CN117594359A - Aluminum electrolytic capacitor anode sintered foil and preparation method thereof - Google Patents
Aluminum electrolytic capacitor anode sintered foil and preparation method thereof Download PDFInfo
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- CN117594359A CN117594359A CN202410072019.0A CN202410072019A CN117594359A CN 117594359 A CN117594359 A CN 117594359A CN 202410072019 A CN202410072019 A CN 202410072019A CN 117594359 A CN117594359 A CN 117594359A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 239000011888 foil Substances 0.000 title claims abstract description 104
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 83
- 239000003990 capacitor Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 67
- 238000000576 coating method Methods 0.000 claims abstract description 52
- 239000002131 composite material Substances 0.000 claims abstract description 51
- 239000011248 coating agent Substances 0.000 claims abstract description 46
- 239000002002 slurry Substances 0.000 claims abstract description 46
- 238000005245 sintering Methods 0.000 claims abstract description 41
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 33
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000010936 titanium Substances 0.000 claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 16
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- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
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- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 3
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- 229940116411 terpineol Drugs 0.000 claims description 3
- 239000001069 triethyl citrate Substances 0.000 claims description 3
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 claims description 3
- 235000013769 triethyl citrate Nutrition 0.000 claims description 3
- 229940036248 turpentine Drugs 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000010408 film Substances 0.000 description 41
- 229910052751 metal Inorganic materials 0.000 description 25
- 239000002184 metal Substances 0.000 description 25
- 239000013077 target material Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 238000004544 sputter deposition Methods 0.000 description 7
- 125000004429 atom Chemical group 0.000 description 6
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- 239000011261 inert gas Substances 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 238000004070 electrodeposition Methods 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The present disclosure provides an aluminum electrolytic capacitor anode sintered foil and a preparation method thereof, and relates to the technical field of capacitors. The preparation method of the anode sintered foil of the aluminum electrolytic capacitor comprises the following steps: spherical aluminum powder is used as an anode, a titanium target is used as a cathode, and an aluminum-titanium composite powder is generated in a magnetron sputtering mode, and a titanium film is coated on the surface of the aluminum-titanium composite powder; preparing target slurry based on aluminum-titanium composite powder, coating the target slurry on two side surfaces of an aluminum foil substrate, and drying to obtain the aluminum foil substrate with powder stacking layers on the two side surfaces; sintering the aluminum foil base material with powder stacking layers on the surfaces of two sides, and performing formation energizing treatment after sintering to prepare the anode sintered foil of the aluminum electrolytic capacitor. The present disclosure can improve the quality of aluminum electrolytic capacitor anode sintered foil.
Description
Technical Field
The disclosure relates to the technical field of capacitors, in particular to a preparation method of an aluminum electrolytic capacitor anode sintered foil and the aluminum electrolytic capacitor anode sintered foil.
Background
Electrolytic capacitors, which are important devices in the electronics industry, have been widely used in many fields such as aerospace, rail transit, industrial control, electronic circuits, new energy sources, and the like. The anode sintered foil is one of key elements of the electrolytic capacitor, and the quality of the anode sintered foil is related to the service life of the electrolytic capacitor, thereby influencing the service life of the whole electronic equipment.
The sintered foil for the aluminum electrolytic capacitor is characterized in that high-purity aluminum powder with purity up to 99.99% is directly sintered on the surface of a high-purity electronic aluminum foil, and a porous powder layer structure is obtained on the surface of the high-purity electronic aluminum foil after energized treatment, so that the aims of expanding the opposing area of the capacitor and increasing the capacitance of the capacitor are fulfilled. However, since the dielectric constant of the surface aluminum oxide film provided in the powder layer is low, further increase in the capacitance of the sintered foil for aluminum electrolytic capacitor is limited by the dielectric constant of the surface aluminum oxide film provided in the powder layer, subject to the limitation that the increase in the opposing area approaches the theoretical value.
In order to improve the performance of the sintered foil for aluminum electrolytic capacitors, the high dielectric metal or its oxide may be combined with an aluminum oxide film by a chemical solution deposition method. However, such methods generally suffer from poor film uniformity, resulting in poor foil quality.
It should be noted that the information disclosed in the above background section is only for enhancing understanding of the background of the present disclosure and thus may include information that does not constitute prior art known to those of ordinary skill in the art.
Disclosure of Invention
The purpose of the present disclosure is to provide a method for preparing an anode sintered foil of an aluminum electrolytic capacitor and an anode sintered foil of an aluminum electrolytic capacitor, so as to overcome the problem of poor quality of the anode sintered foil of the aluminum electrolytic capacitor at least to some extent.
According to a first aspect of the present disclosure, there is provided a method for preparing an anode sintered foil of an aluminum electrolytic capacitor, comprising: spherical aluminum powder is used as an anode, a titanium target is used as a cathode, and an aluminum-titanium composite powder is generated in a magnetron sputtering mode, and a titanium film is coated on the surface of the aluminum-titanium composite powder; preparing target slurry based on aluminum-titanium composite powder, coating the target slurry on two side surfaces of an aluminum foil substrate, and drying to obtain the aluminum foil substrate with powder stacking layers on the two side surfaces; sintering the aluminum foil base material with powder stacking layers on the surfaces of two sides, and performing formation energizing treatment after sintering to prepare the anode sintered foil of the aluminum electrolytic capacitor.
Alternatively, the bias voltage of the magnetron sputtering is 0V to 300V, the power is 100W to 400W, and the processing time is 0.2h to 3h.
Optionally, preparing the target slurry based on the aluminum-titanium composite powder includes: and uniformly mixing and dispersing the aluminum-titanium composite powder, the organic solvent and the functional material to prepare the target slurry.
Optionally, the organic solvent is one or more of ethylene glycol, polyethylene glycol, terpineol, turpentine and triethyl citrate.
Optionally, the functional material is one or more of a binder, a dispersing agent and a film forming agent; the binder is one or more of polyvinyl acetate, polyethylene, carboxyethyl cellulose, phenolic resin and urea resin; the dispersing agent is one or more of methyl cellulose, hydroxypropyl methyl cellulose and polyvinyl alcohol; the film forming agent is one or more of benzyl alcohol, ethylene glycol butyl ether and polyethylene glycol.
Optionally, in the case that the functional material is formed by mixing a binder, a dispersant and a film forming agent, uniformly mixing and dispersing the aluminum-titanium composite powder, the organic solvent and the functional material to prepare the target slurry, wherein the method comprises the following steps of: organic solvent, binder, dispersant and film forming agent according to (80-90): (0.5-10): (0.1-5): (0.1-5) mixing to produce a preformed solvent; and (3) mixing the aluminum-titanium composite powder with a prefabricated solvent according to the following steps: (4-2) mixing to prepare the objective slurry.
Optionally, applying the target slurry to both side surfaces of the aluminum foil substrate includes: the target sizing agent is coated on the two side surfaces of the aluminum foil substrate by any one coating mode of screw roll coating, screen printing and doctor blade coating.
Optionally, sintering the aluminum foil substrate having powder build-up layers on both surfaces comprises: the sintering of the aluminum foil substrate having powder deposit layers on both side surfaces was performed by raising the temperature from room temperature to 400 to 650 ℃.
Optionally, the atmosphere environment of sintering is any one of air, vacuum, inert atmosphere and reducing atmosphere; the inert atmosphere is nitrogen atmosphere, argon atmosphere or mixed atmosphere of nitrogen and argon; the reducing atmosphere is hydrogen atmosphere or alkane atmosphere.
According to a second aspect of the present disclosure, there is provided an aluminum electrolytic capacitor anode sintered foil produced by any one of the above production methods.
In the scheme of the embodiment of the disclosure, on one hand, the magnetron sputtering technology is adopted to modify the surface of spherical aluminum powder to obtain a uniformly distributed high-dielectric metal film, and then the aluminum electrolytic capacitor anode sintered foil with high specific capacitance can be obtained through the processes of slurry preparation, coating, sintering, formation energization and the like. On the other hand, the magnetron sputtering technology is adopted in the method, the uniformity of the coating film is good, and the quality of the foil material can be improved. On the other hand, in the preparation process of the present disclosure, a large amount of organic solvents are not used, and electrochemical corrosion is not performed, so that the step of removing residual acid radical ions after the etching process is omitted, the problem of acid liquor pollution caused by the conventional process is solved, the production process is simplified, and the industrialization cost is saved.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the disclosure and together with the description, serve to explain the principles of the disclosure. It will be apparent to those of ordinary skill in the art that the drawings in the following description are merely examples of the disclosure and that other drawings may be derived from them without undue effort.
Fig. 1 schematically shows a flowchart of a method of manufacturing an aluminum electrolytic capacitor anode sintered foil according to an embodiment of the present disclosure.
Fig. 2 shows a scanning electron microscope image of a cross section of an aluminum titanium composite powder according to some embodiments of the present disclosure.
Fig. 3 illustrates a schematic diagram of preparing a target slurry according to some embodiments of the present disclosure.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. However, the exemplary embodiments may be embodied in many forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the example embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a thorough understanding of embodiments of the present disclosure. One skilled in the relevant art will recognize, however, that the aspects of the disclosure may be practiced without one or more of the specific details, or with other methods, processes, steps, etc. In other instances, well-known technical solutions have not been shown or described in detail to avoid obscuring aspects of the present disclosure.
Furthermore, the drawings are merely schematic illustrations of the present disclosure and are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and thus a repetitive description thereof will be omitted. The flow diagrams depicted in the figures are exemplary only and not necessarily all steps are included. For example, some steps may be decomposed, and some steps may be combined or partially combined, so that the order of actual execution may be changed according to actual situations.
The anode sintered foil of the aluminum electrolytic capacitor is prepared by sintering high-purity aluminum powder with purity up to 99.99% on the surface of a high-purity electronic aluminum foil, and obtaining a porous powder layer structure on the surface of the high-purity electronic aluminum foil after formation energization treatment, so that the aims of expanding the opposite area of a capacitor and increasing the capacitance of the capacitor are fulfilled.
However, since the dielectric constant of the surface aluminum oxide film provided in the powder layer is low, further increase in the capacitance of the sintered foil of the anode of the electrolytic capacitor is limited by the dielectric constant of the surface aluminum oxide film provided in the powder layer, subject to the limitation that the increase in the opposing area approaches the theoretical value.
To solve this problem, the high dielectric metal or its oxide may be combined with the aluminum oxide film by a chemical solution deposition method. The common methods include sol-gel method, hydrolytic deposition method, electrochemical deposition method, etc., and organic solvents are used in large amounts during the introduction process, which is difficult in terms of environmental protection. In addition, the thickness of the composite film prepared by the chemical solution deposition method is difficult to control, the uniformity is poor, and the difficulty in improving the withstand voltage of the capacitor exists.
In view of this, the embodiments of the present disclosure provide a novel method of manufacturing an anode sintered foil of an aluminum electrolytic capacitor, which is independent of a chemical solution deposition method, and is capable of controlling the thickness of a composite aluminum film. The method adopts a magnetron sputtering process to modify the surface of high-purity spherical aluminum powder, so that metal atoms of an anode metal target material are uniformly attached to the surface of the high-purity spherical aluminum powder which uniformly rolls in a cathode vibration disk through sputtering, uniformly distributed high-dielectric metal films are obtained on the surface of the high-purity spherical aluminum powder through adjusting magnetron sputtering process parameters, and then the anode sintered foil of the aluminum electrolytic capacitor with high specific capacitance is obtained through processes of slurry preparation, coating, sintering, formation energization and the like. In the embodiment of the present disclosure, a high dielectric metal thin film uniformly distributed on the surface of the high purity spherical aluminum powder is obtained, and it is noted that the obtained film layer is uniform, and thus, the performance uniformity, which is an effect that cannot be achieved by the electroless plating method, may be caused.
Fig. 1 schematically shows a flowchart of a method of manufacturing an aluminum electrolytic capacitor anode sintered foil according to an embodiment of the present disclosure. Referring to fig. 1, the preparation method may include the steps of:
s12, using spherical aluminum powder as an anode and a titanium target as a cathode, and generating aluminum-titanium composite powder in a magnetron sputtering mode, wherein a titanium film is coated on the surface of the aluminum-titanium composite powder.
In the exemplary embodiment of the present disclosure, the aluminum powder used is spherical aluminum powder, and thus, gaps may be generated after the aluminum powder is stacked, so as to meet the subsequent process requirements and the preparation effect. Wherein the purity of the adopted spherical aluminum powder is more than 99.99%, and the particle size of the aluminum powder can be 1-10 μm.
In addition, the purity of the adopted metal titanium target material is also more than 99.99 percent.
Firstly, spherical aluminum powder can be led into a vibrating disk of a magnetron sputtering device to serve as an anode, a titanium target material serves as a cathode, and a coating chamber is vacuumized. Next, parameters such as the vibration frequency and the vibration amplitude of the anode, bias voltage, power, time and the like of the magnetron sputtering device can be adjusted to generate the aluminum-titanium composite powder, and the surface of the aluminum-titanium composite powder is coated with the titanium film.
Specifically, the bias voltage of the magnetron sputtering may be configured to 0V to 300V, the power may be configured to 100W to 400W, and the process time may be configured to 0.2h to 3h. Fig. 2 shows a scanning electron microscope image of a cross section of an aluminum titanium composite powder according to some embodiments of the present disclosure.
S14, preparing target slurry based on the aluminum-titanium composite powder, coating the target slurry on two side surfaces of the aluminum foil substrate, and drying to obtain the aluminum foil substrate with powder stacking layers on the two side surfaces.
After the aluminum-titanium composite powder is obtained, a target slurry, which is a slurry to be coated on an aluminum foil substrate, may be prepared based on the aluminum-titanium composite powder.
Specifically, the aluminum-titanium composite powder, the organic solvent and the functional material can be uniformly mixed and dispersed to prepare the target slurry.
The organic solvent can be one or more of ethylene glycol, polyethylene glycol, terpineol, turpentine and triethyl citrate.
The functional material can be one or more of a binder, a dispersing agent and a film forming agent.
As the binder, one or more of polyvinyl acetate, polyethylene, carboxyethyl cellulose, phenolic resin, urea resin may be mixed.
As the dispersant, one or more of methylcellulose, hydroxypropyl methylcellulose, and polyvinyl alcohol may be mixed.
For the film forming agent, one or more of benzyl alcohol, ethylene glycol butyl ether and polyethylene glycol can be mixed.
In an embodiment in which the functional material is mixed with a binder, a dispersant, and a film forming agent, a process of preparing the target slurry will be described with reference to fig. 3.
First, an organic solvent, a binder, a dispersant, and a film forming agent may be mixed to produce a preformed solvent.
Specifically, when mixing, the mass ratio of the organic solvent, the binder, the dispersant, and the film forming agent may be, for example, (80-90): (0.5-10): (0.1-5): (0.1-5).
Next, the aluminum-titanium composite powder may be mixed with a pre-prepared solvent to prepare a target slurry.
Specifically, when mixing, the mass ratio of the aluminum-titanium composite powder to the pre-prepared solvent may be, for example, (6-8): (4-2).
In the case where the target slurry has been prepared, the target slurry may be coated on both side surfaces of the aluminum foil substrate. Specifically, the target slurry can be coated on the two side surfaces of the aluminum foil substrate by any one of screw roll coating, screen printing and doctor blade coating. Wherein the thickness of the coated single face is controlled in the range of, for example, 20 μm to 100 μm.
It is understood that for a substrate, coating the target slurry on both side surfaces means coating the target slurry on one surface of the substrate and also coating the target slurry on the surface opposite to the surface.
In some embodiments of the present disclosure, the target coating may be simultaneously applied to both side surfaces of the aluminum foil substrate by means of an apparatus capable of simultaneously coating both sides of the substrate.
In other embodiments of the present disclosure, the target slurry may be coated on one surface of the aluminum foil substrate before being dried and then coated on the other surface of the aluminum foil substrate.
The aluminum foil substrate coated with the target slurry is dried to obtain the aluminum foil substrate with powder stacking layers on two side surfaces. Wherein, the drying process may include raising the temperature from room temperature to 100 ℃ to 250 ℃ and maintaining the temperature for 0.5 to 2 hours. This warming process may be a slow warming process.
S16, sintering the aluminum foil base material with the powder stacking layers on the surfaces of the two sides, and performing formation energizing treatment after sintering to prepare the anode sintered foil of the aluminum electrolytic capacitor.
According to some embodiments of the present disclosure, sintering of the aluminum foil substrate having powder deposit layers on both side surfaces may be performed by increasing the temperature from room temperature to 400 to 650 ℃, which may be a slow temperature increase process. In addition, for sintering, gradient sintering may also be performed at different temperature gradients, which is not limited by the present disclosure.
The atmosphere during sintering may be any of air, vacuum, inert atmosphere, and reducing atmosphere. The inert atmosphere according to some embodiments of the present disclosure may be a nitrogen atmosphere, an argon atmosphere, or a mixed atmosphere of nitrogen and argon, and the reducing atmosphere may be a hydrogen atmosphere or an alkane atmosphere.
After sintering, a formation energizing treatment may be performed to prepare an aluminum electrolytic capacitor anode sintered foil. The formation energizing treatment is to perform standardized formation energizing operation on the foil obtained by sintering according to an electronic industry standard SJ/T11140-2022. The present disclosure is not limited in this regard.
According to the preparation method of the anode sintered foil of the aluminum electrolytic capacitor, on one hand, the magnetron sputtering technology is adopted to modify the surface of spherical aluminum powder to obtain the uniformly distributed high-dielectric metal film, and then the anode sintered foil of the aluminum electrolytic capacitor with high specific capacitance can be obtained through the processes of slurry preparation, coating, sintering, formation energization and the like. On the other hand, the magnetron sputtering technology is adopted in the method, the uniformity of the coating film is good, and the quality of the foil material can be improved. On the other hand, in the preparation process of the present disclosure, a large amount of organic solvents are not used, and electrochemical corrosion is not performed, so that the step of removing residual acid radical ions after the etching process is omitted, the problem of acid liquor pollution caused by the conventional process is solved, the production process is simplified, and the industrialization cost is saved.
In order to better explain the details and effects of the preparation method of the anode sintered foil for the aluminum electrolytic capacitor of the present disclosure, examples and comparative examples of the present disclosure are described below.
Example 1
First, a raw material selection process is performed. Specifically, spherical aluminum powder is poured into a vibration disc of a magnetron sputtering device to be used as matrix powder, the average particle size of the spherical aluminum powder is 1-10 mu m, and the mass purity is more than 99.99%. Pure titanium target material is selected as a cathode, the quality and purity of the target material are also over 99.99 percent, and the coating chamber is vacuumized.
And secondly, executing a composite powder preparation process. Specifically, by adjusting the vibration frequency and amplitude of the anode, the parameters of the magnetron sputtering device are set as follows: and carrying out magnetron sputtering for 1h under the bias voltage of 100V and the power of 100W, so that metal atoms of the anode metal target material are uniformly attached to the surface of the high-purity spherical aluminum powder uniformly rolled in the cathode vibration disk through sputtering, and thus the composite aluminum powder with uniformly distributed high-dielectric metal films on the surface is obtained.
Third, a slurry preparation and coating process is performed. Specifically, organic solvent, binder, dispersant and film forming agent are mixed according to (80-90): (0.5-10): (0.1-5): (0.1-5) and mixing into a prefabricated solvent. The total addition amount of the composite aluminum powder and the prefabricated solvent are as follows (6-8): the mass ratio of (4-2) is mixed to form aluminum paste, namely the target paste. And (3) coating the slurry on two sides of the high-purity aluminum foil by adopting polish rod coating, screw rod rolling coating, screen printing or doctor blade coating to obtain a powder stacking layer formed by stacking composite powder. Wherein the thickness of the coated single side is 20 mu m to 100 mu m, and the thickness of the high-purity aluminum foil is 10 mu m to 100 mu m.
Fourth, a sintering curing process is performed. Specifically, the foil obtained in the third step is sintered and solidified, and the sintering and solidification are that the foil is heated to 600 ℃ from room temperature under the protection of inert gas, and the sintering and the heat preservation are carried out for 8 hours.
And fifthly, performing a formation enabling process. Specifically, the foil obtained in the fourth step is subjected to standardized formation enabling operation according to an electronic industry standard SJ/T11140-2022.
Comparative example one
First, a raw material selection process is performed. Specifically, spherical aluminum powder is poured into a vibration disc of a magnetron sputtering device to be used as matrix powder, the average particle size of the spherical aluminum powder is 1-10 mu m, and the mass purity is more than 99.99%. Pure titanium target material is selected as a cathode, the quality and purity of the target material are also over 99.99 percent, and the coating chamber is vacuumized.
And secondly, executing a composite powder preparation process. Specifically, by adjusting the vibration frequency and amplitude of the anode, the parameters of the magnetron sputtering device are set as follows: and carrying out magnetron sputtering for 1.5 hours under the bias voltage of 100V and the power of 100W, so that metal atoms of the anode metal target material are uniformly attached to the surface of the high-purity spherical aluminum powder which uniformly rolls in the cathode vibration disk through sputtering, and thus the composite aluminum powder with the uniformly distributed high-dielectric metal film on the surface is obtained.
Third, a slurry preparation and coating process is performed. Specifically, organic solvent, binder, dispersant and film forming agent are mixed according to (80-90): (0.5-10): (0.1-5): (0.1-5) and mixing into a prefabricated solvent. The total addition amount of the composite aluminum powder and the prefabricated solvent are as follows (6-8): the mass ratio of (4-2) is mixed to form aluminum paste, namely the target paste. And (3) coating the slurry on two sides of the high-purity aluminum foil by adopting polish rod coating, screw rod rolling coating, screen printing or doctor blade coating to obtain a powder stacking layer formed by stacking composite powder. Wherein the thickness of the coated single side is 20 mu m to 100 mu m, and the thickness of the high-purity aluminum foil is 10 mu m to 100 mu m.
Fourth, a sintering curing process is performed. Specifically, the foil obtained in the third step is sintered and solidified, and the sintering and solidification are that the foil is heated to 600 ℃ from room temperature under the protection of inert gas, and the sintering and the heat preservation are carried out for 8 hours.
And fifthly, performing a formation enabling process. Specifically, the foil obtained in the fourth step is subjected to standardized formation enabling operation according to an electronic industry standard SJ/T11140-2022.
Comparative example two
First, a raw material selection process is performed. Specifically, spherical aluminum powder is poured into a vibration disc of a magnetron sputtering device to be used as matrix powder, the average particle size of the spherical aluminum powder is 1-10 mu m, and the mass purity is more than 99.99%. Pure titanium target material is selected as a cathode, the quality and purity of the target material are also over 99.99 percent, and the coating chamber is vacuumized.
And secondly, executing a composite powder preparation process. Specifically, by adjusting the vibration frequency and amplitude of the anode, the parameters of the magnetron sputtering device are set as follows: and carrying out magnetron sputtering for 1.5 hours under the bias voltage of 100V and the power of 100W, so that metal atoms of the anode metal target material are uniformly attached to the surface of the high-purity spherical aluminum powder which uniformly rolls in the cathode vibration disk through sputtering, and thus the composite aluminum powder with the uniformly distributed high-dielectric metal film on the surface is obtained.
Third, a slurry preparation and coating process is performed. Specifically, organic solvent, binder, dispersant and film forming agent are mixed according to (80-90): (0.5-10): (0.1-5): (0.1-5) and mixing into a prefabricated solvent. The total addition amount of the composite aluminum powder and the prefabricated solvent are as follows (6-8): the mass ratio of (4-2) is mixed to form aluminum paste, namely the target paste. And (3) coating the slurry on two sides of the high-purity aluminum foil by adopting polish rod coating, screw rod rolling coating, screen printing or doctor blade coating to obtain a powder stacking layer formed by stacking composite powder. Wherein the thickness of the coated single side is 20 mu m to 100 mu m, and the thickness of the high-purity aluminum foil is 10 mu m to 100 mu m.
Fourth, a sintering curing process is performed. Specifically, the foil obtained in the third step is sintered and solidified, and the sintering and solidification are that the foil is heated to 610 ℃ from room temperature under the protection of inert gas, and the sintering and the heat preservation are carried out for 12 hours.
And fifthly, performing a formation enabling process. Specifically, the foil obtained in the fourth step is subjected to standardized formation enabling operation according to an electronic industry standard SJ/T11140-2022.
Comparative example three
First, a raw material selection process is performed. Specifically, spherical aluminum powder is poured into a vibration disc of a magnetron sputtering device to be used as matrix powder, the average particle size of the spherical aluminum powder is 1-10 mu m, and the mass purity is more than 99.99%. Pure titanium target material is selected as a cathode, the quality and purity of the target material are also over 99.99 percent, and the coating chamber is vacuumized.
And secondly, executing a composite powder preparation process. Specifically, by adjusting the vibration frequency and amplitude of the anode, the parameters of the magnetron sputtering device are set as follows: and carrying out magnetron sputtering for 2 hours under the bias voltage of 100V and the power of 200W, so that metal atoms of the anode metal target material are uniformly attached to the surface of the high-purity spherical aluminum powder uniformly rolled in the cathode vibration disk through sputtering, and the composite aluminum powder with the uniformly distributed high-dielectric metal film on the surface is obtained.
Third, a slurry preparation and coating process is performed. Specifically, organic solvent, binder, dispersant and film forming agent are mixed according to (80-90): (0.5-10): (0.1-5): (0.1-5) and mixing into a prefabricated solvent. The total addition amount of the composite aluminum powder and the prefabricated solvent are as follows (6-8): the mass ratio of (4-2) is mixed to form aluminum paste, namely the target paste. And (3) coating the slurry on two sides of the high-purity aluminum foil by adopting polish rod coating, screw rod rolling coating, screen printing or doctor blade coating to obtain a powder stacking layer formed by stacking composite powder. Wherein the thickness of the coated single side is 20 mu m to 100 mu m, and the thickness of the high-purity aluminum foil is 10 mu m to 100 mu m.
Fourth, a sintering curing process is performed. Specifically, the foil obtained in the third step is sintered and solidified, and the sintering and solidification are that the foil is heated to 620 ℃ from room temperature under the protection of inert gas, and the sintering and the heat preservation are carried out for 16 hours.
And fifthly, performing a formation enabling process. Specifically, the foil obtained in the fourth step is subjected to standardized formation enabling operation according to an electronic industry standard SJ/T11140-2022.
Comparative example four
First, a raw material selection process is performed. Specifically, spherical aluminum powder is poured into a vibration disc of a magnetron sputtering device to be used as matrix powder, the average particle size of the spherical aluminum powder is 1-10 mu m, and the mass purity is more than 99.99%. Pure titanium target material is selected as a cathode, the quality and purity of the target material are also over 99.99 percent, and the coating chamber is vacuumized.
And secondly, executing a composite powder preparation process. Specifically, by adjusting the vibration frequency and amplitude of the anode, the parameters of the magnetron sputtering device are set as follows: and carrying out magnetron sputtering for 3 hours under the bias voltage of 200V and the power of 300W, so that metal atoms of the anode metal target material are uniformly attached to the surface of the high-purity spherical aluminum powder uniformly rolled in the cathode vibration disk through sputtering, and the composite aluminum powder with the uniformly distributed high-dielectric metal film on the surface is obtained.
Third, a slurry preparation and coating process is performed. Specifically, organic solvent, binder, dispersant and film forming agent are mixed according to (80-90): (0.5-10): (0.1-5): (0.1-5) and mixing into a prefabricated solvent. The total addition amount of the composite aluminum powder and the prefabricated solvent are as follows (6-8): the mass ratio of (4-2) is mixed to form aluminum paste, namely the target paste. And (3) coating the slurry on two sides of the high-purity aluminum foil by adopting polish rod coating, screw rod rolling coating, screen printing or doctor blade coating to obtain a powder stacking layer formed by stacking composite powder. Wherein the thickness of the coated single side is 20 mu m to 100 mu m, and the thickness of the high-purity aluminum foil is 10 mu m to 100 mu m.
Fourth, a sintering curing process is performed. Specifically, the foil obtained in the third step is sintered and solidified, and the sintering and solidification are that the foil is heated to 650 ℃ from room temperature under the protection of inert gas, and the sintering and the heat preservation are carried out for 30 hours.
And fifthly, performing a formation enabling process. Specifically, the foil obtained in the fourth step is subjected to standardized formation enabling operation according to an electronic industry standard SJ/T11140-2022.
Comparative example five
First, a slurry preparation and coating process is performed. Specifically, organic solvent, binder, dispersant and film forming agent are mixed according to (80-90): (0.5-10): (0.1-5): (0.1-5) and mixing into a prefabricated solvent. High-purity spherical aluminum powder with an average particle diameter of 1 μm to 10 μm and a pre-prepared solvent according to (6-8): the mass ratio of (4-2) is mixed to form aluminum paste, namely the target paste. And (3) coating the slurry on two sides of the high-purity aluminum foil by adopting polish rod coating, screw rod rolling coating, screen printing or doctor blade coating to obtain a powder stacking layer formed by stacking composite powder. Wherein the thickness of the coated single side is 20 mu m to 100 mu m, and the thickness of the high-purity aluminum foil is 10 mu m to 100 mu m.
And secondly, performing a sintering and curing process. Specifically, the foil obtained in the first step is sintered and solidified, and the sintering and solidification are that the foil is heated to 600 ℃ from room temperature under the protection of inert gas, and the sintering and the heat preservation are carried out for 8 hours.
And thirdly, performing a formation enabling process. Specifically, the foil obtained in the second step is subjected to standardized formation enabling operation according to an electronic industry standard SJ/T11140-2022.
Samples after the formation and energization of the first, second, third, fourth and fifth examples were tested and their properties are shown in table 1.
TABLE 1
As can be seen from table 1, comparative example five is a sample not subjected to magnetron sputtering coating,the specific capacitance is low, 0.825 mu F/cm 2 The specific capacitances of the first and second, third and fourth examples were all 0.913. Mu.F/cm 2 In the above, it was explained that the uniformly distributed high dielectric metal thin film composite film layer obtained by magnetron sputtering can improve the specific capacitance.
However, the first example and the first, second, third and fourth examples are different in performance, and as the magnetron sputtering power and sputtering time are increased, the film thickness is also increased, and the specific capacitance is also increased. The pressure resistance and the bending times of the third and fourth comparative examples are slightly reduced, because the magnetron sputtering time is too long, which results in the film thickness being too large, and the bonding strength during sintering is slightly affected.
In summary, the specific capacitance of the sintered foil prepared by the preparation method of the embodiment of the disclosure is obviously improved compared with that of the conventional sintered foil, and the better bending times can be kept, so that the comprehensive performance of the sintered foil is greatly improved.
Further, the embodiment of the disclosure also discloses an aluminum electrolytic capacitor anode sintered foil, which is prepared by the preparation method of the aluminum electrolytic capacitor anode sintered foil.
It should be noted that although the steps of the methods in the present disclosure are depicted in the accompanying drawings in a particular order, this does not require or imply that the steps must be performed in that particular order, or that all illustrated steps be performed, to achieve desirable results. Additionally or alternatively, certain steps may be omitted, multiple steps combined into one step to perform, and/or one step decomposed into multiple steps to perform, etc.
Furthermore, the above-described figures are only schematic illustrations of processes included in the method according to the exemplary embodiments of the present disclosure, and are not intended to be limiting. It will be readily appreciated that the processes shown in the above figures do not indicate or limit the temporal order of these processes. In addition, it is also readily understood that these processes may be performed synchronously or asynchronously, for example, among a plurality of modules.
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure herein. This application is intended to cover any adaptations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art to which the disclosure pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.
It is to be understood that the present disclosure is not limited to the precise arrangements and instrumentalities shown in the drawings, and that various modifications and changes may be effected without departing from the scope thereof. The scope of the present disclosure is limited only by the appended claims.
Claims (5)
1. A method for preparing an anode sintered foil of an aluminum electrolytic capacitor, which is characterized by comprising the following steps:
generating aluminum-titanium composite powder by taking spherical aluminum powder as an anode and a titanium target as a cathode in a magnetron sputtering mode, wherein a titanium film is coated on the surface of the aluminum-titanium composite powder;
uniformly mixing and dispersing the aluminum-titanium composite powder, the organic solvent and the functional material to prepare target slurry, coating the target slurry on the two side surfaces of the aluminum foil substrate, and drying to obtain the aluminum foil substrate with powder stacking layers on the two side surfaces;
sintering the aluminum foil base material with the powder stacking layers on the surfaces of the two sides, and performing formation energizing treatment after sintering to prepare an aluminum electrolytic capacitor anode sintered foil;
wherein the functional material is one or more of a binder, a dispersing agent and a film forming agent; the binder is one or more of polyvinyl acetate, polyethylene, carboxyethyl cellulose, phenolic resin and urea resin; the dispersing agent is one or more of methyl cellulose, hydroxypropyl methyl cellulose and polyvinyl alcohol; the film forming agent is one or more of benzyl alcohol, ethylene glycol butyl ether and polyethylene glycol;
under the condition that the functional material is formed by mixing a binder, a dispersing agent and a film forming agent, uniformly mixing and dispersing the aluminum-titanium composite powder, the organic solvent and the functional material to prepare the target slurry, wherein the method comprises the following steps of: mixing the organic solvent, the binder, the dispersant and the film forming agent according to the following ratio (80-90): (0.5-10): (0.1-5): (0.1-5) mixing to produce a preformed solvent; and (3) mixing the aluminum-titanium composite powder with the prefabricated solvent according to the following steps: (4-2) to prepare the target slurry.
2. The preparation method according to claim 1, wherein the organic solvent is one or more of ethylene glycol, polyethylene glycol, terpineol, turpentine, and triethyl citrate.
3. The method of manufacturing according to claim 1, wherein coating the target slurry on both side surfaces of the aluminum foil substrate comprises:
and coating the target slurry on the two side surfaces of the aluminum foil substrate by any one of coating modes of screw roll coating, screen printing and doctor blade coating.
4. The method according to claim 1, wherein the atmosphere for sintering is any one of air, vacuum, inert atmosphere, and reducing atmosphere;
the inert atmosphere is nitrogen atmosphere, argon atmosphere or mixed atmosphere of nitrogen and argon;
the reducing atmosphere is hydrogen atmosphere or alkane atmosphere.
5. An aluminum electrolytic capacitor anode sintered foil prepared by the preparation method according to any one of claims 1 to 4.
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