielectric material, and the volume fraction rather than the mass fraction can be used to reflect the space occupied by the inorganic particles in the composite material.
Example 1
(1) Dissolving 28g of potassium hydroxide in 50ml of deionized water in a 100ml stainless steel reaction kettle with a polytetrafluoroethylene inner container, and stirring at room temperature until the solution is clear; then, 1.06g of niobium pentoxide, 0.442g of tantalum pentoxide and 2.332g of barium titanate (molar ratio 1: 4: 10) were added to the solution, ultrasonically dispersed for 1 hour, stirred at room temperature for 5 hours and repeated once, and then transferred into a forced air drying oven and maintained at 200 ℃ for 24 hours.
(2) After the reaction is finished, naturally cooling to room temperature; and (3) carrying out centrifugal separation to obtain a white precipitate, washing the white precipitate for a plurality of times by using deionized water until the pH value is close to 7, and then drying the white precipitate for 24 hours at the temperature of 60 ℃ to obtain the composite powder of potassium niobate tantalate and barium titanate.
(3) dispersing the potassium tantalate niobate/barium titanate composite powder in deionized water, dispersing 0.2g of the composite powder in 50ml of deionized water, adding 0.1g of AgNO 3 particles, stirring for 1h at normal temperature in a dark place, placing the solution under a 300W xenon lamp for irradiation reaction for 180min, centrifugally washing the powder with deionized water and ethanol, and drying for 12h at 60 ℃ to obtain the silver-loaded potassium tantalate/barium titanate composite powder.
(4) Adding polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene into the N, N-dimethylformamide, wherein the volume ratio of the N, N-dimethylformamide to the added polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene is 80: 1. And stirring the mixed solution until the mixed solution is clarified, and dispersing the silver-loaded potassium niobate tantalate/barium titanate composite powder serving as the filler in the clarified solution to obtain a uniform suspension.
(5) And (3) dropping and coating the uniform suspension to form, drying in a vacuum oven at 60 ℃ for 24 hours, placing the dried product in the vacuum oven at 150 ℃ for heat preservation for 10 minutes, and placing the dried product in ice water for quenching treatment to obtain the required silver/potassium tantalate niobate/barium titanate composite polymer film, wherein the serial numbers are shown in table 1.
in the filler prepared in the step (4), the molar ratio of silver, potassium tantalate niobate and barium titanate is 3: 25; the amount of filler added was controlled to be 5% by volume of the polymer.
(6) Gold with the thickness of 100nm and the diameter of 4mm was respectively coated on both sides of the composite film by a vacuum coater as electrodes for subsequent dielectric property tests, and the results (at 1kHz) are shown in Table 1.
Example 2
(1) dissolving 28g of potassium hydroxide in 50ml of deionized water in a 100ml stainless steel reaction kettle with a polytetrafluoroethylene inner container, and stirring at room temperature until the solution is clear; 1.06g of niobium pentoxide, 0.442g of tantalum pentoxide and 2.332g of barium titanate were then added to the solution, dispersed ultrasonically for 1h, stirred at room temperature for 5h and repeated once, and transferred to a forced air drying oven and held at 180 ℃ for 26 hours.
(2) After the reaction is finished, naturally cooling to room temperature; and (3) carrying out centrifugal separation to obtain a white precipitate, washing the white precipitate for a plurality of times by using deionized water until the pH value is close to 7, and then drying the white precipitate for 24 hours at the temperature of 60 ℃ to obtain the composite powder of potassium niobate tantalate and barium titanate.
(3) Dispersing the potassium tantalate niobate/barium titanate composite powder in deionized water, dispersing 0.2g of the composite powder in 50ml of deionized water, adding 0.1g of AgNO 3 particles, stirring for 1h at normal temperature in a dark place, placing the solution under a 300W xenon lamp for irradiation reaction for 120min, centrifugally washing the powder with deionized water and ethanol, and drying for 12h at 60 ℃ to obtain the silver-loaded potassium tantalate/barium titanate composite powder.
(4) Adding polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene into the N, N-dimethylformamide, wherein the volume ratio of the N, N-dimethylformamide to the added polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene is 80: 1. And stirring the mixed solution until the mixed solution is clarified, and dispersing the silver-loaded potassium niobate tantalate/barium titanate composite powder serving as the filler in the clarified solution to obtain a uniform suspension.
(5) and (3) dropping and coating the uniform suspension to form, drying in a vacuum oven at 60 ℃ for 24 hours, placing the dried product in the vacuum oven at 160 ℃ for heat preservation for 10 minutes, and placing the dried product in ice water for quenching treatment to obtain the required silver/potassium tantalate niobate/barium titanate composite polymer film, wherein the serial numbers are shown in table 1.
In the filler prepared in the step (4), the molar ratio of silver, potassium tantalate niobate and barium titanate is 3: 25; the amount of filler added was controlled to be 10% by volume of the polymer.
(6) Gold with the thickness of 100nm and the diameter of 4mm was respectively coated on both sides of the composite film by a vacuum coater as electrodes for subsequent dielectric property tests, and the results (at 1kHz) are shown in Table 1.
Example 3
(1) Dissolving 28g of potassium hydroxide in 50ml of deionized water in a 100ml stainless steel reaction kettle with a polytetrafluoroethylene inner container, and stirring at room temperature until the solution is clear; 1.06g of niobium pentoxide, 0.442g of tantalum pentoxide and 2.332g of barium titanate were then added to the solution, dispersed ultrasonically for 1h, stirred at room temperature for 5h and repeated once, and transferred to a forced air drying oven and held at 200 ℃ for 22 hours.
(2) After the reaction is finished, naturally cooling to room temperature; and (3) carrying out centrifugal separation to obtain a white precipitate, washing the white precipitate for a plurality of times by using deionized water until the pH value is close to 7, and then drying the white precipitate for 24 hours at the temperature of 60 ℃ to obtain the composite powder of potassium niobate tantalate and barium titanate.
(3) dispersing the potassium tantalate niobate/barium titanate composite powder in deionized water, dispersing 0.2g of the composite powder in 50ml of deionized water, adding 0.1g of AgNO 3 particles, stirring for 1h at normal temperature in a dark place, placing the solution under a 300W xenon lamp for irradiation reaction for 120min, centrifugally washing the powder with deionized water and ethanol, and drying for 12h at 60 ℃ to obtain the silver-loaded potassium tantalate/barium titanate composite powder.
(4) Adding polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene into the N, N-dimethylformamide, wherein the volume ratio of the N, N-dimethylformamide to the added polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene is 80: 1. And stirring the mixed solution until the mixed solution is clarified, and dispersing the silver-loaded potassium niobate tantalate/barium titanate composite powder serving as the filler in the clarified solution to obtain a uniform suspension.
(5) And (3) dropping and coating the uniform suspension to form, drying in a vacuum oven at 60 ℃ for 24 hours, placing the dried product in the vacuum oven at 170 ℃ for heat preservation for 10 minutes, and placing the dried product in ice water for quenching treatment to obtain the required silver/potassium tantalate niobate/barium titanate composite polymer film, wherein the serial numbers are shown in table 1.
In the filler prepared in the step (4), the molar ratio of silver, potassium tantalate niobate and barium titanate is 3: 25; the amount of filler added was controlled to account for 15% by volume of the polymer.
(6) Gold with the thickness of 100nm and the diameter of 4mm was respectively coated on both sides of the composite film by a vacuum coater as electrodes for subsequent dielectric property tests, and the results (at 1kHz) are shown in Table 1.
example 4
(1) Dissolving 28g of potassium hydroxide in 50ml of deionized water in a 100ml stainless steel reaction kettle with a polytetrafluoroethylene inner container, and stirring at room temperature until the solution is clear; then, 1.06g of niobium pentoxide, 0.442g of tantalum pentoxide and 2.332g of barium titanate were added to the solution, ultrasonically dispersed for 1 hour, stirred at room temperature for 5 hours and repeated, and then transferred into a forced air drying oven and maintained at 200 ℃ for 24 hours.
(2) after the reaction is finished, naturally cooling to room temperature; and (3) carrying out centrifugal separation to obtain a white precipitate, washing the white precipitate for a plurality of times by using deionized water until the pH value is close to 7, and then drying the white precipitate for 24 hours at the temperature of 60 ℃ to obtain the composite powder of potassium niobate tantalate and barium titanate.
(3) Dispersing the potassium tantalate niobate/barium titanate composite powder in deionized water, dispersing 0.2g of the composite powder in 50ml of deionized water, adding 0.1g of AgNO 3 particles, stirring for 1h at normal temperature in a dark place, placing the solution under a 300W xenon lamp for irradiation reaction for 90min, centrifugally washing the powder with deionized water and ethanol, and drying for 12h at 60 ℃ to obtain the silver-loaded potassium tantalate/barium titanate composite powder.
(4) Adding polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene into the N, N-dimethylformamide, wherein the volume ratio of the N, N-dimethylformamide to the added polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene is 80: 1. And stirring the mixed solution until the mixed solution is clarified, and dispersing the silver-loaded potassium niobate tantalate/barium titanate composite powder serving as the filler in the clarified solution to obtain a uniform suspension.
(5) And (3) dropping and coating the uniform suspension to form, drying in a vacuum oven at 60 ℃ for 24 hours, placing the dried product in the vacuum oven at 150 ℃ for heat preservation for 10 minutes, and placing the dried product in ice water for quenching treatment to obtain the required silver/potassium tantalate niobate/barium titanate composite polymer film, wherein the serial numbers are shown in table 1.
In the filler prepared in the step (4), the molar ratio of silver, potassium tantalate niobate and barium titanate is 3: 25; the amount of filler added was controlled to be 20% by volume of the polymer.
(6) Gold with the thickness of 100nm and the diameter of 4mm was respectively coated on both sides of the composite film by a vacuum coater as electrodes for subsequent dielectric property tests, and the results (at 1kHz) are shown in Table 1.
Comparative example 1
(1) Polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene is added into N, N-dimethylformamide according to the volume ratio of 1: 80, and the mixture is mixed and stirred at room temperature until the mixture is clear, so that a uniform suspension is obtained. No filler material was added (i.e., 0 vol%);
(2) and (3) forming the uniform suspension by drop coating, drying the uniform suspension in a vacuum oven at the temperature of 60 ℃ for 24 hours, placing the dried product in the vacuum oven at the temperature of 150 ℃ for heat preservation for 10 minutes, and placing the dried product in ice water for quenching treatment to obtain the control group polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene composite film.
(3) gold with the thickness of 100nm and the diameter of 4mm is respectively plated on the two surfaces of the composite membrane by a vacuum coating machine to be used as electrodes for subsequent dielectric property tests. The results (at 1kHz) are shown in Table 1.
Comparative example 2
(1) Polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene is added into N, N-dimethylformamide according to the volume ratio of 1: 80, and the mixture is mixed and stirred at room temperature until the mixture is clear, so that a uniform suspension is obtained. Barium titanate powder (namely the filling material is 20 vol%) is added into the comparative example;
(2) And (3) forming the uniform suspension by drop coating, drying the uniform suspension in a vacuum oven at the temperature of 60 ℃ for 24 hours, placing the dried product in the vacuum oven at the temperature of 150 ℃ for heat preservation for 10 minutes, and placing the dried product in ice water for quenching treatment to obtain the control group barium titanate/polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene composite dielectric material.
(3) Gold with the thickness of 100nm and the diameter of 4mm is respectively plated on the two surfaces of the composite membrane by a vacuum coating machine to be used as electrodes for subsequent dielectric property tests. The results (at 1kHz) are shown in Table 1.
TABLE 1
Examples filling amount (vol%) Dielectric constant (1kHz) Dielectric loss (1kHz)
Example 1 5 60.0 0.079
Example 2 10 73.4 0.082
Example 3 15 83.7 0.087
Example 4 20 109.3 0.088
Comparative example 1 0 33.4 0.072
Comparative example 2 20 47.2 0.084
as can be seen from table 1, when the silver/potassium tantalate niobate/barium titanate composite powder is added as a filler into a polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene matrix, the dielectric constant of the composite material can be significantly improved, and a low dielectric loss can be maintained, so that a composite film with high dielectric properties can be obtained, and the composite film can be widely applied to the fields of energy storage capacitors, flexible electronic devices and the like.
It should be noted that the above-mentioned embodiments are only for illustrating the present invention and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.

Claims (4)

1. A preparation method of a silver/potassium tantalate niobate/barium titanate composite polymer dielectric material is characterized by comprising the following steps:
(1) Adding polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene into N, N-dimethylformamide according to the volume ratio of 1: 80, mixing at room temperature, and stirring until the mixture is clear; dispersing the silver-loaded potassium niobate tantalate/barium titanate composite powder serving as a filler in a clear solution to obtain a uniform suspension;
(2) Forming the suspension by drop coating, drying in a vacuum oven at 60 ℃ for 24 hours, and continuing to perform vacuum heat preservation at 150-170 ℃ for 10 minutes; taking out, placing in ice water for quenching treatment to obtain a film-shaped composite polymer dielectric material;
In the step (1), the mol ratio of silver, potassium tantalate niobate and barium titanate in the filler is 3: 25; the amount of the filler is controlled to be 5 to 20% of the total volume of the composite polymer dielectric material in the form of a film.
2. the method according to claim 1, wherein the dispersing in step (1) is: after 1h of ultrasonic dispersion, the mixture was stirred at room temperature for 5h, and this operation was repeated once.
3. The method according to claim 1, wherein the polyvinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene in the step (1) is a terpolymer, and the molar ratios of the three components are respectively as follows: 64.2 mol% of polyvinylidene fluoride, 27.1 mol% of polytrifluoroethylene and 8.7 mol% of polytrifluorochloroethylene.
4. A method according to any one of claims 1 to 3, characterized in that the filling is obtained by a method comprising:
(1) Dissolving 28g of potassium hydroxide in 50ml of deionized water in a stainless steel reaction kettle with a polytetrafluoroethylene inner container, and stirring at room temperature until the solution is clear; taking powdery niobium pentoxide, tantalum pentoxide and barium titanate according to the mol ratio of 1: 4: 10, dispersing the powdery niobium pentoxide, tantalum pentoxide and barium titanate in a clear solution, and reacting at 180-200 ℃ for 22-26 h; the mass ratio of the potassium hydroxide to the niobium pentoxide is 28: 1.06;
(2) After the reaction is finished, naturally cooling to room temperature; centrifuging the solid product and washing with deionized water until the pH approaches 7; then drying for 24 hours at 60 ℃ to obtain potassium niobate tantalate/barium titanate composite powder;
(3) dispersing the potassium niobate tantalate/barium titanate composite powder in deionized water according to the ratio of 0.2g of composite powder to 50ml of deionized water, then adding 0.1g of AgNO 3 particles, stirring for 1h at normal temperature in the dark place, placing the mixed solution under a 300W xenon lamp for irradiation reaction for 90-180 min, sequentially washing the powder by using deionized water and ethanol in a centrifugal mode, and drying for 12h at 60 ℃ to obtain the silver-loaded potassium niobate tantalate/barium titanate composite powder.
CN201910970526.5A 2019-10-13 2019-10-13 preparation method of silver/potassium tantalate niobate/barium titanate composite polymer dielectric material Pending CN110551305A (en)

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CN102875939A (en) * 2012-10-22 2013-01-16 北京工业大学 Preparation method of potassium niobate/ polyvinylidene fluoride high-dielectric composite material
CN104927254A (en) * 2015-07-07 2015-09-23 北京工业大学 Ferrotitanium niobium/polyvinylidene fluoride high-dielectric composite material and preparing method thereof
CN107434897A (en) * 2016-05-27 2017-12-05 北京化工大学 Barium titanate particles, barium titanate/fluoropolymer composite and preparation method thereof

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CN102875939A (en) * 2012-10-22 2013-01-16 北京工业大学 Preparation method of potassium niobate/ polyvinylidene fluoride high-dielectric composite material
CN104927254A (en) * 2015-07-07 2015-09-23 北京工业大学 Ferrotitanium niobium/polyvinylidene fluoride high-dielectric composite material and preparing method thereof
CN107434897A (en) * 2016-05-27 2017-12-05 北京化工大学 Barium titanate particles, barium titanate/fluoropolymer composite and preparation method thereof

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Application publication date: 20191210