CN113307949A - Parylene film for high-temperature energy storage capacitor and preparation method thereof - Google Patents
Parylene film for high-temperature energy storage capacitor and preparation method thereof Download PDFInfo
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Abstract
A parylene film for a high-temperature energy storage capacitor and a preparation method thereof are disclosed, which comprises the following specific steps: a. purifying three p-xylene dimers of an N type, a C type and a F type; b. placing the purified dimer powder into a sublimation area of a feeding bin, and sublimating the dimer powder into gas; c. the dimer gas and the inert gas are fully mixed and then brought into a cracking zone by the inert gas, and the dimer CH is carried out at high temperature2‑CH2Breaking bonds to generate a p-xylene diradical active monomer which is stable at high temperature; d. under the push of inert gas, the mixture enters a vacuum deposition area with low temperature and is spontaneously polymerized and deposited on the surface of a substrate material to form a film; the invention adopts a chemical vapor deposition method and adopts different types of pairsThe dimethyl benzene ring bi-body is used as a precursor, and different types of parylene films can be prepared; the composition, structure and thickness of the film can be controlled, the surface is smooth and compact, and the film can be used for any substrate and can further modify an active interface.
Description
Technical Field
The invention relates to the technical field of high-temperature-resistant energy storage, in particular to a parylene film for a high-temperature energy storage capacitor and a preparation method thereof.
Background
Dielectric energy storage capacitors are a special kind of energy storage devices, which can be used for very short timesThe stored energy is completely released in the middle (microsecond level). The high power, short duration output makes dielectric capacitors widely used in high pulse applications such as medical defibrillators, advanced electromagnetic systems, and the like. In addition, the high-temperature working fields of avionics, automobiles, underground oil and natural gas exploration and the like also show urgent needs for high-temperature resistant energy storage capacitors. The advantages of polymer dielectrics compared to brittle, difficult to process ceramic materials have been well documented, including high breakdown strength, low mass density, inexpensive production, flexibility, and ease of processing. At present, biaxially oriented polypropylene (BOPP) is adopted as a medium in a mainstream capacitor, but the maximum working temperature of the BOPP is only 105 ℃, the BOPP is difficult to adapt to higher working temperature, a plurality of polymer dielectrics are unstable at high temperature, the loss is sharply increased when the temperature is increased, the energy storage density is reduced, and particularly the temperature reaches TgIn the above case, the physical properties and mechanical properties are abruptly degraded, and thus the heat exchanger is not suitable for high-temperature operation.
To obtain a more temperature resistant dielectric material, it is common to add rigid building blocks to the polymer backbone to prevent rotation and increase the stiffness of the backbone. In addition, the side group can physically limit the rotation of the bond, and when the side group is polar, the rotation can be further limited due to polar interaction, so that the rigidity of the polymer is improved, and the high-temperature resistance of the material is improved.
The main chain of the poly-p-xylene contains a benzene ring rigid structure, polar chlorine atoms and fluorine atom side groups on the benzene ring are substituted to further improve the rigidity of the main chain, so that the C-type and F-type poly-p-xylene films have better rigidity, have better high temperature resistance and energy storage performance on the basis of the N-type poly-p-xylene film, and can be well used in the energy storage fields of high temperature resistant energy storage capacitors and the like.
The parylene film can be prepared by a coating method, a plasma enhanced deposition method, a chemical vapor condensation method, an electrochemical deposition method and the like, but more or less defects exist, for example, the film prepared by the traditional electrochemical deposition method has very low molecular weight and no practical value.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a Parylene film for a high-temperature energy storage capacitor and a preparation method thereof, which relate to the preparation of three types (Parylene N, Parylene C and Parylene F) of Parylene films: namely, the parylene film is prepared by using p-xylene cyclic dimer (N type), chlorine substituted p-xylene cyclic dimer (C type) and fluorine substituted p-xylene cyclic dimer (F type) as raw materials.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a parylene film for a high-temperature energy storage capacitor comprises three types of N type, C type and F type, and the structural formula is as follows:
a preparation method of a parylene film for a high-temperature energy storage capacitor comprises the following specific steps:
a. purifying three p-xylene dimers of an N type, a C type and a F type;
b. placing the purified dimer powder into a sublimation area of a feeding bin, and sublimating the dimer powder into gas;
c. the dimer gas and the inert gas are fully mixed and then brought into a cracking zone by the inert gas, and the dimer CH is carried out at high temperature2-CH2Breaking bonds to generate a p-xylene diradical active monomer which is stable at high temperature;
d. then under the push of inert gas, the mixture enters a low-temperature vacuum deposition area and spontaneously polymerizes and deposits on the surface of the substrate material to form a film;
the N-type, C-type and F-type p-xylene dimers in the step a have the structural formulas respectively as follows:
in the step b, the temperature of the sublimation area is controlled to be 150-170 ℃;
in the step b, the pressure of the sublimation area is controlled to be 0.5-1 mbar;
the inert gas in the step c comprises argon;
in the step c, the temperature of the pyrolysis zone is controlled to be 600-700 ℃;
in the step c, the pressure of the cracking area is controlled to be 0.1-0.2 mbar;
in the step d, the temperature of a deposition area is controlled to be-40-60 ℃;
in the step d, the pressure of the deposition area is controlled to be 0.02-0.05 mbar;
in the step d, the substrate material adopts a silicon wafer or an aluminum base.
The invention has the advantages that:
1. different types of paraxylene films can be prepared by adopting different types of paraxylene cyclic dimers as precursors; convenient operation and no by-product.
2. The main chain of the parylene contains a benzene ring rigid structure, so that the N-type parylene film has good temperature resistance; polar chlorine atoms and fluorine atom side groups on the benzene ring are substituted to further improve the rigidity of the main chain, so that the C-type and F-type parylene films have better high temperature resistance on the basis of the N-type parylene film.
3. The invention adopts Chemical Vapor Deposition (CVD) method to control the composition, structure and thickness (hundreds of nanometers to tens of micrometers) of the film, the process of the prepared film is adjustable, the thickness of the film is controllable, the surface is smooth, the structure is compact, and the film can be used for any substrate and can further modify an active interface.
4. The film prepared by the method has excellent high temperature resistance and excellent dielectric property, is a good linear dielectric medium at normal temperature or high temperature (100 ℃), has higher energy storage capacity, and can be used in the field of high temperature resistant energy storage capacitors.
Drawings
FIG. 1 is a schematic diagram of three types of parylene film fabrication processes;
FIG. 2(a) shows the energy storage density of the parylene film at room temperature under different electric field strengths; FIG. 2(b) is a charge-discharge efficiency spectrum of the parylene film at room temperature under different electric field strengths;
FIG. 3(a) is the energy storage density of the parylene film at 70 deg.C under different electric field strengths; FIG. 3(b) is a charge-discharge efficiency spectrum of the parylene film at 70 ℃ under different electric field strengths;
FIG. 4(a) is the energy storage density of the parylene film at 100 deg.C under different electric field strengths; FIG. 4(b) is a graph showing the charge and discharge efficiency of the parylene film at 100 ℃ under different electric field strengths.
Detailed Description
The invention is further illustrated below with reference to the synthesis scheme.
The invention adopts a chemical vapor deposition method to prepare three films of N type, C type and F type by changing the types of raw materials; the final film thickness is controlled by controlling the raw material content.
Selecting a common thickness to prepare N type, C type and F type parylene films with the thickness of 15 mu m; to investigate the thickness effect, a C-type parylene film with a thickness of 10 μm was simultaneously prepared.
Example one
In this embodiment, a method for preparing an N-type parylene film is provided, using N-type p-xylene cyclic dimer as a raw material, as shown in fig. 1(a), and includes the following steps:
a. purifying 35g of N-type p-xylene dimer;
b. placing the purified dimer powder into a sublimation area of a feeding bin, and sublimating the dimer powder into gas; setting the temperature of the sublimation area at 160 ℃ and the pressure at 0.5 mbar;
c. the dimer gas and the inert gas are fully mixed and then are brought into a cracking zone by the inert gas, the temperature of the cracking zone is 650 ℃, and the pressure is 0.1 mbar; dimer CH at high temperature2-CH2Breaking bonds to generate a p-xylene diradical active monomer which is stable at high temperature;
d. then, under the push of inert gas, the mixture enters a low-temperature vacuum deposition area, the temperature of the deposition area is 20 ℃, the pressure of a chamber is 0.02mbar, and the mixture is spontaneously polymerized and deposited on the surface of the base material to form a film; the resulting film was a Parylene N material with a thickness of 15 μm.
The specific experimental steps are as follows:
first, preparation work
(1) Cleaning all chambers, platforms and pipelines of a sublimation area, a pyrolysis area and a deposition area in the whole film preparation device, wiping with distilled water, and wiping with ethanol and dust-free cloth to ensure clean preparation environment;
(2) turning on a power switch of the device, and setting the temperature of a sublimation area to be 160 ℃ and the pressure to be 0.5 mbar; setting the temperature of a cracking zone at 650 ℃ and the pressure at 0.1 mbar; the deposition zone temperature was 20 ℃ and the chamber pressure was 0.02 mbar.
(3) Weighing 35g of N-type p-xylene ring two-body powdery raw materials, placing the raw materials on clean tin foil paper, placing the tin foil paper containing the raw materials into a feeding pipeline of a sublimation area, and placing a cleaned silicon wafer substrate into a deposition area.
(4) And pre-pumping the device: air was evacuated to a pressure of 3mbar and then evacuated to 10mbar twice.
Secondly, the preparation is carried out
And (5) performing air extraction for the third time, and adjusting the sublimation area and the cracking area to a heating working state when the pressure in the chamber reaches 0.5mbar, so that the preparation is started.
Thirdly, the preparation is finished
After the deposition process is finished, when the temperature of the chamber is cooled to be below 45 ℃, the instrument is closed; slowly and intermittently deflating, and taking out the substrate; the resulting film was a Parylene N material with a thickness of 15 μm.
Example two
This example provides a method for preparing a C-type parylene film, as shown in fig. 1(b), which is different from example 1 in that the raw material for the preparation is C-type parylene dimer. The remaining pre-preparation work, operating procedures and parameter settings remained the same as in example 1. The resulting film was a Parylene C material with a thickness of 15 μm.
EXAMPLE III
This example provides a method for preparing an F-type parylene film, as shown in fig. 1(c), which is different from example 1 in that the starting material is F-type p-xylylene dimer. The remaining pre-preparation work, operating procedures and parameter settings remained the same as in example 1. The resulting film was a Parylene F material with a thickness of 15 μm.
Example four
This example provides a method for preparing a C-type parylene film, which is different from example 1 in that the preparation raw material is C-type p-xylylene ring dimer; unlike example 2, only 25g of the starting materials were weighed, and the remaining preparation work, operation procedures and parameter settings were the same as in example 1. The resulting film was a Parylene C material with a thickness of 10 μm.
The films obtained from the above four examples were subjected to relevant tests, as shown in fig. 2, 3, and 4. The parylene film prepared by the method has good energy storage performance: the energy storage density of the C-type and F-type films is kept at 3J/cm at 70 DEG C3@400MV/m or more, is BOPP (1.6J/cm) under the same conditions3) 2 times of the charge-discharge efficiency, the charge-discharge efficiency is also kept above 80%, and the stability is still better at 100 ℃ (the charge-discharge efficiency is still above 60% at 400 MV/m), so that the high-temperature-resistant energy-storage capacitor can be well used in the energy-storage field such as high-temperature-resistant energy-storage capacitors.
Claims (7)
1. A parylene film for a high-temperature energy storage capacitor is characterized by comprising three types of N type, C type and F type, and the structural formula is as follows:
2. the preparation method of the parylene film for the high-temperature energy storage capacitor according to claim 1, is characterized by comprising the following specific steps:
a. purifying three p-xylene dimers of an N type, a C type and a F type;
b. placing the purified dimer powder into a sublimation area of a feeding bin, and sublimating the dimer powder into gas;
c. the dimer gas and the inert gas are fully mixed and then brought into a cracking zone by the inert gas, and the dimer CH is carried out at high temperature2-CH2Breaking bonds to generate a p-xylene diradical active monomer which is stable at high temperature;
d. then enters a low-temperature vacuum deposition area under the driving of inert gas, and spontaneously polymerizes and deposits to be a film on the surface of the base material.
3. The method as claimed in claim 2, wherein the three p-xylene dimers of N-type, C-type and F-type in step a are represented by the following structural formulas:
4. the method of claim 2, wherein the parylene film is a parylene film for a high temperature energy storage capacitor,
in the step b, the temperature of the sublimation area is controlled to be 150-170 ℃;
and in the step b, the pressure of the sublimation area is controlled to be 0.5-1 mbar.
5. The method of claim 2, wherein the parylene film is a parylene film for a high temperature energy storage capacitor,
the inert gas in the step c comprises argon;
in the step c, the temperature of the pyrolysis zone is controlled to be 600-700 ℃;
and c, controlling the pressure of the cracking area in the step c to be 0.1-0.2 mbar.
6. The method of claim 2, wherein the parylene film is a parylene film for a high temperature energy storage capacitor,
in the step d, the temperature of a deposition area is controlled to be-40-60 ℃;
and in the step d, the pressure of the deposition area is controlled to be 0.02-0.05 mbar.
7. The method of claim 2, wherein the parylene film is a parylene film for a high temperature energy storage capacitor,
in the step d, the substrate material adopts a silicon wafer or an aluminum base.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114086116A (en) * | 2021-11-17 | 2022-02-25 | 安徽通灵仿生科技有限公司 | Corrosion-resistant coating on surface of motor rotor of catheter pump and preparation process thereof |
| CN115007415A (en) * | 2022-05-24 | 2022-09-06 | 西安交通大学 | High-performance polypropylene-based capacitor film and preparation method and application thereof |
| CN115463803A (en) * | 2021-12-15 | 2022-12-13 | 上海交通大学 | Chemical vapor deposition device and preparation method of high-thickness Parylene-N film |
| CN116252502A (en) * | 2023-03-13 | 2023-06-13 | 天津大学 | Method for improving dielectric property of polypropylene film based on interface deposition modification |
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| JPS61228019A (en) * | 1985-04-02 | 1986-10-11 | Murata Mfg Co Ltd | Production of organic thin film |
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2021
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3319141A (en) * | 1962-12-27 | 1967-05-09 | Union Carbide Corp | Thin film capacitors |
| JPS61228019A (en) * | 1985-04-02 | 1986-10-11 | Murata Mfg Co Ltd | Production of organic thin film |
Non-Patent Citations (3)
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| JAY J. SENKEVICH，ET AL: ""Molecular Layer Chemistry via Parylenes"", 《CHEM. VAP. DEPOSITION》 * |
| JAY J. SENKEVICH，ET AL: ""Poly(tetraflouro-p-xylylene), a low dielectric constant chemical vapor polymerized polymer"", 《APPL. PHYS. LETT.》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114086116A (en) * | 2021-11-17 | 2022-02-25 | 安徽通灵仿生科技有限公司 | Corrosion-resistant coating on surface of motor rotor of catheter pump and preparation process thereof |
| CN115463803A (en) * | 2021-12-15 | 2022-12-13 | 上海交通大学 | Chemical vapor deposition device and preparation method of high-thickness Parylene-N film |
| CN115463803B (en) * | 2021-12-15 | 2023-09-22 | 上海交通大学 | Chemical vapor deposition device and preparation method of high-thickness Parylene-N film |
| CN115007415A (en) * | 2022-05-24 | 2022-09-06 | 西安交通大学 | High-performance polypropylene-based capacitor film and preparation method and application thereof |
| CN116252502A (en) * | 2023-03-13 | 2023-06-13 | 天津大学 | Method for improving dielectric property of polypropylene film based on interface deposition modification |
| CN116252502B (en) * | 2023-03-13 | 2023-10-27 | 天津大学 | Method for improving dielectric property of polypropylene film based on interface deposition modification |
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