CN115725101A - Preparation method of nano alumina/polyimide high-temperature dielectric composite film - Google Patents

Preparation method of nano alumina/polyimide high-temperature dielectric composite film Download PDF

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Publication number
CN115725101A
CN115725101A CN202211454363.3A CN202211454363A CN115725101A CN 115725101 A CN115725101 A CN 115725101A CN 202211454363 A CN202211454363 A CN 202211454363A CN 115725101 A CN115725101 A CN 115725101A
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alumina
composite film
nano
dielectric composite
preparing
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沈洋
南策文
孙滨洲
江建勇
潘家雨
胡澎浩
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Wu Zhenshiyanshi
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Wu Zhenshiyanshi
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a preparation method of a nano alumina/polyimide high-temperature dielectric composite film, which comprises the following steps: s1, adding an aluminum source and a dispersing agent into distilled water, continuously adding nitric acid, heating in a water bath to obtain alumina sol, and calcining the sol in an argon atmosphere to obtain alumina nanoparticles; s2, directly adding the alumina nanoparticles into the polyacrylic acid solution, magnetically stirring to obtain an alumina/PAA mixed solution which is uniformly mixed, and then obtaining the nano alumina/polyimide film through a coating process, thereby solving the problems that the nanoparticles are difficult to disperse in a polymer matrix and the high-temperature energy storage performance is poor in the prior art.

Description

Preparation method of nano alumina/polyimide high-temperature dielectric composite film
Technical Field
The invention relates to the field of dielectric energy storage materials, in particular to a preparation method of a nano aluminum oxide/polyimide high-temperature dielectric composite film.
Background
The poor high temperature stability of polymer dielectric materials limits their applications in electromagnetic catapulting, weapon systems, new energy vehicles, and the like. Currently, the operating temperature of commercial Biaxially oriented polypropylene BOPP (Biaxially oriented polypropylene) is 105 ℃, and when the temperature reaches 80 ℃, the dielectric properties thereof are drastically reduced. In order to continue using BOPP films in high temperature environments, an additional cooling system is required to maintain the ambient temperature at 60-80 ℃. This will undoubtedly increase the quality of the overall system and increase costs. Therefore, the development of new high temperature dielectric materials is imminent.
Polyimide is a polymer containing imide cyclic imide groups on the main chain and is obtained by condensation polymerization of dibasic acid and diamine. Polyimide film is the film insulating material with the best performance in the world at present, and because PI has excellent thermal property, electrical property, mechanical property and chemical stability, the polyimide film is widely applied to various fields of aerospace, spacecrafts, navigation, rocket missiles, automobiles, electrical appliance insulation, atomic energy industry, satellites, nuclear submarines, microelectronics, liquid crystal display, medical treatment, packaging precision machinery and the like. Research in the present stage mainly aims to reduce the leakage conduction loss of the polymer in a high-temperature state by adding a small amount of nanoparticles with high forbidden band width, but the nanoparticles are difficult to be uniformly dispersed in a polymer matrix due to large specific surface area, so that the improvement on the high-temperature energy storage performance of the polymer is limited.
Disclosure of Invention
The invention provides a preparation method of a nano-alumina/polyimide high-temperature dielectric composite film, which solves the problems that nano-particles are difficult to disperse in a polymer matrix and the high-temperature energy storage performance is poor in the prior art.
In order to solve the technical problem, the invention provides the following technical scheme:
the preparation method of the nano aluminum oxide/polyimide high-temperature dielectric composite film comprises the following steps:
s1, adding an aluminum source and a dispersing agent into distilled water, continuously adding nitric acid, heating in a water bath to obtain alumina sol, and calcining the sol in an argon atmosphere to obtain alumina nanoparticles;
s2, directly adding the alumina nanoparticles into the polyacrylic acid solution, magnetically stirring to obtain an alumina/PAA mixed solution which is uniformly mixed, and then obtaining the nano alumina/polyimide film through a coating process.
The dispersing agent is added in the preparation process of the alumina nano particles, and the alumina with the surfactant can be obtained after calcination, so that the uniform dispersion of the alumina in a preparation system is facilitated, and the secondary agglomeration phenomenon cannot occur.
The alumina nano particles are directly added into the polyacrylic acid solution to obtain a uniform alumina/PAA mixed solution, and the process is suitable for industrial production;
compared with a commercial biaxially oriented polypropylene film or a single-layer polyether sulfone and polyether sulfone based composite film, the amidation process of changing PAA into PI by heating has excellent high-temperature energy storage performance.
Preferably, the aluminum source is aluminum isopropoxide, and the dispersant is aluminum carboxylate.
Aluminum isopropoxide is the main aluminum source, aluminum ions in the aluminum carboxylate provide the aluminum source, and carboxylate ions are adsorbed on the surface of the aluminum oxide corresponding to the dispersant.
Preferably, the adding amount ratio of the aluminum isopropoxide to the deionized water is 1:5-10 percent of aluminum carboxylate, wherein the adding weight of the aluminum carboxylate accounts for 1-3 percent of the adding amount of aluminum isopropoxide.
Preferably, the concentration of the nitric acid is 1mol/L, and the adding mass of the nitric acid accounts for 10-20% of the adding mass of the aluminum isopropoxide.
Preferably, the temperature of the water bath heating in the step S1 is 60-70 ℃, and the time is 20-24h.
Preferably, the calcination temperature in the step S1 is 1000-1200 ℃ and the calcination time is 1-3h.
Preferably, the alumina particles in step S1 have a particle size of 30 to 200nm.
Preferably, the amount of the alumina nanoparticles added in step S1 is 0.5 to 10% by mass of the polyacrylic acid solution.
Preferably, the magnetic stirring time is 30min.
Compared with the prior art, the invention has the following advantages:
during the preparation process of the alumina, the dispersant is added, and the alumina with the surfactant can be obtained after calcination, which is beneficial to uniform dispersion of the alumina in a preparation system and does not generate secondary agglomeration.
In addition, compared with a commercial biaxially oriented polypropylene film or a single-layer polyether sulfone and polyether sulfone based composite film, the film prepared by the coating method has excellent high-temperature energy storage performance.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a scanning electron micrograph of alumina nanoparticles prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the alumina/PI composite film prepared in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of the alumina/PI composite film prepared in comparative example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limiting the present invention.
Example 1
(1) Preparing alumina nanoparticles: adding 1g of aluminum isopropoxide and 0.01g of aluminum carboxylate into 5g of deionized water, adding 0.1g of nitric acid with the concentration of 1mol/L, and heating in a water bath at 60 ℃ for 20 hours to obtain alumina sol; calcining at 1200 ℃ for 1h under the argon atmosphere condition to obtain alumina nano particles;
(2) Preparing an alumina/PI film: adding alumina particles with the mass being 2 percent of that of the polyacrylic acid solution into the PAA solution, magnetically stirring the mixture for 30min at room temperature to obtain an alumina/PAA solution which is uniformly mixed, and preparing the alumina/PI film by a coating method.
Example 2
(1) Preparing alumina nanoparticles: adding 3g of aluminum isopropoxide and 0.09g of aluminum carboxylate into 30g of deionized water, adding 0.6g of nitric acid with the concentration of 1mol/L, and heating in a water bath at 65 ℃ for 22h to obtain alumina sol; calcining for 2 hours at 1100 ℃ under the argon atmosphere condition to obtain alumina nano particles;
(2) Preparing an alumina/PI film: adding alumina particles with the mass being 2 percent of that of the polyacrylic acid solution into the PAA solution, magnetically stirring the mixture for 30min at room temperature to obtain an alumina/PAA solution which is uniformly mixed, and preparing the alumina/PI film by a coating method.
Example 3
(1) Preparing alumina nanoparticles: adding 3g of aluminum isopropoxide and 0.06g of aluminum carboxylate into 20g of deionized water, adding 0.45g of nitric acid with the concentration of 1mol/L, and heating in a water bath at 70 ℃ for 24 hours to obtain alumina sol; calcining for 3 hours at 1000 ℃ under the argon atmosphere condition to obtain alumina nano particles;
(2) Preparing an alumina/PI film: adding alumina particles with the mass being 2 percent of that of the polyacrylic acid solution into the PAA solution, magnetically stirring the mixture for 30min at room temperature to obtain an alumina/PAA solution which is uniformly mixed, and preparing the alumina/PI film by a coating method.
Comparative example 1
(1) Preparing alumina nanoparticles: adding 3g of aluminum isopropoxide into 15g of deionized water, adding 0.3g of nitric acid with the concentration of 1mol/L, and heating in a water bath at 60 ℃ for 20 hours to obtain alumina sol; calcining for 1h at 1100 ℃ under the argon atmosphere condition to obtain alumina nano particles;
(2) Preparing an alumina/PI film: adding alumina particles with the mass being 2 percent of that of the polyacrylic acid solution into the PAA solution, magnetically stirring the mixture for 30min at room temperature to obtain an alumina/PI solution which is uniformly mixed, and preparing the alumina/PI film by a coating method.
Comparative example 2
Adding 0.02g of commercial 30nm alumina nanoparticles into 5mL of N-methylpyrrolidone, ultrasonically stirring for 30min, then adding the mixed solution into 3g of PAA solution, heating in a water bath at 60 ℃ for 30min to obtain a uniform alumina/PAA solution, and preparing the alumina/PI film by a coating method.
Performance testing
The films of examples 1 to 3 and comparative examples 1 to 2 were vacuum-deposited to prepare metal circular electrodes, and their properties were measured.
And (3) testing: a ferroelectric tester (PK-CPE 1701) is adopted to carry out a ferroelectric hysteresis loop test, and the energy storage density and the charge and discharge efficiency are obtained by calculating the ferroelectric hysteresis loop.
The above examples 1 to 3 and comparative examples 1 to 2 were recorded during the preparation process, and the energy storage density at a frequency of 10Hz was measured, respectively, and the results of the relevant performance tests are shown in table 1 below.
TABLE 1
Performance index Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
Dispersibility Is excellent in Is excellent in Is excellent in Good effect Difference (D)
Compatibility Is excellent in Is excellent in Is excellent in Is good Difference (D)
Energy storage Density (J/cm) 3 ,150℃) 3.23 3.41 3.68 2.9 2.4
As can be seen from table 1, examples 1 to 3 have excellent nanoparticle dispersibility and compatibility in preparation, and have excellent high-temperature energy storage properties; however, in comparative examples 1 and 2, since no dispersant was added, the nanoparticles were not uniformly dispersed, and the high temperature energy storage performance was decreased. FIG. 1 is a scanning electron micrograph of alumina particles having a uniform particle size distribution; fig. 2-3 are scanning electron micrographs of the alumina/PI composite films prepared in examples 1 and 3, and further confirm that the alumina nanoparticles have good dispersibility and compatibility in the PI film, which are closely related to the excellent high-temperature energy storage performance.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. The preparation method of the nano aluminum oxide/polyimide high-temperature dielectric composite film is characterized by comprising the following steps:
s1, adding an aluminum source and a dispersing agent into distilled water, continuously adding nitric acid, heating in a water bath to obtain alumina sol, and calcining the sol in an argon atmosphere to obtain alumina nanoparticles;
s2, directly adding the alumina nanoparticles into the polyacrylic acid solution, magnetically stirring to obtain an alumina/PAA mixed solution which is uniformly mixed, and then obtaining the nano alumina/polyimide film through a coating process.
2. The method for preparing a nano alumina/polyimide high temperature dielectric composite film according to claim 1, wherein the aluminum source is aluminum isopropoxide and the dispersant is aluminum carboxylate.
3. The preparation method of the nano aluminum oxide/polyimide high-temperature dielectric composite film according to claim 2, wherein the addition amount ratio of aluminum isopropoxide to deionized water is 1:5-10, wherein the adding weight of the aluminum carboxylate accounts for 1-3% of the adding amount of the aluminum isopropoxide.
4. The method for preparing the nano alumina/polyimide high-temperature dielectric composite film according to claim 1, wherein the concentration of the nitric acid is 1mol/L, and the addition mass of the nitric acid accounts for 10-20% of the addition mass of the aluminum isopropoxide.
5. The method for preparing a nano alumina/polyimide high temperature dielectric composite film according to claim 1, wherein the temperature of the water bath heating in the step S1 is 60-70 ℃ and the time is 20-24h.
6. The method for preparing a nano alumina/polyimide high temperature dielectric composite film according to claim 1, wherein the calcination temperature in the step S1 is 1000-1200 ℃ and the calcination time is 1-3h.
7. The method for preparing a nano alumina/polyimide high temperature dielectric composite film according to claim 1, wherein the alumina particles in the step S1 have a particle size of 30-200nm.
8. The method for preparing a nano alumina/polyimide high temperature dielectric composite film according to claim 1, wherein the alumina nano particles of the step S1 are added in an amount of 0.5-10% by mass based on the polyacrylic acid solution.
9. The method for preparing a nano alumina/polyimide high temperature dielectric composite film according to claim 1, wherein the magnetic stirring time is 30min.
CN202211454363.3A 2022-11-21 2022-11-21 Preparation method of nano alumina/polyimide high-temperature dielectric composite film Pending CN115725101A (en)

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CN112789326A (en) * 2020-12-18 2021-05-11 清华大学 High-temperature energy storage hybrid polyetherimide dielectric film and preparation method and application thereof
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