CN116110722A - Solid electrolytic capacitor and preparation method thereof - Google Patents
Solid electrolytic capacitor and preparation method thereof Download PDFInfo
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- CN116110722A CN116110722A CN202310232146.8A CN202310232146A CN116110722A CN 116110722 A CN116110722 A CN 116110722A CN 202310232146 A CN202310232146 A CN 202310232146A CN 116110722 A CN116110722 A CN 116110722A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/15—Solid electrolytic capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The application provides a solid electrolytic capacitor and a preparation method thereof, and relates to the field of semiconductor devices. The preparation method of the solid electrolytic capacitor comprises the following steps: obtaining an anode block with the surface covered with an electrolyte layer; forming a strengthening layer on the surface of the anode block based on a prefabricated strengthening solution; the strengthening solution is a mixed solution of silica sol, manganese dioxide powder and graphite solution; a solid electrolytic capacitor is prepared based on the anode block formed with the reinforcing layer. The solid electrolytic capacitor prepared by the method can improve the electrical property stability of the solid electrolytic capacitor.
Description
Technical Field
The application relates to the field of semiconductor devices, in particular to a solid electrolytic capacitor and a preparation method thereof.
Background
ESR (Equivalent Series Resistance ) is an important condition for measuring capacitor performance.
However, the solid electrolytic capacitor prepared by the current manufacturing process has an electric property greatly affected by extreme environments, particularly ESR. For example, in a high-temperature environment, the internal structure of the solid electrolytic capacitor is affected by thermal stress, mechanical stress, and the like, and the contact resistance increases due to delamination or the like in the internal structure of the solid electrolytic capacitor, which increases ESR. In a low-temperature environment, holes or cracks of the internal material of the solid electrolytic capacitor can generate tiny capacitance, resistance and the like due to moisture absorption, so that the ESR of the solid electrolytic capacitor is increased and other parameters are changed.
Disclosure of Invention
In view of the above, the present application aims to provide a solid electrolytic capacitor and a method for manufacturing the same, so as to improve the capability of the solid electrolytic capacitor against external influences and improve the electrical performance stability of the solid electrolytic capacitor.
In a first aspect, the present application provides a method for manufacturing a solid electrolytic capacitor, including: obtaining an anode block with the surface covered with an electrolyte layer; forming a strengthening layer on the surface of the anode block based on a prefabricated strengthening solution; the strengthening solution is a mixed solution of silica sol, manganese dioxide powder and graphite powder; a solid electrolytic capacitor is prepared based on the anode block formed with the reinforcing layer.
In the embodiment of the application, the reinforcing layer can be formed on the surface of the electrolyte layer by using the reinforcing solution, and has a certain thickness, so that the capability of the anode block body for resisting the influence of external stress can be effectively improved. Meanwhile, since the strengthening solution includes silica sol, particles of silica adhere to the surface of the electrolyte layer after moisture of the silica sol is evaporated or dried, forming a silica coating film, which can reduce infiltration of moisture. In addition, the silica sol has the following characteristics: large specific surface area and adsorption capacity; the dispersibility is good, and the porous material can be fully filled into solid matters and porous matters; the composite material has the characteristics of good cohesiveness, gel structure formed by adding granular materials, drying and curing, large cohesiveness and the like, and improves the sedimentation rate of original strengthening liquid, more holes of a manganese dioxide layer, poor bonding strength and the like. Therefore, the strengthening solution comprising silica sol is used for forming the strengthening layer on the surface of the anode block, so that the influence of temperature on each layer of the anode block can be effectively reduced, and the deformation of the solid electrolytic capacitor caused by mechanical or environmental stress can be reduced. The strengthening solution further comprises manganese dioxide and graphite, the manganese dioxide and the graphite have good conductivity, and adverse effects of silicon dioxide on the conductivity of the capacitor can be effectively reduced, so that the solid electrolytic capacitor with the strengthening layer can have good external influence resistance and improve the electrical property stability of the solid electrolytic capacitor while the electrical property is not influenced.
In one embodiment, the strengthening solution is prepared by: mixing and stirring silica sol, manganese dioxide powder 1-3 parts and graphite solution 0.1-0.3 part in mass range of 5-10 parts respectively to obtain the strengthening solution, wherein the stirring time is between 4 hours and 50 hours.
In the embodiment of the application, 5 to 10 parts of silica sol is used, so that after the reinforcing layer is formed, silica in the silica sol can play a role in improving the external influence resistance of the solid electrolytic capacitor, thereby improving the electrical property stability of the solid electrolytic capacitor, and reducing the adverse effect on the electrical property of the solid electrolytic capacitor due to excessive use of the silica sol. Meanwhile, the strengthening solution comprises 1 to 3 parts of manganese dioxide powder and 0.1 to 0.3 part of graphite solution, so that adverse effects of silicon dioxide in the silica sol on conductivity can be effectively reduced, and the condition of cost increase caused by excessive materials is avoided. The stirring time of the mixing and stirring is between 4 hours and 50 hours, so that the condition of uneven mixing can be effectively reduced, and the influence of the stirring time process on the preparation efficiency is reduced.
In one embodiment, the silica sol is a mixed solution of nanoparticles of silica and an organic solvent, and the weight ratio of the silica in the silica sol is in the range of 1% to 80%.
In the embodiment of the application, the silica sol comprises the silica with the nano particles, and the nano particles have larger specific surface area, so that the surface tension of a coating film formed after the silica is dried can be improved. The weight ratio of the silicon dioxide in the silica sol is in the range of 1-80%, so that the silicon dioxide can be fully adhered to the surface of the anode block, the situation that the stability of the solid electrolytic capacitor cannot be improved due to a reinforcing layer which is not adhered or is not adhered enough is reduced, and meanwhile, the situation that the conductivity of the solid electrolytic capacitor is reduced due to excessive silicon dioxide is reduced.
In one embodiment, the manganese dioxide powder is nano particles, and the content of manganese dioxide in the manganese dioxide powder is more than 99%; the graphite solution is a graphite aqueous colloidal dispersion obtained by mixing nano-particle graphite powder with water, the solid weight content of the dispersion ranges from 5% to 30%, and the resistivity of the dispersion is less than 0.1 ohm cm.
In the embodiment of the application, the manganese dioxide powder with the manganese dioxide content being more than 99% is selected, and the graphite solution with the solid content range of 5-30% in the dispersion and the specific resistance of the dispersion being less than 0.1 ohm cm is selected, so that the reinforced solution has better conductivity after being dried, and the adverse effect of silica sol on the conductivity is effectively reduced. In addition, since the manganese dioxide powder and the graphite powder are nano particles together with the silicon dioxide, the particles can be uniformly mixed, thereby reducing adverse effects on conductivity due to particle size.
In one embodiment, the anode block is slowly immersed in the strengthening solution; slowly withdrawing the anode block after the strengthening solution submerges the anode block; and drying the anode block to form the reinforcing layer.
In the embodiment of the application, since the strengthening solution is composed of the silica sol and the graphite solution, the adhesion force of the strengthening solution is strong, so that the anode block is slowly immersed and taken out, the strengthening solution can be uniformly distributed and fully adhered on the surface of the anode block, the occurrence of the condition that the strengthening solution is not adhered or bubbles exist is reduced, and the electric performance stability of the solid electrolytic capacitor can be effectively improved by the strengthening layer formed by the strengthening solution.
In one embodiment, the drying the anode block includes: drying the anode block at a first temperature, a second temperature and a third temperature in sequence, wherein the first temperature is less than the second temperature, and the second temperature is less than the third temperature; and carrying out empty decomposition on the dried anode block to form the reinforced layer.
In this embodiment of the application, use first temperature, second temperature and third temperature to dry the positive pole block by stages, can effectively reduce the inconsistent condition of the inside and outside stoving degree of enhancement layer to make enhancement layer stoving more even, reduce the steam existence in the enhancement layer, and then improve the roughness of enhancement layer, reduce solid electrolytic capacitor's ESR.
In one embodiment, after the anode block coated with the electrolyte layer on the surface is obtained, the method further comprises immersing the anode block in a second manganese nitrate solution; and decomposing the second manganese nitrate solution impregnated on the surface of the anode block under a second preset decomposition condition.
In this embodiment of the application, through dipping the anode block body with the surface coated with the electrolyte layer into the second manganese nitrate solution and decomposing, the manganese nitrate can be decomposed into manganese dioxide in the electrolyte layer, so that the electrolyte layer is more compact, the capability of the electrolyte layer for resisting external influence is improved, the conductivity of the electrolyte layer is improved, and the electrical property stability of the solid electrolytic capacitor is further improved. The electrolyte layer is denser, so that the flatness of the electrolyte layer is higher, and therefore, the contact resistance between the electrolyte layer and the reinforcing layer and between the electrolyte layer and the anode block can be effectively reduced, and the ESR of the solid electrolytic capacitor is reduced.
In one embodiment, the preparing a solid electrolytic capacitor based on an anode block formed with the reinforcing layer includes: dipping a conductive layer material on the surface of the reinforced layer; the conductive layer material comprises graphite and/or silver paste; and drying the conductive layer material based on a fourth temperature and a fifth temperature in sequence to form a conductive layer, wherein the fourth temperature is smaller than the fifth temperature, and the fourth temperature is room temperature.
In this embodiment, when the conducting layer formed by conducting layer material is formed on the surface of the strengthening layer, through using different temperatures to dry the conducting layer material by stages, the bubble and the dry crack phenomenon generated on the conducting layer due to the rapid evaporation of water vapor can be effectively reduced, the adverse effect on the electrical performance of the solid electrolytic capacitor due to the abnormal occurrence of the conducting layer is reduced, and therefore the contact resistance between the conducting layer and the strengthening layer is reduced, the preparation yield of the solid electrolytic capacitor is improved, and the ESR of the solid electrolytic capacitor is reduced.
In one embodiment, after the forming a strengthening layer on the surface of the anode block based on the preformed strengthening solution, the method further comprises: impregnating the anode block with a first manganese nitrate solution; carrying out dehydration treatment on the anode block; and under a first preset decomposition condition, carrying out thermal decomposition on the anode block with the surface immersed with the first manganese nitrate solution.
In the embodiment of the application, after the reinforcing layer is formed, the anode block is immersed in the first manganese nitrate solution, and dehydration treatment and thermal decomposition are performed, so that the reinforcing layer is more compact, the flatness of the reinforcing layer is improved, the capability of the reinforcing layer for resisting external environment influence is improved, the conductivity of the reinforcing layer is improved, and the electrical performance stability of the solid electrolytic capacitor under different environments is improved. In addition, the strengthening layer is more dense and flat, so that the contact resistance between the strengthening layer and the electrolyte layer can be effectively reduced, and the ESR of the solid electrolytic capacitor is reduced.
In a second aspect, the present application provides a solid electrolytic capacitor comprising: the anode block is connected with the anode, an oxide film is formed on the surface of the anode block, and an electrolyte layer is covered on the surface of the dielectric oxide film; the reinforcing layer is covered on the surface of the electrolyte layer; the strengthening layer comprises silica sol, manganese dioxide powder and graphite; and the conductive layer is connected with the negative electrode.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a solid electrolytic capacitor according to an embodiment of the present application;
fig. 2 is a flowchart of a method for manufacturing a solid electrolytic capacitor according to an embodiment of the present application.
Icon: an anode block 110; an electrolyte layer 120; a reinforcing layer 130; a conductive layer 140; a positive electrode 210; a negative electrode 220.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the present application.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a solid electrolytic capacitor according to an embodiment of the present application. The solid electrolytic capacitor provided by the embodiment of the application comprises: anode block 110, positive electrode 210, and negative electrode 220.
The anode block 110 is covered with an electrolyte layer 120 on the surface, the inside of the anode block 110 is electrically connected with the positive electrode 210, and the electrolyte layer 120 is used for electrically connecting with the negative electrode 220.
Anode block 110 is a block made of anode material such as tantalum, aluminum, etc., and the shape of anode block 110 includes, but is not limited to, a cube, cylinder, table, etc., in some embodiments, anode block 110 may also be a grooved block shape or other irregularly shaped block shape.
Wherein, since the anode block 110 is made of anode metal, a dielectric oxide film is formed on the surface of the anode block 110, for example, when the anode block 110 is a tantalum block, the dielectric oxide film is tantalum pentoxide, and when the anode block 110 is an aluminum block, the dielectric oxide film is aluminum oxide.
The surface of the anode block 110 is also covered with an electrolyte layer 120, and the electrolyte layer 120 is covered on the surface of the dielectric oxide film. The electrolyte layer 120 is formed of a cathode material, for example, a cathode layer covered with a tantalum surface may be a manganese dioxide layer, and an aluminum surface may be covered with a cathode layer made of a high molecular conductive polymer material.
In the solid electrolytic capacitor, the anode block 110 is used as an anode, the electrolyte layer 120 is used as a cathode, and the dielectric oxide film separates the anode from the cathode to form a capacitor, so that the anode block 110 and the electrolyte layer 120 are respectively connected with the positive electrode and the negative electrode, the function of the capacitor can be realized, and the basic principle and the structure of the solid electrolytic capacitor can refer to the prior art and are not developed any more.
The surface of the anode block 110 of the solid electrolytic capacitor provided in the present application is also covered with a reinforcing layer 130. The reinforcement layer 130 covers the surface of the electrolyte layer 120 such that the electrolyte layer 120 is connected to the negative electrode through the reinforcement layer 130. Wherein the strengthening layer 130 comprises silica sol, manganese dioxide powder and graphite.
In some embodiments, the surface of the strengthening layer 130 is covered with a conductive layer 140 formed by sequentially covering graphite and silver paste, and the negative electrode 220 electrode may be electrically connected to the electrolyte layer 120 through the conductive layer 140 and the strengthening layer 130. Meanwhile, the solid electrolytic capacitor can also be provided with packaging shells such as epoxy resin materials, ceramic shells, copper shells, silver shells and the like.
Next, a description will be given of a solid electrolytic capacitor provided in the present application in conjunction with a method of manufacturing a solid electrolytic capacitor provided in the present embodiment.
Referring to fig. 2, fig. 2 is a flowchart of a method for manufacturing a solid electrolytic capacitor according to an embodiment of the present application, where the method for manufacturing a solid electrolytic capacitor includes:
s110, an anode block with the surface covered with an electrolyte layer is obtained.
And S120, forming a strengthening layer on the surface of the anode block body based on the prefabricated strengthening solution.
S130, a solid electrolytic capacitor is prepared based on the anode block formed with the reinforcing layer.
Next, a method for manufacturing the solid electrolytic capacitor according to the embodiment of the present application will be described by taking the anode block as an example of the tantalum block.
In S110, acquiring the anode block surface-coated with the electrolyte layer may include: an anode block obtained by compression molding or cutting with a mold is obtained, a dielectric oxide film is formed on the surface of the anode block by an oxidizing solution, for example, a tantalum block is placed in an oxidizing solution prepared from phosphoric acid, nitric acid, ethylene glycol and the like, and the oxidizing solution is electrically conducted at room temperature or high temperature, so that the dielectric oxide film is formed on the surface of the anode block. It will be appreciated that the process of obtaining an anode block coated with an electrolyte layer on the surface may refer to the prior art and will not be described in detail herein.
In some embodiments, after the anode block surface-coated with the electrolyte layer is obtained through S110, the anode block surface-coated with the electrolyte layer may be further impregnated with a second manganese nitrate solution, and then the surface-impregnated second manganese nitrate solution of the anode block is decomposed under a second preset decomposition condition, and the process is repeated a plurality of times.
In this embodiment, the second preset decomposition conditions include: the specific gravity of the second manganese nitrate solution is in the range of 1.0g/cm 3 To 1.6g/cm 3 The decomposition temperature is between 200 ℃ and 350 ℃, and the water vapor is between 0.005 and 0.01 Mpa. The decomposition process comprises the following steps: and (3) placing the film furnace with the surface impregnated with the second manganese nitrate solution into the film furnace containing water vapor for decomposition, wherein the temperature in the film furnace is between 200 ℃ and 350 ℃, and after the second manganese nitrate solution is completely decomposed, soaking the second manganese nitrate solution again and decomposing, and repeating the process for a plurality of times.
The number of repeating the impregnation and the decomposition may be set according to the thickness of the electrolyte layer, for example, when the electrolyte layer is thick, the impregnation and the decomposition may be repeated more times, and when the electrolyte layer is thin, the impregnation and the decomposition may be repeated less times. In addition, the number of repetitions may be limited by the process production efficiency, and too many repetitions may affect the production efficiency of the solid electrolytic capacitor, and thus, too many repetitions are not preferable. Illustratively, in some embodiments, the number of repetitions may be 2 to 5.
It will be appreciated that manganese nitrate in the manganese nitrate solution may be decomposed into manganese dioxide, and the anode block coated with the electrolyte layer is impregnated with the second manganese nitrate solution, so that the second manganese nitrate solution permeates into the electrolyte layer, and thus, the second manganese nitrate solution on the surface of the anode block is decomposed, and the second manganese nitrate solution is decomposed into manganese dioxide, so that the electrolyte layer is more compact, the conductivity of the electrolyte layer is improved, and meanwhile, the binding force inside the electrolyte layer is improved, and the permeation of external water vapor is reduced, so that the capability of the manufactured capacitor against environmental influences is improved. The electrolyte layer is more dense, so that the contact surfaces between the electrolyte layer and the dielectric oxide film and between the electrolyte layer and the reinforcing layer are smoother, and the ESR of the manufactured solid electrolytic capacitor can be reduced.
In S120, the strengthening solution is a mixed solution of silica sol, manganese dioxide powder and graphite powder, and the strengthening solution may be prepared by the following method: mixing and stirring 5 to 10 parts of silica sol, 1 to 3 parts of manganese dioxide powder and 0.1 to 0.3 part of graphite solution to obtain a reinforced solution, wherein the stirring time is between 4 and 50 hours.
The silica sol is a mixed solution of nano particles of silicon dioxide and an organic solvent, and the weight ratio of the silicon dioxide in the silica sol is in the range of 1-80%. When the anode block is immersed in the silica sol, and the moisture of the silica sol is evaporated or dried, the particles of the silica are adhered to the surface of the electrolyte layer to form a coating film, so that the penetration of water vapor can be reduced, and meanwhile, as the silica in the silica sol is nano particles, namely the specific surface area of the silica is larger, the surface tension of the anode block can be effectively improved, the influence of temperature on each layer of the anode block is reduced, and the deformation of a solid electrolytic capacitor caused by mechanical or environmental stress is reduced. Meanwhile, the silica sol has the following characteristics: large specific surface area and adsorption capacity; the dispersibility is good, and the porous material can be fully filled into solid matters and porous matters; the anode block has the characteristics of better cohesiveness, gel structure formed by adding granular materials, drying and curing, larger cohesiveness and the like, improves the sedimentation rate of original strengthening liquid, more holes of a manganese dioxide layer, poor bonding strength and the like, and can effectively improve the capability of the anode block for resisting external influence. The organic solvents for preparing the silica sol can be referred to in the prior art and are not developed here.
However, since silica has poor conductivity, too much silica may lower the conductivity of the anode block surface, and thus manganese dioxide powder and graphite are also included in the strengthening solution. Wherein the manganese dioxide powder is nano particles, and the content of manganese dioxide in the manganese dioxide powder is more than 99 percent; the graphite solution is a graphite aqueous colloidal dispersion obtained by mixing nano-particle graphite powder with water, the weight content of solids in the dispersion ranges from 5% to 30%, and the resistivity of the dispersion is less than 0.1 ohm cm.
The manganese dioxide and the graphite have better conductivity, and manganese dioxide powder with the manganese dioxide content being more than 99 percent and the graphite aqueous colloidal dispersion with the solid content ranging from 5 percent to 30 percent and the resistivity being less than 0.1 ohm cm are selected, and after the strengthening solution is dried, the manganese dioxide and the graphite can be attached to the surface of an anode block, so that the adverse effect of silicon dioxide on the conductivity of the capacitor is effectively reduced. The manganese dioxide powder and the graphite powder are nano particles, and can be uniformly mixed after stirring, so that the manganese dioxide and the graphite can be uniformly distributed in the reinforcing layer, and the conductivity is improved.
In the process, the silica sol, the manganese dioxide powder and the graphite solution are stirred for 4 to 50 hours, so that the silica, the manganese dioxide and the graphite are uniformly distributed in the strengthening solution, various particles in the formed strengthening layer are uniformly distributed, the adverse effect of the silica on conductivity is reduced, and the adverse effect is mainly reflected in that the conductivity is reduced or even poor conductivity.
In one embodiment, forming a reinforcement layer on the surface of the anode block based on a preformed reinforcement solution comprises: slowly dipping the anode block into the strengthening solution; slowly taking out the anode block after the strengthening solution submerges the anode block; and drying the anode block to form a reinforcing layer.
Because the strengthening solution comprises silica sol and graphite aqueous colloidal dispersion, the strengthening solution has good dispersibility such as specific surface area and adsorption capacity, and can be fully filled into solid matters and porous matters; the adhesive has the characteristics of good cohesiveness, gel structure formed by adding granular materials, drying and curing, large cohesiveness and the like, so that the adhesive force of the strengthening solution is strong. If the anode block is put into the strengthening solution more quickly, bubbles may occur in the anode block, and thus the uniform and dense strengthening solution cannot be adhered. Therefore, in this embodiment, when the anode block is immersed in the strengthening solution, the anode block is slowly immersed in the strengthening solution, and when the anode block below the surface of the strengthening solution is sufficiently adhered with the strengthening solution, the anode block is further immersed in the strengthening solution, and the process is repeated until the upper end surface of the anode block is sufficiently immersed in the strengthening solution.
Meanwhile, when the anode block immersed with the strengthening solution is taken out, the anode block is slowly taken out, so that the situation that the surface of the anode block is uneven or uneven due to the strong adsorption between the strengthening solutions is reduced. For example, the strengthening solution in the container and the strengthening solution on the surface of the anode block have strong viscosity, and when the anode block is taken out relatively quickly, the strengthening solution on the surface of the anode block may be affected by the strengthening solution in the container, and a large amount of strengthening solution exists and is unevenly adhered, so that slow taking out is beneficial to even and smooth adhesion of the strengthening solution on the surface of the anode block. Wherein the slow withdrawal rate may be the same as or less than the rate at which the anode block is placed into the strengthening solution during immersion, and in some embodiments, the slow withdrawal may continue with lifting a portion of the anode block until the anode block is completely withdrawn when there is no significant drop of strengthening solution from the surface of the anode block above the level of the strengthening solution in the container.
Thus, the strengthening solution on the surface of the anode block can be uniformly adhered, and a uniform strengthening layer can be formed. In addition, since the anode block is slowly immersed in and slowly taken out of the strengthening solution, the surface of the anode block may have more strengthening solution, and in some embodiments, paper may be used to remove the excess strengthening solution at the bottom of the anode block, so that the strengthening solution on the surface of the anode block can be uniformly and evenly adhered.
In addition, the formed strengthening layer has a certain thickness, so that the capability of the solid electrolytic capacitor for resisting the influence of external stress can be improved, the protection of the internal structure of the solid electrolytic capacitor is realized, and the performance of the solid electrolytic capacitor is more stable.
In one embodiment, drying the anode block comprises: drying the anode block at a first temperature, a second temperature and a third temperature in sequence, wherein the first temperature is less than the second temperature, and the second temperature is less than the third temperature; and carrying out empty decomposition on the dried anode block to form a reinforcing layer. Wherein the first temperature ranges from 25 ℃ to 75 ℃, the second temperature ranges from 75 ℃ to 105 ℃, and the third temperature ranges from 135 ℃ to 185 ℃.
In this embodiment, the anode block with the strengthening solution attached to the surface may be put into a drying oven at a first temperature, and pre-dried at the first temperature for 5 to 30 minutes, where after no obvious moisture is present on the surface of the anode block, the temperature of the drying oven is raised to a second temperature, and dried at the second temperature for 5 to 30 minutes, and after it is determined that the tantalum core has no bubble, crack, etc., the temperature of the drying oven may be raised to a third temperature, and dried at the third temperature for 10 to 50 minutes.
Through the stage-by-stage drying, and the temperature rises stage by stage, more steam can be made to evaporate in the lower stage of temperature, and remaining steam can be realized evaporating in the higher stage of temperature to can make the liquid in the enhancement layer more thoroughly that can dry, compare in the mode of directly using single temperature to dry, can effectively reduce the inhomogeneous condition of enhancement layer stoving degree and appear, for example, reduce the outer stoving of enhancement layer and the condition that the inlayer is not dried. Meanwhile, the anode block can be prevented from being directly placed into a high-temperature environment for drying, so that bubbles and cracks appear when water vapor evaporates too quickly, and the combination compactness of layers is improved. In addition, when drying in different stages is accomplished, can in time observe positive pole block surface state to when appearing unusual, can in time adjust, improve the yields, reduce the cost of preparation of condenser. It can be understood that in addition, when drying in stages, the strengthening liquid gradually rises at lower temperature, objects such as water vapor in the liquid are slowly discharged from the inside, and the strengthening liquid in the inside is fully connected with the manganese dioxide layer in the inside, so that the compactness and compactness of the inside of the anode block are improved, and the occurrence of phenomena such as bubbles, layering and cracks in the inside is reduced.
After the reinforcing layer is dried, the anode block can be put into a film furnace for empty decomposition, so that all substances of the anode block react completely, and the influence of the unreacted substances on the performance of the capacitor is reduced. In this embodiment, the empty decomposition may be that the anode block is dried and then the dried anode block is placed in an environment with a preset temperature, so that the substance on the surface of the anode block is completely decomposed.
In one embodiment, after the surface of the anode block is covered with the reinforcing layer, the reinforcing layer on the surface of the anode block may be subjected to a densification process, where the densification process includes: dipping the anode block into a first manganese nitrate solution; carrying out dehydration treatment on the anode block; under a first preset decomposition condition, thermally decomposing the anode block with the surface immersed in the first manganese nitrate solution.
In this embodiment, the first manganese nitrate solution is impregnated on the surface of the strengthening layer. Which is a kind ofIn which the first manganese nitrate solution may have a density in the range of 1.3g/cm 3 To 1.85g/cm 3 The manganese nitrate solution of (2) can be added with a catalyst, wherein the catalyst can be ammonium nitrate, urea, methanol and other materials.
After the impregnation of the first manganese nitrate solution, the anode block may be subjected to a dehydration treatment, which in some embodiments may be a drying of the first manganese nitrate solution on the surface of the anode block, the dehydration treatment being at a temperature between 50 ℃ and 130 ℃ for a time ranging from 5 minutes to 15 minutes.
After the anode block is dehydrated, the anode block may be put into a film furnace containing water vapor for thermal decomposition. The thermal decomposition means that after the anode block is dried, the anode block is placed in an environment with a preset temperature to react, so that the compound on the surface of the anode block is completely decomposed, for example, manganese nitrate is decomposed into manganese dioxide. The temperature of the empty decomposition is between 180 ℃ and 250 ℃, the decomposition time is between 5 minutes and 15, and the steam pressure is between 0.01Mpa and 0.05 Mpa.
It is understood that manganese nitrate can be decomposed into manganese dioxide, and thus, by the densification treatment, the voids of the reinforcing layer can be reduced, the infiltration of moisture can be reduced, and the capability of the solid electrolytic capacitor against the influence of external stress can be improved. The processes of immersing the second manganese nitrate, dehydrating and decomposing the second manganese nitrate in the air can be repeated for a plurality of times, so that the reinforcing layer is sufficiently densely treated, and the capability of the solid electrolytic capacitor for resisting the environmental influence is further improved. In addition, since the dense treatment fills the gaps of the reinforcing layer, the flatness of the reinforcing layer can be improved, thereby reducing the contact resistance between the reinforcing layer and other layers, and thus reducing the ESR of the solid electrolytic capacitor.
S130 may include: covering a conductive layer on the surface of the reinforced layer; and electrically connecting the negative electrode with the conductive layer, electrically connecting the positive electrode with the anode material in the anode block to obtain a capacitor main body, and finally packaging the capacitor main body to obtain the solid electrolytic capacitor. The specific process of preparing the solid electrolytic capacitor based on the anode block can refer to the prior art, and is not developed here. In one embodiment, covering the surface of the strengthening layer with a conductive layer includes: impregnating a conductive layer material on the surface of the reinforcing layer, wherein the conductive layer material comprises graphite and/or silver paste; and drying the conductive layer material based on the fourth temperature and the fifth temperature in sequence to form the conductive layer.
The surface of the reinforcing layer is covered with a conductive layer formed of graphite and silver paste, and the conductive layer is connected with the negative electrode, whereby the conductivity between the capacitor and the electrode can be further improved. Wherein, the graphite layer of conducting layer covers the enhancement layer, and the silver thick liquid layer covers the graphite layer. The materials used to form the graphite layer and the silver paste layer can be referred to in the prior art and are not developed here.
In this embodiment, when forming the conductive layer, the material of the covered conductive layer may be baked in stages, and different temperatures may be used in different stages.
For example, after the surface of the strengthening layer is covered with graphite or silver paste material, the anode block may be left to air dry at a fourth temperature, which may be room temperature ranging from 20 ℃ to 30 ℃ for 15 minutes to 60 minutes. After determining that the surface of the anode block has no obvious moisture, placing the anode block into an oven at room temperature, and raising the temperature to a fifth temperature, and drying the anode block at the fifth temperature which is in the range of 150-210 ℃. When the graphite or silver paste is covered at the same time, the graphite layer can be covered by the process, and after the graphite layer is dried, the silver paste layer can be covered by the process.
Through drying in stages and at different temperatures, the phenomena of air bubbles and cracking generated by vapor evaporation in the drying process can be effectively reduced, the yield of the prepared solid electrolytic capacitor is improved, the abnormality of the solid electrolytic capacitor is reduced, and the capability and the stability of the solid electrolytic capacitor for resisting external influences are improved. The principle and effect of staged drying are similar to those described above and will not be described again.
In the embodiment of the application, the reinforcing layer can be formed on the surface of the electrolyte layer by using the reinforcing solution, and has a certain thickness, so that the capability of the anode block body for resisting the influence of external stress can be effectively improved. Meanwhile, since the strengthening solution includes silica sol, particles of silica adhere to the surface of the electrolyte layer after moisture of the silica sol is evaporated or dried, forming a silica coating film, which can reduce infiltration of moisture. In addition, the silica sol has the following characteristics: large specific surface area and adsorption capacity; the dispersibility is good, and the porous material can be fully filled into solid matters and porous matters; the composite material has the characteristics of good cohesiveness, gel structure formed by adding granular materials, drying and curing, large cohesiveness and the like, and improves the sedimentation rate of original strengthening liquid, more holes of a manganese dioxide layer, poor bonding strength and the like. Therefore, the strengthening solution comprising silica sol is used for forming the strengthening layer on the surface of the anode block, so that the influence of temperature on each layer of the anode block can be effectively reduced, and the deformation of the solid electrolytic capacitor caused by mechanical or environmental stress can be reduced. The strengthening solution further comprises manganese dioxide and graphite, the manganese dioxide and the graphite have good conductivity, and adverse effects of silicon dioxide on the conductivity of the capacitor can be effectively reduced, so that the solid electrolytic capacitor with the strengthening layer can have good external influence resistance and improve the electrical property stability of the solid electrolytic capacitor while the electrical property is not influenced.
Next, the performance of the solid electrolytic capacitor provided in the present application will be described by way of example. Referring to table 1, table 1 provides a table for comparing the performance of the solid electrolytic capacitor obtained by the preparation method and the tantalum core of the solid electrolytic capacitor prepared by the existing preparation method. The group I is a solid electrolytic capacitor obtained by the solid electrolytic capacitor preparation method, the group II is a solid electrolytic capacitor prepared by the existing preparation method, the specifications of the two groups of solid electrolytic capacitors are 6.3V680 mu F-H shell products, and the equipment used for preparing the two groups of solid electrolytic capacitors is the same.
Table 1 comparison of properties
As can be seen from table 1, the capacity, loss and leakage current performance of the two groups of solid electrolytic capacitors of the same specification are not very different, whereas the solid electrolytic capacitors of group I have a smaller ESR than the solid electrolytic capacitors of group II.
Table 2, table 3, table 4 are comparative tables of the performances of the solid electrolytic capacitor obtained by the preparation method provided in the present application and the tantalum core of the solid electrolytic capacitor obtained by the existing preparation method, which were tested by high and low temperature screening (25 ℃, -55 ℃ and 85 ℃) after bonding molding, end treatment, bar cutting, aging, temperature impact, aging.
Referring to Table 2, table 2 shows a comparison of room temperature (25 ℃) test provided in the examples of the present application.
TABLE 2 comparison Table for room temperature (25 ℃ C.) test
In this test, two sets of solid electrolytic capacitors were placed at room temperature to test electrical properties, and as can be seen from table 2, the capacity and leakage current of the two sets of solid electrolytic capacitors differ less, whereas the solid electrolytic capacitor of set I has smaller loss and ESR than the solid electrolytic capacitor of set II, i.e., the capacitor prepared by the preparation method of the solid electrolytic capacitor provided by the present application has smaller loss and ESR.
Referring to Table 3, table 3 shows a comparison of low temperature (-55deg.C) tests provided in the examples of the present application.
TABLE 3 Low temperature (-55 ℃) test comparison Table
In the test, two groups of solid electrolytic capacitors are placed at a low temperature of-55 ℃ to test the electrical performance, and as can be seen from table 3, at the low temperature, the group I solid electrolytic capacitors have smaller loss and ESR than the group II solid electrolytic capacitors, and the group I capacity change is smaller, namely, the capacitor prepared by the preparation method of the solid electrolytic capacitors provided by the application has smaller electrical performance change and better stability at the low temperature.
Referring to Table 4, table 4 shows a comparison of the high temperature (85 ℃) test provided in the examples of the present application.
TABLE 4 high temperature (85 ℃) test comparison Table
In the test, two groups of solid electrolytic capacitors are placed at a high temperature of 85 ℃ to test the electrical performance, and as can be seen from table 4, the leakage current changes of the two groups of solid electrolytic capacitors are obviously changed at the high temperature, and compared with the solid electrolytic capacitor of group II, the solid electrolytic capacitor of group I has smaller loss and ESR, and the capacity change of group I is smaller, namely, the capacitor prepared by the preparation method of the solid electrolytic capacitor provided by the application has smaller electrical performance change and better stability at the low temperature.
As can be seen from the comparison of tables 1 to 4, the preparation method of the solid electrolytic capacitor provided by the application can effectively improve the capability of the solid electrolytic capacitor against external influence and improve the stability of the solid electrolytic capacitor.
The foregoing is merely specific embodiments of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art can easily think about changes or substitutions within the technical scope of the present application, and the changes and substitutions are intended to be covered by the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
It should be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
Claims (10)
1. A method for manufacturing a solid electrolytic capacitor, comprising:
obtaining an anode block with the surface covered with an electrolyte layer;
forming a strengthening layer on the surface of the anode block based on a prefabricated strengthening solution; the strengthening solution is a mixed solution of silica sol, manganese dioxide powder and graphite solution;
a solid electrolytic capacitor is prepared based on the anode block formed with the reinforcing layer.
2. The method for producing a solid electrolytic capacitor according to claim 1, wherein the strengthening solution is produced by: mixing and stirring silica sol, manganese dioxide powder 1-3 parts and graphite solution 0.1-0.3 part in mass range of 5-10 parts respectively to obtain the strengthening solution, wherein the stirring time is between 4 hours and 50 hours.
3. The method of manufacturing a solid electrolytic capacitor according to claim 2, wherein the silica sol is a mixed solution of nanoparticles of silica and an organic solvent, and the weight ratio of the silica in the silica sol is in a range of 1% to 80%.
4. The method for manufacturing a solid electrolytic capacitor according to claim 2, wherein the manganese dioxide powder is nanoparticles, and the content of manganese dioxide in the manganese dioxide powder is more than 99%;
the graphite solution is a graphite aqueous colloidal dispersion obtained by mixing nano-particle graphite powder with water, the solid weight content of the dispersion ranges from 5% to 30%, and the resistivity of the dispersion is less than 0.1 ohm cm.
5. The method of manufacturing a solid electrolytic capacitor according to claim 1, wherein the forming a reinforcement layer on the surface of the anode block based on the pre-formed reinforcement solution comprises:
slowly dipping the anode block into the strengthening solution;
slowly withdrawing the anode block after the strengthening solution submerges the anode block;
and drying the anode block to form the reinforcing layer.
6. The method of manufacturing a solid electrolytic capacitor according to claim 5, wherein the drying the anode block comprises:
drying the anode block at a first temperature, a second temperature and a third temperature in sequence, wherein the first temperature is less than the second temperature, and the second temperature is less than the third temperature;
and carrying out empty decomposition on the dried anode block to form the reinforced layer.
7. The method for producing a solid electrolytic capacitor according to claim 1, wherein after the anode block having the surface covered with the electrolyte layer is obtained, the method further comprises:
impregnating the anode block with a second manganese nitrate solution; and decomposing the second manganese nitrate solution impregnated on the surface of the anode block under a second preset decomposition condition.
8. The method for manufacturing a solid electrolytic capacitor according to claim 1, wherein the manufacturing a solid electrolytic capacitor based on the anode block formed with the reinforcing layer comprises:
dipping a conductive layer material on the surface of the reinforced layer; the conductive layer material comprises graphite and silver paste;
and drying the conductive layer material based on a fourth temperature and a fifth temperature in sequence to form a conductive layer, wherein the fourth temperature is smaller than the fifth temperature, and the fourth temperature is room temperature.
9. The method for producing a solid electrolytic capacitor according to any one of claims 1 to 8, wherein after the formation of a reinforcing layer on the surface of the anode block based on the preformed reinforcing solution, the method further comprises:
impregnating the anode block with a first manganese nitrate solution;
carrying out dehydration treatment on the anode block;
and under a first preset decomposition condition, carrying out thermal decomposition on the anode block with the surface immersed with the first manganese nitrate solution.
10. A solid electrolytic capacitor, characterized by comprising:
the anode block is electrically connected with the anode, a dielectric oxide film is formed on the surface of the anode block, and an electrolyte layer is covered on the surface of the dielectric oxide film;
the reinforcing layer is covered on the surface of the electrolyte layer and is electrically connected with the negative electrode; the strengthening layer comprises silica sol, manganese dioxide and graphite.
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