CN110643129A - Polymer-ceramic composite dielectric energy storage material and preparation method thereof - Google Patents
Polymer-ceramic composite dielectric energy storage material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/18—Manufacture of films or sheets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
Abstract
A polymer-ceramic composite dielectric energy storage material comprising the following components: polymethyl methacrylate (PMMA) is used as a matrix, and Barium Strontium Titanate (BST) nano particles are used as a filler; the preparation steps are as follows: 1) weighing; 2) preparing a PMMA solution; 3) preparing PMMA-BST mixed solution; 4) preparing a PMMA-BST composite material film; 5) heat treatment; 6) and preparing an electrode. The film sample has uniform and compact microstructure, good transparency and flexibility; the energy storage density of the material is far higher than that of biaxially oriented polypropylene, the charge-discharge efficiency of the material is far higher than that of a composite dielectric material system taking a ferroelectric polymer as a matrix, and the material meets the practical application requirements of high energy storage density and high charge-discharge efficiency.
Description
Technical Field
The invention belongs to the field of polymer-ceramic composite dielectric energy storage materials, and particularly relates to a polymer-ceramic composite dielectric energy storage material and a preparation method thereof, which have high energy storage density and high charge-discharge efficiency.
Background
With the continuous increase of the demand of the modern society for efficient and convenient power systems, the high-power and high-energy-density electric energy storage technology receives high attention and extensive research. Compared with electrochemical energy storage technologies (such as batteries, super capacitors and the like), dielectric energy storage is considered to be an advanced electric energy storage technology which can be used in modern electric power equipment and national defense weapons due to the fact that the dielectric energy storage has high power density and can meet the application requirements of high voltage and rapid charging and discharging, and the dielectric energy storage has wide application prospects.
Polymer-ceramic composite dielectric materials are one of the most interesting dielectric energy storage materials today. By introducing the ceramic nanoparticles with high dielectric constant into the polymer matrix with high electrical breakdown strength, the dielectric constant and the electrical breakdown strength of the material can be synergistically regulated and controlled, so that the energy storage density of the material is improved. The research of polymer-ceramic composite dielectric materials as energy storage dielectrics must be based on the energy storage characteristics of polymer materials and ceramic materials, and needs to consider a plurality of factors influencing the material performance, such as: film preparation technology, ceramic particle morphology, polymer matrix and ceramic nanoparticle interface, and the like. In related studies, PVDF-based ferroelectric polymers are widely used as polymer matrices of composite dielectric energy storage materials due to their high dielectric constants and electrical breakdown strengths; while ferroelectric ceramic nanoparticles with very high dielectric constants, e.g. BaTiO3(BT)、(Ba,Sr)TiO3(BST)、Pb(Zr,Ti)O3(PZT), etc., are widely used as ceramic fillers.
The polymer-ceramic composite dielectric energy storage materials widely adopted at present all adopt ferroelectric polymers and fillers, and particularly adopt PVDF-based polymers with larger electric polarization hysteresis as matrixes. Due to the remarkable ferroelectric characteristics of the materials, the corresponding composite material systems have the problem of low charging and discharging efficiency which is difficult to overcome. The low charging and discharging efficiency can not only reduce the use efficiency of energy, but also can seriously convert the energy which cannot be effectively released by electric energy into heat energy, the accumulated heat energy can cause the temperature of the energy storage device to rise, and once the temperature exceeds the use temperature, the polymer-based composite dielectric energy storage material is fatally influenced to the practical application. Therefore, how to improve the charge-discharge efficiency of the polymer-ceramic composite dielectric energy storage material is a technical problem which needs to be solved urgently by research in the field at present.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a polymer-ceramic composite dielectric energy storage material and a preparation method thereof, and the polymer-ceramic composite dielectric energy storage material has high energy storage density and high charge and discharge efficiency. The preparation method has the advantages that the non-ferroelectric polar polymer PMMA is selected as a composite material matrix, BST nano particles with extremely small electric polarization hysteresis and high dielectric constant are selected as the filler, so that the requirements on process stability in the preparation of the composite material can be met, the microcosmic uniformity and compactness of the composite material are easy to realize, the characteristic that the composite material is expressed as a linear dielectric at room temperature (far lower than the glass transition temperature of the polymer matrix) can be met, and the application requirements on the polymer-ceramic composite dielectric energy storage material with high energy storage density and high charge and discharge efficiency are met from the aspects of process and performance. The polymer-ceramic composite dielectric energy storage material comprises PMMA-xBST, wherein x is the mass fraction of BST in the composite material, and can be selected from 1-65% according to requirements. The method has the advantages of simple components and process steps, easy operation, good repeatability and great economic value.
In order to achieve the purpose, the invention adopts the technical scheme that:
a polymer-ceramic composite dielectric energy storage material comprises the following components in percentage by mass:
polymethyl methacrylate (PMMA) is used as 35-99% of a matrix;
barium Strontium Titanate (BST) nano-particles are used as filler 1-65%.
A preparation method of a polymer-ceramic composite dielectric energy storage material comprises the following steps:
1) weighing: weighing 35-99% of PMMA particles and 1-65% of BST nano particles according to the proportion of each component in the PMMA-BST composite material and the mass fraction;
2) preparing a PMMA solution: fully dissolving PMMA particles weighed in the step 1) in N, N-Dimethylformamide (DMF), wherein the mass ratio of PMMA to DMF is 1: 10;
3) preparing a PMMA-BST mixed solution: adding the BST nano-particles weighed in the step 1) into the PMMA solution prepared in the step 2), and fully dispersing the BST nano-particles through stirring and ultrasonic vibration to form uniform and stable PMMA-BST mixed solution;
4) preparing a PMMA-BST film: uniformly coating the PMMA-BST mixed solution prepared in the step 3) on a clean glass plate to form a thin film through a spin coating process; placing the glass plate and the film thereon in an oven for drying at 80 ℃ for 1 hour; stripping the dried and cured PMMA-BST composite material film from the glass substrate;
5) and (3) heat treatment: carrying out heat treatment on the stripped PMMA-BST composite material film obtained in the step 4), wherein the temperature is 140 ℃, and the time is 24 hours;
6) preparing an electrode: preparing silver electrodes on two surfaces of the PMMA-BST composite material film subjected to heat treatment in the step 5) by using a magnetron sputtering method, wherein the thickness of the electrodes is about 150 nm.
Compared with the existing polymer-ceramic composite dielectric energy storage material, the invention has the following beneficial technical effects:
the polymer-ceramic composite dielectric energy storage material disclosed by the invention selects a non-ferroelectric polar polymer as a matrix, and takes ferroelectric ceramic nanoparticles with extremely small electric polarization hysteresis and higher dielectric constant as fillers, so that a novel composite dielectric material system with high energy storage density and high charge-discharge efficiency is developed.
The invention discloses a polymer-ceramic composite dielectric energy storage material and a preparation method thereof, wherein PMMA is used as a polymer matrix, BST nano particles are used as a filler, and the polymer-ceramic composite dielectric energy storage material which has high energy storage density and high charge-discharge efficiency, namely a PMMA-BST composite dielectric film, is prepared by adopting the technical processes of solution mixing, spin coating film making, drying and curing and the like. The invention has simple components and process steps, easy operation, good repeatability, high yield and good application value.
The composite material system has a uniform and compact microstructure, and a film sample of the composite material system has good transparency and flexibility; the energy storage density of the material is far higher than that of biaxially oriented polypropylene, the charge-discharge efficiency of the material is far higher than that of a composite dielectric material system taking a ferroelectric polymer as a matrix, and the material meets the practical application requirements of high energy storage density and high charge-discharge efficiency.
Drawings
FIG. 1 is a photograph of an actual sample of PMMA-BST composite dielectric energy storage material film prepared by the present invention.
FIG. 2(a) is an electric polarization-electric field curve of a PMMA substrate selected by the present invention during charging and discharging processes; FIG. 2(b) is a graph showing the energy storage performance of the PMMA-BST composite dielectric film of the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the following embodiments are clearly and completely described in order to make the advantages and features of the present invention more easily understood by those skilled in the art, and thus the protection scope of the present invention is more clearly and clearly defined.
Example 1
A polymer-ceramic composite dielectric energy storage material comprising the following components:
polymethyl methacrylate (PMMA) is used as a matrix, and the mass fraction of the PMMA in the composite material is 99%;
barium Strontium Titanate (BST) nano-particles are used as filler, and the mass fraction of the Barium Strontium Titanate (BST) nano-particles in the composite material is 1%.
Example 2
A polymer-ceramic composite dielectric energy storage material comprising the following components:
polymethyl methacrylate (PMMA) is used as a matrix, and the mass fraction of the PMMA in the composite material is 69%;
barium Strontium Titanate (BST) nano-particles are used as fillers, and the mass fraction of the Barium Strontium Titanate (BST) nano-particles in the composite material is 31%.
Example 3
A polymer-ceramic composite dielectric energy storage material comprising the following components:
polymethyl methacrylate (PMMA) is used as a matrix, and the mass fraction of the PMMA in the composite material is 49%;
barium Strontium Titanate (BST) nano-particles are used as fillers, and the mass fraction of the Barium Strontium Titanate (BST) nano-particles in the composite material is 51%.
Example 4
A polymer-ceramic composite dielectric energy storage material comprising the following components:
polymethyl methacrylate (PMMA) is used as a matrix, and the mass fraction of the PMMA in the composite material is 35 percent;
barium Strontium Titanate (BST) nano-particles are used as filler, and the mass fraction of the Barium Strontium Titanate (BST) nano-particles in the composite material is 65%.
Example 5
A polymer-ceramic composite dielectric energy storage material comprises the following components: polymethyl methacrylate (PMMA) is used as a matrix (the mass fraction is 99 percent), and Barium Strontium Titanate (BST) nano particles are used as fillers (the mass fraction is 1 percent).
The preparation method comprises the following steps:
1) weighing: weighing 1g of PMMA particles and 0.01g of BST nano particles according to the proportion of each component in the PMMA-BST composite material;
2) preparing a PMMA solution: fully dissolving PMMA particles weighed in the step 1) in N, N-Dimethylformamide (DMF), wherein the mass ratio of PMMA to DMF is 1: 10;
3) preparing a PMMA-BST mixed solution: adding the BST nano-particles weighed in the step 1) into the PMMA solution prepared in the step 2), and fully dispersing the BST nano-particles through stirring and ultrasonic vibration to form uniform and stable PMMA-BST mixed solution;
4) preparing a PMMA-BST film: uniformly coating the PMMA-BST mixed solution prepared in the step 3) on a clean glass plate to form a thin film through a spin coating process; placing the glass plate and the film thereon in an oven for drying at 80 ℃ for 1 hour; stripping the dried and cured PMMA-BST composite material film from the glass substrate;
5) and (3) heat treatment: carrying out heat treatment on the stripped PMMA-BST composite material film obtained in the step 4), wherein the temperature is 140 ℃, and the time is 24 hours;
6) preparing an electrode: preparing silver electrodes on two surfaces of the PMMA-BST composite material film subjected to heat treatment in the step 5) by using a magnetron sputtering method, wherein the thickness of the electrodes is about 150 nm.
Example 6
A polymer-ceramic composite dielectric energy storage material comprises the following components: polymethyl methacrylate (PMMA) is used as a matrix (the mass fraction is 69%), and Barium Strontium Titanate (BST) nano particles are used as a filler (the mass fraction is 31%);
the preparation method comprises the following steps:
1) weighing: weighing 1g of PMMA particles and 0.46g of BST nano particles according to the proportion of each component in the PMMA-BST composite material;
2) preparing a PMMA solution: fully dissolving PMMA particles weighed in the step 1) in N, N-Dimethylformamide (DMF), wherein the mass ratio of PMMA to DMF is 1: 10;
3) preparing a PMMA-BST mixed solution: adding the BST nano-particles weighed in the step 1) into the PMMA solution prepared in the step 2), and fully dispersing the BST nano-particles through stirring and ultrasonic vibration to form uniform and stable PMMA-BST mixed solution;
4) preparing a PMMA-BST film: uniformly coating the PMMA-BST mixed solution prepared in the step 3) on a clean glass plate to form a thin film through a spin coating process; placing the glass plate and the film thereon in an oven for drying at 80 ℃ for 1 hour; stripping the dried and cured PMMA-BST composite material film from the glass substrate;
5) and (3) heat treatment: carrying out heat treatment on the stripped PMMA-BST composite material film obtained in the step 4), wherein the temperature is 140 ℃, and the time is 24 hours;
6) preparing an electrode: preparing silver electrodes on two surfaces of the PMMA-BST composite material film subjected to heat treatment in the step 5) by using a magnetron sputtering method, wherein the thickness of the electrodes is about 150 nm.
Example 7
A polymer-ceramic composite dielectric energy storage material comprises the following components: polymethyl methacrylate (PMMA) is used as a matrix (mass fraction is 49%), and Barium Strontium Titanate (BST) nano particles are used as a filler (mass fraction is 51%);
the preparation method comprises the following steps:
1) weighing: weighing 1g of PMMA particles and 1.04g of BST nano particles according to the proportion of each component in the PMMA-BST composite material;
2) preparing a PMMA solution: fully dissolving PMMA particles weighed in the step 1) in N, N-Dimethylformamide (DMF), wherein the mass ratio of PMMA to DMF is 1: 10;
3) preparing a PMMA-BST mixed solution: adding the BST nano-particles weighed in the step 1) into the PMMA solution prepared in the step 2), and fully dispersing the BST nano-particles through stirring and ultrasonic vibration to form uniform and stable PMMA-BST mixed solution;
4) preparing a PMMA-BST film: uniformly coating the PMMA-BST mixed solution prepared in the step 3) on a clean glass plate to form a thin film through a spin coating process; placing the glass plate and the film thereon in an oven for drying at 80 ℃ for 1 hour; stripping the dried and cured PMMA-BST composite material film from the glass substrate;
5) and (3) heat treatment: carrying out heat treatment on the stripped PMMA-BST composite material film obtained in the step 4), wherein the temperature is 140 ℃, and the time is 24 hours;
6) preparing an electrode: preparing silver electrodes on two surfaces of the PMMA-BST composite material film subjected to heat treatment in the step 5) by using a magnetron sputtering method, wherein the thickness of the electrodes is about 150 nm.
Example 8
A polymer-ceramic composite dielectric energy storage material comprises the following components: polymethyl methacrylate (PMMA) is used as a matrix (the mass fraction is 35%), and Barium Strontium Titanate (BST) nano particles are used as a filler (the mass fraction is 65%);
the preparation method comprises the following steps:
1) weighing: weighing 1g of PMMA particles and 1.85g of BST nano particles according to the proportion of each component in the PMMA-BST composite material;
2) preparing a PMMA solution: fully dissolving PMMA particles weighed in the step 1) in N, N-Dimethylformamide (DMF), wherein the mass ratio of PMMA to DMF is 1: 10;
3) preparing a PMMA-BST mixed solution: adding the BST nano-particles weighed in the step 1) into the PMMA solution prepared in the step 2), and fully dispersing the BST nano-particles through stirring and ultrasonic vibration to form uniform and stable PMMA-BST mixed solution;
4) preparing a PMMA-BST film: uniformly coating the PMMA-BST mixed solution prepared in the step 3) on a clean glass plate to form a thin film through a spin coating process; placing the glass plate and the film thereon in an oven for drying at 80 ℃ for 1 hour; stripping the dried and cured PMMA-BST composite material film from the glass substrate;
5) and (3) heat treatment: carrying out heat treatment on the stripped PMMA-BST composite material film obtained in the step 4), wherein the temperature is 140 ℃, and the time is 24 hours;
6) preparing an electrode: preparing silver electrodes on two surfaces of the PMMA-BST composite material film subjected to heat treatment in the step 5) by using a magnetron sputtering method, wherein the thickness of the electrodes is about 150 nm.
Referring to fig. 1, fig. 1 shows a photo of an actual sample of the PMMA-BST composite dielectric energy storage material thin film prepared by the present invention. As can be seen from FIG. 1, the PMMA-BST composite film prepared by the invention has good uniformity and flexibility, the thickness of the film sample is about 5 μm, and the size of the sample can be cut.
Referring to fig. 2(a) - (b), the PMMA-BST composite material thin film prepared by the present invention is represented by a linear dielectric similar to the PMMA thin film, the charge and discharge efficiency (η) thereof is close to 100%, and as the BST content increases, the energy storage density of the composite material is improved under the same electric field.
The above-described embodiments are only a part of the embodiments of the present invention, and do not limit the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. All the components or equivalent processes which are changed by using the contents of the specification and the drawings of the invention, or are directly or indirectly applied to other related technical fields, are included in the scope of the invention.
Claims (7)
1. A polymer-ceramic composite dielectric energy storage material is characterized by comprising the following components in percentage by mass:
polymethyl methacrylate (PMMA) is used as 35-99% of a matrix;
barium Strontium Titanate (BST) nano-particles are used as filler 1-65%.
2. A preparation method of a polymer-ceramic composite dielectric energy storage material is characterized by comprising the following steps:
1) weighing: weighing 35-99% of PMMA particles and 1-65% of BST nano particles according to the proportion of each component in the PMMA-BST composite material and the mass fraction;
2) preparing a PMMA solution: fully dissolving PMMA particles weighed in the step 1) in N, N-Dimethylformamide (DMF);
3) preparing a PMMA-BST mixed solution: adding the BST nano particles weighed in the step 1) into the PMMA solution prepared in the step 2) and fully dispersing to form uniform and stable PMMA-BST mixed solution;
4) preparing a PMMA-BST composite material film: uniformly coating the PMMA-BST mixed solution prepared in the step 3) on a clean glass plate to form a film; placing the glass plate and the film thereon in an oven for drying at 80 ℃ for 1 hour; stripping the dried and cured PMMA-BST composite material film from the glass substrate;
5) and (3) heat treatment: carrying out heat treatment on the stripped PMMA-BST composite material film obtained in the step 4), wherein the temperature is 140 ℃, and the time is 24 hours;
6) preparing an electrode: preparing silver electrodes on two surfaces of the PMMA-BST composite material film subjected to heat treatment in the step 5) by using a magnetron sputtering method, wherein the thickness of the electrodes is about 150 nm.
3. The method of claim 1, wherein the PMMA has a molecular weight of 2 x 106The BST nanoparticles have a Ba content0.5Sr0.5TiO3。
4. The method of claim 1, wherein the BST nanoparticles are 100nm in size.
5. The method for preparing the polymer-ceramic composite dielectric energy storage material according to claim 2, wherein the mass ratio of PMMA to DMF in the step 2) is 1: 10.
6. The method for preparing the polymer-ceramic composite dielectric energy storage material as claimed in claim 2, wherein the step 3) of mixing and dispersing the BST nanoparticles in the PMMA solution is performed under the action of stirring and ultrasonic vibration.
7. The method for preparing the polymer-ceramic composite dielectric energy storage material according to claim 2, wherein the thin film preparation process in the step 4) is spin coating film preparation.
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Cited By (6)
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| CN111303576A (en) * | 2020-02-29 | 2020-06-19 | 杭州电子科技大学 | High-temperature-resistant composite film material based on submicron ceramic filler and preparation method thereof |
| CN111850493A (en) * | 2020-07-21 | 2020-10-30 | 哈尔滨理工大学 | Energy storage polymer composite film based on inorganic insulating layer modification and preparation method thereof |
| CN112625279A (en) * | 2020-12-16 | 2021-04-09 | 西安科技大学 | Shell thickness-controllable PAMMA @ BT/PP nano composite dielectric film and preparation method thereof |
| CN112646213A (en) * | 2020-11-26 | 2021-04-13 | 中国科学院深圳先进技术研究院 | Preparation method of charge storage polymer-based composite material |
| CN114350103A (en) * | 2021-12-22 | 2022-04-15 | 杭州电子科技大学 | Application of ABS-based ceramic nanoparticle composite material as energy storage material at high temperature |
| CN115966402A (en) * | 2022-12-05 | 2023-04-14 | 中南大学 | Flexible nano composite dielectric mixed liquid, flexible nano composite dielectric and application |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111303576A (en) * | 2020-02-29 | 2020-06-19 | 杭州电子科技大学 | High-temperature-resistant composite film material based on submicron ceramic filler and preparation method thereof |
| CN111850493A (en) * | 2020-07-21 | 2020-10-30 | 哈尔滨理工大学 | Energy storage polymer composite film based on inorganic insulating layer modification and preparation method thereof |
| CN112646213A (en) * | 2020-11-26 | 2021-04-13 | 中国科学院深圳先进技术研究院 | Preparation method of charge storage polymer-based composite material |
| CN112646213B (en) * | 2020-11-26 | 2022-09-27 | 中国科学院深圳先进技术研究院 | Preparation method of charge storage polymer-based composite material |
| CN112625279A (en) * | 2020-12-16 | 2021-04-09 | 西安科技大学 | Shell thickness-controllable PAMMA @ BT/PP nano composite dielectric film and preparation method thereof |
| CN114350103A (en) * | 2021-12-22 | 2022-04-15 | 杭州电子科技大学 | Application of ABS-based ceramic nanoparticle composite material as energy storage material at high temperature |
| CN114350103B (en) * | 2021-12-22 | 2023-12-29 | 杭州电子科技大学 | Application of ABS-based ceramic nanoparticle composite material as energy storage material at high temperature |
| CN115966402A (en) * | 2022-12-05 | 2023-04-14 | 中南大学 | Flexible nano composite dielectric mixed liquid, flexible nano composite dielectric and application |
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