CN115188593B - Interface treatment method for manganese dioxide cathode layer of tantalum capacitor - Google Patents
Interface treatment method for manganese dioxide cathode layer of tantalum capacitor Download PDFInfo
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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
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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
- H01G9/0029—Processes of manufacture
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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
- H01G9/15—Solid electrolytic capacitors
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- 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 invention belongs to the technical field of interface treatment of a manganese dioxide cathode layer of a tantalum capacitor, and particularly relates to a method for interface treatment of a manganese dioxide cathode layer of a tantalum capacitor, which comprises the steps of immersing an anode block forming the manganese dioxide cathode layer in interface treatment liquid, taking out, sequentially standing at room temperature, drying in a 180 ℃ oven, cooling, immersing in a manganese nitrate solution, taking out, drying in a 60-120 ℃ oven until no liquid trace exists on the surface of the anode block, and then decomposing in a 180-250 ℃ oven for 5-8min; after coating the graphite layer, putting the tantalum block into a reactor for high-temperature heat treatment at 250 ℃, and finally coating a silver paste layer; the method improves the interface state of the manganese dioxide cathode layer, reduces the contact resistance, and enhances the external thermal and electric impact stress resistance at the same time, so that the ESR value and the parameter stability of the product are improved, the operation is simple, the efficiency is high, complex equipment is not needed, and the input cost is low.
Description
Technical Field
The invention belongs to the technical field of interface treatment of a manganese dioxide cathode layer of a tantalum capacitor, and particularly relates to a method for interface treatment of a manganese dioxide cathode layer of a tantalum capacitor.
Background
Based on the composition of the chip tantalum capacitor, its Equivalent Series Resistance (ESR) mainly comprises Ta 2 O 5 Dielectric oxide film resistance (rmediate), cathode manganese dioxide electrolyte resistance (rsolution), tantalum metal resistance (rgold), and the likeThe contact resistance (rcontact) between the material layers, the equivalent series resistance of the capacitor is calculated as: r=r Medium (C) +r Solution +r Gold alloy +r Interface(s) . At a test frequency of 100KHz, r Gold alloy And r Medium (C) Can be ignored. Therefore, on the premise that the current manganese dioxide manufacturing technology tends to be mature, the ESR of the chip tantalum capacitor mainly comes from r Interface(s) . At present, in an environmental stress test, the ESR stability of chip tantalum capacitor products in the market is poor, the ESR can be continuously increased when the chip tantalum capacitor products are applied in long-term storage or severe environments, and finally the whole machine is in fault, and meanwhile, at low temperature, the ESR value can be greatly increased due to the change of the contact performance of a material interface, and finally the whole machine is in fault at low temperature.
At present, the patent with publication number of CN109887751B discloses a preparation method of a tantalum core for a chip tantalum capacitor and a cathode thereof and a chip tantalum capacitor, wherein the anode tantalum core is continuously immersed in each group of manganese nitrate solution for 1-5 times, each immersion time is immediately carried out on the immersed tantalum core to carry out high-temperature water vapor thermal decomposition to form a hollow manganese dioxide cathode layer, the manganese nitrate solution contains a nonionic surfactant, and the manganese nitrate solution enables the tantalum core for the chip tantalum capacitor to have ultralow equivalent series resistance through improving a manganese dioxide structure, but the scheme has no effect on ESR stability, particularly stability under high-temperature and high-humidity environment, and the inventor improves and modifies a manganese dioxide interface on the basis of earlier study so as to improve the ESR stability and have application values in the application fields requiring high-temperature and high-humidity environment or low-temperature environment such as automobile electronic application, low-temperature application and the like.
Disclosure of Invention
The invention provides a method for processing a manganese dioxide cathode layer interface of a tantalum capacitor, which is used for manufacturing a chip tantalum capacitor with low Equivalent Series Resistance (ESR) and excellent stability under high-temperature high-humidity environment application.
The method is realized by the following technical scheme:
a tantalum capacitor manganese dioxide cathode layer interface treatment method comprises the following steps:
1) Immersing anode blocks forming a manganese dioxide cathode layer in the interface treatment liquid for 10-30 s, and taking out and dipping in the bottom redundant solution;
2) Standing at room temperature until no liquid trace exists on the surface of the anode block;
3) Placing the anode block after standing in a 180 ℃ oven for drying for 15-30min, taking out and cooling;
4) Immersing the dried and cooled anode block into a manganese nitrate solution at the temperature of 30-60 ℃ for 1-6min, taking out and dipping in the bottom redundant solution;
5) Drying the anode block immersed in the manganese nitrate solution in a baking oven at 60-120 ℃ until no liquid trace exists on the surface of the anode block, and then placing the anode block in a baking oven at 180-250 ℃ for decomposition for 5-8min;
6) Directly coating a graphite layer on the cooled anode block, and after the graphite layer is solidified, placing the anode block in a 250 ℃ oven for heat treatment for 30-60min;
7) After the heat treatment is finished, the anode block is directly coated with a silver paste layer and solidified.
The interface treatment liquid is flexible ink and consists of one or more of graphite, water-soluble acrylic resin, water, ethanol, triethylamine and an auxiliary agent.
The pH value of the interface treatment liquid is 8-12.
Preferably, the interface treatment fluid consists of graphite, water-soluble acrylic resin, water, ethanol, triethylamine and an auxiliary agent, wherein the mass ratio of the components is as follows: 3-8% of graphite, 2.5-3.5% of acrylic resin, 85-95% of water, 0.5-1.5% of ethanol, 0.5-1.0% of triethylamine and 0.1-1.0% of auxiliary agent.
The auxiliary agent is one or more of dispersing agent, flatting agent, slip agent and cross-linking agent.
The pH value of the manganese nitrate solution is 1-3.
The manganese nitrate solution is a hexahydrate manganese nitrate solution with the mass concentration of 50 percent.
The graphite layer is low-temperature graphite with high conductivity, and the conductivity of the graphite is less than 30 omega m -2 The curing temperature is more than 200 ℃.
The silver paste layer is low-temperature silver paste with high conductivity, and the conductivity of the silver paste is less than 0.015 omega.m -2 The curing temperature is less than 150 ℃.
The preparation method of the anode block for forming the manganese dioxide cathode layer comprises the following steps:
step 1: the valve metal powder is molded and sintered in vacuum to form porous anode block with lead wire, the specific volume of the valve metal powder is 1000-150000 mu F/g, and the sintered density is 4.5-12 g/cm 3 ；
Step 2: formation of dielectric oxide film: immersing the anode block into a dilute phosphoric acid solution to form a dielectric oxide film through electrochemical reaction;
step 3: formation of manganese dioxide layer: and placing the anode block with the dielectric oxide film into a manganese nitrate solution, and forming a manganese dioxide layer on the surface of the anode block through pyrolysis reaction.
The valve metal refers to metal tantalum, niobium, titanium or aluminum.
The beneficial effects are that:
the invention provides a manganese dioxide cathode layer interface treatment method, which uses the prepared interface treatment liquid for the interface treatment of a manganese dioxide cathode layer, and reduces Equivalent Series Resistance (ESR) by improving the surface state of manganese dioxide and the contact effect of external conductive graphite and silver paste, thereby improving the stability of the ESR of a chip tantalum capacitor under a complex environment, particularly under high humidity and high temperature.
The method has the advantages of simple operation, high efficiency, no need of complex equipment and low input cost, improves the interface state of the manganese dioxide cathode layer, reduces the contact resistance, and enhances the external thermal and electric impact stress resistance, thereby improving the ESR value and parameter stability of the product and greatly helping to improve the reliability of the capacitor in complex environments.
The solid electrolytic capacitor produced by the method has an ultralow equivalent series resistance ERS value which is obviously lower than 50% of the industry standard, particularly under the high-temperature and high-humidity environment and the low-temperature environment, the ESR change rate is not more than 50% when being placed under the double-85 environment (85 ℃ and 85%RH), the ESR change rate is not more than 150% under the low temperature (-55 ℃) at the same time, the technical level is higher, the impedance frequency characteristic is good, the ESR value can be kept stable within the range of 10 KHz-1000 KHz, and the special requirements of modern 5G communication base stations and automobile electrons on the capacitance can be completely met.
Detailed Description
The following detailed description of the invention is provided in further detail, but the invention is not limited to these embodiments, any modifications or substitutions in the basic spirit of the present examples, which still fall within the scope of the invention as claimed.
Example 1
Selecting tantalum powder with CV value of 10000Fv/g, pressing into tablet, sintering into anode porous sintered block (sintered block for short) containing tantalum lead under high temperature and high vacuum at 1700 ℃, forming dielectric oxide film layer by sintering the sintered block in dilute phosphoric acid water solution, coating manganese dioxide layer outside the dielectric oxide film, and preparing and carrying out cathode layer interface treatment according to the following steps:
1) Immersing the anode block forming the manganese dioxide cathode layer in the interface treatment liquid for 10s, and taking out and dipping in the bottom redundant solution;
2) Standing at room temperature until no liquid trace exists on the surface of the anode block;
3) Placing the anode block after standing in a 180 ℃ oven to dry for 15min, taking out and cooling;
4) Immersing the dried and cooled anode block in a manganese nitrate solution at 30 ℃ for 6min, taking out and dipping in the bottom redundant solution;
5) Drying the anode block immersed in the manganese nitrate solution in a baking oven at 60 ℃ until no liquid trace exists on the surface of the anode block, and then placing the anode block in a baking oven at 180 ℃ for decomposition for 8min;
6) And (3) directly coating and solidifying the cooled anode block with a graphite layer, after the graphite layer is solidified, placing the anode block in a 250 ℃ oven for heat treatment for 30min, and finally coating and solidifying the anode block with a silver paste layer.
The interface treatment liquid is flexible ink, and consists of graphite, water-soluble acrylic resin, water, ethanol, triethylamine and an auxiliary agent, wherein the mass ratio of the components is as follows: 3% of graphite, 3.5% of acrylic resin, 91.9% of water, 1% of ethanol, 0.5% of triethylamine and 0.1% of auxiliary agent;
the pH value of the interface treatment liquid is 11;
the auxiliary agent is a dispersing agent;
the pH value of the manganese nitrate solution is 1;
the manganese nitrate solution is a 50wt% manganese nitrate hexahydrate solution;
the graphite layer is low-temperature graphite with high conductivity, and the conductivity of the graphite is less than 30 omega m -2 The curing temperature is more than 200 ℃;
the silver paste layer is low-temperature silver paste with high conductivity, and the conductivity of the silver paste is less than 0.015 omega.m -2 The curing temperature is less than 150 ℃.
Example 2
Selecting tantalum powder with CV value of 10000Fv/g, pressing into tablet, sintering into anode porous sintered block (sintered block for short) containing tantalum lead under high temperature and high vacuum at 1700 ℃, forming dielectric oxide film layer by sintering the sintered block in dilute phosphoric acid water solution, coating manganese dioxide layer outside the dielectric oxide film, and preparing and carrying out cathode layer interface treatment according to the following steps:
1) Immersing the anode block forming the manganese dioxide cathode layer in the interface treatment liquid for 30s, and taking out and dipping in the bottom redundant solution;
2) Standing at room temperature until no liquid trace exists on the surface of the anode block;
3) Placing the anode block after standing in a 180 ℃ oven to dry for 30min, taking out and cooling;
4) Immersing the dried and cooled anode block in a manganese nitrate solution at 60 ℃ for 1min, taking out and dipping in the bottom redundant solution;
5) Drying the anode block immersed in the manganese nitrate solution in a baking oven at 60 ℃ until no liquid trace exists on the surface of the anode block, and then placing the anode block in a baking oven at 250 ℃ for 5min for decomposition;
6) And (3) directly coating and solidifying the cooled anode block with a graphite layer, after the graphite layer is solidified, placing the anode block in a 250 ℃ oven for heat treatment for 30min, and finally coating and solidifying the anode block with a silver paste layer.
The interface treatment liquid is flexible ink, and consists of graphite, water-soluble acrylic resin, water, ethanol, triethylamine and an auxiliary agent, wherein the mass ratio of the components is as follows: 3% of graphite, 3.5% of acrylic resin, 91.9% of water, 1% of ethanol, 0.5% of triethylamine and 0.1% of auxiliary agent;
the pH value of the interface treatment liquid is 11;
the auxiliary agent is a leveling agent;
the pH value of the manganese nitrate solution is 1;
the manganese nitrate solution is a 50wt% manganese nitrate hexahydrate solution;
the graphite layer is low-temperature graphite with high conductivity, and the conductivity of the graphite is less than 30 omega m -2 The curing temperature is more than 200 ℃;
the silver paste layer is low-temperature silver paste with high conductivity, and the conductivity of the silver paste is less than 0.015 omega.m -2 The curing temperature is less than 150 ℃.
Example 3
Selecting tantalum powder with CV value of 10000Fv/g, pressing into tablet, sintering into anode porous sintered block (sintered block for short) containing tantalum lead under high temperature and high vacuum at 1700 ℃, forming dielectric oxide film layer by sintering the sintered block in dilute phosphoric acid water solution, coating manganese dioxide layer outside the dielectric oxide film, and preparing and carrying out cathode layer interface treatment according to the following steps:
1) Immersing the anode block forming the manganese dioxide cathode layer in the interface treatment liquid for 20s, and taking out and dipping in the bottom redundant solution;
2) Standing at room temperature until no liquid trace exists on the surface of the anode block;
3) Placing the anode block after standing in a 180 ℃ oven to dry for 20min, taking out and cooling;
4) Immersing the dried and cooled anode block into a manganese nitrate solution with the temperature of 45 ℃ for 3min, taking out and dipping the anode block in the bottom redundant solution;
5) Drying the anode block immersed in the manganese nitrate solution in a drying oven at 90 ℃ until no liquid trace exists on the surface of the anode block, and then placing the anode block in a drying oven at 220 ℃ for decomposition for 7min;
6) And (3) directly coating and solidifying the cooled anode block with a graphite layer, after the graphite layer is solidified, placing the anode block in a 250 ℃ oven for heat treatment for 30min, and finally coating and solidifying the anode block with a silver paste layer.
The interface treatment liquid is flexible ink, and consists of graphite, water-soluble acrylic resin, water, ethanol, triethylamine and an auxiliary agent, wherein the mass ratio of the components is as follows: 3% of graphite, 3.5% of acrylic resin, 91.9% of water, 1% of ethanol, 0.5% of triethylamine and 0.1% of auxiliary agent;
the pH value of the interface treatment liquid is 11;
the auxiliary agent is a leveling agent;
the pH value of the manganese nitrate solution is 1;
the manganese nitrate solution is a 50wt% manganese nitrate hexahydrate solution;
the graphite layer is low-temperature graphite with high conductivity, and the conductivity of the graphite is less than 30 omega m -2 The curing temperature is more than 200 ℃;
the silver paste layer is low-temperature silver paste with high conductivity, and the conductivity of the silver paste is less than 0.015 omega.m -2 The curing temperature is less than 150 ℃.
Comparative example 1
Tantalum powder with CV value of 10000Fv/g is selected, pressed into tablets, sintered into anode porous sintered blocks (sintered blocks for short) containing tantalum leads at 1700 ℃ under high temperature and high vacuum, the sintered blocks are formed into dielectric oxide film layers in dilute phosphoric acid aqueous solution, manganese dioxide layers are coated outside the dielectric oxide film, and finally graphite layers and silver paste layers are coated in sequence, so that the comparative example does not carry out corresponding interface treatment.
Comparative example 2
Selecting tantalum powder with CV value of 10000Fv/g, pressing into tablet, sintering at 1700 deg.C under high temperature and high vacuum to anode porous sintered block (sintered block for short) containing tantalum lead, forming dielectric oxide film layer in dilute phosphoric acid water solution, coating manganese dioxide layer outside the dielectric oxide film, directly coating graphite layer on cooled anode block and solidifying, placing anode block in 250 deg.C oven for heat treatment for 30min after graphite layer is solidified, finally coating silver paste layer on anode block and solidifying.
Comparative example 3
Selecting tantalum powder with CV value of 10000Fv/g, pressing into tablet, sintering into anode porous sintered block (sintered block for short) containing tantalum lead under high temperature and high vacuum at 1700 ℃, forming dielectric oxide film layer by sintering the sintered block in dilute phosphoric acid water solution, coating manganese dioxide layer outside the dielectric oxide film, and preparing and carrying out cathode layer interface treatment according to the following steps:
1) Immersing the anode block forming the manganese dioxide cathode layer in the interface treatment liquid for 20s, and taking out and dipping in the bottom redundant solution;
2) Standing at room temperature until no liquid trace exists on the surface of the anode block;
3) Placing the anode block after standing in a 180 ℃ oven to dry for 20min, taking out and cooling;
4) Immersing the dried and cooled anode block into a manganese nitrate solution with the temperature of 45 ℃ for 3min, taking out and dipping the anode block in the bottom redundant solution;
5) Drying the anode block immersed in the manganese nitrate solution in a drying oven at 90 ℃ until no liquid trace exists on the surface of the anode block, and then placing the anode block in a drying oven at 220 ℃ for decomposition for 7min;
6) The cooled anode block is directly coated with a graphite layer and solidified, and high-temperature heat treatment is not performed.
The interface treatment liquid is flexible ink, and consists of graphite, water-soluble acrylic resin, water, ethanol, triethylamine and an auxiliary agent, wherein the mass ratio of the components is as follows: 3% of graphite, 3.5% of acrylic resin, 91.9% of water, 1% of ethanol, 0.5% of triethylamine and 0.1% of auxiliary agent;
the pH value of the interface treatment liquid is 11;
the auxiliary agent is a leveling agent;
the pH value of the manganese nitrate solution is 1;
the manganese nitrate solution is a 50wt% manganese nitrate hexahydrate solution;
the graphite layer is low-temperature graphite with high conductivity, and the conductivity of the graphite is less than 30 omega m -2 The curing temperature is more than 200 ℃;
the silver paste layer is low-temperature silver paste with high conductivity, and the conductivity of the silver paste is less than 0.015 omega.m -2 The curing temperature is less than 150 ℃.
The tantalum anodes in the above examples and comparative examples are dissolved into diluted phosphoric acid to form a dielectric oxide film product with a specification of 35V10 mu F, after all the processes of the examples or comparative examples are completed, the anodes and cathodes of the lead frames are welded in sequence to complete the encapsulation of the resin layers to form a solid electrolytic capacitor, the equivalent series resistance is tested at 100KHz to be initial value, then the product is put into a HAST test box to carry out 9 accelerated lifetime test under the conditions of 121 ℃, 85% RH, 0.08MPa and 63h, after the test is finished, the product is placed at room temperature for 1-2h to carry out normal temperature ESR test, after the completion, the product is placed at low temperature of-55 ℃ to carry out ESR test again after the constant temperature is kept for half an hour, and the data are shown in tables 1-3:
TABLE 1 initial ESR measurement at ambient temperature
TABLE 2 ESR values after 1000 hours of "double 85
TABLE 3 Low temperature (-55 ℃) ESR values
As can be seen from the data in the table, the electrolytic capacitor produced by the technical scheme of the invention has a lower ESR value, in comparative example 2, the electrolytic capacitor is not treated by using the interface treatment liquid, and in comparative example 3, the ESR is improved compared with comparative example 1, but the best ideal effect is not achieved, and the ESR can be improved to the best effect by combining the two interface treatment methods.
Claims (7)
1. The interface treatment method of the manganese dioxide cathode layer of the tantalum capacitor is characterized by comprising the following steps:
1) Immersing anode blocks forming a manganese dioxide cathode layer in the interface treatment liquid for 10-30 s, and taking out and dipping in the bottom redundant solution;
2) Standing at room temperature until no liquid trace exists on the surface of the anode block;
3) Placing the anode block after standing in a 180 ℃ oven for drying for 15-30min, taking out and cooling;
4) Immersing the dried and cooled anode block into a manganese nitrate solution at the temperature of 30-60 ℃ for 1-6min, taking out and dipping in the bottom redundant solution;
5) Drying the anode block immersed in the manganese nitrate solution in a baking oven at 60-120 ℃ until no liquid trace exists on the surface of the anode block, and then placing the anode block in a baking oven at 180-250 ℃ for decomposition for 5-8min;
6) Directly coating a graphite layer on the cooled anode block, and after the graphite layer is solidified, placing the anode block in a 250 ℃ oven for heat treatment for 30-60min;
7) After the heat treatment is finished, directly coating a silver paste layer on the anode block and curing;
the interface treatment liquid consists of graphite, water-soluble acrylic resin, water, ethanol, triethylamine and an auxiliary agent, wherein the mass ratio of the components is as follows: 3-8% of graphite, 2.5-3.5% of acrylic resin, 85-95% of water, 0.5-1.5% of ethanol, 0.5-1.0% of triethylamine and 0.1-1% of auxiliary agent.
2. The method of claim 1, wherein the pH of the interface treatment solution is 8-12.
3. The method for treating an interface of a manganese dioxide cathode layer of a tantalum capacitor according to claim 1, wherein the auxiliary agent is one or more of a dispersing agent, a leveling agent, a slip agent and a crosslinking agent.
4. The method of claim 1, wherein the pH of the manganese nitrate solution is 1-3.
5. The method for treating an interface of a manganese dioxide cathode layer of a tantalum capacitor according to claim 1, wherein said manganese nitrate solution is a 50wt% concentration manganese nitrate hexahydrate solution.
6. The method for interface treatment of manganese dioxide cathode layer of tantalum capacitor according to claim 1, wherein said graphite layer is low temperature graphite with high conductivity, and the conductivity of said graphite is less than 30Ω.m -2 The curing temperature is more than 200 ℃.
7. The method for processing interface of manganese dioxide cathode layer of tantalum capacitor according to claim 1, wherein said silver paste layer is low temperature silver paste with high conductivity, and the conductivity of said silver paste is less than 0.015 Ω.m -2 The curing temperature is less than 150 ℃.
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