CN115331965A - Electrode foil, preparation method thereof and capacitor - Google Patents
Electrode foil, preparation method thereof and capacitor Download PDFInfo
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- CN115331965A CN115331965A CN202210938340.3A CN202210938340A CN115331965A CN 115331965 A CN115331965 A CN 115331965A CN 202210938340 A CN202210938340 A CN 202210938340A CN 115331965 A CN115331965 A CN 115331965A
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- 239000011888 foil Substances 0.000 title claims abstract description 230
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003990 capacitor Substances 0.000 title claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 125
- 238000011282 treatment Methods 0.000 claims abstract description 45
- 238000005245 sintering Methods 0.000 claims abstract description 28
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- 238000000034 method Methods 0.000 claims description 33
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 19
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 17
- 239000004925 Acrylic resin Substances 0.000 claims description 13
- 229920000178 Acrylic resin Polymers 0.000 claims description 13
- 239000001856 Ethyl cellulose Substances 0.000 claims description 13
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 13
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- 238000004519 manufacturing process Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 11
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 10
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 10
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 10
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- 238000009835 boiling Methods 0.000 claims description 9
- 230000000087 stabilizing effect Effects 0.000 claims description 9
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- 150000007524 organic acids Chemical class 0.000 claims description 8
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- 229910052782 aluminium Inorganic materials 0.000 description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
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- 238000007796 conventional method Methods 0.000 description 1
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- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Ceramic Capacitors (AREA)
Abstract
The invention provides an electrode foil, a preparation method thereof and a capacitor, wherein the preparation method of the electrode foil comprises the following steps: clamping the base foil from two opposite sides of the base foil by using a mold clamping plate, wherein the mold clamping plate is provided with a slurry coating window; coating slurry in the slurry coating windows on the two opposite sides of the base foil to form a slurry layer; drying and sintering the base foil coated with the slurry and the mold clamping plate together to form sintered layers on the opposite two sides of the base foil to obtain an unformed foil; the unformed foil and the mold clamp plate were subjected to chemical conversion treatment together to obtain an electrode foil. According to the preparation method, the thickness of the electrode foil slurry layer can reach the standard, the shape of the slurry layer is neat, and the formed electrode foil cannot be bent and deformed.
Description
Technical Field
The invention relates to the technical field of electrode foils, in particular to an electrode foil, a preparation method thereof and a capacitor.
Background
The bulk electrode foil is mainly used in capacitors with high capacity requirements. The paste layer on the surface of the base foil of the bulk electrode foil is thicker than that of the conventional electrode foil (the paste thickness is generally about 50 μm). When the electrode foil is used in an electronic circuit with high capacity requirement, the assembly process can be simplified compared with the traditional electrode foil, and the volume is smaller (if the traditional electrode foil is adopted, the electrode foil is required to be stacked and combined by a plurality of sheet layers).
Currently, the preparation process of the bulk electrode foil is to coat the slurry on the surface of the base foil, and then obtain the finished electrode foil after drying, sintering and formation. Because the slurry layer in the block-shaped electrode foil is thick (generally 100-400 μm), the slurry is easy to overflow after the slurry layer is coated on the base foil, so that the shape of the slurry layer is irregular and the thickness of the slurry layer cannot meet the requirement. Moreover, after the formation step, the electrode foil is easily subjected to bending deformation.
Disclosure of Invention
Therefore, the electrode foil which has the standard thickness of the slurry layer and is regular in shape and free from bending after formation, the preparation method thereof and the capacitor need to be provided aiming at the problems that the traditional preparation method of the block electrode foil is easy to generate irregular slurry layer shape, irregular thickness and bending deformation after formation of the electrode foil.
In order to solve the above problems, the technical solution proposed by the present invention is as follows:
according to an aspect of the present invention, there is provided a method of manufacturing an electrode foil, including the steps of:
clamping the base layer foil from two opposite sides of the base layer foil by using a mold clamping plate, wherein the mold clamping plate is provided with a slurry coating window;
coating slurry in the slurry coating windows on the two opposite sides of the base foil to form slurry layers;
drying and sintering the base foil coated with the slurry and the mold clamping plate together to form sintered layers on opposite sides of the base foil to obtain an unformed foil; and
and carrying out chemical conversion treatment on the unformed foil and the die clamping plate together to obtain the electrode foil.
In some of these embodiments, applying a slurry in the slurry application windows on opposite sides of the base foil comprises the steps of:
coating a slurry in the slurry coating window on one side of the base foil, turning the base foil and the mold clamp plate together so that the other side of the base foil faces upward, and then coating a slurry in the slurry coating window on the other side of the base foil.
In some of these embodiments, the formation process comprises the steps of:
placing the unformed foil and the mold clamping plate into an aqueous solution of an organic acid, and boiling for 15-40 min at 95-100 ℃; and
subjecting the un-formed foil after poaching and the mold jaws together to a multi-stage formation process.
In some of these embodiments, the multi-stage formation process includes the steps of:
first-stage formation: putting the boiled unformed foil and the mold clamping plate into a forming solution together, and heating at 83-93 ℃ under 450-520V voltage of 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 3000-7500 s under current;
primary heat treatment: treating the unformed foil and the die clamping plate together at the temperature of 350-550 ℃ for 1-5 min;
secondary formation: putting the unformed foil and the die clamping plate into a forming liquid together, and carrying out treatment at 83-93 ℃ under the conditions of 450-520V of voltage and 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 500-1500 s under the current;
and (3) phosphoric acid treatment: placing the unformed foil and the die clamping plate together in a phosphoric acid solution with the conductivity of 25000 mu s/cm-45000 mu s/cm, and treating for 5-10 min at the temperature of 55-70 ℃;
carrying out three-stage formation: putting the unformed foil and the die clamping plate into a forming liquid together, and carrying out treatment at 83-93 ℃ under the conditions of 450-520V of voltage and 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 500-1500 s under the current;
secondary heat treatment: treating the unformed foil and the mold clamp plate together at 350-550 ℃ for 1-5 min;
carrying out four-stage formation: putting the unformed foil and the die clamping plate into a forming liquid together, and carrying out treatment at 83-93 ℃ under the conditions of 450-520V of voltage and 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 500-1500 s under the current; and
ammonium dihydrogen phosphate treatment: putting the unformed foil and the die clamping plate into ammonium dihydrogen phosphate solution with the concentration of 1 g/L-3 g/L, and treating for 2 min-8 min at the temperature of 55-70 ℃.
In some embodiments, the sintering process comprises the steps of:
and (3) treating the dried unformed foil and the mold clamping plate for 1 to 6 hours at the temperature of between 200 and 400 ℃ under the protection of inert gas, and then treating for 1 to 24 hours at the temperature of between 560 and 660 ℃.
In some of these embodiments, the slurry comprises, in weight percent: 40-60% of aluminum powder, 20-55% of solvent, 0.1-10% of ethyl cellulose and 0.1-10% of acrylic resin.
In some of these embodiments, the solvent is one or both of ethyl acetate and butyl diglycol.
According to another aspect of the present invention, there is provided an electrode foil comprising a base foil and sintered layers provided on opposite sides of the base foil, the electrode foil being produced by the above-described production method of the present invention.
In some of these embodiments, the sintered layers on opposite sides of the base foil each have a thickness of 100-400 μm.
According to another aspect of the present invention, there is provided a capacitor, wherein at least one electrode of the capacitor is the above-mentioned electrode foil.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the electrode foil is improved, the base layer foil is clamped from two opposite sides of the base layer foil by adopting a mold clamping plate, and a slurry coating window is arranged on the mold clamping plate; coating slurry in the slurry coating windows on the two opposite sides of the base foil to form a slurry layer; carrying out subsequent drying treatment, sintering treatment and formation treatment on the base foil coated with the slurry and the mold clamping plate; the thickness of the slurry layer can reach the standard, the shape of the slurry layer is neat, and the formed electrode foil cannot be bent and deformed.
In addition, the proportion of the slurry components is reasonably adjusted, so that the slurry has proper viscosity, the thickness of the slurry layer can reach the standard, the shape of the slurry layer is neat, and the coating uniformity of the slurry layer is good.
Furthermore, by adding organic acid into the boiling liquid during boiling and properly prolonging the formation and pressure stabilization treatment time, the formation uniformity of the sintered layer in the thickness direction is effectively improved, and the electrical performance of the electrode foil is improved.
Drawings
FIG. 1 is a schematic view of a mold clamp plate;
FIG. 2 is a schematic diagram of a side view of the mold clamping plate after clamping the base foil;
FIG. 3 is a photograph of an electrode foil prepared in example 1;
FIG. 4 is a photograph of the slurry in comparative example 2 overflowing after coating;
FIG. 5 is a front photograph of the electrode foil prepared in comparative example 3;
fig. 6 is a side photograph of the electrode foil prepared in comparative example 3.
Description of reference numerals:
10. a mold clamp plate; 11. coating a window with slurry; 100. a base foil.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings, which illustrate embodiments of the present invention. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, as those skilled in the art will recognize without departing from the spirit and scope of the present invention.
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. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Referring to fig. 1 and 2, some embodiments of the present invention provide a method for preparing an electrode foil, including the following steps S100 to S400.
Step S100: the base foil 100 is sandwiched from opposite sides of the base foil 100 by mold clamping plates 10, the mold clamping plates 10 being provided with paste application windows 11.
In the conventional method for manufacturing the electrode foil, the slurry is directly coated on the opposite surfaces of the base foil 10 to form slurry layers, and then the subsequent drying, sintering and formation processes are performed. Since the slurry has a certain fluidity, the slurry may overflow after the slurry is coated on the base foil 10, so that the thickness of the slurry layer cannot meet the requirement, and the shape of the slurry layer is irregular, which affects the product quality of the electrode foil. This problem is particularly pronounced in bulk electrode foils having a thick slurry layer.
In order to solve the above problem, the present invention employs two mold clamping plates 10 to clamp the base foil 100 from opposite sides of the base foil 100, respectively, before applying the slurry on the base foil 10. The die clamping plate 10 is provided with the slurry coating window 11, and the slurry coating window 11 can be used for containing slurry coated on the base foil 100 and limiting the coated slurry so as to reduce the overflow of the slurry and enable the shape and the thickness of the slurry layer to meet the expected requirements. The structure of the mold clamping plate 10 is shown in fig. 1, and the schematic view of the mold clamping plate 10 clamping the base foil 100 is shown in fig. 2.
Through adopting mould splint 10 to follow basic unit's foil 100 of relative both sides centre gripping basic unit's foil 100 respectively, can carry on spacingly to thick liquids through thick liquids coating window 11 on the mould splint 10, reduce the excessive of thick liquids, make the shape on thick liquids layer keep for the shape of thick liquids coating window 11, and then also can guarantee the thickness on thick liquids layer.
Specifically, the shape of the slurry application window 11 on the mold splint 10 may be set according to the shape of the desired slurry layer; the thickness of the slurry coating window 11 can also be set according to the thickness of the slurry layer to be obtained, and the thickness of the slurry coating window 11 should be greater than or equal to the thickness of the slurry layer. The number of the size application windows 11 on the mold clamping plate 10 can be specifically set according to actual production needs.
Step S200: the slurry is applied in the slurry application windows 11 on the opposite sides of the base layer foil 100 to form slurry layers.
After the base foil 100 is sandwiched from the opposite sides of the base foil 100 by the mold cramping plates 10, the slurry is coated in the slurry coating windows 11 of the opposite sides of the base foil 100, thereby forming slurry layers on the opposite sides of the base foil 100, respectively.
Specifically, the coating amount and thickness of the slurry layer may be set as needed. For the bulk electrode foil, the slurry layers on the opposite sides of the base foil 100 are generally applied to a thickness of 100 μm to 400 μm. That is, the coating thickness of the slurry layer on one surface of the base foil 100 is 100 μm to 400 μm.
In some of these embodiments, the application of the paste in the paste application windows 11 on opposite sides of the base foil 100 specifically comprises the steps of: first applying a paste in the paste application window 11 on one side of the base layer foil 100; then the base foil 100 is turned over together with the mold clamp 10 with the other side of the base foil 100 facing upwards; the slurry is applied in the slurry application window 11 on the surface (the upward side) of the base layer foil 100. In this manner, the slurry layer can be applied to the opposite sides of the base foil 100. By using the die chuck 10, the base foil 100 can be made to better maintain its shape during the inversion process after the application of the slurry to one side thereof.
In some of the examples, the slurry used comprises the following components in weight percent: 40-60% of aluminum powder, 20-55% of solvent, 0.1-10% of ethyl cellulose and 0.1-10% of acrylic resin. Wherein the solvent is one or two of ethyl acetate and diethylene glycol butyl ether; ethyl cellulose is used as a binder, so that the aluminum powder and the base foil 100 can be well bonded together; the acrylic resin is used as a pore-expanding agent, so that the porosity of a sintered layer formed after the slurry layer is sintered can be expanded.
The preparation method of the slurry comprises the following steps: mixing aluminum powder, solvent, ethyl cellulose and acrylic resin according to a ratio, and then homogenizing in a homogenizer to completely and uniformly mix the raw materials.
By adopting the raw materials to form the slurry, the slurry has proper viscosity, the overflow problem of the slurry in the slurry layer is further solved, the thickness and the shape of the slurry layer are more favorably ensured, and the slurry layer with uniform thickness can be formed. If the viscosity of the slurry is too low, the slurry layer is easy to overflow, and the thickness and the shape of the slurry layer are not kept favorably; if the viscosity of the slurry layer is too high, the base foil 100 is easily deformed during the coating process, resulting in uneven slurry coating.
It is understood that the mass percentage content of the aluminum powder in the slurry can be, but is not limited to, 40%, 45%, 50%, 55%, 60%; the mass percentage content of the solvent can be, but is not limited to, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%; the content of ethyl cellulose in percentage by mass may be, but is not limited to, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%; the acrylic resin may be contained in an amount of, but not limited to, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10% by mass.
Step S300: the base foil 100 coated with the slurry is subjected to a drying process and a sintering process together with the mold cramp plate 10 to form sintered layers on the opposite sides of the base foil 100, resulting in an unformed foil.
After the slurry is applied to the base foil 100, the base foil 100 and the mold cramp 10 are subjected to a drying process together to remove the solvent in the slurry layer; and then sintering treatment is carried out, and residual solvent and binder in the slurry layer are removed to form a sintering layer with larger porosity. Specifically, the temperature and the drying time of the drying treatment can be determined according to the kind and the amount of the solvent actually used.
In some embodiments, the sintering process specifically comprises the steps of: firstly, degreasing the dried unformed foil and a mold clamping plate 10 for 1 to 6 hours in a vacuum sintering furnace at the temperature of between 200 and 400 ℃ under the protection of inert gas; then sintering at 560-660 ℃ for 1-24 h. Wherein, the degreasing treatment mainly can remove the residual solvent and binder after drying; the sintering process can partially melt the surface of the aluminum powder and form better bonding with the base foil.
It is understood that the temperature of the degreasing treatment can be, but is not limited to, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃, and the time of the degreasing treatment can be, but is not limited to, 1h, 2h, 3h, 4h, 5h, 6h; the temperature of the sintering treatment can be, but is not limited to, 560 ℃, 580 ℃, 600 ℃, 620 ℃, 640 ℃ and 660 ℃; the time of the sintering treatment can be but is not limited to 1h, 2h, 5h, 8h, 10h, 12h, 15h, 18h, 20h, 22h and 24h; the inert gas may be argon.
In some of the embodiments, the sintered layers on the opposite sides of the base layer foil 100 each have a thickness of 100 μm to 400 μm, and the electrode foil formed is a bulk electrode foil.
Step S400: the unformed foil is subjected to chemical conversion treatment together with the mold clamp 10 to obtain an electrode foil.
After the non-formed foil is obtained by the sintering process, the manufacturing method of the present invention continues to perform the formation process of the non-formed foil together with the mold cramping plate 10, and forms a layer of oxide film on the surface of the aluminum particles in the sintered layer by the formation process.
In some of these embodiments, the formation process includes the steps of: firstly, putting unformed foil and a mold clamping plate 10 into an aqueous solution of organic acid, and carrying out water boiling treatment at the temperature of 95-100 ℃ for 15-40 min; the boiled, unformed foil is then subjected to a multi-stage formation process with the mold clamp 10. The organic acid may be citric acid, adipic acid, azelaic acid, etc.
Specifically, the specific steps of the multistage formation treatment are as follows:
first-stage formation: putting the boiled unformed foil and the mold clamp plate 10 into the forming solution together, and heating at 83-93 ℃ under 450-520V voltage of 0.5A/cm 3 ～2.5A/cm 3 Under the current, stabilizing the voltage for 3000-7500 s; to preliminarily form an oxide film on the surface of the aluminum particles;
primary heat treatment: treating the unformed foil and the die clamp plate 10 together at the temperature of 350-550 ℃ for 1-5 min; so that the part where the compact oxide film is not formed is cracked, the formation liquid can more easily enter the inside of the sintering layer, and the crystal form of the oxide film can be converted;
secondary formation: putting the unformed foil and the die clamp plate 10 into the forming solution together, and heating at 83-93 ℃ under 450-520V voltage of 0.5A/cm 3 ～2.5A/cm 3 Under the current, the voltage stabilization treatment is carried out for 500-1500 s; so as to repair the oxide film and simultaneously form the oxide film on the sintering layer closer to the inside;
and (3) phosphoric acid treatment: placing the unformed foil and the die clamping plate 10 into a phosphoric acid solution with the conductivity of 25000 mu s/cm-45000 mu s/cm together, and treating for 5 min-10 min at the temperature of 55-70 ℃; the unstable hydrated film is dissolved, so that a stable oxide film is conveniently formed in the subsequent process, and the stability of the electrode foil is improved;
carrying out three-stage formation: putting the unformed foil and the die clamp plate 10 into a forming solution together, and heating at 83-93 ℃, 450-520V and 0.5A/cm 3 ～2.5A/cm 3 Under the current, the voltage stabilization treatment is carried out for 500-1500 s; to repair the defective oxide film while allowing the sintered layer closer to the inside to form an oxide film;
secondary heat treatment: treating the unformed foil and the die clamp plate 10 together at the temperature of 350-550 ℃ for 1-5 min; so that the part without the compact oxide film is cracked, the formed liquid can enter the inside of the sintering layer more easily, and the crystal form of the oxide film can be converted;
quaternization into: putting the unformed foil and the die clamp plate 10 into a forming solution together, and heating at 83-93 ℃, 450-520V and 0.5A/cm 3 ～2.5A/cm 3 Under the current, the voltage stabilization treatment is carried out for 500-1500 s; to repair the defective oxide film while allowing the sintered layer closer to the inside to form an oxide film;
ammonium dihydrogen phosphate treatment: putting the unformed foil and the die clamping plate 10 into ammonium dihydrogen phosphate solution with the concentration of 1 g/L-3 g/L, and treating for 2 min-8 min at the temperature of 55-70 ℃; phosphate radical occupies active sites of water molecules combined with the oxide film, and the damage of water to the oxide film is avoided.
Because the coating layer of the bulk electrode foil is thick, if the sintered layer after sintering does not have sufficient porosity, the formation liquid cannot enter one side (i.e., the inner side of the sintered layer) close to the base layer foil 100 along with the growth of the oxide film in the formation process, and then the oxide film cannot well grow on the aluminum balls in the sintered layer close to one side of the base layer foil 100, so that the sintered layer is not uniform in the thickness direction, and the bulk electrode foil cannot reach the expected withstand voltage value.
In order to solve the above problems, the manufacturing method of the present invention includes a formation processing step of subjecting an unformed foil and the mold clamp 10 to a water boiling process in an aqueous solution of an organic acid, and adding an organic acid to the water boiling solution to adjust the water boiling solution to be weakly acidic, thereby reducing the rate of hydration reaction, facilitating the formation of a uniform hydrated layer in the sintered layer, and making the sintered layer more uniform in the thickness direction. Combined with the appropriate extension of the voltage stabilization treatment time in the subsequent multi-stage formation step (longer compared with the traditional method), the sintering layer can be formed into a uniform oxide film in the thickness direction.
In addition, when the conventional manufacturing method applies the slurry layer on the second surface of the base foil 100, the base foil 100 may be bent downward to some extent by the gravity of the slurry layer on the first surface, resulting in non-uniform thickness of the slurry layers on both sides of the base foil 100. In this way, in the formation step, the degree of oxide film formation in the sintered layers on both sides is not uniform, and the pressing force of the oxide film against the base layer foil 100 is different, which leads to bending deformation of the bulk electrode foil.
In the preparation method of the present invention, the die holder 10 is always used to hold the foil sheet for operation from the slurry coating and drying process to the formation process, and the force applied to the base foil 100 by the die holder 10 can reduce the degree of downward bending of the base foil 100 when the slurry layer is coated on the second surface of the base foil 100, so that the thicknesses of the slurry layers on both sides of the base foil 100 are substantially the same. In this way, in the formation step, the bulk electrode foil does not bend and deform due to the difference in the pressing force of the oxide films on both sides against the base layer foil 100.
Specifically, after each of the formation treatment, the phosphoric acid treatment and the ammonium dihydrogen phosphate treatment, a water washing step is provided to wash off the excess agent on the foil. In the above-mentioned chemical conversion treatments, the chemical conversion solution used may be an aqueous boric acid solution having a concentration of 50g/L to 100 g/L.
In general, the invention enables the slurry to have proper viscosity by reasonably adjusting the component proportion of the slurry; adjusting the preparation process, and clamping two surfaces of the base foil 100 by using the mold clamping plates 10 all the time in the steps of slurry coating, drying treatment, sintering treatment and formation treatment; the structural design is carried out on the mold clamping plate 10, and a slurry coating window 11 is arranged on the mold clamping plate 10; by combining the slurry component adjustment, the preparation process adjustment and the mold structure design, the thickness of the slurry layer can reach the standard, the shape of the slurry layer is neat, and the formed electrode foil cannot be bent and deformed; by adding organic acid during boiling and properly prolonging the formation pressure stabilization treatment time, the formation uniformity of the sintering layer in the thickness direction is effectively improved. By combining the technical means, the product quality of the electrode foil is effectively improved.
The electrode foil prepared by the invention can be used as an electrode of an aluminum electrolytic capacitor, and particularly can be used as an anode of the aluminum electrolytic capacitor.
The present invention will be further described with reference to specific examples and comparative examples, which should not be construed as limiting the scope of the present invention.
Example 1:
mixing aluminum powder, solvent (ethyl acetate and diethylene glycol monobutyl ether), ethyl cellulose and acrylic resin, and homogenizing in a homogenizer to obtain slurry. Wherein the mass content of the aluminum powder is 40%, the mass content of the ethyl acetate is 48%, the mass content of the diethylene glycol butyl ether is 6%, the mass content of the ethyl cellulose is 3%, and the mass content of the acrylic resin is 3%.
Arranging two mould clamping plates 10, wherein the mould clamping plates 10 are provided with slurry coating windows 11; the base foil 100 is sandwiched between two mold clamping plates 10 and fixed prior to slurry application; then coating the slurry in the slurry coating window 11 on one side of the base foil 100 to form a slurry layer; turning over the base foil 100 and the mold clamp plate 10 together, and coating slurry in the slurry coating window 11 on the other surface of the base foil 100 to form a slurry layer; the mold cramp 10 after coating the slurry is dried together with the base foil 100.
Putting the dried mold clamping plate 10 and the base layer foil 100 into a vacuum sintering furnace, and carrying out degreasing treatment for 1h at 200 ℃ under the protection of inert gas; then degreasing for 1h at 400 ℃; then sintering for 6h at 630 ℃.
The sintered mold clamp 10 and the base foil 100 are boiled in water at 95 ℃ for 20min, and citric acid is added to the boiled liquid to adjust the pH of the boiled liquid to 5.
First-stage formation: the mold clamping plate 10 and the base foil 100 are put together in a forming liquid for forming treatment. The formation solution is 80g/L boric acid aqueous solution, the formation temperature is 88 ℃, the voltage is 450V, and the current is 0.75A/cm 3 The voltage stabilization time is 5500s; and washing with water after the formation is finished.
Primary heat treatment: the mold splint 10 and the base foil 100 are placed together in a heat treatment furnace to be heat-treated. The heat treatment temperature is 500 deg.C, and the time is 2min.
Secondary formation: the formation solution is 80g/L boric acid aqueous solution, the formation temperature is 88 ℃, the voltage is 450V, and the current is 0.75A/cm 3 The voltage stabilization time is 1000s; and washing with water after the formation is finished.
And (3) phosphoric acid treatment: the temperature is 60 ℃, the conductivity of the phosphoric acid solution is 25000 mu s/cm-60000 mu s/cm, and the time is 7min; and washing with water after the treatment is finished.
Carrying out three-stage formation; the mold clamping plate 10 and the base foil 100 are put together in a forming liquid for forming treatment. The formation solution is 80g/L boric acid aqueous solution, the formation temperature is 88 ℃, the voltage is 450V, and the current is 0.75A/cm 3 The voltage stabilization time is 1000s; and washing with water after the formation is finished.
Secondary heat treatment: the mold cramp plate 10 and the base foil 100 are put together in a heat treatment furnace to be heat-treated. The heat treatment temperature is 500 deg.C, and the time is 2min.
Carrying out four-stage formation: the mold clamping plate 10 and the base foil 100 are put together in a forming liquid for forming treatment. The formation solution is 80g/L boric acid aqueous solution, the formation temperature is 88 ℃, the voltage is 450V, and the current is 0.75A/cm 3 The voltage stabilization time is 1000s; and washing with water after the formation is finished.
Ammonium dihydrogen phosphate treatment: the mold jaws 10 and the base foil 100 are treated together in a solution of ammonium dihydrogen phosphate. The temperature is 60 ℃, the concentration of ammonium dihydrogen phosphate is 3g/L, and the treatment time is 4min; and after the treatment is finished, washing with water, and removing the template clamp 10 to obtain the electrode foil.
In the process of preparing the electrode foil, the slurry layer can reach the expected thickness, the slurry layer does not overflow, the shape is neat, and the electrode foil does not bend and deform after being formed. A photograph of the front surface of the prepared electrode foil is shown in fig. 3. And (3) carrying out performance test on the prepared electrode foil by using an LCR digital bridge, wherein the test frequency is 120Hz, and the electrolyte is ammonium pentaborate. Specific test results are shown in table 1.
Example 2:
this example was prepared essentially the same as example 1 except that the slurry composition was different: in the example, the mass content of the aluminum powder in the slurry was 40%, the mass content of the ethyl acetate was 54%, the mass content of the ethyl cellulose was 3%, and the mass content of the acrylic resin was 3%.
In the process of preparing the electrode foil, the slurry layer can reach the expected thickness, the slurry layer does not overflow and is neat in shape, and the electrode foil is not bent and deformed after being formed. The prepared electrode foil was subjected to a performance test using an LCR digital bridge under the same test conditions as in example 1. The specific test results are shown in table 1.
Example 3:
this example was prepared essentially identically to example 1, except that the slurry was of a different composition: in the example, the mass content of the aluminum powder in the slurry was 60%, the mass content of ethyl acetate was 34%, the mass content of ethyl cellulose was 3%, and the mass content of the acrylic resin was 3%.
In the process of preparing the electrode foil, the slurry layer can reach the expected thickness, the slurry layer does not overflow and is neat in shape, and the electrode foil is not bent and deformed after being formed. The prepared electrode foil was subjected to a performance test using an LCR digital bridge under the same test conditions as in example 1. Specific test results are shown in table 1.
Example 4:
this example was prepared essentially the same as example 1 except that the slurry composition was different: in the example, the mass content of the aluminum powder in the slurry is 40%, the mass content of the ethyl acetate is 52.8%, the mass content of the ethyl cellulose is 4.2%, and the mass content of the acrylic resin is 3%.
In the process of preparing the electrode foil, the slurry layer can reach the expected thickness, the slurry layer does not overflow and is neat in shape, and the electrode foil is not bent and deformed after being formed. The prepared electrode foil was subjected to a performance test using an LCR digital bridge under the same test conditions as in example 1. Specific test results are shown in table 1.
Comparative example 1:
the comparative example was prepared essentially the same as example 1, except that the slurry was of a different composition: in the example, the mass content of the aluminum powder in the slurry was 40%, the mass content of ethyl acetate was 51%, the mass content of diethylene glycol butyl ether was 6%, the mass content of ethyl cellulose was 3%, and no acrylic resin was added.
In the process of preparing the electrode foil by the comparative example, the slurry layer can reach the expected thickness, the slurry layer does not overflow, the shape is neat, and the electrode foil is not bent and deformed after being formed. The prepared electrode foil was subjected to a performance test using an LCR digital bridge under the same test conditions as in example 1. Specific test results are shown in table 1.
Comparative example 2:
the preparation method of this comparative example is different from that of example 1 in the composition of the slurry: in the comparative example, the mass content of aluminum powder was 30%, the mass content of ethyl acetate was 56%, the mass content of diethylene glycol butyl ether was 7%, the mass content of ethyl cellulose was 3.5%, and the mass content of acrylic resin was 3.5%.
In the process of preparing the electrode foil according to the comparative example, the homogenized slurry is too thin, the slurry layer overflows seriously during coating, and the slurry layer cannot reach the expected thickness and shape. The photograph of the slurry after coating is shown in fig. 4. No subsequent steps are performed after the slurry layer is applied.
Comparative example 3:
the comparative example was prepared essentially the same as example 1 except that: after the slurry layer is formed by coating the slurry on the mold cramping plate 10, the mold cramping plate 10 is removed, and then the subsequent steps of drying, sintering, and forming are performed without providing the mold cramping plate 10.
In the preparation method of the comparative example, the electrode foil is subjected to severe bending deformation in the formation process. Fig. 5 shows a front photograph and fig. 6 shows a side photograph of the electrode foil after formation. As can be seen from fig. 5 and 6, the formed electrode foil has severe bending deformation due to the absence of the template jig 10. The electrode foil was not subjected to a performance test.
TABLE 1 Performance parameters of the electrode foils of the examples and comparative examples
| Examples/comparative examples | Pressure resistance value (V) | Capacity (. Mu.F/cm) 2 ) | Loss of power | Bulk foil thickness (μm) |
| Example 1 | 501 | 37.6 | 0.10 | 425 |
| Example 2 | 511 | 32.5 | 0.09 | 416 |
| Example 3 | 482 | 40.3 | 0.13 | 422 |
| Example 4 | 466 | 39.5 | 0.26 | 423 |
| Comparative example 1 | 480 | 22.1 | 0.11 | 418 |
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (10)
1. The preparation method of the electrode foil is characterized by comprising the following steps of:
clamping the base foil from opposite sides of the base foil with mold clamping plates, the mold clamping plates having slurry coating windows;
coating slurry in the slurry coating windows on the two opposite sides of the base foil to form slurry layers;
carrying out drying treatment and sintering treatment on the base foil coated with the slurry and the mold clamping plate together to form sintered layers on two opposite sides of the base foil to obtain an unformed foil; and
and carrying out chemical conversion treatment on the unformed foil and the die clamping plate together to obtain the electrode foil.
2. The method for preparing an electrode foil as claimed in claim 1, wherein the step of coating the slurry in the slurry coating windows of the opposite sides of the base foil comprises the steps of:
coating a slurry in the slurry coating window on one side of the base foil, turning the base foil and the mold clamp plate together so that the other side of the base foil faces upward, and then coating a slurry in the slurry coating window on the other side of the base foil.
3. The method for producing an electrode foil as claimed in claim 1, wherein the formation treatment comprises the steps of:
putting the unformed foil and the mold clamping plate into an organic acid aqueous solution, and boiling for 15-40 min at 95-100 ℃; and
subjecting the un-formed foil after poaching and the mold clamp plate together to a multi-stage formation process.
4. The method for producing an electrode foil as claimed in claim 3, wherein the multistage formation process comprises the steps of:
first-stage formation: putting the boiled unformed foil and the mold clamping plate into a forming solution together, and heating at 83-93 ℃ under 450-520V voltage of 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 3000-7500 s under current;
primary heat treatment: treating the unformed foil and the die clamping plate together at the temperature of 350-550 ℃ for 1-5 min;
secondary formation: putting the unformed foil and the die clamping plate into a forming solution together, and heating at 83-93 ℃, 450-520V voltage and 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 500-1500 s under current;
and (3) phosphoric acid treatment: placing the unformed foil and the die clamping plate together in a phosphoric acid solution with the conductivity of 25000 mu s/cm-45000 mu s/cm, and treating for 5 min-10 min at the temperature of 55-70 ℃;
carrying out three-stage formation: putting the unformed foil and the die clamping plate into a forming solution together, and heating at 83-93 ℃, 450-520V voltage and 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 500-1500 s under the current;
secondary heat treatment: treating the unformed foil and the mold clamp plate together at 350-550 ℃ for 1-5 min;
quaternization into: placing the unformed foil and the mold clamp plate into a forming liquid together at 83-93 deg.CTemperature, 450V-520V voltage, 0.5A/cm 3 ～2.5A/cm 3 Stabilizing the voltage for 500-1500 s under the current; and
ammonium dihydrogen phosphate treatment: putting the unformed foil and the die clamping plate into ammonium dihydrogen phosphate solution with the concentration of 1 g/L-3 g/L, and treating for 2 min-8 min at the temperature of 55-70 ℃.
5. The method of manufacturing an electrode foil according to claim 1, wherein the sintering process includes the steps of:
and (3) treating the dried unformed foil and the mold clamping plate together for 1 to 6 hours at the temperature of between 200 and 400 ℃ under the protection of inert gas, and then treating for 1 to 24 hours at the temperature of between 560 and 660 ℃.
6. The method for producing an electrode foil as claimed in any one of claims 1 to 5, wherein the slurry comprises, in weight percent: 40-60% of aluminum powder, 20-55% of solvent, 0.1-10% of ethyl cellulose and 0.1-10% of acrylic resin.
7. The method of manufacturing an electrode foil according to claim 6, wherein the solvent is one or both of ethyl acetate and diethylene glycol butyl ether.
8. An electrode foil comprising a base foil and sintered layers provided on opposite sides of the base foil, the electrode foil being produced by the production method according to any one of claims 1 to 7.
9. The electrode foil according to claim 8, wherein the sintered layers on the opposite sides of the base foil each have a thickness of 100 to 400 μm.
10. A capacitor, wherein at least one electrode of the capacitor is the electrode foil according to claim 8 or 9.
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