CN115223798A - Manufacturing method of axially-led organic polymer tantalum fixed capacitor - Google Patents
Manufacturing method of axially-led organic polymer tantalum fixed capacitor Download PDFInfo
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- CN115223798A CN115223798A CN202210905178.5A CN202210905178A CN115223798A CN 115223798 A CN115223798 A CN 115223798A CN 202210905178 A CN202210905178 A CN 202210905178A CN 115223798 A CN115223798 A CN 115223798A
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 239000003990 capacitor Substances 0.000 title claims abstract description 93
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 62
- 229920000620 organic polymer Polymers 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 80
- 229920000642 polymer Polymers 0.000 claims abstract description 52
- 239000000047 product Substances 0.000 claims abstract description 52
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 32
- 239000010439 graphite Substances 0.000 claims abstract description 32
- 229910052709 silver Inorganic materials 0.000 claims abstract description 32
- 239000004332 silver Substances 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 31
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- 229910052802 copper Inorganic materials 0.000 claims description 25
- 239000010949 copper Substances 0.000 claims description 25
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- DSSYKIVIOFKYAU-XVKPBYJWSA-N (1s,4r)-4,7,7-trimethylbicyclo[2.2.1]heptan-3-one Chemical compound C1C[C@@]2(C)C(=O)C[C@H]1C2(C)C DSSYKIVIOFKYAU-XVKPBYJWSA-N 0.000 claims description 16
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
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- 239000000243 solution Substances 0.000 description 68
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 11
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- 239000002245 particle Substances 0.000 description 9
- 239000011230 binding agent Substances 0.000 description 5
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- 238000010586 diagram Methods 0.000 description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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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
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
- H01G13/006—Apparatus or processes for applying terminals
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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
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
- H01G13/04—Drying; Impregnating
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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
- H01G9/0029—Processes of manufacture
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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
- H01G9/0029—Processes of manufacture
- H01G9/0036—Formation of the solid electrolyte layer
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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
- H01G9/004—Details
- H01G9/008—Terminals
- H01G9/012—Terminals specially adapted for solid capacitors
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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
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
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- H—ELECTRICITY
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- 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
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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- 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
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Abstract
The invention belongs to the technical field of capacitor manufacturing, and mainly comprises the pressing of an anode blank; calcining the anode blank to form an anode body; energizing the anode body, and dipping the anode body by using a high molecular solution in a vacuum dipping tank to form a high molecular polymer layer; firstly coating a graphite layer on a high polymer layer, then coating a silver paste layer to form a semi-finished product, assembling the semi-finished product to form a finished product, and carrying out aging screening on the finished product; the axially-led organic polymer tantalum fixed capacitor produced by the method comprises the following components: good high-frequency performance, high safety, large ripple and surge current impact resistance, strong self-repairing capability and high voltage, large capacity, no secondary damage of the oxide film, small leakage current, high production efficiency, environmental protection and the like.
Description
Technical Field
The invention belongs to the technical field of capacitor manufacturing, and particularly relates to a manufacturing method of an axially-led organic polymer tantalum fixed capacitor.
Background
The development of the tantalum capacitor industry and the continuous breakthrough of the technology are accelerated by the progress of the electronic technology in the current society, and the tantalum capacitor is not only applied to the aerospace field but also is widely matched with high-precision military electronic equipment in the fields of ships, weapons and the like. With the large-scale application of low impedance and high frequency circuits, higher demands are placed on tantalum capacitors. The solid electrolyte tantalum capacitor has the characteristics of low ESR (Equivalent Series Resistance), low loss tangent value, high stability, long service life, high reliability and the like. Therefore, the circuit is widely applied to the circuit of the whole machine.
At present, solid electrolyte tantalum capacitors taking manganese dioxide as electrolyte need to be decomposed at high temperature in the manufacturing process, gas released after thermal decomposition is not environment-friendly, and the dielectric film is easily damaged at high temperature. Thereby affecting the electrical performance of the capacitor. The Mn02 has high oxygen content, and when defects exist in the dielectric layer, the dielectric layer is easy to burn under the action of an external voltage. Manganese dioxide as an electrolyte has low conductivity and poor capacity-frequency characteristics. With increasing frequency, capacity fading is severe. Therefore, the polymer conductive polymer material, PEDOT for short, is the mainstream of development in the market, and is a new generation of conductive polymer developed by German scientists in the middle and later 80 years of the 20 th century. PEDOT not only has very high conductivity (about 300 s/era), but also has very high stability in an oxidized state, most of the high-molecular conductive polymers adopted as electrolytes in the current market are chip tantalum capacitors, and due to small volume, limited capacity is led out, and resin plastic packaging is adopted, so that the electrical performance parameters can be influenced by moisture when the packages are placed in the air for a long time.
Disclosure of Invention
The invention mainly aims to solve the defects of tantalum capacitors taking polymers as electrolytes in the market and the performance problem of traditional manganese dioxide as electrolytes, and provides a manufacturing method for axially leading out an organic polymer tantalum fixed capacitor by combining the polymerization characteristic of high conductivity of a polymer material, so that the electrical properties (including capacity, leakage current, ESR and loss) are very stable in various complex environments, and the organic polymer tantalum fixed capacitor manufactured by the method has the advantages of high voltage resistance and the like.
The technical scheme of the invention is as follows:
a manufacturing method of an axially-led organic polymer tantalum fixed capacitor is characterized by comprising the following steps:
the method comprises the following steps: placing tantalum powder and a tantalum wire into a die cavity, and applying pressure to the tantalum powder in the die cavity by using a forming machine to form an anode blank with a tantalum core;
step two: putting the pressed anode blank into a sintering furnace for calcining to form an anode body with a micro-porous structure;
step three: welding the tantalum cores of the anode bodies on the steel bars by using a spot welder to form a group, placing the steel bars on a process frame, and energizing the anode bodies by using an electrochemical method to form a layer of compact Ta on the surfaces of the anode bodies 2 O 5 An oxide film;
step four: carrying a high polymer material solution by using a vacuum impregnation tank, and impregnating the anode body of the oxide film generated in the third step under the pressure condition of (-60 to-80 kpa) + -2 kpa, wherein the high polymer material solution is PEDOT solution, the solid content in the PEDOT solution is 0.8-9%, and the viscosity value is 1000-2500 mPa.S; the vacuum impregnation tank is automatically descended, the lifting speed is 0.01-0.03 mm/s, and the impregnation time is 10-15 min;
step five: airing the impregnated anode body at normal temperature for 5-8 min, then curing at high temperature, raising the temperature to 125 ℃, and keeping the constant temperature for 10-15 min after reaching the target temperature;
step six: repeating the processes of the fourth step and the fifth step for 12 to 25 times according to the specification of the capacitor, and forming a high polymer layer on the surface of the oxide film of the anode body;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high polymer layer of the anode body after the six steps are completed, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, and drying at the following temperatures: 150 +/-3 ℃; raising the temperature from room temperature to a target temperature, keeping the constant temperature for 30min +/-3 min, and then lap-welding a tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and D, aging and screening the finished products in the step eight, and removing unqualified products.
Further, the process of energizing the anode body by adopting the electrochemical method in the third step is that the anode body is put into energizing liquid at the temperature of 80 ℃, and an energizing constant voltage of 24V-320V is applied for 240min according to the specification of the capacitor; the energizing liquid is selected in relation to the energizing voltage when the energizing voltage is applied<80V, energized liquid selected to have a concentration of 0.1% HNO 3 A solution; when the energizing voltage is 80V or less and less than 180V, the selective concentration of the energizing liquid is 0.1% 3 PO 4 Mixing with 20% glycol; energized voltage of 180V or less<300V energized liquid selection concentration 0.1% 3 PO 4 Mixing with 50% glycol; an energizing voltage of not less than 300V an energizing liquid having a selected concentration of 0.1% 3 PO 4 Mixing with 75% ethylene glycol.
Further, when the process from the fourth step to the fifth step is repeated in the sixth step, the solid content of the polymer material solution in the fourth step needs to be measured before each product with one specification is soaked, the polymer material solution needs to be supplemented if the condition is not met, and the polymer solution needs to be stirred for 5-7 min by using a stirring paddle after the solution is supplemented until no obvious agglomeration exists; and the viscosity of the stirred polymer solution is measured.
Further, the method for measuring the viscosity of the polymer solution comprises the steps of pouring the polymer material solution into a 1000mL beaker, adjusting a viscometer to a horizontal position, selecting a rotor with the range of 0-25000 mPa & S, selecting the rotating speed of 120r/min, starting a main machine of the viscometer to ensure that the solution can not exceed the specified scale on the rotor, starting measurement, recording the read data after the value is stable, pressing a reset button, measuring three groups of data, and taking the average value of the three groups of data to obtain the viscosity value of the solution.
Further, camphor powder is uniformly mixed in the tantalum powder in the step one, and the mass of the camphor powder is 3% of that of the tantalum powder.
Further, in the ninth step, the aging process is to apply an aging voltage 1.1 to 1.2 times of the rated voltage of the finished product axially led out of the organic polymer tantalum fixed capacitor.
Further, the high-temperature curing process in the fifth step is that the temperature is increased to 55 ℃ from room temperature and is kept for 6min, then the temperature is increased to 85 ℃ and is kept for 1min, then the temperature is increased to 105 ℃ and is kept for 3min, finally the temperature is increased to 125 ℃ and is kept for 10-15 min according to the process.
The invention adopting the technical scheme can bring the following beneficial effects:
1. high frequency performance advantage
The high polymer material has conductivity dozens of times higher than that of the traditional MnO2 to form the high polymer electrolyte on the tantalum core of the solid tantalum capacitor, and the high-frequency performance is improved by the manufacturing method of the invention. The conventional manganese dioxide solid electrolyte tantalum capacitor loses more than half of its capacity at 100KHZ frequency, the commercial polymer used as the electrolyte tantalum capacitor loses more than eighty percent of its capacity at 100KHZ frequency, and the axial organic polymer tantalum fixed capacitor retains at least ninety-five percent of its capacity at 100KHZ frequency. The sudden reduction of capacitance below the frequency of 100KHZ improves the circuit filtering performance of the capacitor in the frequency range of the DC-DC conversion circuit.
2. Has high safety
When the organic polymer tantalum fixed capacitor fails, the cathode polymer generates oxygen absorption reaction, so that the contact between anode tantalum powder and oxygen is isolated, combustion cannot occur even if the product fails, and the organic polymer tantalum fixed capacitor has safety.
3. Resistant big ripple and surge current impact
The organic polymer tantalum fixed capacitor manufactured by the method of the present invention has high capacitance and small loss tangent in a high frequency range, and can accommodate larger ripple current.
4. Strong self-repairing ability
Compared with the prior art, the polymer electrolyte layer manufactured by the manufacturing method has denser molecular gap micron-scale, when a capacitor is damaged, current can be collected at a flaw position, and the polymer at the flaw position can be gasified by local overheating to repair the flaw.
5. High voltage and large capacity
The high molecular impregnation work in the vacuum impregnation equipment breaks the tension between molecules, more molecules can be brought in under the vacuum state, and compared with the organic high molecular material in the market, the product of the invention has better capacity extraction as electrolyte and compact film layer and high pressure resistance.
6. Avoid the secondary damage of the oxide film and reduce the leakage current
The temperature of the whole process of the polymer used as the electrolyte manufacturing process does not exceed 150 ℃, the damage caused by the fact that the oxide film exceeds the bearable temperature range is avoided, and the leakage current level is improved.
7. High production efficiency and environmental protection
The whole manufacturing process of the invention has no environmental pollution, the most important polymer is used as the electrolyte manufacturing process and adopts a physical polymerization mode, compared with the chemical polymerization mode on the market, the whole process has no residue and needs cleaning, the operation is simple, the production efficiency is high, no chemical product is generated, and the invention is environment-friendly.
Drawings
FIG. 1 is a schematic structural diagram of an axially-leaded organic polymer tantalum fixed capacitor manufactured by the method of the present invention;
FIG. 2 is a block diagram of a process flow of the present invention;
FIG. 3 is a graph of curing temperature versus time for the present invention.
In the figure, 1-anode lead, 2-tantalum wire3-copper shell, 4-tantalum core, 5-solder, 6-Ta 2 O 5 An oxide film, a 7-high polymer layer, an 8-graphite layer and a 9-silver paste layer. 10-cathode lead.
Detailed Description
As shown in fig. 2, a method for manufacturing an axially-extended organic polymer tantalum fixed capacitor includes the following steps:
the method comprises the following steps: placing tantalum powder and a tantalum wire into a die cavity, and applying pressure to the tantalum powder in the die cavity by using a forming machine to form an anode blank with a tantalum core;
step two: putting the pressed anode blank into a sintering furnace for calcining to form an anode body with a micro porous structure;
step three: welding the tantalum cores of the anode bodies on the steel bars by using a spot welder to form a group, placing the steel bars on a process frame, and energizing the anode bodies by using an electrochemical method to form a layer of compact Ta on the surfaces of the anode bodies 2 O 5 An oxide film;
step four: carrying a high molecular material solution by using a vacuum impregnation tank, and impregnating the anode body with the oxide film generated in the third step under the pressure condition of (-60 to-80 kpa) + -2 kpa, wherein the high molecular material solution is PEDOT solution, the solid content in the PEDOT solution is 0.8 to 9 percent, and the viscosity value is 1000 to 2500mPa.S; the vacuum impregnation tank bearing automatically descends, the lifting speed is 0.01-0.03 mm/s, and the impregnation time is 10-15 min;
step five: airing the impregnated anode body at normal temperature for 5-8 min, then curing at high temperature, raising the temperature to 125 ℃, and keeping the constant temperature for 10-15 min after reaching the target temperature;
step six: repeating the processes of the fourth step and the fifth step for 12 to 25 times according to the specification of the capacitor, and forming a high polymer layer on the surface of the oxide film of the anode body;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high polymer layer of the anode body after the six steps are completed, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa.s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, wherein the drying temperature of the graphite layer and the silver paste layer is as follows: 150 +/-3 ℃; raising the temperature from room temperature to a target temperature, keeping the constant temperature for 30min +/-3 min, and then lap-welding a tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and D, aging and screening the finished products in the step eight, and removing unqualified products.
Further, the process of energizing the anode body by adopting the electrochemical method in the third step is that the anode body is put into energizing liquid at the temperature of 80 ℃, and an energizing constant voltage of 24V-320V is applied for 240min according to the specification of the capacitor; selecting an energizing liquid in relation to an energizing voltage, the energizing liquid being selected to be a solution having a concentration of 0.1% HNO3 when the energizing voltage is < 80V; when the energizing voltage is less than or equal to 80V and less than 180V, the energizing liquid is selected from a mixed solution of H3PO4 and 20 percent of glycol with the concentration of 0.1 percent; energizing voltage of 180V or less and energizing voltage of 300V, the concentration of the energizing liquid is 0.1 percent, the H3PO4 and 50 percent of glycol mixed solution are selected; the energizing voltage is more than or equal to 300V, the concentration of the energizing liquid is 0.1 percent, and the energizing liquid is mixed with 75 percent of glycol.
Further, when the process from the fourth step to the fifth step is repeated in the sixth step, the solid content of the polymer material solution in the fourth step needs to be measured before each product with one specification is soaked, the polymer material solution needs to be supplemented if the condition is not met, and the polymer solution needs to be stirred for 5-7 min by using a stirring paddle after the solution is supplemented until no obvious agglomeration exists; and the viscosity of the stirred polymer solution is measured. Further, the method for measuring the viscosity of the polymer solution comprises the steps of pouring the polymer material solution into a 1000mL beaker, adjusting a viscometer to a horizontal position, selecting a rotor with the range of 0-25000 mPa & S, selecting the rotating speed of 120r/min, starting a main machine of the viscometer to ensure that the solution can not exceed the specified scale on the rotor, starting measurement, recording the read data after the value is stable, pressing a reset button, measuring three groups of data, and taking the average value of the three groups of data to obtain the viscosity value of the solution.
Further, camphor powder is uniformly mixed in the tantalum powder in the step one, and the mass of the camphor powder is 3% of that of the tantalum powder.
Further, in the ninth step, the aging process is to apply an aging voltage 1.1 to 1.2 times of the rated voltage of the finished product axially led out of the organic polymer tantalum fixed capacitor.
Further, in the fifth step, the high-temperature curing process is to raise the temperature from room temperature to 55 ℃, maintain for 6min, then raise the temperature to 85 ℃, maintain for 1min, then raise the temperature to 105 ℃, maintain for 3min, finally raise the temperature to 125 ℃, maintain for 10-15 min, the temperature raising process refers to the curing curve diagram of fig. 3, in the diagram, the horizontal axis is time, the vertical axis is temperature, and the room temperature is 25 ℃, although the temperature raising rate is fast, the physical polymerization speed is also accelerated, but as the curing temperature rises, the curing speed is accelerated, larger particles are easy to form, on one hand, the immersion property is reduced, so that air bubble residues still exist in the tantalum block; on the other hand, some branched chains may be formed in the main chain of the polymer, thereby changing the conjugated structure of the main chain, so that the self-conductivity is reduced. Finally, ESR and loss of the capacitor are increased, and the surface of a high polymer electrolyte layer formed after high polymer impregnation and curing can be dense and flat according to a curing curve.
Example 1
The manufacturing specification is as follows: 16V and 680 muF to axially lead out an organic polymer tantalum fixed capacitor;
the method comprises the following steps: uniformly mixing 2251mg of tantalum powder and 67.53mg of camphor powder, putting the mixture into a die cavity with the size of phi 7mm x 9mm, inserting a tantalum wire with the size of phi 0.6mm into the center of the mixed powder for pressing, wherein the camphor powder is used as a binder, and putting an anode blank formed by pressing and forming the tantalum wire core with the size of phi 0.6mm into a sintering furnace for calcining to form an anode body with a micro-porous structure;
step three: welding tantalum cores of anode bodies on the steel bar by using a spot welder to form a group, placing the steel bar on a process frame, and energizing the anode bodies by using an electrochemical method to form a layer of compact Ta2O5 oxide film on the surfaces of the anode bodies, wherein the specific process comprises the steps of putting the anode bodies into an ethylene glycol energizing liquid with the concentration of 0.1% HNO3+20% at the temperature of 80 ℃, applying 80V energizing constant voltage and keeping the voltage for 240min;
step four: carrying a PEDOT solution by using a vacuum impregnation tank, and impregnating the anode body with the oxide film generated in the third step under the vacuum state of-60 kpa +/-2 kpa, wherein the solid content in the PEDOT solution is 0.8-9%, and the viscosity value is 1500mPa.S; the vacuum impregnation tank is automatically descended, the lifting speed is 0.03mm/s, the impregnation time is 12min, the liquid level of high polymer is required to be level in the manufacturing process, the overflow is consistent, no air bubble exists, no turbidity phenomenon exists and any visible impurities exist, and as the particles are unevenly distributed in the particle size of each molecule impregnated in the high polymer material solution to form tension on the surface of the product, the vacuum negative pressure value and the impregnation automation parameters are set, so that each molecule breaks through the tension formed on the surface of the product in the whole impregnation process and is impregnated into the pores in the tantalum core;
step five: airing the impregnated anode body at normal temperature for 6min, then curing the aired anode body, and referring to a curing temperature curve in fig. 3, raising the temperature from room temperature to 55 ℃ for 6min, then raising the temperature to 85 ℃ for 1min, then raising the temperature to 105 ℃ for 3min, finally raising the temperature to 125 ℃ for 10min, wherein the horizontal axis is time, the vertical axis is temperature, and the room temperature is 25 ℃;
step six: repeating the process of the fourth step to the fifth step for 22 times to form a high polymer layer on the surface of the oxide film of the anode body, wherein the solid content of the high polymer material solution in the fourth step needs to be measured before dipping a product with a specification when the process of the fourth step to the sixth step is repeated, the high polymer material solution needs to be supplemented if the condition is not met, and the high polymer solution needs to be stirred by a stirring paddle for 5-7 min after the solution is supplemented until no obvious agglomeration exists; measuring the viscosity of the stirred polymer solution until the fixed content reaches a set value;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high-molecular polymer layer of the anode body after the six processes are finished, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa.s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, wherein the drying temperature of the graphite layer and the silver paste layer is as follows: 150 +/-3 ℃; after the temperature is increased from room temperature to the target temperature along with the temperature, the drying time is as follows: timing when the target temperature is reached within 30 +/-3 min, and lap-welding the tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and e, applying a voltage 1.2 times the rated voltage of the finished product in the step eight to carry out aging screening, and removing unqualified products.
The manufacture by the method of example 1 is given in table 1 below: comparison of loss, ESR and leakage of 169v, 680uF axially-led organic polymer tantalum fixed capacitor with the existing polymer electrolyte capacitor with the same specification and chip tantalum polymer electrolyte capacitor with the same specification:
TABLE 1
Example 2
The manufacturing specification is as follows: an organic polymer tantalum fixed capacitor is led out axially from the capacitor at 4V,5600 muF;
the method comprises the following steps: uniformly mixing 4000mg of tantalum powder and 120mg of camphor powder, putting the mixture into a die cavity with the size of phi 7mm x 16mm, inserting a tantalum wire with the size of phi 0.6mm into the center of the mixed powder for pressing, wherein the camphor powder is used as a binder, and putting an anode blank formed by pressing in a tantalum wire core with the size of phi 0.6mm into a sintering furnace for calcining so as to form an anode body with a micro-porous structure;
step three: welding the tantalum cores of the anode bodies on the steel bars by a spot welding machine to form a group, placing the steel bars on a process frame,energizing the anode body by an electrochemical method to form a layer of compact Ta on the surface of the anode body 2 O 5 Oxide film, wherein the specific process is to put the anode body into the concentration of 0.1% HNO under the condition of 80 deg.C 3 Applying 13V energizing constant voltage in the energizing liquid for 240min;
step four: carrying a PEDOT solution by using a vacuum impregnation tank, and impregnating the anode body with the oxide film generated in the third step under the vacuum state of-60 kpa +/-2 kpa, wherein the solid content in the PEDOT solution is 0.8-9%, and the viscosity value is 1500mPa.S; the vacuum impregnation tank is automatically descended, the lifting speed is 0.03mm/s, the impregnation time is 15min, the liquid level of a high polymer is required to be horizontal in the manufacturing process, the overflow is consistent, no bubbles exist, no turbidity phenomenon exists and any visible impurities exist, and as the particles of all molecules impregnated in the high polymer material solution are unevenly distributed to form tension on the surface of a product, the vacuum negative pressure value and the impregnation automation parameters are set, so that all molecules break through the tension formed on the surface of the product in the whole impregnation process to be impregnated into the internal pores of the tantalum core;
step five: drying the impregnated anode body in the air at normal temperature for 6min, then curing the dried anode body, referring to a curing temperature curve in FIG. 3, raising the temperature from room temperature to 55 ℃, keeping for 6min, then raising the temperature to 85 ℃, keeping for 1min, then raising the temperature to 105 ℃, keeping for 3min, finally raising the temperature to 125 ℃, keeping for 10min, wherein the horizontal axis in the figure is time, the vertical axis is temperature, and the room temperature is 25 ℃;
step six: repeating the process of the fourth step and the sixth step for 25 times to form a high polymer layer on the surface of the oxide film of the anode body, wherein when the process of the fourth step and the sixth step is repeated, the solid content of the high polymer material solution in the fourth step needs to be measured before dipping a product with a specification, the high polymer material solution needs to be supplemented if the condition is not met, and the high polymer solution needs to be stirred by a stirring paddle for 5-7 min after the solution is supplemented until no obvious agglomeration exists; measuring the viscosity of the stirred polymer solution until the fixed content reaches a set value;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high polymer layer of the anode body after the six steps are completed, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa.s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, wherein the drying temperature of the graphite layer and the silver paste layer is as follows: 150 +/-3 ℃; after the temperature is increased from room temperature to the target temperature along with the temperature, the drying time is as follows: timing when the target temperature is reached within 30min +/-3 min, and lap-welding the tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and e, applying a voltage 1.2 times the rated voltage of the finished product in the step eight to carry out aging screening, and removing unqualified products.
The results obtained by the method of example 2 are given in table 2 below: comparing the loss, ESR and leakage of the 4V,5600uF axially-led organic polymer tantalum fixed capacitor with those of the existing polymer electrolyte capacitor with the same specification and the chip tantalum polymer electrolyte capacitor with the same specification:
TABLE 2
Example 3
The manufacturing specification is as follows: 125V,68 muF of axial lead-out organic polymer tantalum fixed capacitor;
the method comprises the following steps: uniformly mixing 6028mg tantalum powder and 180.84mg camphor powder, putting the mixture into a die cavity with the size phi of 8mm x 15mm, inserting a tantalum wire with the size phi of 0.6mm into the center of the mixed powder for pressing, wherein the camphor powder is used as a binder, and putting an anode blank formed by pressing in a tantalum wire core with the size phi of 0.6mm into a sintering furnace for calcining so as to form an anode body with a micro-porous structure;
step three: applying tantalum to the anode body by means of a spot welderThe core is welded on the steel bar to form a group, the steel bar is arranged on a process frame, and the anode body is energized by an electrochemical method, so that a layer of compact Ta is formed on the surface of the anode body 2 O 5 Oxide film, wherein the specific process is that the anode body is put into a concentration of 0.1% H under the condition of 80 ℃ 3 PO 4 Applying 310V energizing constant voltage to +75% ethylene glycol energizing liquid for 240min;
step four: carrying PEDOT solution by using a vacuum impregnation tank, and impregnating the anode body with the oxide film generated in the third step under the vacuum state of-65 kpa +/-2 kpa, wherein the solid content in the PEDOT solution is 0.8-9%, and the viscosity value is 1500mPa.S; the vacuum impregnation tank is automatically descended, the lifting speed is 0.03mm/s, the impregnation time is 10min, the liquid level of a high polymer is required to be horizontal in the manufacturing process, the overflow is consistent, no bubbles exist, no turbidity phenomenon exists and any visible impurities exist, and as the particles of all molecules impregnated in the high polymer material solution are unevenly distributed to form tension on the surface of a product, the vacuum negative pressure value and the impregnation automation parameters are set, so that all molecules break through the tension formed on the surface of the product in the whole impregnation process to be impregnated into the internal pores of the tantalum core;
step five: airing the impregnated anode body at normal temperature for 6min, then curing the aired anode body, and referring to a curing temperature curve in fig. 3, raising the temperature from room temperature to 55 ℃ for 6min, then raising the temperature to 85 ℃ for 1min, then raising the temperature to 105 ℃ for 3min, finally raising the temperature to 125 ℃ for 10min, wherein the horizontal axis is time, the vertical axis is temperature, and the room temperature is 25 ℃;
step six: repeating the process of the fourth step and the sixth step for 25 times to form a high polymer layer on the surface of the oxide film of the anode body, wherein when the process of the fourth step and the sixth step is repeated, the solid content of the high polymer material solution in the fourth step needs to be measured before dipping a product with a specification, the high polymer material solution needs to be supplemented if the condition is not met, and the high polymer solution needs to be stirred by a stirring paddle for 5-7 min after the solution is supplemented until no obvious agglomeration exists; measuring the viscosity of the stirred polymer solution until the fixed content reaches a set value;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high polymer layer of the anode body after the six steps are completed, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa.s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, wherein the drying temperature of the graphite layer and the silver paste layer is as follows: 150 +/-3 ℃; after the temperature is increased from room temperature to the target temperature, the drying time is as follows: timing when the target temperature is reached within 30min +/-3 min, and lap-welding the tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and e, applying a voltage 1.1 times the rated voltage of the finished product in the step eight to carry out aging screening, and removing unqualified products.
The results produced by the method of example 3 are given in table 3 below: comparison of loss, ESR and leakage of 125V,68 muF axially-led organic polymer tantalum fixed capacitor with the existing polymer electrolyte capacitor with the same specification and chip tantalum polymer electrolyte capacitor with the same specification:
TABLE 3
Example 4
The manufacturing specification is as follows: an organic polymer tantalum fixed capacitor is axially led out from the capacitor body of 4V,4.7 muF;
the method comprises the following steps: uniformly mixing 17mg of tantalum powder and 0.51mg of camphor powder, putting the mixture into a die cavity with the size phi of 1.5mm x 1.5mm, inserting tantalum wires with the size phi of 0.4mm into the center of the mixed powder for pressing, wherein the camphor powder is used as a binder, and putting an anode blank formed by pressing in a tantalum wire core with the size phi of 0.6mm into a sintering furnace for calcining to form an anode body with a micro-porous structure;
step three: welding the tantalum cores of the anode bodies on the steel bars by using a spot welder to form a group, placing the steel bars on a process frame, and energizing the anode bodies by using an electrochemical method to form a layer of compact Ta on the surfaces of the anode bodies 2 O 5 Oxide film, wherein the specific process is to put the anode body into the concentration of 0.1% HNO under the condition of 80 deg.C 3 In the energizing liquid, 60V energizing constant voltage is applied for 240min;
step four: carrying a PEDOT solution by using a vacuum impregnation tank, and impregnating the anode body with the oxide film generated in the third step under the vacuum state of-65 kpa +/-2 kpa, wherein the solid content in the PEDOT solution is 0.8-9%, and the viscosity value is 1500mPa.S; the vacuum impregnation tank is automatically descended, the lifting speed is 0.03mm/s, the impregnation time is 10min, the liquid level of high polymer is required to be level in the manufacturing process, the overflow is consistent, no air bubble exists, no turbidity phenomenon exists and any visible impurities exist, and as the particles are unevenly distributed in the particle size of each molecule impregnated in the high polymer material solution to form tension on the surface of the product, the vacuum negative pressure value and the impregnation automation parameters are set, so that each molecule breaks through the tension formed on the surface of the product in the whole impregnation process and is impregnated into the pores in the tantalum core;
step five: drying the impregnated anode body in the air at normal temperature for 6min, then curing the dried anode body, referring to a curing temperature curve in FIG. 3, raising the temperature from room temperature to 55 ℃, keeping for 6min, then raising the temperature to 85 ℃, keeping for 1min, then raising the temperature to 105 ℃, keeping for 3min, finally raising the temperature to 125 ℃, keeping for 10min, wherein the horizontal axis in the figure is time, the vertical axis is temperature, and the room temperature is 25 ℃;
step six: repeating the process of the fourth step to the sixth step for 12 times to form a high polymer layer on the surface of the oxide film of the anode body, wherein the solid content of the high polymer material solution in the fourth step needs to be measured before dipping a product with a specification when the process of the fourth step to the sixth step is repeated, the high polymer material solution needs to be supplemented when the condition is not met, and the high polymer solution needs to be stirred by a stirring paddle for 5-7 min after the solution is supplemented until no obvious agglomeration exists; measuring the viscosity of the stirred polymer solution until the fixed content reaches a set value;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high polymer layer of the anode body after the six steps are completed, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, wherein the drying temperature of the graphite layer and the silver paste layer is as follows: 150 +/-3 ℃; after the temperature is increased from room temperature to the target temperature along with the temperature, the drying time is as follows: timing when the target temperature is reached within 30min +/-3 min, and lap-welding a tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and e, applying a voltage 1.2 times the rated voltage of the finished product in the step eight to carry out aging screening, and removing unqualified products.
The results obtained by the method of example 4 are given in table 4 below: comparing the loss, ESR and leakage of the axial lead-out organic polymer tantalum fixed capacitor of 4V,4.7 muF with the loss, ESR and leakage of the existing polymer electrolyte capacitor and the chip tantalum polymer electrolyte capacitor of the same specification:
TABLE 4
Example 5
The manufacturing specification is as follows: 50V,280 muF of organic polymer tantalum fixed capacitors are axially led out;
the method comprises the following steps: uniformly mixing 6899mg of tantalum powder and 206.97mg of camphor powder, putting the mixture into a die cavity with the size phi 8.3mm x 17mm, inserting tantalum wire with the size phi 0.6mm into the center of the mixed powder for pressing, wherein the camphor powder is used as a binder, and putting an anode blank formed by pressing in a tantalum wire core with the size phi 0.6mm into a sintering furnace for calcining to form an anode body with a micro-porous structure;
step three: welding the tantalum cores of the anode body on the steel bar into a group by using a spot welding machine, arranging the steel bar on a process rack, and energizing the anode body by using an electrochemical method to form a layer of compact Ta on the surface of the anode body 2 O 5 Oxide film, wherein the specific process is putting the anode body into a concentration of 0.1% H under the condition of 80 ℃% 3 PO 4 Applying 197V energizing constant voltage to +50% ethylene glycol energizing liquid for 240min;
step four: carrying a PEDOT solution by using a vacuum impregnation tank, and impregnating the anode body with the oxide film generated in the third step under the vacuum state of-65 kpa +/-2 kpa, wherein the solid content in the PEDOT solution is 0.8-9%, and the viscosity value is 1500mPa.S; the vacuum impregnation tank is automatically descended, the lifting speed is 0.03mm/s, the impregnation time is 10min, the liquid level of high polymer is required to be level in the manufacturing process, the overflow is consistent, no air bubble exists, no turbidity phenomenon exists and any visible impurities exist, and as the particles are unevenly distributed in the particle size of each molecule impregnated in the high polymer material solution to form tension on the surface of the product, the vacuum negative pressure value and the impregnation automation parameters are set, so that each molecule breaks through the tension formed on the surface of the product in the whole impregnation process and is impregnated into the pores in the tantalum core;
step five: drying the impregnated anode body in the air at normal temperature for 6min, then curing the dried anode body, referring to a curing temperature curve in FIG. 3, raising the temperature from room temperature to 55 ℃, keeping for 6min, then raising the temperature to 85 ℃, keeping for 1min, then raising the temperature to 105 ℃, keeping for 3min, finally raising the temperature to 125 ℃, keeping for 10min, wherein the horizontal axis in the figure is time, the vertical axis is temperature, and the room temperature is 25 ℃;
step six: repeating the process of the fourth step to the sixth step for 24 times to form a high polymer layer on the surface of the oxide film of the anode body, wherein the solid content of the high polymer material solution in the fourth step needs to be measured before dipping a product with a specification when the process of the fourth step to the sixth step is repeated, the high polymer material solution needs to be supplemented when the condition is not met, and the high polymer solution needs to be stirred by a stirring paddle for 5-7 min after the solution is supplemented until no obvious agglomeration exists; measuring the viscosity of the stirred polymer solution until the fixed content reaches a set value;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high polymer layer of the anode body after the six steps are completed, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa.s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, wherein the drying temperature of the graphite layer and the silver paste layer is as follows: 150 +/-3 ℃; after the temperature is increased from room temperature to the target temperature along with the temperature, the drying time is as follows: timing when the target temperature is reached within 30min +/-3 min, and lap-welding a tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and e, applying a voltage 1.2 times the rated voltage of the finished product in the step eight to carry out aging screening, and removing unqualified products.
The results obtained by the method of example 5 are given in table 5 below: 50V, comparison of loss, ESR and leakage of a 280 mu F axial extraction organic polymer tantalum fixed capacitor with the existing polymer electrolyte capacitor with the same specification and a chip type tantalum polymer electrolyte capacitor with the same specification:
TABLE 5
By utilizing the manufacturing method of the axially-led organic polymer tantalum fixed capacitor provided by the invention, the axially-led organic polymer tantalum fixed capacitor with the rated voltage of 4-125V, the capacity of 4.7-5600 muF and the ESR of 30-500 m omega can be manufactured, on one hand, compared with the product performance of the same specification in the prior art, on the other hand, the product performance is greatly improved, on the other hand, the market blank is filled, and the method has extremely high popularization value.
Claims (7)
1. A manufacturing method of an axially-led organic polymer tantalum fixed capacitor is characterized by comprising the following steps:
the method comprises the following steps: placing tantalum powder and a tantalum wire into a die cavity, and applying pressure to the tantalum powder in the die cavity by using a forming machine to form an anode blank with a tantalum core;
step two: putting the pressed anode blank into a sintering furnace for calcining to form an anode body with a micro-porous structure;
step three: welding the tantalum cores of the anode body on the steel bar into a group by using a spot welding machine, arranging the steel bar on a process rack, and energizing the anode body by using an electrochemical method to form a layer of compact Ta on the surface of the anode body 2 O 5 An oxide film;
step four: carrying a high polymer material solution by using a vacuum impregnation tank, and impregnating the anode body of the oxide film generated in the third step under the pressure condition of (-60 to-80 kpa) + -2 kpa, wherein the high polymer material solution is PEDOT solution, the solid content in the PEDOT solution is 0.8-9%, and the viscosity value is 1000-2500 mPa.S; the vacuum impregnation tank is automatically descended, the lifting speed is 0.01-0.03 mm/s, and the impregnation time is 10-15 min;
step five: airing the impregnated anode body at normal temperature for 5-8 min, then curing at high temperature, raising the temperature to 125 ℃, and keeping the constant temperature for 10-15 min after reaching the target temperature;
step six: repeating the processes of the fourth step and the fifth step for 12 to 25 times according to the specification of the capacitor, and forming a high polymer layer on the surface of the oxide film of the anode body;
step seven: and (3) sequentially coating a graphite layer and a silver paste layer on the high polymer layer of the anode body after the six steps are completed, wherein the graphite viscosity requirement is as follows: 300 to 500 mPas; the viscosity requirement of the silver paste is as follows: 2000-3000 mPa s viscosity, coating at normal temperature, drying after the graphite layer and the silver paste layer are coated for 30min, and drying at the following temperatures: 150 +/-3 ℃; raising the temperature from room temperature to a target temperature, keeping the constant temperature for 30min +/-3 min, and then lap-welding a tantalum wire to lead out an anode lead of the capacitor to form a semi-finished product;
step eight: arranging the semi-finished product in the seventh step on a copper shell in a soldering mode, leading out a pole lead of a cathode capacitor from the bottom of the copper shell, and sealing the upper part of the copper shell by adopting glass insulating powder to form a finished product of the fixed capacitor with the organic polymer tantalum axially led out;
step nine: and D, aging and screening the finished products in the step eight, and removing unqualified products.
2. The method for manufacturing an axially-extended organic polymer tantalum fixed capacitor according to claim 1, wherein the method comprises the following steps: the process of energizing the anode body by adopting the electrochemical method in the third step is that the anode body is put into energizing liquid at the temperature of 80 ℃, and 24-320V energizing constant voltage is applied according to the specification of the capacitor for 240min; the energizing liquid is selected in relation to the energizing voltage when the energizing voltage is applied<80V, energized liquid selected to have a concentration of 0.1% HNO 3 A solution; when the energizing voltage is 80V or less and less than 180V, the selective concentration of the energizing liquid is 0.1% 3 PO 4 Mixing with 20% glycol; energized voltage of 180V or less<300V energized liquid selection concentration 0.1% 3 PO 4 Mixing with 50% glycol; an energizing voltage of not less than 300V an energizing liquid having a selected concentration of 0.1% 3 PO 4 Mixing with 75% ethylene glycol.
3. The method for manufacturing an axially-extracted organic polymer tantalum fixed capacitor according to claim 1, wherein the method comprises the following steps: when the process from the fourth step to the fifth step is repeated in the sixth step, the solid content of the polymer material solution in the fourth step needs to be measured before each product with one specification is soaked, the polymer material solution needs to be supplemented if the condition is not met, and the polymer solution needs to be stirred for 5-7 min by using a stirring paddle after the solution is supplemented until no obvious agglomeration exists; and the viscosity of the stirred polymer solution is measured.
4. The method for manufacturing an axially-extended organic polymer tantalum fixed capacitor according to claim 3, wherein the method comprises the following steps: the method for measuring the viscosity of the high polymer solution comprises the steps of pouring the high polymer material solution into a 1000mL beaker, adjusting a viscometer to a horizontal position, selecting a rotor with the range of 0-25000 mPa.S, selecting 120r/min as a rotating speed, starting a main machine of the viscometer to start measurement if the solution is ensured to be capable of submerging specified scales on the rotor, recording read data after the value is stable, and then pressing a reset button to measure three groups of data and taking the average value of the three groups of data to obtain the viscosity value of the solution.
5. The method for manufacturing an axially-extended organic polymer tantalum fixed capacitor according to claim 1, wherein the method comprises the following steps: in the first step, camphor powder is uniformly mixed in the tantalum powder, and the mass of the camphor powder is 3% of that of the tantalum powder.
6. The method for manufacturing an axially-extracted organic polymer tantalum fixed capacitor according to claim 1, wherein the method comprises the following steps: and the aging process in the ninth step is to apply aging voltage which is 1.1 to 1.2 times of the rated voltage of the finished product axially led out of the organic polymer tantalum fixed capacitor.
7. The method for manufacturing an axially-extended organic polymer tantalum fixed capacitor according to claim 1, wherein the method comprises the following steps: and the high-temperature curing process in the step five is that the temperature is increased to 55 ℃ from room temperature and is kept for 6min, then the temperature is increased to 85 ℃ and is kept for 1min, then the temperature is increased to 105 ℃ and is kept for 3min, and finally the temperature is increased to 125 ℃ and is kept for 10-15 min.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100265634A1 (en) * | 2009-04-20 | 2010-10-21 | Yuri Freeman | High voltage and high efficiency polymer electrolytic capacitors |
CN102270535A (en) * | 2011-05-13 | 2011-12-07 | 株洲宏达电子有限公司 | Method for manufacturing polymer ethylenedioxythiophene (PEDT) cathode plate type tantalum electrolytic capacitor by two-step method |
CN104319103A (en) * | 2014-11-10 | 2015-01-28 | 株洲宏达电子有限公司 | Metal shell packaged polymer tantalum capacitor and preparation method thereof |
CN111696786A (en) * | 2020-05-19 | 2020-09-22 | 北京七一八友益电子有限责任公司 | Preparation method of high-voltage chip type solid electrolyte tantalum capacitor |
CN114360911A (en) * | 2021-11-01 | 2022-04-15 | 北京七一八友益电子有限责任公司 | Method for preparing chip type solid electrolyte tantalum capacitor |
-
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- 2022-07-29 CN CN202210905178.5A patent/CN115223798A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100265634A1 (en) * | 2009-04-20 | 2010-10-21 | Yuri Freeman | High voltage and high efficiency polymer electrolytic capacitors |
CN102270535A (en) * | 2011-05-13 | 2011-12-07 | 株洲宏达电子有限公司 | Method for manufacturing polymer ethylenedioxythiophene (PEDT) cathode plate type tantalum electrolytic capacitor by two-step method |
CN104319103A (en) * | 2014-11-10 | 2015-01-28 | 株洲宏达电子有限公司 | Metal shell packaged polymer tantalum capacitor and preparation method thereof |
CN111696786A (en) * | 2020-05-19 | 2020-09-22 | 北京七一八友益电子有限责任公司 | Preparation method of high-voltage chip type solid electrolyte tantalum capacitor |
CN114360911A (en) * | 2021-11-01 | 2022-04-15 | 北京七一八友益电子有限责任公司 | Method for preparing chip type solid electrolyte tantalum capacitor |
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