CN112992550A - Industrial production method of capacitor material - Google Patents
Industrial production method of capacitor material Download PDFInfo
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- CN112992550A CN112992550A CN202110284098.8A CN202110284098A CN112992550A CN 112992550 A CN112992550 A CN 112992550A CN 202110284098 A CN202110284098 A CN 202110284098A CN 112992550 A CN112992550 A CN 112992550A
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- 239000003990 capacitor Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000009776 industrial production Methods 0.000 title abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 54
- 238000000576 coating method Methods 0.000 claims abstract description 54
- 239000002002 slurry Substances 0.000 claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract 4
- 239000002131 composite material Substances 0.000 claims description 47
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 29
- 239000011889 copper foil Substances 0.000 claims description 29
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 239000011888 foil Substances 0.000 claims description 14
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- 239000004408 titanium dioxide Substances 0.000 claims description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 6
- 239000005751 Copper oxide Substances 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 229910000431 copper oxide Inorganic materials 0.000 claims description 6
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- 239000003822 epoxy resin Substances 0.000 description 11
- 229920000647 polyepoxide Polymers 0.000 description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 9
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- 238000001816 cooling Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
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- 238000005096 rolling process Methods 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
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- 150000003839 salts Chemical class 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- 238000004140 cleaning Methods 0.000 description 2
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
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- 229910000420 cerium oxide Inorganic materials 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
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- 239000013072 incoming material Substances 0.000 description 1
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- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
本发明公开了一种电容材料的工业化生产方法，属于电容材料制备技术领域。本发明的制备方法包括以下步骤：(1)将电容原料研磨并制备成浆料；(2)将得到的浆料涂覆于金属基材的一个表面并进行烘烤，形成表面具有干膜的金属基材；(3)使用两个复合辊，对两片表面具有干膜的金属基材进行干膜对干膜的复合，得到复合后的材料；(4)将复合后的材料进行固化，得到电容材料。本发明的电容材料制备方法，操作步骤简单，工艺条件相对宽松，能够有效节约经济成本，有利于快速应用于工业化生产，且制备得到的电容材料性能优异。
The invention discloses an industrialized production method of a capacitor material, and belongs to the technical field of capacitor material preparation. The preparation method of the present invention includes the following steps: (1) grinding the capacitor raw material and preparing it into a slurry; (2) coating the obtained slurry on one surface of a metal substrate and baking it to form a dry film on the surface. metal substrate; (3) using two compounding rollers to perform dry film-to-dry film compounding on two metal substrates with dry films on their surfaces to obtain a compounded material; (4) curing the compounded material, Get capacitor material. The preparation method of the capacitor material of the present invention has simple operation steps and relatively loose process conditions, can effectively save the economic cost, is conducive to rapid application in industrial production, and the prepared capacitor material has excellent performance.
Description
Technical Field
The invention relates to the field of preparation of capacitor materials, in particular to an industrial production method of a capacitor material.
Background
Since the 21 st century, the human society has faced a serious challenge of energy crisis and environmental pollution, and all countries and energy researchers in the world are continuously seeking cleaner green energy, and the capacitor as one of the green energy has raised a technical trend in the world, and the capacitor material as a determining factor for determining the performance of the capacitor is becoming the focus of the current research.
The capacitance material as a key component of the capacitor determines the basic characteristics of the super capacitor.
In the prior art, the preparation method of the capacitor material with good performance mainly comprises the following steps: (1) adding high-surface-area carbon powder into a metal salt aqueous solution, infiltrating the metal salt aqueous solution into the surface and holes of the carbon powder, adding sodium hydroxide (NaOH) or potassium hydroxide (KOH) to form metal oxide, removing water, adding Polytetrafluoroethylene (PTFE), and rolling to form a capacitor material; (2) preparation of amorphous thin film capacitor material: adding alcohol to a metal salt aqueous solution to form a gelatinous precipitate, washing and vacuum-drying to form a metal oxide, adding activated carbon to an organic solution to form a gelatinous precipitate, and performing heat treatment at a temperature of 200 to 300 ℃ under an inert atmosphere to form a capacitor material.
However, the existing preparation method of the capacitor material including the above preparation method is only suitable for laboratory production or small-scale production, the process flow is complicated, the process conditions are strict, and the method cannot be quickly applied to industrial production. Therefore, it is an urgent technical problem to provide an industrial production method of a capacitor material with good performance.
Disclosure of Invention
The invention aims to provide an industrial production method of a capacitor material, which solves the problems in the prior art, enables the performance of the capacitor material to be excellent and can meet the requirement of industrial production.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides an industrial production method of a capacitor material, which comprises the following steps:
(1) grinding the capacitor raw material and preparing into slurry;
(2) coating the obtained slurry on one surface of a metal base material and baking to form the metal base material with a dry film on the surface;
(3) compounding the dry film to the dry film on two pieces of metal base materials with the dry films on the surfaces by using two compounding rollers to obtain a compounded material;
(4) and curing the compounded material to obtain the capacitor material.
Further, the metal base material is an aluminum foil or a copper foil, and the thickness of the metal base material is 6-60 micrometers.
Further, the viscosity of the slurry is 0.01-2.0 Pascal-second, and the coating thickness of the slurry is 1-20 microns.
Further, the capacitor raw material comprises titanium dioxide, barium oxide, copper oxide, calcium carbonate or rare earth oxide.
Further, the step (1) also comprises the step of baking the capacitor raw material.
Further, the baking temperature in the step (2) is 50-350 ℃, and the baking time is 1-20 min.
Further, the two composite rollers are both rubber rollers, or one of the two composite rollers is a rubber roller, and the other composite roller is a smooth roller or a rubber roller; the Rockwell hardness of the rubber surface of the rubber roller is 30-70.
Further, the surface temperature of the two composite rollers is 80-250 ℃, the pressure of the compression roller is 0.2-2.0 MPa, and the included angle of the two metal base films with the dry films when the two metal base films pass between the two composite rollers is 10-80 degrees.
Further, the curing process adopts constant-temperature baking.
Further, the constant temperature baking process is divided into three stages: the first stage is constant temperature baking at 70-100 deg.C for 50-70 min; the second stage constant temperature baking temperature is 140-; the constant-temperature baking temperature in the third stage is 170-350 ℃, and the constant-temperature time is 50-70 min; and naturally cooling to 30-50 ℃ after the third-stage constant-temperature baking is finished.
The invention discloses the following technical effects:
the preparation method of the capacitor material has simple operation steps and relatively loose process conditions, can effectively save economic cost, and is favorable for being rapidly applied to industrial production.
The capacitor material prepared by the invention has excellent performances in the aspects of peel strength resistance, dielectric constant, dielectric loss, dielectric layer thickness, plate explosion, water absorption and insulation resistance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a process flow diagram of example 1 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "parts" in the present invention are all parts by mass unless otherwise specified.
The solvent for dissolving the raw material according to the present invention includes: ether alcohols (such as n-butanol), ketones (such as cyclohexanone, acetone, butanone, pentanone, etc.), esters (such as ethyl acetate), etc.
Example 1
1. Weighing the raw materials according to the molar ratio of the titanium dioxide to the barium oxide to the copper oxide to the calcium carbonate to the cerium oxide of 98:96:1:1.9: 0.9.
2. Putting the weighed raw materials into a ball milling tank, adding ethanol serving as a ball milling medium into the ball milling tank to uniformly mix the powder, removing a solvent, compacting the mixed powder, baking in an oven, wherein the baking temperature curve is that the temperature is raised to 60 ℃ at the rate of 2 ℃/min for one hour, then the temperature is raised to 200 ℃ at the rate of 5 ℃/min for 0.5 hour, and then the temperature is raised to 750 ℃ at the rate of 10 ℃/min for 120 minutes, and then the temperature is naturally reduced to room temperature to obtain powder A.
3. Weighing epoxy resin accounting for 10% of the powder A by mass, and dissolving the epoxy resin with n-butyl alcohol (the temperature is controlled below 30 ℃ during dissolving) to obtain a solution A; then putting a certain amount of powder A and solution A into a ball milling tank, screwing a handle, setting the linear velocity of a central shaft of the ball milling tank to be 50 m/min, the running time to be 15 hours and the ambient temperature to be 10 ℃, obtaining a mixture comprising the slurry and a grinding ball after ball milling is finished, and obtaining the slurry with the viscosity of 0.01 Pascal per second;
the operation mode of the ball milling tank is bidirectional operation, the single operation time is 50min, and the waiting time for each shutdown is 1 min.
4. Separating the slurry and the grinding balls in the mixture by using a strainer;
5. standing the slurry for 20min, transferring the slurry to a storage bin of a coating device, coating the slurry on an electrolytic copper foil (the thickness is 10 microns), wherein the coating device is a continuous coating device, the coating mode adopts scraper blade coating, the coating head adopts secondary purification, the purification grade is thousands grade, the coating speed is 1 m/min, and the coating width is 500 mm; the coating thickness is 12 microns, and the deviation is less than 1 micron;
the width of the copper foil is 520 mm, and the tension is 25N;
setting the baking temperature of the baking oven at 100 ℃, baking time for 2min, and effectively baking the copper foil for more than 6m to obtain the electrolytic copper foil with the dry film on the surface.
5. Placing two pieces of electrolytic copper foils with dry films on the surfaces at unreeling stations of two composite rollers respectively, compounding the dry films by using the two pieces of electrolytic copper foils entering the two composite rollers, and reeling the two pieces of electrolytic copper foils by using a reeling rod (a steel pipe of DN 150) after compounding to obtain a compounded coiled material;
the two composite rollers comprise an upper composite roller and a lower composite roller, and the diameters of the two composite rollers are both 1000 mm;
during compounding, the two compound rollers are heated, the surface temperatures of the two compound rollers are controlled to be 220 ℃, one of the two compound rollers is a rubber roller, the Rockwell hardness of the rubber surface of the rubber roller is 50, the other compound roller is a smooth roller, the pressure of the two compound rollers is 0.2 MPa, and the included angle between the two compound rollers when two pieces of electrolytic copper foil pass through the two compound rollers is 10 degrees.
6. Moving the coiled material after compounding to the baking oven, vertically placing, and going on the pine book, taking out the rolling pole after the pine book, divide three constant temperature stage in proper order to toast the coiled material according to the temperature from low to high, wherein, the programming rate 1 ℃/min, three constant temperature stage includes: the first-stage constant temperature is 100 ℃, the first-stage constant temperature duration is 60min, the second-stage constant temperature is 150 ℃, the second-stage constant temperature duration is 50min, the third-stage constant temperature is 200 ℃, and the third-stage constant temperature duration is 70 min; and after the third-stage constant temperature is finished, naturally cooling to 50 ℃, opening the box door, putting the winding rod in the box door and tightly winding the winding rod.
7. Under the condition that the environmental temperature is 10 ℃ and the cleanliness requires ten thousand-level purification, the coiled material is moved to the unwinding position of the slitting machine, the width of each 25mm of each cut two sides is set, namely only 450mm in the middle is reserved, a DN150 plastic pipe is used for winding, the coiled material is moved to the unwinding position of the slitting machine after the edge cutting and winding are completed, the length of each cut sheet is set to be 550mm, and the slitting machine is started to cut the coiled material into required product sizes.
The performance of the capacitor material prepared in example 1 was measured, and the measurement results are shown in table 1:
TABLE 1
Example 2
1. According to titanium dioxide, barium oxide and La2O3Weighing raw materials according to a molar ratio of 100:94:6, putting the weighed raw materials into a ball milling tank, adding ethanol serving as a ball milling medium into the ball milling tank to uniformly mix the powder, removing a solvent, compacting the mixed powder, baking the powder in a muffle furnace, wherein the baking temperature curve is that the temperature is raised to 100 ℃ at the speed of 2 ℃/min for one hour, then the temperature is raised to 200 ℃ at the speed of 5 ℃/min for 0.5 hour, then the temperature is raised to 900 ℃ at the speed of 10 ℃/min for 120 minutes, and then the temperature is naturally lowered to room temperatureTo obtain powder B.
2. Weighing epoxy resin with 50% of the powder A by mass, and dissolving with butanone (the temperature is controlled below 30 ℃ during dissolving) to obtain a solution C; then putting a certain amount of the powder B and the solution C into a ball milling tank, screwing a handle, setting the linear velocity of a central shaft of the ball milling tank to be 50 m/min, the running time to be 24 hours and the ambient temperature to be 10 ℃, obtaining a mixture comprising the slurry and a grinding ball after ball milling is finished, and obtaining the slurry with the viscosity of 0.2 Pascal per second;
the operation mode of the ball milling tank is bidirectional operation, the single operation time is 60min, and the waiting time for each shutdown is 10 min.
3. And separating the slurry and the grinding balls in the mixture by using a filter screen.
4. Standing the slurry for 40min, transferring the slurry to a storage bin of a coating device, coating the slurry on an electrolytic copper foil (with the thickness of 18 microns), wherein the coating device is a continuous coating device, extrusion coating is adopted as a coating mode, secondary purification is adopted at a coating head, the purification grade is thousands, the coating speed is 15 m/min, and the coating width is 500 mm; the coating thickness is 6 microns, and the deviation is less than 1 micron;
the width of the electrolytic copper foil is 520 mm, and the tension is 20N;
setting the baking temperature of the baking oven at 100 ℃, baking time for 2min, and effective baking length equal to 6m to obtain the electrolytic copper foil with the dry film on the surface.
5. Placing two pieces of electrolytic copper foils with dry films on the surfaces at unreeling stations of two composite rollers respectively, compounding the dry films by using the two pieces of electrolytic copper foils entering the two composite rollers, and reeling the two pieces of electrolytic copper foils by using a reeling rod (a steel pipe of DN 150) after compounding to obtain a compounded coiled material;
the two composite rollers comprise an upper composite roller and a lower composite roller, and the diameters of the two composite rollers are both 600 mm;
during compounding, the two compound rollers are heated, the surface temperatures of the two compound rollers are controlled to be 100 ℃, one of the two compound rollers is a rubber roller, the Rockwell hardness of the rubber surface of the rubber roller is 70, the other compound roller is a rubber roller, the pressure of the pressing rollers of the two compound rollers is 2.0 MPa, and the included angle between the two compound rollers when two pieces of electrolytic copper foil pass through the two compound rollers is 80 degrees.
6. Moving the coiled material after compounding to the baking oven, vertically placing, and carrying out the uncoiling, taking out the rolling rod after the uncoiling, and baking the coiled material according to three constant temperature stages of temperature from low to high in proper order, wherein, the heating rate is 10 ℃/min, and three constant temperature stages include: the first-stage constant temperature is 70 ℃, the first-stage constant temperature duration is 70min, the second-stage constant temperature is 140 ℃, the second-stage constant temperature duration is 70min, the third-stage constant temperature is 170 ℃, and the third-stage constant temperature duration is 50 min; and after the third-stage constant temperature is finished, naturally cooling to 30 ℃, opening the box door, putting the winding rod in the box door and tightly winding the winding rod.
7. And under the condition that the environmental temperature is 30 ℃ and the cleanliness requires ten thousands of levels of purification, the edge trimmer is used for trimming the cured coiled material product, and the coiled material product is cut into the required size of a sample.
The performance of the capacitor material prepared in example 2 was measured, and the measurement results are shown in table 2:
TABLE 2
| Performance of | Parameter range |
| Dielectric constant | 22.6(1000Hz) |
| Dielectric loss | 0.013(1000Hz) |
| Dielectric thickness | 12 micron |
| Water absorption rate | 0.015％ |
| Glass transition temperature | 110℃ |
| Temperature of thermal cracking | 300.71℃(N2) |
| Compressive strength | 2201KV/mm |
| Peel strength at 90 ° | 1.0N/cm |
| Insulation resistance | 3.89×104Ω |
Example 3
1. According to the formula titanium dioxide, barium oxide, copper oxide, calcium carbonate and Er2O3Weighing raw materials according to a molar ratio of 99:97: 0.9: 2: 1.1, putting the weighed raw materials into a ball milling tank, adding ethanol serving as a ball milling medium into the ball milling tank to uniformly mix the powder, removing a solvent, compacting the mixed powder, baking in an oven, wherein the baking temperature curve is that the temperature is raised to 100 ℃ at the rate of 2 ℃/min for one hour, then the temperature is continuously raised to 200 ℃ at the rate of 5 ℃/min for 0.5 hour, and then the temperature is raised to 900 ℃ at the rate of 10 ℃/min for 120 minutes, and then naturally cooled to room temperature to obtain powder D.
2. Weighing epoxy resin with the mass of 50% of the powder A, dissolving the epoxy resin with a mixed solution of acetone and butanone (the temperature is controlled below 30 ℃ during dissolving), and performing ultrasonic dispersion treatment (the ultrasonic frequency is 20 kilohertz and the power is 3 kilowatts) during dissolving to obtain a solution D; then putting a certain amount of powder D and solution D into a ball milling tank, screwing down a handle, setting the linear velocity of a central shaft of the ball milling tank to be 65 m/min, the running time to be 20h and the ambient temperature to be 15 ℃, obtaining a mixture comprising the slurry and a grinding ball after ball milling is finished, and obtaining the slurry with the viscosity of 0.3 Pascal per second;
the operation mode of the ball milling tank is bidirectional operation, the single operation time is 55min, and the waiting time for each shutdown is 8 min.
3. Separating the slurry and the grinding balls in the mixture by using a filter screen;
4. standing the slurry for 30min, transferring the slurry to a storage bin of a coating device, coating the slurry on an electrolytic aluminum foil (with the thickness of 50 microns), wherein the coating device is a continuous coating device, the coating mode adopts transfer coating, a coating head adopts secondary purification, the purification grade is thousands, the coating speed is 10 m/min, and the coating width is 1000 mm; the coating thickness is 8 microns, and the deviation is less than 1 micron;
the width of the electrolytic copper foil is 500 mm, and the tension is 25N;
setting the baking temperature of a baking oven at 80 ℃, baking time for 5min, and opening the baking oven for 10 meters (opening 5 sections of baking ovens with 2 meters per section) to obtain the electrolytic copper foil with the dry film on the surface.
5. Respectively placing two electrolytic copper foils or electrolytic aluminum foils with dry films on the surfaces at unwinding stations of two composite rollers, compounding the dry films by using the two electrolytic copper foils entering the two composite rollers, and winding the two electrolytic copper foils by using a winding rod (a steel pipe of DN 150) after compounding to obtain a compounded coiled material;
the two composite rollers comprise an upper composite roller and a lower composite roller, and the diameters of the two composite rollers are both 800 mm;
during compounding, the two compound rollers are heated, the surface temperatures of the two compound rollers are controlled to be 80 ℃, one of the two compound rollers is a rubber roller, the Rockwell hardness of the rubber surface of the rubber roller is 30, the other compound roller is a rubber roller, the pressure of the compression rollers of the two compound rollers is 1 MPa, and the included angle between the two electrolytic aluminum foils when the two electrolytic aluminum foils pass through the two compound rollers is 30 degrees.
6. Move the coiled material after compounding to the baking oven in, vertically place, take out the rolling rod after the pine is rolled up, divide three constant temperature stage in proper order to toast the coiled material according to the temperature from low to high, the baking process goes on under nitrogen protection gas environment, the programming rate 8 ℃/min, three constant temperature stage includes: the first-stage constant temperature is 80 ℃, the first-stage constant temperature duration is 50min, the second-stage constant temperature is 170 ℃, the second-stage constant temperature duration is 60min, the third-stage constant temperature is 190 ℃, and the third-stage constant temperature duration is 60 min; and after the third-stage constant temperature is finished, naturally cooling to 40 ℃, opening the box door, putting the winding rod in the box door and tightly winding the winding rod.
7. And under the condition that the environmental temperature is 20 ℃ and the cleanliness requires ten thousands of levels of purification, the edge trimmer is used for trimming the cured coiled material product, and the coiled material product is cut into the required size of a sample.
The performance of the capacitor material prepared in example 3 was measured, and the measurement results are shown in table 3:
TABLE 3
| Performance of | Parameter range |
| Dielectric constant | 34.3(1000Hz) |
| Dielectric loss | 0.014(1000Hz) |
| Dielectric thickness | 16 micron |
| Water absorption rate | 0.017％ |
| Glass transition temperature | 163℃ |
| Temperature of thermal cracking | 310.22℃(N2) |
| Compressive strength | 21.64KV/mm |
| Peel strength at 90 ° | 0.97N/cm |
| Insulation resistance | 4.56×104Ω |
Example 4
1. According to the formula of titanium dioxide, barium oxide, copper oxide, calcium carbonate and Dy2O3Weighing raw materials according to a molar ratio of 99:97:1.1:1.9:0.9, putting the weighed raw materials into a ball milling tank, adding ethanol serving as a ball milling medium into the ball milling tank to uniformly mix the powder, removing a solvent, compacting the mixed powder, baking in an oven, raising the temperature to 100 ℃ at a baking temperature curve of 2 ℃/min for one hour, continuing to maintain the temperature to 200 ℃ at a temperature of 5 ℃/min for 0.5 hour, raising the temperature to 700 ℃ at a temperature of 10 ℃/min for 120 minutes, and naturally cooling to room temperature to obtain powder E.
2. Weighing epoxy resin accounting for 30% of the powder A by mass, dissolving the epoxy resin with a mixed solution of pentanone and butanone (the temperature is controlled below 30 ℃ during dissolving), and performing ultrasonic dispersion treatment (the ultrasonic frequency is 20 kilohertz and the power is 3 kilowatts) during dissolving to obtain a solution D; then putting a certain amount of powder D and solution D into a ball milling tank, screwing down a handle, setting the linear velocity of a central shaft of the ball milling tank to be 55 m/min, the running time to be 18h and the ambient temperature to be 18 ℃, obtaining a mixture comprising the slurry and a grinding ball after ball milling is finished, and obtaining the slurry with the viscosity of 0.3 Pascal per second;
the operation mode of the ball milling tank is bidirectional operation, the single operation time is 50min, and the waiting time for each shutdown is 7 min.
3. Separating the slurry and the grinding balls in the mixture by using a strainer;
4. standing the slurry for 40min, transferring the slurry to a storage bin of a coating device, coating the slurry on an electrolytic aluminum foil (the thickness is 40 microns), wherein the coating device is a continuous coating device, the coating mode adopts transfer coating, a coating head adopts secondary purification, the purification grade is thousand grades, the coating speed is 13 m/min, and the coating width is 500 mm; the coating thickness is 20 microns, and the deviation is less than 1 micron;
the width of the electrolytic aluminum foil is 500 mm, and the tension is 25N;
setting the baking temperature of the baking oven at 200 ℃, baking time for 15min, and opening the baking oven for 10 meters (opening 5 sections of baking oven with 2 meters per section) to obtain the electrolytic aluminum foil with the dry film on the surface.
5. Placing two electrolytic aluminum foils with dry films on the surfaces at unwinding stations of two composite rollers respectively, compounding the dry films by using the two electrolytic aluminum foils entering the two composite rollers, and winding the two electrolytic aluminum foils by using a winding rod (a steel pipe of DN 150) after compounding to obtain a compounded coiled material;
the two composite rollers comprise an upper composite roller and a lower composite roller, and the diameters of the two composite rollers are 900 millimeters;
during compounding, the two composite rollers are heated, the surface temperatures of the two composite rollers are controlled to be 130 ℃, the two composite rollers are rubber rollers, the Rockwell hardness of the rubber surfaces of the rubber rollers is 45, the pressure of the compression rollers of the two composite rollers is 0.5 MPa, and the included angle between the two electrolytic aluminum foils when the two electrolytic aluminum foils pass through the two composite rollers is 30 degrees.
6. Move the coiled material after compounding to the baking oven in, vertically place to the unwrapping wire, take out the rolling pole after the unwrapping wire, the baking oven is toasted the coiled material according to the three constant temperature stage of temperature from low to high in proper order, and the baking process goes on under helium protective gas environment, and the programming rate 9 ℃/min, three constant temperature stage include: the first-stage constant temperature is 90 ℃, the first-stage constant temperature duration is 60min, the second-stage constant temperature is 160 ℃, the second-stage constant temperature duration is 70min, the third-stage constant temperature is 180 ℃, and the third-stage constant temperature duration is 50 min; and after the third-stage constant temperature is finished, naturally cooling to 45 ℃, opening the box door, putting the winding rod in the box door and tightly winding the winding rod.
7. And (3) under the condition that the environmental temperature is 15 ℃ and the cleanliness requires ten thousands of levels of purification, using an edge trimmer to perform edge cutting processing on the cured coiled material product, and cutting the coiled material product into the required size of a sample.
The performance of the capacitor material prepared in example 4 was measured, and the measurement results are shown in table 4:
TABLE 4
| Performance of | Parameter range |
| Dielectric constant | 37 |
| Dielectric loss | 0.0153(1000KHz) |
| Dielectric thickness | 20 micron |
| Water absorption rate | 0.02％ |
| Glass transition temperature | 100℃ |
| Temperature of thermal cracking | 345.33℃(N2) |
| Compressive strength | 28.08KV/mm |
| Peel strength at 90 ° | 1.30N/cm |
| Burst plate test | Constant temperature of 300 ℃ for 70min without plate explosion |
| Insulation resistance | 4.00×104Ω |
Example 5
1. According to titanium dioxide, copper oxide, calcium carbonate and Pr2O3Weighing raw materials according to a molar ratio of 100:1:2.1:1, putting the weighed raw materials into a ball milling tank, adding ethanol serving as a ball milling medium into the ball milling tank to uniformly mix the powder, removing a solvent, compacting the mixed powder, baking in an oven, wherein the baking temperature curve is that the temperature is raised to 100 ℃ at a speed of 2 ℃/min for one hour, then the temperature is raised to 200 ℃ at a speed of 5 ℃/min for 0.5 hour, and then the temperature is raised to 700 ℃ at a speed of 10 ℃/min for 120 minutes, and then the temperature is naturally lowered to room temperature to obtain powder F.
2. Weighing epoxy resin accounting for 40% of the powder A by mass, dissolving the epoxy resin with a mixed solution of acetone, pentanone and butanone (the temperature is controlled below 30 ℃ during dissolving), and performing ultrasonic dispersion treatment (the ultrasonic frequency is 20 kilohertz and the power is 3 kilowatts) during dissolving to obtain a solution F; then putting a certain amount of powder F and solution F into a ball milling tank, screwing down a handle, setting the linear velocity of a central shaft of the ball milling tank to be 55 m/min, the running time to be 18h and the ambient temperature to be 18 ℃, obtaining a mixture comprising the slurry and a grinding ball after ball milling is finished, and obtaining the slurry with the viscosity of 0.3 Pascal per second;
the operation mode of the ball milling tank is bidirectional operation, the single operation time is 60min, and the waiting time for each shutdown is 6 min.
3. Separating the slurry and the grinding balls in the mixture by using a strainer;
4. standing the slurry for 20min, transferring the slurry to a storage bin of a coating device, coating the slurry on an electrolytic copper foil (the thickness is 35 microns), wherein the coating device is a continuous coating device, the coating mode adopts transfer coating, a coating head adopts two-stage purification, the purification grade is thousand grades, the coating speed is 1.5 m/min, and the coating width is 500 mm; the coating thickness is 6 microns, and the deviation is less than 1 micron;
the width of the electrolytic copper foil is 520 mm, and the tension is 25N;
setting the baking temperature of a baking oven at 100 ℃, baking time for 12min, and opening the baking oven for 10 meters (opening 5 sections of baking ovens with 2 meters per section) to obtain the electrolytic copper foil with the dry film on the surface.
5. Placing two pieces of electrolytic copper foils with dry films on the surfaces at unreeling stations of two composite rollers respectively, compounding the dry films by using the two pieces of electrolytic copper foils entering the two composite rollers, and reeling the two pieces of electrolytic copper foils by using a reeling rod (a steel pipe of DN 150) after compounding to obtain a compounded coiled material;
the two composite rollers comprise an upper composite roller and a lower composite roller, and the diameters of the two composite rollers are 700 millimeters;
during compounding, the two compound rollers are heated, the surface temperatures of the two compound rollers are controlled to be 150 ℃, one of the two compound rollers is a rubber roller, the Rockwell hardness of the rubber surface of the rubber roller is 60, the other compound roller is a rubber roller, the pressure of the two compound rollers is 0.2 MPa, and the included angle between the two compound rollers when two pieces of electrolytic copper foil pass through the two compound rollers is 40 degrees.
6. Move the coiled material after compounding to the baking oven in, vertically place to the unwrapping wire, take out the rolling pole after the unwrapping wire, divide three constant temperature stage in proper order to toast the coiled material according to the temperature from low to high, the baking process goes on under argon gas protective gas's environment, and the programming rate 2 ℃/min, three constant temperature stage include: the first-stage constant temperature is 100 ℃, the first-stage constant temperature duration is 55min, the second-stage constant temperature is 150 ℃, the second-stage constant temperature duration is 50min, the third-stage constant temperature is 190 ℃, and the third-stage constant temperature duration is 55 min; and after the third-stage constant temperature is finished, naturally cooling to 40 ℃, opening the box door, putting the winding rod in the box door and tightly winding the winding rod.
7. And (3) under the condition that the environmental temperature is 18 ℃ and the cleanliness requires ten thousands of levels of purification, using an edge trimmer to perform edge cutting processing on the cured coiled material product, and cutting the coiled material product into the required size of a sample.
The performance of the capacitor material prepared in example 5 was measured, and the measurement results are shown in table 5:
TABLE 5
| Performance of | Parameter range |
| Dielectric constant | 41 |
| Dielectric thickness | 6 micron |
| Water absorption rate | 0.022％ |
| Glass transition temperature | 125℃ |
| Temperature of thermal cracking | 338.33℃(N2) |
| Compressive strength and withstand voltage | 21.13KV/mm， |
| Peel strength at 90 ° | 0.95N/cm |
| Burst plate test | Constant temperature of 300 ℃ for 70min without plate explosion |
| Insulation resistance | 3.98×104Ω |
The purity of the solvent in the capacitor raw material is more than 75%, the solvent needs to be controlled in the incoming material process, the temperature of the storage environment is controlled to be 10-30 ℃, the humidity is below 60%, the ventilation is good, direct sunlight is forbidden, and the capacitor raw material is sealed and stored.
Cleaning the colander or the filter screen immediately after use, removing residual slurry and the like in pores of the colander or the filter screen, drying the colander or the filter screen by blowing or airing, and storing the colander or the filter screen in a clean tool box; cleaning the grinding balls and the ball milling tank immediately, drying the solvent in the grinding balls and the ball milling tank, and sealing and storing the grinding balls and the ball milling tank;
if the filtered slurry is not used immediately, the filtered slurry is sealed and temporarily stored, the ambient temperature is 10-20 ℃, the ambient humidity is below 60 percent, the slurry is transferred under the above conditions, and the viscosity of the slurry is kept between 0.01 and 2.0 Pascal per second.
The added epoxy resin can bond the powder to the maximum extent, so that the epoxy resin and the ceramic powder form a uniform composite material with certain flexibility; the invention can also add various surfactants for the capacitor material into the capacitor raw material, and the addition of the surfactants can not influence the performance of the capacitor material.
The trimming method of the invention comprises the steps of orienting two-edge separation cutting (such as a blade), opposite tearing cutting (such as scissors), high-temperature melting cutting (such as laser cutting), and grinding cutting (such as a grinding wheel and a water jet).
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
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