CN116206902A - Manganese dioxide cathode of welding-resistant tantalum electrolytic capacitor, capacitor and preparation method of manganese dioxide cathode - Google Patents
Manganese dioxide cathode of welding-resistant tantalum electrolytic capacitor, capacitor and preparation method of manganese dioxide cathode Download PDFInfo
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 234
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title claims abstract description 208
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 90
- 239000003990 capacitor Substances 0.000 title claims abstract description 86
- 238000003466 welding Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 230000005484 gravity Effects 0.000 claims abstract description 67
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 65
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 32
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 32
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 4
- ICGLPKIVTVWCFT-UHFFFAOYSA-N 4-methylbenzenesulfonohydrazide Chemical compound CC1=CC=C(S(=O)(=O)NN)C=C1 ICGLPKIVTVWCFT-UHFFFAOYSA-N 0.000 claims description 4
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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
- H01G9/0425—Electrodes or formation of dielectric layers thereon characterised by the material specially adapted for cathode
-
- 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
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/032—Inorganic semiconducting electrolytes, e.g. MnO2
-
- 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
-
- 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 discloses a manganese dioxide cathode of a welding-resistant tantalum electrolytic capacitor, a capacitor and a preparation method thereof, wherein the preparation method of the manganese dioxide cathode comprises the following steps: providing a tantalum core anode coated with a tantalum pentoxide dielectric film, immersing in manganese nitrate solutions with different specific gravities within a first specific gravity range, performing high-temperature vapor decomposition, and forming an inner cathode layer on the tantalum pentoxide dielectric film after repeated operation for a plurality of times; immersing the sample in manganese nitrate solution with a decomposition accelerator in a second specific gravity range for multiple times, taking out the sample after each immersion, pre-drying the sample, and carrying out surface homogenization treatment; and carrying out thermal decomposition on the sample to form an outer cathode layer on the surface of the sample. The method can improve the compactness and uniformity of the manganese dioxide outer layer, and greatly improve the welding heat resistance of the tantalum electrolytic capacitor and the use stability of the tantalum electrolytic capacitor while maintaining the excellent performance of the tantalum electrolytic capacitor.
Description
Technical Field
The invention relates to the field of ceramic capacitors, in particular to a manganese dioxide cathode of a welding-resistant tantalum electrolytic capacitor, a capacitor and a preparation method thereof.
Background
With the rapid development of the electronic information industry, integration, miniaturization, high frequency and high density have become major trends in the development of electronic devices. The tantalum electrolytic capacitor has higher volume specific capacity, good temperature stability and frequency stability, and is widely applied to small-sized complete machine electronic equipment such as mobile communication, notebook computers, palm computers, automobile electronics and the like, and has good application prospects in the aspects of aviation, aerospace, petroleum drilling and the like.
The electrolyte layer of the common sheet type solid electrolyte tantalum electrolytic capacitor consists of manganese dioxide, and the prior art is formed by decomposing manganese nitrate under a certain temperature condition. However, in the actual manufacturing process, a certain temperature and time are required for decomposing manganese nitrate into manganese dioxide, and particularly after a viscosity reducer is added into the manganese nitrate solution, the fluidity of the manganese nitrate solution is enhanced, and the manganese nitrate on the surface of the tantalum electrolytic capacitor is subjected to the influence of gravity or other factors before being decomposed, so that the manganese dioxide formed after being decomposed has the problem of partial accumulation, and the problem of poor structural uniformity of a surface electrolyte layer is caused. Therefore, the prepared tantalum electrolytic capacitor has the problem that the thickness uniformity of the manganese dioxide layer on the surface is poor, in the actual use process of the capacitor, particularly in the SMT process, the uneven manganese dioxide layer easily causes the dielectric layer inside the capacitor to be damaged in the heat expansion and cold contraction process, the leakage current is increased and invalid, and the yield after welding is reduced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a manganese dioxide cathode of a welding-resistant tantalum electrolytic capacitor, the capacitor and a preparation method thereof.
In order to achieve the above object, the technical scheme of the present invention is as follows:
a preparation method of a manganese dioxide cathode of a welding-resistant tantalum electrolytic capacitor comprises the following steps:
1) Providing a tantalum core anode coated with a tantalum pentoxide dielectric film, immersing in manganese nitrate solutions with different specific gravities within a first specific gravity range, performing high-temperature vapor decomposition, and forming an inner cathode layer on the tantalum pentoxide dielectric film after repeated operation for a plurality of times;
2) Immersing the sample obtained in the step 1 into a manganese nitrate solution with a decomposition accelerator in a second specific gravity range for multiple times, taking out the sample after each immersion, placing the sample at a temperature of 75-180 ℃, placing the sample at a water vapor pressure of 0.02-0.05 MPa, pre-drying the sample for 5-10 minutes under the condition that the mass percentage concentration of oxygen is 7-10%, and carrying out surface homogenization treatment;
3) And (3) carrying out thermal decomposition on the sample obtained in the step (2) to form an outer cathode layer on the surface of the sample.
Preferably, the decomposition accelerator is one or more of citric acid, p-toluenesulfonyl hydrazide, urea and ammonium nitrate.
Preferably, the mass fraction of the decomposition accelerator in the manganese nitrate solution having the decomposition accelerator in the second specific gravity range is 0.01% to 8%.
Preferably, the first specific gravity range is 1.00g/cm 3 ～1.30g/cm 3 。
Preferably, the second specific gravity range is 1.30g/cm 3 ～2.00g/cm 3 。
Preferably, the specific gravity of the manganese nitrate solution in the step S2 has a gradient change, which is a first specific gravity, a second specific gravity, and a third specific gravity in this order, wherein the first specific gravity is smaller than the second specific gravity, and the second specific gravity is greater than the third specific gravity.
Preferably, the conditions for thermal decomposition in the step 3 are as follows: the temperature is 200-280 ℃, the vapor pressure is 0.02-0.05 MPa, and the decomposition is carried out for 5-7 minutes under the condition that the oxygen mass percentage concentration is 6-12%.
The manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor is prepared by adopting the preparation method of the manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor.
A preparation method of a solid sheet type tantalum electrolytic capacitor comprises a preparation step of a tantalum core anode, a preparation step of a tantalum pentoxide dielectric film and a preparation method of a manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor.
The solid sheet type tantalum electrolytic capacitor is prepared by adopting the preparation method of the solid sheet type tantalum electrolytic capacitor.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the process of decomposing manganese nitrate into manganese dioxide is controlled by improving the solution formula and the preparation process, so that the structural consistency of a manganese dioxide electrolyte layer on the surface of the tantalum electrolytic capacitor is effectively improved, the surface uniformity of a manganese dioxide cathode of the prepared tantalum electrolytic capacitor is good, the welding resistance of the tantalum electrolytic capacitor is greatly improved while the excellent performance of the tantalum electrolytic capacitor is maintained, and the use stability of the tantalum electrolytic capacitor is improved.
(2) According to the invention, a decomposition accelerator is added into a manganese nitrate solution for preparing manganese dioxide, a manganese nitrate homogenization treatment process is designed in the process of decomposing manganese nitrate into manganese dioxide, and before the manganese nitrate solution on the surface of a tantalum capacitor is decomposed into manganese dioxide, the decomposition accelerator is decomposed before manganese nitrate, so that manganese nitrate is uniformly distributed on the surface of the tantalum capacitor, and finally a uniformly distributed manganese dioxide layer is obtained by decomposition.
(3) The manganese dioxide layer on the surface of the tantalum electrolytic capacitor after being coated is uniformly distributed, good in consistency and higher in qualification rate after finished product aging, and the welding heat resistance test is carried out in a reflow soldering mode, so that the phenomena of leakage current increase, short circuit failure and the like are avoided.
Drawings
The accompanying drawings are included to provide a further understanding of the embodiments and are incorporated in and constitute a part of this specification. The drawings illustrate embodiments and together with the description serve to explain the principles of the invention. Many of the intended advantages of other embodiments and embodiments will be readily appreciated as they become better understood by reference to the following detailed description.
FIG. 1 is a surface morphology of manganese dioxide cathode of tantalum electrolytic capacitor of comparative example 1 of the present application;
FIG. 2 is a surface state diagram of a tantalum electrolytic capacitor produced in comparative example 1 of the present application after being coated;
FIG. 3 is a surface morphology of manganese dioxide cathode of tantalum electrolytic capacitor of example 1 of the present application;
fig. 4 is a surface state diagram of a product after coating of a tantalum electrolytic capacitor produced in example 1 of the present application.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
The embodiment of the invention provides a preparation method of a manganese dioxide cathode of a welding-resistant tantalum electrolytic capacitor, which comprises the following steps:
1) Providing a tantalum core anode coated with a tantalum pentoxide dielectric film, and placing the anode in a reactor having a specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Dipping in manganese nitrate solutions with different specific gravities, decomposing with high temperature steam, and repeatedly operating to form an inner cathode layer on the tantalum pentoxide dielectric film;
2) Immersing the sample obtained in step 1 into the solution with specific gravity of 1.30g/cm for multiple times 3 ～2.00g/cm 3 In the manganese nitrate solution with the decomposition accelerator of 0.01 to 8 percent by mass, the decomposition accelerator is one or a plurality of compounds of citric acid, p-toluenesulfonyl hydrazine, urea and ammonium nitrate. Taking out after each impregnation, placing the impregnated product at the temperature of 75-180 ℃ and the vapor pressure of 0.02-0.05 MPa, and pre-drying the impregnated product for 5-10 minutes under the condition that the mass percentage concentration of oxygen is 7-10%, so as to perform surface homogenization treatment;
3) And (3) decomposing the sample obtained in the step (2) for 5-7 minutes under the conditions that the temperature is 200-280 ℃, the water vapor pressure is 0.02-0.05 MPa and the oxygen mass percentage concentration is 6-12%, so as to carry out thermal decomposition, and forming an outer cathode layer on the surface of the sample.
Further, in the step S2, the specific gravity of the manganese nitrate solution has a gradient change, which is a first specific gravity, a second specific gravity, and a third specific gravity in this order, the first specific gravity is smaller than the second specific gravity, and the second specific gravity is larger than the third specific gravity. In order to further improve the compactness of the manganese dioxide outer layer, when preparing the outer cathode layer, the specific gravity of the manganese nitrate solution used is a certain gradient, namely, firstly the manganese nitrate solution with smaller specific gravity is used, then the manganese nitrate solution with larger specific gravity is used, and finally the manganese nitrate solution with smaller specific gravity is used for preparing the manganese nitrate.
The manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor is prepared by adopting the preparation method of the manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor.
A preparation method of a solid sheet type tantalum electrolytic capacitor comprises a preparation step of a tantalum core anode, a preparation step of a tantalum pentoxide dielectric film, a preparation method of a manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor and a packaging step. The preparation method of the tantalum core anode and the preparation method of the tantalum pentoxide dielectric film are both carried out in the conventional mode, and the tantalum core anode is formed by compression molding and sintering at high temperature under vacuum conditions. The tantalum pentoxide dielectric film is prepared by adopting an electrochemical mode.
The solid chip tantalum electrolytic capacitor is basically the same as the traditional chip solid electrolyte tantalum electrolytic capacitor in structure mode, and is prepared by the preparation method of the solid chip tantalum electrolytic capacitor. Firstly, according to the design, the tantalum powder particles are pressed and molded, vacuum sintering is carried out to obtain a tantalum core anode, then a tantalum pentoxide dielectric film is formed in an electrochemical mode, manganese dioxide is coated on the tantalum core anode as a cathode, finally, core block assembly is carried out, and products are molded and sealed by epoxy resin. However, the preparation method of the manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor is adopted in the preparation process of the manganese dioxide cathode because of being a high-safety product, and a new preparation process and a manganese nitrate solution formula are adopted to finally prepare the high-stability tantalum electrolytic capacitor.
In order to achieve the aim of controlling the process of decomposing manganese nitrate into manganese dioxide, the invention adds a decomposition accelerator into manganese nitrate solution for preparing manganese dioxide. In the process of decomposing manganese nitrate into manganese dioxide, a manganese nitrate homogenization treatment process is designed, and before a manganese nitrate solution on the surface of a tantalum electrolytic capacitor is decomposed into manganese dioxide, a decomposition accelerator is decomposed before manganese nitrate, so that manganese nitrate is uniformly distributed on the surface of the tantalum electrolytic capacitor, and finally a uniformly distributed manganese dioxide layer is obtained by decomposition.
The present invention is further illustrated by the following examples, which are not intended to limit the scope or applicability of the invention.
Example 1
The embodiment provides a preparation method of a solid sheet type tantalum electrolytic capacitor, which comprises the following steps:
1) Anode design: tantalum metal powder with uniform particle size is selected, the weight of the tantalum powder is calculated, tantalum wires are inserted into the tantalum powder and pressed into square blocks, and then the tantalum powder is sintered into the porous substrate tantalum core anode under the conditions of high temperature and vacuum.
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution.
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Soaking in manganese nitrate solution with different specific gravity, decomposing with high temperature vapor, and repeating the operation for several times to form manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.50g/cm 3 、2.00g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Wherein, 0.01 percent of p-toluenesulfonyl hydrazide by mass percentage is added into the manganese nitrate solution. Taking out after each impregnation and placing at 110 ℃ to ensure the vapor pressurePre-drying for 5 minutes under the condition that the strength is 0.02MPa and the oxygen mass percentage concentration is 10%. Then decomposing the tantalum core for 5 minutes under the conditions that the temperature is 230 ℃, the vapor pressure is 0.05MPa and the oxygen mass percentage concentration is 8%, and obtaining a sample surface which is a manganese dioxide outer cathode layer.
5) Assembling a high-stability chip tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode obtained in the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Example 2:
the embodiment provides a preparation method of a solid sheet type tantalum electrolytic capacitor, which comprises the following steps:
1) Anode design: tantalum metal powder with uniform particle size is selected, the weight of the tantalum powder is calculated, tantalum wires are inserted into the tantalum powder and pressed into square blocks, and then the tantalum powder is sintered into the porous substrate tantalum core anode under the conditions of high temperature and vacuum.
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution.
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Soaking in manganese nitrate solution with different specific gravity, decomposing with high temperature vapor, and repeating the operation for several times to form manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.50g/cm 3 、2.00g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Wherein, ammonium nitrate with the mass fraction of 0.1% is added into the manganese nitrate solution. Taking out after each soaking and placing at 150 ℃ to obtain water vapor with pressurePre-drying for 7 minutes under the condition of 0.03MPa and oxygen mass percentage concentration of 8 percent. Then decomposing the tantalum core for 5 minutes under the conditions that the temperature is 260 ℃, the vapor pressure is 0.05MPa and the oxygen mass percentage concentration is 8%, and obtaining a sample surface which is a manganese dioxide outer cathode layer.
5) Assembling a high-stability chip tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode obtained in the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Example 3:
the embodiment provides a preparation method of a solid sheet type tantalum electrolytic capacitor, which comprises the following steps:
1) Anode design: tantalum metal powder with uniform particle size is selected, the weight of the tantalum powder is calculated, tantalum wires are inserted into the tantalum powder and pressed into square blocks, and then the tantalum powder is sintered into the porous substrate tantalum core anode under the conditions of high temperature and vacuum.
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution.
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Soaking in manganese nitrate solution with different specific gravity, decomposing with high temperature vapor, and repeating the operation for several times to form manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.40g/cm 3 、1.90g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Wherein 8% of urea by mass is added into the manganese nitrate solution. Taking out after each soaking, placing at 160deg.C, water vapor pressure of 0.02MPa, and oxygenPre-drying for 10 minutes under the condition that the mass percentage concentration of the air is 10 percent. Then decomposing the tantalum core for 6 minutes under the conditions that the temperature is 220 ℃, the vapor pressure is 0.05MPa and the oxygen mass percentage concentration is 8%, and obtaining a sample surface which is a manganese dioxide outer cathode layer.
5) Assembling a high-stability chip tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode obtained in the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Comparative example 1:
the comparative example proposes a method for manufacturing a solid sheet type tantalum electrolytic capacitor, comprising the following steps:
1) Anode design: selecting tantalum metal powder with uniform particle size, calculating the weight of the tantalum powder, inserting tantalum wires into the tantalum powder, pressing the tantalum wire into square blocks, and sintering the tantalum wire into a porous substrate tantalum core anode under the conditions of high temperature and vacuum;
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution;
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Dipping in manganese nitrate solution, decomposing with high temperature steam, and repeating the operation for several times to form the manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.50g/cm 3 、2.00g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Taking out after each soaking, and pre-drying for 10 minutes under the conditions that the temperature is 120 ℃, the water vapor pressure is 0.02MPa and the oxygen mass percentage concentration is 10%. The tantalum core is then heated to 260 DEG CThe water vapor pressure is 0.05MPa, and the sample is decomposed for 5 minutes under the condition that the mass percentage concentration of oxygen is 8 percent, and the surface of the obtained sample is a manganese dioxide outer cathode layer.
5) Assembled sheet type tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode after the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Comparative example 2
The comparative example proposes a method for manufacturing a solid sheet type tantalum electrolytic capacitor, comprising the following steps:
1) Anode design: selecting tantalum metal powder with uniform particle size, calculating the weight of the tantalum powder, inserting tantalum wires into the tantalum powder, pressing the tantalum wire into square blocks, and sintering the tantalum wire into a porous substrate tantalum core anode under the conditions of high temperature and vacuum;
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution;
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Dipping in manganese nitrate solution, decomposing with high temperature steam, and repeating the operation for several times to form the manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing the tantalum core anode with the manganese dioxide inner layer into the solution with the specific gravity of 1.70g/cm for multiple times 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Taking out after each soaking, and pre-drying for 10 minutes under the conditions that the temperature is 120 ℃, the water vapor pressure is 0.02MPa and the oxygen mass percentage concentration is 10%. Then decomposing the tantalum core for 5 minutes under the conditions that the temperature is 260 ℃, the vapor pressure is 0.05MPa and the oxygen mass percentage concentration is 8%, and obtaining a sample surface which is a manganese dioxide outer cathode layer.
5) Assembled sheet type tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode after the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Comparative example 3
The comparative example proposes a method for manufacturing a solid sheet type tantalum electrolytic capacitor, comprising the following steps:
1) Anode design: selecting tantalum metal powder with uniform particle size, calculating the weight of the tantalum powder, inserting tantalum wires into the tantalum powder, pressing the tantalum wire into square blocks, and sintering the tantalum wire into a porous substrate tantalum core anode under the conditions of high temperature and vacuum;
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution;
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Dipping in manganese nitrate solution, decomposing with high temperature steam, and repeating the operation for several times to form the manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.50g/cm 3 、2.00g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Then decomposing the tantalum core for 5 minutes under the conditions that the temperature is 260 ℃, the vapor pressure is 0.05MPa and the oxygen mass percentage concentration is 8%, and obtaining a sample surface which is a manganese dioxide outer cathode layer.
5) Assembled sheet type tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode after the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Comparative example 4
The comparative example proposes a method for manufacturing a solid sheet type tantalum electrolytic capacitor, comprising the following steps:
1) Anode design: selecting tantalum metal powder with uniform particle size, calculating the weight of the tantalum powder, inserting tantalum wires into the tantalum powder, pressing the tantalum wire into square blocks, and sintering the tantalum wire into a porous substrate tantalum core anode under the conditions of high temperature and vacuum;
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution;
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Dipping in manganese nitrate solution, decomposing with high temperature steam, and repeating the operation for several times to form the manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.50g/cm 3 、2.00g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Wherein, 5% ethanol is added to the manganese nitrate solution as a dispersing agent. Then decomposing the tantalum core for 5 minutes under the conditions that the temperature is 260 ℃, the vapor pressure is 0.05MPa and the oxygen mass percentage concentration is 8%, and obtaining a sample surface which is a manganese dioxide outer cathode layer.
5) Assembled sheet type tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode after the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Comparative example 5
The comparative example proposes a method for manufacturing a solid sheet type tantalum electrolytic capacitor, comprising the following steps:
1) Anode design: selecting tantalum metal powder with uniform particle size, calculating the weight of the tantalum powder, inserting tantalum wires into the tantalum powder, pressing the tantalum wire into square blocks, and sintering the tantalum wire into a porous substrate tantalum core anode under the conditions of high temperature and vacuum;
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution;
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Dipping in manganese nitrate solution, decomposing with high temperature steam, and repeating the operation for several times to form the manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.50g/cm 3 、2.00g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Wherein, 1% sodium lignin sulfonate is added in manganese nitrate solution as viscosity reducer, then tantalum core is decomposed for 5 minutes under the conditions of 260 ℃ temperature, 0.05MPa water vapor pressure and 8% oxygen mass percentage concentration, and the obtained sample surface is manganese dioxide outer cathode layer.
5) Assembled sheet type tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode after the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
Comparative example 6
The comparative example proposes a method for manufacturing a solid sheet type tantalum electrolytic capacitor, comprising the following steps:
1) Anode design: selecting tantalum metal powder with uniform particle size, calculating the weight of the tantalum powder, inserting tantalum wires into the tantalum powder, pressing the tantalum wire into square blocks, and sintering the tantalum wire into a porous substrate tantalum core anode under the conditions of high temperature and vacuum;
2) Forming a dielectric film: nitric acid is used as electrolyte to prepare aqueous solution as forming solution, and the tantalum core anode is electrochemically formed into a tantalum pentoxide dielectric film with uniform thickness and good consistency on the surface of the tantalum core anode in the forming solution;
3) Manufacturing a manganese dioxide inner cathode layer: placing the tantalum core anode with the formed tantalum pentoxide dielectric film into a reactor with the specific gravity of 1.00g/cm 3 ～1.30g/cm 3 Dipping in manganese nitrate solution, decomposing with high temperature steam, and repeating the operation for several times to form the manganese dioxide inner cathode layer.
4) Manufacturing a manganese dioxide outer cathode layer: immersing tantalum core anode with manganese dioxide inner layer into the solution with specific gravity of 1.50g/cm 3 、2.00g/cm 3 And 1.30g/cm 3 Each impregnation time was 5 minutes in the manganese nitrate solution. Wherein, 1% sodium lignin sulfonate is added into the manganese nitrate solution as a viscosity reducer, and 5% ethanol is added into the manganese nitrate solution as a dispersing agent. Then decomposing the tantalum core for 5 minutes under the conditions that the temperature is 260 ℃, the vapor pressure is 0.05MPa and the oxygen mass percentage concentration is 8%, and obtaining a sample surface which is a manganese dioxide outer cathode layer.
5) Assembled sheet type tantalum electrolytic capacitor: and (3) preparing a graphite layer and a silver layer outside the tantalum core anode after the step (4) in sequence in a dipping mode, then attaching the tantalum core anode on a lead frame cathode by using silver paste, connecting a tantalum wire of the tantalum core anode with a positive lead frame in a resistance welding mode, and then carrying out mould pressing encapsulation, ageing and testing by using epoxy resin.
The solid sheet type tantalum electrolytic capacitors prepared in examples 1 to 3 and comparative example were subjected to an aging test, a leakage test and a reflow soldering test, and the results shown in table 1 were obtained.
Table 1 comparative and example burn-in, leakage and reflow test yield statistics
Fig. 1 and 2 show the surface morphology of manganese dioxide and the surface state of the coated product of comparative example 1, and fig. 3 and 4 show the surface morphology of manganese dioxide and the surface state of the coated product of example 1, respectively, and it can be seen from comparison that the surface particles of the manganese dioxide layer of comparative example 1 are coarse, the manganese dioxide layer at the edge portion of the tantalum block is obviously raised, the surface of the manganese dioxide layer of example 1 is obviously flatter, and the thickness of the manganese dioxide layer at the edge and other portions of the tantalum block is uniform. As can be seen from the figure: the manganese dioxide layer on the surface of the tantalum electrolytic capacitor after being coated is uniformly distributed, the uniformity is good, the qualification rate of the finished product after aging is higher, and the product has no leakage current increase or short circuit failure after being subjected to a welding heat resistance test in a reflow soldering mode.
According to the invention, the process of decomposing manganese nitrate into manganese dioxide is controlled by improving the formula of the manganese nitrate solution and the preparation process, so that the purpose of improving the structural consistency of the manganese dioxide electrolyte layer on the surface of the tantalum electrolytic capacitor is achieved, the welding heat resistance of the tantalum electrolytic capacitor is greatly improved while the excellent performance of the tantalum electrolytic capacitor is maintained, and the use stability of the tantalum electrolytic capacitor is improved.
While the present invention has been described with reference to the specific embodiments thereof, the scope of the present invention is not limited thereto, and any changes or substitutions will be apparent to those skilled in the art within the scope of the present invention, and are intended to be covered by the present invention. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (10)
1. The preparation method of the manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor is characterized by comprising the following steps of:
1) Providing a tantalum core anode coated with a tantalum pentoxide dielectric film, immersing in manganese nitrate solutions with different specific gravities within a first specific gravity range, performing high-temperature vapor decomposition, and forming an inner cathode layer on the tantalum pentoxide dielectric film after repeated operation for a plurality of times;
2) Immersing the sample obtained in the step 1 into a manganese nitrate solution with a decomposition accelerator in a second specific gravity range for multiple times, taking out the sample after each immersion, placing the sample at a temperature of 75-180 ℃, placing the sample at a water vapor pressure of 0.02-0.05 MPa, pre-drying the sample for 5-10 minutes under the condition that the mass percentage concentration of oxygen is 7-10%, and carrying out surface homogenization treatment;
3) And (3) carrying out thermal decomposition on the sample obtained in the step (2) to form an outer cathode layer on the surface of the sample.
2. The method for preparing the manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor of claim 1, wherein the decomposition accelerator is one or more of citric acid, p-toluenesulfonyl hydrazide, urea and ammonium nitrate.
3. The method for producing a manganese dioxide cathode for a weld-resistant tantalum electrolytic capacitor according to claim 1 or 2, wherein the mass fraction of the decomposition accelerator in the manganese nitrate solution having the decomposition accelerator in the second specific gravity range is 0.01 to 8%.
4. The method of producing a manganese dioxide cathode for a weld-resistant tantalum electrolytic capacitor according to claim 1, wherein said first specific weight range is 1.00g/cm 3 ～1.30g/cm 3 。
5. The method for producing a manganese dioxide cathode for a tantalum electrolytic capacitor of claim 1 wherein said second specific gravity range is 1.30g/cm 3 ～2.00g/cm 3 。
6. The method for producing a manganese dioxide cathode for a tantalum electrolytic capacitor resistant to welding according to claim 1, wherein the manganese nitrate solution in step S2 has a gradient change in specific gravity, in order of a first specific gravity, a second specific gravity, and a third specific gravity, the first specific gravity being smaller than the second specific gravity, and the second specific gravity being larger than the third specific gravity.
7. The method for preparing a manganese dioxide cathode for a welding-resistant tantalum electrolytic capacitor according to claim 1, wherein the conditions for thermal decomposition in said step 3 are: the temperature is 200-280 ℃, the vapor pressure is 0.02-0.05 MPa, and the decomposition is carried out for 5-7 minutes under the condition that the oxygen mass percentage concentration is 6-12%.
8. A manganese dioxide cathode for a weld-resistant tantalum electrolytic capacitor prepared by the method of any one of claims 1 to 7.
9. A method for preparing a solid sheet type tantalum electrolytic capacitor, which is characterized by comprising a step for preparing a tantalum core anode, a step for preparing a tantalum pentoxide dielectric film and a method for preparing a manganese dioxide cathode of the welding-resistant tantalum electrolytic capacitor as claimed in any one of claims 1 to 7.
10. A solid-chip tantalum electrolytic capacitor, which is characterized by being prepared by the preparation method of the solid-chip tantalum electrolytic capacitor as claimed in claim 9.
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