CN109880292B - Preparation method of polymer-based high-dielectric composite material based on three-dimensional skeleton with core-shell structure - Google Patents
Preparation method of polymer-based high-dielectric composite material based on three-dimensional skeleton with core-shell structure Download PDFInfo
- Publication number
- CN109880292B CN109880292B CN201910057398.5A CN201910057398A CN109880292B CN 109880292 B CN109880292 B CN 109880292B CN 201910057398 A CN201910057398 A CN 201910057398A CN 109880292 B CN109880292 B CN 109880292B
- Authority
- CN
- China
- Prior art keywords
- composite material
- nickel
- barium titanate
- preparation
- epoxy resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention discloses a preparation method of a polymer-based high-dielectric composite material based on a three-dimensional skeleton with a core-shell structure, which relates to the technical field of high-dielectric composite materials, and the preparation process comprises the following steps: the preparation method comprises the steps of foam nickel pretreatment, preparation of a foam nickel/barium titanate composite material and preparation of a polymer-based high-dielectric composite material, wherein the polymer-based high-dielectric composite material is divided into three types, namely foam nickel/barium titanate/epoxy resin, nickel oxide/barium titanate/epoxy resin composite material and nickel oxide (nickel)/barium titanate/epoxy resin composite material. The polymer-based high-dielectric composite material prepared by the invention can obtain a dielectric constant as high as 8000 under the condition that the loss is lower than 0.1, can conveniently change the dielectric constant and the loss by adjusting the electrophoretic deposition amount, the sintering temperature and the oxidation temperature, and has the advantages of simple preparation method, easy operation, strong applicability and practicability and the like.
Description
Technical Field
The invention relates to the technical field of high-dielectric composite materials, in particular to a preparation method of a polymer-based high-dielectric composite material based on a three-dimensional skeleton with a core-shell structure.
Background
The high dielectric composite material is widely applied to filters, sensors, antennas, energy storage devices and the like, and along with the development of electronic devices towards high integration, the dielectric constant of the existing dielectric material needs to be greatly improved, and meanwhile, the low loss is kept. In view of the advantages of low dielectric loss, high breakdown field strength, easy processing and forming and the like of the high polymer material, the high polymer-based high-dielectric composite material becomes a hot point of domestic and foreign research.
At present, there are two main approaches to improve the dielectric constant of polymer composite materials: (1) high dielectric filler is introduced into the insulating polymer matrix, so that the dipole concentration can be improved, and the interface can be increased, thereby improving the polarization strength and the dielectric constant; (2) conductive filler is introduced into the insulating polymer matrix, and the percolation effect is utilized to greatly improve the interface polarization and the dielectric constant.
The problems of improving the dielectric constant of the polymer composite material are as follows: the high dielectric ceramic phase is added into the polymer matrix, so that the dielectric constant can be improved, but the dielectric constant is obviously improved only when the content of the ceramic phase is very high, so that the mechanical property and the processing property of the material are greatly reduced, and the loss is greatly increased; a dielectric constant much higher than that of the matrix can be obtained by incorporating a conductive phase in the insulating polymeric matrix, but the presence of the conductive phase results in a significant increase in losses.
In summary, how to make the polymer-based dielectric composite material obtain significantly improved dielectric constant while maintaining low loss is still a difficult problem in the field of high dielectric material research.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a preparation method of a polymer-based high-dielectric composite material based on a three-dimensional skeleton with a core-shell structure, and the high-dielectric composite material with high dielectric property and low loss is obtained.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a polymer-based high-dielectric composite material based on a three-dimensional skeleton with a core-shell structure comprises the following steps: the preparation process comprises the following steps: the preparation method comprises the steps of foam nickel pretreatment, preparation of a foam nickel/barium titanate composite material and preparation of a polymer-based high-dielectric composite material, wherein the polymer-based high-dielectric composite material is divided into three types, namely foam nickel/barium titanate/epoxy resin, nickel oxide/barium titanate/epoxy resin composite material and nickel oxide (nickel)/barium titanate/epoxy resin composite material.
Further, the preparation process of the nickel oxide/barium titanate/epoxy resin composite material also comprises the preparation of the nickel oxide/barium titanate composite material, and the oxidation temperature is higher than 900 ℃.
Further, the preparation process of the nickel (nickel) oxide/barium titanate/epoxy resin composite material also comprises the preparation of the nickel (nickel) oxide/barium titanate composite material, and the oxidation temperature is lower than 900 ℃.
Further, a foam nickel pretreatment step:
(1) trimming the foamed nickel into blocks of 2cm multiplied by 2cm, putting the blocks into a beaker, adding an acetone solution to immerse the foamed nickel, and ultrasonically cleaning the blocks for 30 min;
(2) pouring off the acetone solution, adding deionized water, and continuing to perform ultrasonic treatment for 15 min;
(3) then absolute ethyl alcohol is added for cleaning by ultrasonic treatment for 15 min.
Further, the preparation steps of the foamed nickel/barium titanate composite material are as follows:
(1) adding 0.8-1.0g of barium titanate powder and 0.5-0.7g of Polyethyleneimine (PEI) into a beaker, adding 50mL of isopropanol, stirring for 4h at room temperature, and then carrying out ultrasonic treatment for 30min to obtain a uniformly dispersed barium titanate mixed solution;
(2) performing electrophoretic deposition by using a direct current power supply, taking two platinum sheets as anodes, taking pretreated foamed nickel as a cathode, and depositing for 20min at 40V voltage, wherein the distance between the foamed nickel and the platinum sheets is 17 mm;
(3) and then, under the nitrogen atmosphere, controlling the sintering temperature to be 700-1300 ℃, and sintering for 2h to obtain a series of foamed nickel/barium titanate composite materials with different sintering temperatures.
Further, preparation of foamed nickel/barium titanate/epoxy resin composite material: and (3) placing a series of foamed nickel/barium titanate composite materials with different sintering temperatures prepared by electrophoretic deposition in a mould, injecting a mixed solution of epoxy resin, and curing at 100 ℃ for 6 hours to obtain a series of foamed nickel/barium titanate/epoxy resin composite materials.
Further, the preparation steps of the nickel oxide/barium titanate/epoxy resin and nickel oxide (nickel)/barium titanate/epoxy resin composite material are as follows: calcining the foamed nickel/barium titanate composite material prepared by electrophoretic deposition at 1300 ℃ for 2h in nitrogen atmosphere, controlling the oxidation temperature at 300-1300 ℃ in air atmosphere to convert part or all of nickel into nickel oxide, preparing the nickel oxide (nickel)/barium titanate composite material when the nickel is partially oxidized, and preparing the nickel oxide/barium titanate composite material when the nickel is fully oxidized.
Further, the nickel oxide/barium titanate composite material and the nickel oxide (nickel)/barium titanate composite material prepared in the above manner are placed in a mold, a mixed solution of epoxy resin is injected, and curing is carried out for 6 hours at 100 ℃ to obtain the nickel oxide/barium titanate/epoxy resin composite material or the nickel oxide (nickel)/barium titanate/epoxy resin composite material.
Further, a preparation method of the mixed solution of the epoxy resin comprises the following steps: mixing epoxy resin, 4-methyltetrahydrophthalic anhydride and 2-ethyl-4-methylimidazole according to the weight ratio of 10:8:0.1, wherein 8-14g of epoxy resin, 6.4-11.2g of 4-methyltetrahydrophthalic anhydride and 0.08-0.14g of 2-ethyl-4-methylimidazole are stirred at 50 ℃ for 30min and then at 70 ℃ for 30min to prepare a mixed solution of the epoxy resin.
The beneficial effect of the invention is that,
1. depositing a barium titanate ceramic layer on the walls of the foamed nickel pores by electrophoretic deposition technique, and controlling electrophoretic deposition parameters, such as electrophoretic deposition voltage, deposition time, and BaTiO3The concentration of the inorganic oxide can control the amount of electrophoretic deposition, so that ceramic layers with different thicknesses can be obtained;
2. the polymer-based high-dielectric composite material with different components and microstructures is obtained by calcining the core-shell structure porous metal ceramic in nitrogen and air atmosphere for a certain time and temperature respectively and impregnating and filling epoxy resin.
The polymer-based high-dielectric composite material prepared by the invention can obtain a dielectric constant as high as 8000 under the condition that the loss is lower than 0.1, can conveniently change the dielectric constant and the loss by adjusting the electrophoretic deposition amount, the sintering temperature and the oxidation temperature, and has the advantages of simple preparation method, easy operation, strong applicability and practicability and the like.
Drawings
FIG. 1 is a schematic diagram of an experimental procedure according to the present invention;
FIG. 2 is a graph of dielectric constant (dispersion) of a nickel foam/barium titanate/epoxy composite at different sintering temperatures;
FIG. 3 is a graph showing the loss dispersion of the nickel foam/barium titanate/epoxy resin composite material at different sintering temperatures;
FIG. 4 is a graph showing the variation of dielectric constant of the nickel foam/barium titanate/epoxy resin composite material with sintering temperature;
FIG. 5 is a graph of dielectric loss versus sintering temperature for a nickel foam/barium titanate/epoxy composite;
FIG. 6 is a graph of dielectric constant for polymer-based high dielectric composites of different oxidation temperatures;
FIG. 7 is a graph of loss dispersion for polymer-based high dielectric composites at different oxidation temperatures;
FIG. 8 is a graph of dielectric constant of a polymer-based high dielectric composite material as a function of the oxidation temperature of nickel foam;
FIG. 9 is a graph of dielectric loss versus nickel foam oxidation temperature for a polymer-based high dielectric composite.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
The preparation method of the polymer-based high-dielectric composite material based on the three-dimensional skeleton of the core-shell structure comprises the following steps of:
firstly, a foamed nickel pretreatment step:
(1) trimming the foamed nickel into blocks of 2cm multiplied by 2cm, putting the blocks into a beaker, adding an acetone solution to immerse the foamed nickel, and ultrasonically cleaning the blocks for 30 min;
(2) pouring off the acetone solution, adding deionized water, and continuing to perform ultrasonic treatment for 15 min;
(3) then absolute ethyl alcohol is added for cleaning by ultrasonic treatment for 15 min.
Secondly, preparing the foamed nickel/barium titanate composite material:
(1) adding 1.0g of barium titanate powder and 0.7g of Polyethyleneimine (PEI) into a beaker, adding 50mL of isopropanol, stirring for 4h at room temperature, and then carrying out ultrasonic treatment for 30min to obtain a uniformly dispersed barium titanate mixed solution;
(2) performing electrophoretic deposition by using a direct current power supply, taking two platinum sheets as anodes, taking pretreated foamed nickel as a cathode, and depositing for 20min at 40V voltage, wherein the distance between the foamed nickel and the platinum sheets is 17 mm;
(3) and then, under the nitrogen atmosphere, controlling the sintering temperature to be 700 ℃, and sintering for 2h to obtain the foamed nickel/barium titanate composite material with the sintering temperature of 700 ℃.
Thirdly, preparing the foamed nickel/barium titanate/epoxy resin composite material:
and (3) placing the foamed nickel/barium titanate composite material with the sintering temperature of 700 ℃ prepared by electrophoretic deposition in a mould, injecting the mixed solution of epoxy resin, and curing for 6 hours at 100 ℃ to obtain the foamed nickel/barium titanate/epoxy resin composite material with the sintering temperature of 700 ℃.
The preparation method of the mixed solution of the epoxy resin comprises the following steps: mixing epoxy resin, 4-methyltetrahydrophthalic anhydride and 2-ethyl-4-methylimidazole according to the weight ratio of 10:8:0.1, wherein 10g of epoxy resin, 8g of 4-methyltetrahydrophthalic anhydride and 0.1g of 2-ethyl-4-methylimidazole are firstly stirred at 50 ℃ for 30min and then at 70 ℃ for 30min to prepare a mixed solution of the epoxy resin.
Example 2
Compared with the embodiment 1, the embodiment of the preparation method of the polymer-based high-dielectric composite material based on the three-dimensional skeleton with the core-shell structure and the preparation process of the foamed nickel/barium titanate/epoxy resin composite material is different in that: controlling the sintering temperature to be 1000 ℃, and preparing the foamed nickel/barium titanate/epoxy resin composite material with the sintering temperature of 1000 ℃.
Example 3
The preparation method of the polymer-based high-dielectric composite material based on the three-dimensional skeleton of the core-shell structure comprises the following steps of: this example is different from example 1 in that: controlling the sintering temperature to be 1300 ℃, and preparing the foamed nickel/barium titanate/epoxy resin composite material with the sintering temperature of 1300 ℃.
Example 4
The preparation method of the polymer-based high-dielectric composite material based on the three-dimensional skeleton of the core-shell structure comprises the following steps of:
firstly, a foamed nickel pretreatment step:
(1) trimming the foamed nickel into blocks of 2cm multiplied by 2cm, putting the blocks into a beaker, adding an acetone solution to immerse the foamed nickel, and ultrasonically cleaning the blocks for 30 min;
(2) pouring off the acetone solution, adding deionized water, and continuing to perform ultrasonic treatment for 15 min;
(3) then absolute ethyl alcohol is added for cleaning by ultrasonic treatment for 15 min.
Secondly, preparing the foamed nickel/barium titanate composite material:
(1) adding 1.0g of barium titanate powder and 0.7g of Polyethyleneimine (PEI) into a beaker, adding 50mL of isopropanol, stirring for 4h at room temperature, and then carrying out ultrasonic treatment for 30min to obtain a uniformly dispersed barium titanate mixed solution;
(2) performing electrophoretic deposition by using a direct-current power supply, taking two platinum sheets as anodes, taking pretreated foamed nickel as a cathode, and depositing for 20min at 40V voltage, wherein the distance between the foamed nickel and the platinum sheets is 17 mm;
(3) and then, under the nitrogen atmosphere, controlling the sintering temperature to be 1300 ℃ and sintering for 2h to obtain the foamed nickel/barium titanate composite material with the sintering temperature of 1300 ℃.
Thirdly, preparing the nickel oxide (nickel)/barium titanate composite material:
and (2) calcining the foam nickel/barium titanate composite material prepared by electrophoretic deposition at the sintering temperature of 1300 ℃ for 2h at the high temperature of 1300 ℃ in a nitrogen atmosphere, and then controlling the oxidation temperature of 900 ℃ in an air atmosphere to convert part or all of nickel into nickel oxide so as to prepare the nickel oxide (nickel)/barium titanate composite material at the oxidation temperature of 900 ℃.
Fourthly, preparing the nickel oxide (nickel)/barium titanate/epoxy resin composite material:
and (2) placing the (nickel)/barium titanate composite material in a mould, injecting the epoxy resin mixed solution, and curing for 6 hours at 100 ℃ to obtain the nickel oxide (nickel)/barium titanate/epoxy resin composite material with the oxidation temperature of 900 ℃.
Example 5
This example differs from example 4 in that:
in the preparation step of the nickel (nickel) oxide/barium titanate composite material, the oxidation temperature is controlled to be 500 ℃, nickel is partially oxidized, and the nickel (nickel) oxide/barium titanate/epoxy resin composite material with the oxidation temperature of 500 ℃ is prepared.
Example 6
This example differs from example 5 in that:
in the preparation step of the nickel (nickel) oxide/barium titanate composite material, the oxidation temperature is controlled to be 700 ℃, nickel is partially oxidized, and the nickel (nickel) oxide/barium titanate/epoxy resin composite material with the oxidation temperature of 700 ℃ is prepared.
Example 7
This example differs from example 6 in that:
in the preparation step of the nickel (nickel) oxide/barium titanate composite material, the oxidation temperature is controlled to be 300 ℃, nickel is partially oxidized, and the nickel (nickel) oxide/barium titanate/epoxy resin composite material with the oxidation temperature of 300 ℃ is prepared.
Example 8
This example differs from example 4 in that:
in the preparation step of the nickel oxide/barium titanate composite material, the oxidation temperature is controlled at 1100 ℃, nickel is completely oxidized, and the nickel oxide/barium titanate/epoxy resin composite material with the oxidation temperature of 1100 ℃ is prepared.
Example 9
This example differs from example 8 in that:
in the preparation step of the nickel oxide/barium titanate composite material, the oxidation temperature is controlled to be 1300 ℃, nickel is completely oxidized, and the nickel oxide/barium titanate/epoxy resin composite material with the oxidation temperature of 1300 ℃ is prepared.
Tests were carried out on the nickel foam/barium titanate/epoxy composite obtained in examples 1 to 3: FIG. 2 is a graph of dielectric constant (dispersion) of a nickel foam/barium titanate/epoxy composite at different sintering temperatures; FIG. 3 is a graph showing the loss dispersion of the nickel foam/barium titanate/epoxy resin composite material at different sintering temperatures; FIG. 4 is a graph showing the variation of dielectric constant of the nickel foam/barium titanate/epoxy resin composite material with sintering temperature; fig. 5 is a graph of dielectric loss versus sintering temperature for a nickel foam/barium titanate/epoxy composite.
It can be seen from the figure that:the dielectric constant is gradually increased along with the increase of the temperature, when the temperature reaches 1300 ℃, the polymer-based high-dielectric composite material shows excellent dielectric property, and the dielectric constant reaches 6397 (10) at the maximum4Hz) of about pure BaTiO3The loss is only 0.04, which is 5.18 times the dielectric constant.
It is known that the dielectric constant of metal is high, but the dielectric loss is also high, but the loss value is greatly reduced but the dielectric constant is not greatly reduced by depositing a barium titanate ceramic layer on the foamed nickel.
The results show that the prepared nickel foam/barium titanate/epoxy resin composite material has the advantages of high dielectric and low loss by adding a ceramic layer on the surface of the metal.
The polymer-based high dielectric composites prepared in examples 4-9 were tested: FIG. 4 is a graph showing the variation of dielectric constant of the nickel foam/barium titanate/epoxy resin composite material with sintering temperature; FIG. 5 is a graph of dielectric loss versus sintering temperature for a nickel foam/barium titanate/epoxy composite; FIG. 6 is a graph of dielectric constant (dispersion) for polymer-based high dielectric composites at different oxidation temperatures; FIG. 7 is a graph of loss dispersion for polymer-based high dielectric composites at different oxidation temperatures; FIG. 8 is a graph of dielectric constant of a polymer-based high dielectric composite material as a function of the oxidation temperature of nickel foam; FIG. 9 is a graph of dielectric loss versus nickel foam oxidation temperature for a polymer-based high dielectric composite.
It can be seen from the figure that: the dielectric constant increases and then decreases with increasing oxidation temperature, and reaches 15744 (10) at an oxidation temperature of 500 DEG C4Hz) which is about one order of magnitude higher than the dielectric constant of pure barium titanate, but the loss factor also reaches 0.21; comprehensive analysis shows that when the oxidation temperature is 700 ℃, the composite material shows excellent dielectric property; at a frequency of 104The dielectric constant of the material is up to 9220 at Hz and is about pure BaTiO37.47 times the dielectric constant and a loss factor of only 0.13.
The results show that the composite material with high dielectric property and low loss is successfully prepared by oxidizing the nickel foam to different degrees, and the high dielectric composite material with more excellent dielectric property is expected to be obtained by further adjusting the oxidation temperature of the nickel foam.
The invention takes foam nickel as a substrate, and barium titanate (BaTiO) is deposited on the pore wall of the foam nickel by an electrophoretic deposition technology3) And sintering the particles at high temperature in a nitrogen atmosphere to obtain a barium titanate ceramic layer, and then calcining the barium titanate ceramic layer at different temperatures and times in an air atmosphere to partially or completely convert the foamed nickel into a nickel oxide (NiO) layer. And finally, impregnating and filling the prepared three-dimensional porous framework with epoxy resin to obtain a series of epoxy resin-based high-dielectric composite materials.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make modifications, alterations, additions or substitutions within the spirit and scope of the present invention.
Claims (7)
1. A preparation method of a polymer-based high-dielectric composite material based on a three-dimensional skeleton with a core-shell structure is characterized by comprising the following steps: the preparation method comprises the following steps of foam nickel pretreatment, preparation of a foam nickel/barium titanate composite material and preparation of a polymer-based high-dielectric composite material, wherein the polymer-based high-dielectric composite material is divided into three types, namely a foam nickel/barium titanate/epoxy resin composite material, a nickel oxide/barium titanate/epoxy resin composite material and a nickel oxide-nickel/barium titanate/epoxy resin composite material;
the preparation steps of the foamed nickel/barium titanate composite material are as follows:
(1) adding 0.8-1.0g of barium titanate powder and 0.5-0.7g of Polyethyleneimine (PEI) into a beaker, adding 50mL of isopropanol, stirring for 4h at room temperature, and then carrying out ultrasonic treatment for 30min to obtain a uniformly dispersed barium titanate mixed solution;
(2) performing electrophoretic deposition by using a direct-current power supply, taking two platinum sheets as anodes, taking pretreated foamed nickel as a cathode, and depositing for 20min at 40V voltage, wherein the distance between the foamed nickel and the platinum sheets is 17 mm;
(3) then, under the nitrogen atmosphere, controlling the sintering temperature to be 700-1300 ℃, and sintering for 2h to obtain a series of foamed nickel/barium titanate composite materials with different sintering temperatures;
the preparation method comprises the following steps of:
calcining the foamed nickel/barium titanate composite material prepared by the electrophoretic deposition method at 1300 ℃ for 2h in a nitrogen atmosphere, controlling the oxidation temperature at 300-1300 ℃ in an air atmosphere to convert part or all of nickel into nickel oxide, preparing the nickel oxide-nickel/barium titanate composite material when the nickel is partially oxidized, and preparing the nickel oxide/barium titanate composite material when the nickel is fully oxidized.
2. The method for preparing the polymer-based high-dielectric composite material based on the three-dimensional skeleton with the core-shell structure according to claim 1, wherein the oxidation temperature is higher than 900 ℃ in the preparation process of the nickel oxide/barium titanate composite material.
3. The method for preparing the polymer-based high-dielectric composite material based on the three-dimensional skeleton with the core-shell structure according to claim 1, wherein the oxidation temperature is lower than 900 ℃ in the preparation process of the nickel oxide-nickel/barium titanate composite material.
4. The preparation method of the polymer-based high dielectric composite material based on the three-dimensional skeleton of the core-shell structure according to claim 1, 2 or 3, wherein the foamed nickel pretreatment step is as follows:
(1) trimming the foamed nickel into blocks of 2cm multiplied by 2cm, putting the blocks into a beaker, adding an acetone solution to immerse the foamed nickel, and ultrasonically cleaning the blocks for 30 min;
(2) pouring off the acetone solution, adding deionized water, and continuing to perform ultrasonic treatment for 15 min;
(3) then absolute ethyl alcohol is added for cleaning by ultrasonic treatment for 15 min.
5. The preparation method of the polymer-based high dielectric composite material based on the three-dimensional skeleton of the core-shell structure according to claim 1, wherein the preparation steps of the foamed nickel/barium titanate/epoxy resin composite material are as follows: and (3) placing a series of foamed nickel/barium titanate composite materials with different sintering temperatures prepared by the electrophoretic deposition method in a mould, injecting a mixed solution of epoxy resin, and curing at 100 ℃ for 6 hours to obtain a series of foamed nickel/barium titanate/epoxy resin composite materials.
6. The preparation method of the polymer-based high dielectric composite material based on the three-dimensional skeleton with the core-shell structure according to claim 1, wherein the prepared nickel oxide/barium titanate composite material or nickel oxide-nickel/barium titanate composite material is placed in a mold, a mixed solution of epoxy resin is injected, and curing is performed for 6 hours at 100 ℃ to obtain the nickel oxide/barium titanate/epoxy resin composite material or nickel oxide-nickel/barium titanate/epoxy resin composite material.
7. The preparation method of the polymer-based high-dielectric composite material based on the three-dimensional skeleton with the core-shell structure according to claim 6, wherein the preparation method of the mixed solution of the epoxy resin comprises the following steps: mixing epoxy resin, 4-methyltetrahydrophthalic anhydride and 2-ethyl-4-methylimidazole according to the weight ratio of 10:8:0.1, wherein 8-14g of epoxy resin, 6.4-11.2g of 4-methyltetrahydrophthalic anhydride and 0.08-0.14g of 2-ethyl-4-methylimidazole are stirred at 50 ℃ for 30min and then at 70 ℃ for 30min to prepare a mixed solution of the epoxy resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910057398.5A CN109880292B (en) | 2019-01-22 | 2019-01-22 | Preparation method of polymer-based high-dielectric composite material based on three-dimensional skeleton with core-shell structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910057398.5A CN109880292B (en) | 2019-01-22 | 2019-01-22 | Preparation method of polymer-based high-dielectric composite material based on three-dimensional skeleton with core-shell structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109880292A CN109880292A (en) | 2019-06-14 |
| CN109880292B true CN109880292B (en) | 2020-03-06 |
Family
ID=66926547
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910057398.5A Active CN109880292B (en) | 2019-01-22 | 2019-01-22 | Preparation method of polymer-based high-dielectric composite material based on three-dimensional skeleton with core-shell structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109880292B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110746742A (en) * | 2019-10-10 | 2020-02-04 | 深圳市峰泳科技有限公司 | Flexible dielectric material with high dielectric constant and preparation method thereof |
| CN110964294A (en) * | 2019-12-02 | 2020-04-07 | 江苏科技大学 | Epoxy resin-based high-dielectric composite material, preparation method and application |
| CN112280297B (en) * | 2020-10-26 | 2021-12-28 | 中国海洋大学 | Barium titanate/polyetherimide dielectric composite material and preparation method thereof |
| CN113956618B (en) * | 2021-11-23 | 2023-05-30 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of three-dimensional porous barium titanate composite dielectric material |
| CN114874582B (en) * | 2022-03-24 | 2023-02-28 | 华北电力大学 | Electroluminescent material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105914046A (en) * | 2016-04-14 | 2016-08-31 | 深圳大学 | Preparation method for hydroxyl-cobalt-carbonate thin-film super capacitor electrode material |
| CN108250677A (en) * | 2016-12-29 | 2018-07-06 | 中国科学院深圳先进技术研究院 | A kind of polymer matrix composite comprising filler grain three-dimensional network and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MY124934A (en) * | 2000-06-30 | 2006-07-31 | Taiyo Yuden Kk | Dielectric ceramic composition and ceramic capacitor |
| US20100110608A1 (en) * | 2008-11-06 | 2010-05-06 | Frank Wei | Core-shell structured dielectric particles for use in multilayer ceramic capacitors |
-
2019
- 2019-01-22 CN CN201910057398.5A patent/CN109880292B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105914046A (en) * | 2016-04-14 | 2016-08-31 | 深圳大学 | Preparation method for hydroxyl-cobalt-carbonate thin-film super capacitor electrode material |
| CN108250677A (en) * | 2016-12-29 | 2018-07-06 | 中国科学院深圳先进技术研究院 | A kind of polymer matrix composite comprising filler grain three-dimensional network and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109880292A (en) | 2019-06-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109880292B (en) | Preparation method of polymer-based high-dielectric composite material based on three-dimensional skeleton with core-shell structure | |
| CN101712784B (en) | Core-shell structured packing/polymer-based composite material and preparation method thereof | |
| CN112280297B (en) | Barium titanate/polyetherimide dielectric composite material and preparation method thereof | |
| KR102293297B1 (en) | all solid state battery and its making method | |
| KR20140027131A (en) | Method for improving the electrical parameters in capacitors containing pedot/pss as a solid electrolyte by polyglycerol | |
| CN103474247A (en) | Method for manufacturing solid polymer electrolytic condenser | |
| CN102709055B (en) | A kind of conducting high polymers thing catholyte solution and Synthesis and applications thereof | |
| WO2011001147A1 (en) | Ceramic material | |
| CN103864435B (en) | Preparation method of wide-temperature, high-pressure-resistant and high-energy-density ceramic dielectric material | |
| CN102775626B (en) | Preparation method of high-energy storage density solid dielectric composite material | |
| CN102800480A (en) | Preparation method for cathode of Nb capacitor | |
| CN104292764A (en) | Composite dielectric material for high energy-storage capacitor and preparation method of composite dielectric material | |
| CN109265880B (en) | Core-shell structure powder and dielectric composite material prepared from same | |
| JP4831108B2 (en) | Manufacturing method of solid electrolytic capacitor | |
| CN202363267U (en) | Solid electrolytic capacitor | |
| CN101805179A (en) | Preparation method for barium strontium titanate (BST) thick film material | |
| JP2003037024A (en) | Method of manufacturing solid electrolytic capacitor | |
| CN109592662B (en) | Preparation method of biochar negative electrode material for lithium-sulfur battery | |
| CN101007892A (en) | Core-shell structure polymer base composite material and its preparing process | |
| Zheng et al. | An in situ (K 0.5 Na 0.5) NbO 3-doped barium titanate foam framework and its cyanate ester resin composites with temperature-stable dielectric properties and low dielectric loss | |
| CN105239131A (en) | Electrolyte for in-situ growth of barium strontium titanium ferroelectric film on surface of titanium substrate and preparing method of film | |
| CN114559579A (en) | High-density flexible graphite bipolar plate and preparation method and application thereof | |
| EP3984727A1 (en) | Method for manufacturing composite material, and composite material | |
| CN108147831A (en) | A kind of preparation method of C/C composite materials high-temperature oxidation resistant coating | |
| CN113480815A (en) | Polymethyl methacrylate/polyvinylidene fluoride composite material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |