CN112024892A - Method for manufacturing aluminum electrolytic capacitor anode foil by electric field auxiliary sintering - Google Patents
Method for manufacturing aluminum electrolytic capacitor anode foil by electric field auxiliary sintering Download PDFInfo
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- CN112024892A CN112024892A CN202010876862.6A CN202010876862A CN112024892A CN 112024892 A CN112024892 A CN 112024892A CN 202010876862 A CN202010876862 A CN 202010876862A CN 112024892 A CN112024892 A CN 112024892A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
- B22F2007/047—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method non-pressurised baking of the paste or slurry containing metal powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/06—Use of electric fields
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
A method for manufacturing an aluminum electrolytic capacitor anode foil by electric field auxiliary sintering comprises the following steps: 1) mixing the slurry, namely uniformly mixing aluminum powder or aluminum alloy powder in the slurry; 2) forming a film formed of the mixed slurry manufactured in step 1) on an aluminum foil substrate, and curing; 3) placing the aluminum foil cured in the step 2) between two parallel electrodes, and coating a silver paint coating between the electrodes and the aluminum foil; 4) putting the aluminum foil together with the electrode in the step 3) into a sintering furnace, raising the temperature to 300-550 ℃, and keeping the temperature for 4-60 minutes under a protective atmosphere; and (3) starting to electrify direct current to the two electrodes, gradually increasing the electric field intensity between the two electrodes until the flash burning phenomenon occurs, and obtaining the sintered anode foil. In the invention, the electric field is used for assisting sintering, so that the flash sintering phenomenon is generated, the sintering time of the anode foil is short, the sintering temperature is low, and the phenomenon of grain growth in the sintering process can be inhibited.
Description
Technical Field
The invention relates to a sintering method of an aluminum electrolytic capacitor anode foil, in particular to a manufacturing method of an aluminum electrolytic capacitor anode foil by electric field auxiliary sintering.
Background
The surface of the anode foil of the conventional aluminum electrolytic capacitor is subjected to etching treatment to obtain a large surface area, but in order to obtain the anode foil of the aluminum electrolytic capacitor used for the capacitor of medium and high voltage, patent No. 2008801287834, an electrode material for the aluminum electrolytic capacitor and a method for manufacturing the electrode material; a sintered anode foil is disclosed. The anode foil is formed by sintering aluminum powder or aluminum alloy powder on an aluminum foil substrate. Researches show that the sintering process has long sintering time, high temperature, easy abnormal growth of crystal grains and high energy consumption; when the sintered aluminum grains are abnormally long, a large number of connected voids become closed voids, and the capacity of the anode foil is reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for manufacturing an anode foil of an aluminum electrolytic capacitor by electric field assisted sintering, so that the sintering time is shortened, and the abnormal length of crystal grains can be inhibited.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for manufacturing an aluminum electrolytic capacitor anode foil by electric field auxiliary sintering comprises the following steps:
1) mixing the slurry, namely uniformly mixing aluminum powder or aluminum alloy powder in the slurry;
2) forming a film formed of the mixed slurry manufactured in step 1) on an aluminum foil substrate, and curing;
3) placing the aluminum foil cured in the step 2) between two parallel electrodes, and coating a silver paint coating between the electrodes and the aluminum foil;
4) putting the aluminum foil together with the electrode in the step 3) into a sintering furnace, raising the temperature to 300-550 ℃, and keeping the temperature for 4-60 minutes under a protective atmosphere; starting to electrify direct current to the two electrodes, gradually increasing the electric field intensity between the two electrodes until a flash burning phenomenon occurs, and obtaining a sintered anode foil; the electric field intensity between the electrodes is 10-80V/cm; the current of the direct current power supply is lower than 8A;
the above method for manufacturing an aluminum electrolytic capacitor anode foil by electric field assisted sintering preferably further comprises: 5) putting the sintered anode foil obtained in the step 4) into pure water, and carrying out ultrasonic oscillation for 0.1-1 hour;
6) soaking the anode foil treated in the step 5) in a phosphoric acid solution for 30 seconds to 10 minutes; the concentration of the phosphoric acid solution is between 0.5 and 3 percent.
In the above method for manufacturing an aluminum electrolytic capacitor anode foil by electric field assisted sintering, preferably, the slurry in step 1) includes a solvent and an organic binder, and the solvent includes one or more of alcohol, ethylene glycol, glycerol, NMP, PVDF, xylene, and methanol.
In the above method for manufacturing an aluminum electrolytic capacitor anode foil by electric field assisted sintering, preferably, the electrodes are two parallel copper electrodes.
In the method for manufacturing the anode foil of the aluminum electrolytic capacitor by electric field assisted sintering, preferably, the porosity of the aluminum powder or aluminum alloy powder film is 10-50%, and the total thickness of the aluminum powder layer is 50-500 μm.
Compared with the prior art, the invention has the advantages that: in the invention, the electric field is used for assisting sintering, so that the flash sintering phenomenon is generated, the sintering time of the anode foil is short, the sintering temperature is low, and the phenomenon of grain growth in the sintering process can be inhibited.
Drawings
FIG. 1 is a circuit diagram of a sintered anode foil in example 1.
FIG. 2 is a graph of power consumption as a function of furnace temperature.
Fig. 3 is a scanning electron microscope image of the anode foil produced in example 1.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
It should be particularly noted that when an element is referred to as being "fixed to, connected to or communicated with" another element, it can be directly fixed to, connected to or communicated with the other element or indirectly fixed to, connected to or communicated with the other element through other intermediate connecting components.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
A method for manufacturing an aluminum electrolytic capacitor anode foil by electric field auxiliary sintering comprises the following steps:
1) mixing the slurry, namely uniformly mixing aluminum powder or aluminum alloy powder in the slurry; the porosity of the aluminum powder or aluminum alloy powder film is 10-50%, and the total thickness of the aluminum powder layer is 50-500 μm.
2) Forming a film formed of the mixed slurry manufactured in step 1) on an aluminum foil substrate, and curing;
3) placing the aluminum foil cured in the step 2) between two parallel copper electrodes, and coating a silver paint coating layer of 10-40 μm between the electrodes and the aluminum foil to reduce the contact resistance as much as possible;
4) putting the aluminum foil together with the electrode in the step 3) into a sintering furnace, raising the temperature to 300-550 ℃, and keeping the temperature for 4-60 minutes under a protective atmosphere; starting to electrify direct current to the two electrodes, gradually increasing the electric field intensity between the two electrodes until a flash burning phenomenon occurs, and obtaining a sintered anode foil; the electric field intensity between the electrodes is 10-80V/cm; the current of the direct current power supply is lower than 8A. As shown in fig. 2, when the flash occurs, the power consumption of the power supply suddenly increases from 0, the voltage decreases, and the current increases.
5) Putting the sintered anode foil obtained in the step 4) into pure water, and carrying out ultrasonic oscillation for 0.1-1 hour; and putting the anode foil into pure water for ultrasonic oscillation, so that aluminum powder or aluminum alloy powder which is not sintered together can oscillate out.
6) Soaking the anode foil treated in the step 5) in a phosphoric acid solution for 30 seconds to 10 minutes; the concentration of the phosphoric acid solution is between 0.5 and 3 percent. In this example, an electron microscope scanning image of the prepared anode foil is shown in fig. 3.
In the anode foil of the embodiment, when the anode foil is subjected to the step 5), the associated alumina is formed on the surface of the sintered film, the alumina colloid with high plume-shaped water content is generated on the outermost layer of the anode foil, and the alumina colloid is difficult to be converted into anhydrous alumina during formation, so that the quality of the oxide film and the specific capacity after formation are affected, and the external plume-shaped hydrated alumina colloid can be dissolved by treating the anode foil with dilute phosphoric acid alone, so that the quality of the oxide film and the specific capacity of the sintered film are improved. The ultrasonic oscillation in step 5) also causes a certain damage to alumina colloids with high plume water content, and since the anode foil is always in water, the alumina colloids are always present and need to be removed by phosphoric acid. Meanwhile, in the phosphoric acid solution, the spines and fine powder particles on the surface of a part of the sintered film can be dissolved, so that the uniformity of the surface resistance of the sintered film is helped. It is to be noted that the treatment of the anode foil with dilute phosphoric acid in step 6) is completely different from the treatment of the surface of the anode foil with acid at the time of etching.
In the present implementation, the slurry in step 1) includes a solvent and an organic binder, and the solvent includes one or more of alcohol, ethylene glycol, glycerol, NMP, PVDF, xylene, and methanol. The organic binder may be one or more of known organic binders, such as one or more of polyvinyl alcohol resin, polyester resin, epoxy resin, phenolic resin.
Electric field assisted sintering (Elelctronic field assisted sintering) refers to the process of applying an electric field to a sample in a conventional pressureless sintering process, wherein the sample is subjected to a temperature which is provided by a sintering furnace on one hand, and joule heat generated under the action of a direct current electric field can greatly promote the densification of the sample on the other hand. Flash Sintering (Flash Sintering) refers to that in the process of electric field assisted Sintering, when the electric field strength reaches a certain value, a sample is sharply shrunk to be compact at a certain Sintering temperature, and the process is completed within a few seconds. As a novel sintering method, the electric field assisted sintering has the advantages of low sintering temperature, short sintering time, capability of inhibiting the growth of crystal grains in the sintering process and the like, and can save a large amount of time and energy, thereby being very beneficial to cost control and environmental protection.
As shown in fig. 1, in the present example, sintering was performed using a tube furnace; the platinum gold wire connects the DC power supply, the ammeter and the sample in series to form a closed loop, and the sample is placed in the tube furnace. The electric sintering process is subjected not only to heat from the tube furnace but also to joule heat generated by the electric current. The temperature rise rate of the tube furnace is 2-30 ℃/min, the tube furnace is heated to 550 ℃ at the temperature of 300 ℃ to maintain the temperature for 4-30 minutes under the protective atmosphere. The power supply provides the electric field intensity at 10-80V/cm according to the length of the foil, and in order to prevent the damage to equipment and samples caused by overlarge current in the whole loop, the upper current limit of the direct current power supply is set to be 8A. When the current reaches 0.1-5A, the power supply is automatically switched to current control. This is because the sudden onset of sintering is accompanied by a likewise sudden increase in the conductivity of the sample (flash firing occurs), as in fig. 2. The power supply must be immediately switched to current control to prevent excessive current and temperature damage to the sample and equipment. During the current control phase, the power consumed by the power supply on the sample decreases because the resistance of the sample continues to decrease. The temperature of the sample gradually rises to a steady value due to the flow restriction. When subjected to the current limiting process, the power consumed by the power supply acts on the sample primarily in the form of joule heating, which accelerates the sintering process.
In the embodiment, the electric field is used for assisting sintering, so that the flash sintering phenomenon occurs, the sintering time of the anode foil is short, the sintering temperature is low, and the phenomenon of grain growth in the sintering process can be inhibited.
Claims (5)
1. A method for manufacturing an aluminum electrolytic capacitor anode foil by electric field auxiliary sintering is characterized in that: the method comprises the following steps:
1) mixing the slurry, namely uniformly mixing aluminum powder or aluminum alloy powder in the slurry;
2) forming a film formed of the mixed slurry manufactured in step 1) on an aluminum foil substrate, and curing;
3) placing the aluminum foil cured in the step 2) between two parallel electrodes, and coating a silver paint coating between the electrodes and the aluminum foil;
4) putting the aluminum foil together with the electrode in the step 3) into a sintering furnace, raising the temperature to 300-550 ℃, and keeping the temperature for 4-60 minutes under a protective atmosphere; starting to electrify direct current to the two electrodes, gradually increasing the electric field intensity between the two electrodes until a flash burning phenomenon occurs, and obtaining a sintered anode foil; the electric field intensity between the electrodes is 10-80V/cm; the current of the direct current power supply is lower than 8A.
2. The method for manufacturing an aluminum electrolytic capacitor anode foil by electric field assisted sintering according to claim 1, wherein the method comprises the following steps: further comprising: 5) putting the sintered anode foil obtained in the step 4) into pure water, and carrying out ultrasonic oscillation for 0.1-1 hour;
6) soaking the anode foil treated in the step 5) in a phosphoric acid solution for 30 seconds to 10 minutes; the concentration of the phosphoric acid solution is between 0.5 and 3 percent.
3. The method for manufacturing an aluminum electrolytic capacitor anode foil by electric field assisted sintering according to claim 1, wherein the method comprises the following steps: the slurry in the step 1) comprises a solvent and an organic binder, wherein the solvent comprises one or more of alcohol, ethylene glycol, glycerol, NMP, PVDF, xylene and methanol.
4. The method for manufacturing an aluminum electrolytic capacitor anode foil by electric field assisted sintering according to claim 1, wherein the method comprises the following steps: the electrodes are two parallel copper electrodes.
5. The method for manufacturing an aluminum electrolytic capacitor anode foil by electric field assisted sintering according to claim 1, wherein the method comprises the following steps: the porosity of the aluminum powder or aluminum alloy powder film is 10-50%, and the total thickness of the aluminum powder layer is 50-500 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115083784A (en) * | 2022-07-15 | 2022-09-20 | 新疆众和股份有限公司 | Slurry for sintered foil, preparation method of sintered foil and aluminum electrolytic capacitor |
| CN116100027A (en) * | 2023-04-04 | 2023-05-12 | 南通海星电子股份有限公司 | Preparation method of laser scanning assisted laminated foil |
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| CN110606751A (en) * | 2019-09-18 | 2019-12-24 | 上海交通大学 | Method for graphene-assisted room-temperature flash firing of ceramic material |
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2020
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Cited By (3)
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| CN115083784A (en) * | 2022-07-15 | 2022-09-20 | 新疆众和股份有限公司 | Slurry for sintered foil, preparation method of sintered foil and aluminum electrolytic capacitor |
| CN115083784B (en) * | 2022-07-15 | 2024-01-02 | 新疆众和股份有限公司 | Slurry for sintered foil, preparation method of sintered foil and aluminum electrolytic capacitor |
| CN116100027A (en) * | 2023-04-04 | 2023-05-12 | 南通海星电子股份有限公司 | Preparation method of laser scanning assisted laminated foil |
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