CN111180212A - Tantalum capacitor anode and energizing process thereof, tantalum capacitor and preparation method thereof - Google Patents
Tantalum capacitor anode and energizing process thereof, tantalum capacitor and preparation method thereof Download PDFInfo
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- CN111180212A CN111180212A CN201911424328.5A CN201911424328A CN111180212A CN 111180212 A CN111180212 A CN 111180212A CN 201911424328 A CN201911424328 A CN 201911424328A CN 111180212 A CN111180212 A CN 111180212A
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- tantalum
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- acid
- tantalum core
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 167
- 239000003990 capacitor Substances 0.000 title claims abstract description 55
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000008569 process Effects 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 97
- 238000010438 heat treatment Methods 0.000 claims abstract description 66
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 238000005554 pickling Methods 0.000 claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 26
- 230000015572 biosynthetic process Effects 0.000 claims description 26
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 150000007522 mineralic acids Chemical class 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229920001940 conductive polymer Polymers 0.000 abstract description 15
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000003466 welding Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000013073 enabling process Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 63
- 238000009835 boiling Methods 0.000 description 58
- 238000005507 spraying Methods 0.000 description 49
- 239000008367 deionised water Substances 0.000 description 32
- 229910021641 deionized water Inorganic materials 0.000 description 32
- 239000000243 solution Substances 0.000 description 32
- 230000006872 improvement Effects 0.000 description 16
- 230000000295 complement effect Effects 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 238000005476 soldering Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- H01G9/14—Structural combinations or circuits for modifying, or compensating for, electric characteristics of electrolytic capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Powder Metallurgy (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention provides a tantalum capacitor anode, an enabling process thereof, a tantalum capacitor and a preparation method thereof. The energized process includes the steps of pickling, forming, heat treating, and post-forming. According to the energizing process, impurities, particularly metal impurities, in the sintered tantalum core are removed through acid washing, a more uniform and compact dielectric oxide film is obtained through optimization of conditions such as current density, boosting time, formed liquid temperature and heat treatment temperature, the probability of short circuit breakdown of the conductive polymer chip tantalum capacitor when the conductive polymer chip tantalum capacitor is electrified for the first time after high-temperature welding is reduced, and the welding heat resistance of the conductive polymer chip tantalum capacitor dielectric oxide film is improved.
Description
Technical Field
The invention relates to the field of capacitors, in particular to a tantalum capacitor anode and an enabling process thereof, a tantalum capacitor and a preparation method thereof.
Background
With the wide application of the conductive polymer chip type tantalum capacitor, the quality requirements of users on electronic components are gradually improved in the application process of the conductive polymer chip type tantalum capacitor, wherein the requirements are particularly significant in the fields of automobile industry and military industry.
At present, a small part of conductive polymer chip tantalum capacitors can generate short circuit failure when being electrified for the first time after being welded at high temperature in the use process. In order to reduce the probability of short circuit failure of the conductive polymer chip tantalum capacitor when the conductive polymer chip tantalum capacitor is electrified for the first time after high-temperature welding, the process needs to be optimized and improved, so that the welding heat resistance of the conductive polymer chip tantalum capacitor is improved.
Disclosure of Invention
The invention aims to provide a tantalum capacitor anode, an enabling process of the tantalum capacitor anode, a tantalum capacitor and a preparation method of the tantalum capacitor.
In order to achieve the above object, the present invention provides the following technical solutions.
In a first aspect, the invention provides a process for energizing an anode of a tantalum capacitor, comprising:
pickling the sintered tantalum core, removing the pickling solution on the surface of the tantalum core, and then drying;
electrifying the dried tantalum core to form a tantalum core, wherein the temperature of a forming liquid is 45-90 ℃, boosting the tantalum core to a forming voltage by constant current in the forming process, then performing constant voltage treatment, wherein the current density is 1.5-6.5 mA/piece, and the boosting time is 3-12 hours;
removing residual forming liquid on the surface of the tantalum core, and then carrying out heat treatment, wherein the temperature of the heat treatment is 255-365 ℃;
and (4) cooling the tantalum core after the heat treatment is finished, and then performing compensation formation.
As a further improvement of the above technical solution, the acid washing solution includes at least one of an organic acid solution and an inorganic acid solution, the organic acid solution includes at least one of acetic acid, citric acid and acetic acid, and the inorganic acid solution includes at least one of a nitric acid solution, phosphoric acid and sulfuric acid.
As a further improvement of the technical scheme, the concentration of the pickling solution is 10 wt% -50 wt%.
As a further improvement of the technical scheme, the pickling time is 30-60 min.
As a further improvement of the technical scheme, the acid washing solution for removing the surface of the tantalum core is removed by water washing, and the time of the water washing is 30-120 min.
As a further improvement of the above technical solution, the drying is drying.
As a further improvement of the technical scheme, the drying temperature is 120-150 ℃, and the drying time is 30-60 min.
As a further improvement of the above technical means, the forming liquid contains at least one of phosphoric acid, nitric acid, and acetic acid.
As a further improvement of the technical scheme, the concentration of the forming liquid is 0.5-1 g/L.
As a further improvement of the technical scheme, the forming voltage is 48-128V.
As a further improvement of the technical scheme, the constant-pressure treatment time is 3-12 hours.
As a further improvement of the technical scheme, the forming liquid for removing the residual on the surface of the tantalum core is removed by spraying and boiling.
As a further improvement of the technical scheme, the spraying liquid used for spraying is deionized water, and the spraying time is 2-10 min.
As a further improvement of the technical scheme, the boiling and washing liquid used for boiling and washing is deionized water, the boiling and washing temperature is 25-95 ℃, and the boiling and washing time is 30-90 min.
As a further improvement of the technical scheme, the heat treatment time is 20 min-60 min.
As a further improvement of the technical scheme, the temperature reduction condition is that the temperature is reduced to room temperature after being placed at room temperature.
As a further improvement of the technical scheme, the complementary forming condition is constant pressure for 3-4 hours.
In a second aspect, the invention provides a tantalum capacitor anode, which is obtained by subjecting a sintered tantalum core to the energizing process described in the first aspect.
In a third aspect, the present invention provides a method for producing a tantalum capacitor, comprising the energization process as described in the first aspect.
In a fourth aspect, the present invention provides a tantalum capacitor comprising the tantalum capacitor anode of the second aspect.
The invention has the beneficial effects that: in the tantalum capacitor anode energizing process, impurities, particularly metal impurities, in a sintered tantalum core are removed through acid washing, a more uniform and compact dielectric oxide film is obtained through optimization of conditions such as current density, boosting time, formed liquid temperature, heat treatment temperature and the like, the probability of short circuit breakdown problem of the conductive polymer chip tantalum capacitor when the conductive polymer chip tantalum capacitor is electrified for the first time after high-temperature welding is reduced, and the welding heat resistance of the conductive polymer chip tantalum capacitor dielectric oxide film is improved.
Detailed Description
The terms as used herein:
"prepared from … …" is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of … …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of … …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "1 ~ 5" is disclosed, the ranges described should be construed to include the ranges "1 ~ 4", "1 ~ 3", "1 ~ 2 and 4 ~ 5", "1 ~ 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In these examples, the parts and percentages are by mass unless otherwise indicated.
"part by mass" means a basic unit of measure indicating a mass ratio of a plurality of components, and 1 part may represent any unit mass, for example, 1g or 2.689 g. If we say that the part by mass of the component A is a part by mass and the part by mass of the component B is B part by mass, the ratio of the part by mass of the component A to the part by mass of the component B is a: b. alternatively, the mass of the A component is aK and the mass of the B component is bK (K is an arbitrary number, and represents a multiple factor). It is unmistakable that, unlike the parts by mass, the sum of the parts by mass of all the components is not limited to 100 parts.
"and/or" is used to indicate that one or both of the illustrated conditions may occur, e.g., a and/or B includes (a and B) and (a or B).
In a first aspect, the invention provides a process for energizing an anode of a tantalum capacitor, comprising:
pickling the sintered tantalum core, removing the pickling solution on the surface of the tantalum core, and then drying;
electrifying the dried tantalum core to form a tantalum core, wherein the temperature of a forming liquid is 45-90 ℃, boosting the tantalum core to a forming voltage by constant current in the forming process, then performing constant voltage treatment, wherein the current density is 1.5-6.5 mA/piece, and the boosting time is 3-12 hours;
removing residual forming liquid on the surface of the tantalum core, and then carrying out heat treatment, wherein the temperature of the heat treatment is 255-365 ℃;
and (4) cooling the tantalum core after the heat treatment is finished, and then performing compensation formation.
According to the invention, in the energizing process of the anode of the tantalum capacitor, impurities, especially metal impurities, in the sintered tantalum core are removed by acid washing, the boosting is carried out by adopting a lower current density, the boosting time is prolonged, the influence of high-current density boosting on the heating of the tantalum core is relieved, meanwhile, a dielectric oxide film is subjected to high-temperature treatment by adopting higher forming liquid temperature and higher heat treatment temperature, the high-temperature resistance of the dielectric oxide film is improved by complementary formation repair, the leakage current increasing amplitude and the breakdown voltage reducing amplitude of the conductive polymer chip tantalum capacitor after reflow soldering can be effectively reduced, the soldering heat resistance of the conductive polymer chip tantalum capacitor is improved, and more directly, the probability of short circuit failure of the conductive polymer chip tantalum capacitor after high-temperature soldering can be reduced.
The acid washing solution may be an organic acid solution, an inorganic acid solution, or a mixed solution of an organic acid and an inorganic acid, the organic acid solution may be at least one of acetic acid, citric acid, and acetic acid, and the inorganic acid solution may be at least one of a nitric acid solution, phosphoric acid, and sulfuric acid.
In some embodiments of the invention, the concentration of the acid wash solution is between 10 wt% and 50 wt%.
In some embodiments of the present invention, the pickling time is 30 to 60 min.
And removing the pickling solution on the surface of the tantalum core after pickling by washing with water, wherein the washing time is 30-120 min. After washing, the tantalum core can be dried in a drying mode, the drying temperature can be 120-150 ℃, and the drying time can be 30-60 min.
In some embodiments of the present invention, the forming liquid contains at least one of phosphoric acid, nitric acid, and acetic acid.
In some embodiments of the present invention, the concentration of the forming liquid is 0.5 to 1 g/L.
In some embodiments of the present invention, the forming voltage is 48-128V.
In some embodiments of the present invention, the constant pressure treatment time is 3 to 12 hours.
And forming liquid is remained on the surface of the tantalum core subjected to constant-pressure treatment, the remaining forming liquid can be removed in a spraying mode, the used spraying liquid is generally deionized water, and the spraying time can be 2-10 min. In order to remove the residual forming liquid completely, the tantalum core can be further boiled and washed after being sprayed, the boiling and washing liquid used for boiling and washing is generally deionized water, the boiling and washing temperature can be 25-95 ℃, and the boiling and washing time can be 30-90 min.
In some embodiments of the invention, the heat treatment time is 20min to 60 min.
And cooling the tantalum core after the heat treatment to room temperature, and then performing subsequent complementary formation treatment, wherein the room temperature is about 25 ℃.
In some embodiments of the present invention, the formation conditions are constant pressure for 3-4 hours, and the forming liquid, the forming liquid temperature, the forming voltage, the current density, etc. are the same as those in the forming step.
In a second aspect, the invention provides a tantalum capacitor anode, which is obtained by subjecting a sintered tantalum core to the energizing process described in the first aspect.
In a third aspect, the present invention provides a method for producing a tantalum capacitor, comprising the energization process as described in the first aspect.
In a fourth aspect, the present invention provides a tantalum capacitor comprising the tantalum capacitor anode of the second aspect.
Embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
Take 16V220 muF (7.3X 4.3X 2.8) and tantalum powder as an example, 16V70000 muF.V/g. The energizing process of the tantalum capacitor anode comprises the following steps:
(1) acid washing: 20000g of deionized water and 20000g of nitric acid are uniformly mixed, then poured into a pickling tank, the sintered tantalum core is pickled for 60 minutes, washed with water for 120 minutes after pickling, and then placed into an oven to be dried for 60 minutes at 150 ℃.
(2) Preparing a forming solution: with 50000g of deionized water and 30g of phosphoric acid, a mixture was prepared and placed in a forming (energized) apparatus, and the forming liquid was subjected to water circulation and water heating to heat the forming liquid to 45 ℃.
(3) Forming: and (3) putting the tantalum core after the acid washing into a forming (energizing) device for electrification, forming by electrifying at the rate of 6.5 mA/piece, boosting for 4 hours to form voltage of 48V, and performing constant voltage for 4 hours.
(4) Spraying: and (3) putting the tantalum core after the constant pressure is finished into a spraying groove, and spraying the tantalum core by using spraying liquid, wherein the spraying liquid is deionized water, and the spraying time is 10 min.
(5) Boiling and washing: and (3) putting the sprayed tantalum core into a boiling and washing tank, and boiling and washing the tantalum core by using a boiling and washing liquid, wherein the boiling and washing liquid is deionized water, the boiling and washing temperature is 25 ℃, and the boiling and washing time is 90 min.
(6) And (3) heat treatment: and (3) carrying out high-temperature heat treatment on the boiled tantalum core, wherein the heat treatment temperature is 255 ℃, the heat treatment time is 30 minutes, and the tantalum core is placed to the room temperature after the heat treatment is finished.
(7) Complementary formation (energization): the tantalum core after heat treatment is placed into a forming (energizing) device again for electrification forming, and the constant pressure is kept for 4 hours.
And after the completion of the formation, washing the tantalum core with water to remove the residual formation liquid, wherein the washing time is 90 minutes.
Example 2
Take 16V220 muF (7.3X 4.3X 2.8) and tantalum powder as an example, 16V70000 muF.V/g. The energizing process of the tantalum capacitor anode comprises the following steps:
(1) acid washing: 20000g of deionized water and 20000g of nitric acid are uniformly mixed, then poured into a pickling tank, the sintered tantalum core is pickled for 60 minutes, washed with water for 120 minutes after pickling, and then placed into an oven to be dried for 60 minutes at 150 ℃.
(2) Preparing a forming solution: with 50000g of deionized water and 30g of phosphoric acid, a mixture was prepared and placed in a forming (energized) apparatus, and the forming liquid was subjected to water circulation and water heating, and the forming liquid was heated to 65 ℃.
(3) Forming: and (3) putting the tantalum core after the acid washing into a forming (energizing) device for electrification, forming by electrifying at a rate of 4.5 mA/piece, boosting the pressure for 7 hours to form a voltage of 48V, and performing constant voltage for 8 hours.
(4) Spraying: and (3) putting the tantalum core after the constant pressure is finished into a spraying groove, and spraying the tantalum core by using spraying liquid, wherein the spraying liquid is deionized water, and the spraying time is 10 min.
(5) Boiling and washing: and (3) putting the sprayed tantalum core into a boiling and washing tank, and boiling and washing the tantalum core by using a boiling and washing liquid, wherein the boiling and washing liquid is deionized water, the boiling and washing temperature is 25 ℃, and the boiling and washing time is 90 min.
(6) And (3) heat treatment: and (3) carrying out high-temperature heat treatment on the boiled tantalum core, wherein the heat treatment temperature is 315 ℃, the heat treatment time is 30 minutes, and the tantalum core is placed to the room temperature after the heat treatment is finished.
(7) Complementary formation (energization): the tantalum core after heat treatment is placed into a forming (energizing) device again for electrification forming, and the constant pressure is kept for 4 hours.
And after the completion of the formation, washing the tantalum core with water to remove the residual formation liquid, wherein the washing time is 90 minutes.
Example 3
Take 16V220 muF (7.3X 4.3X 2.8) and tantalum powder as an example, 16V70000 muF.V/g. The energizing process of the tantalum capacitor anode comprises the following steps:
(1) acid washing: 20000g of deionized water and 20000g of nitric acid are uniformly mixed, then poured into a pickling tank, the sintered tantalum core is pickled for 60 minutes, washed with water for 120 minutes after pickling, and then placed into an oven to be dried for 30 minutes at 150 ℃.
(2) Preparing a forming solution: a mixture of 50000g of deionized water and 30g of phosphoric acid was prepared and placed in forming (energized) equipment, and the forming liquor was subjected to water circulation and water heating, at 85 ℃.
(3) Forming: and (3) putting the tantalum core after the acid washing into a forming (energizing) device for electrification, forming by electrifying at the rate of 2.5 mA/piece, boosting the pressure for 12 hours to form a voltage of 48V, and performing constant voltage for 12 hours.
(4) Spraying: and (3) putting the tantalum core after the constant pressure is finished into a spraying groove, and spraying the tantalum core by using spraying liquid, wherein the spraying liquid is deionized water, and the spraying time is 10 min.
(5) Boiling and washing: and (3) putting the sprayed tantalum core into a boiling and washing tank, and boiling and washing the tantalum core by using a boiling and washing liquid, wherein the boiling and washing liquid is deionized water, the boiling and washing temperature is 95 ℃, and the boiling and washing time is 90 min.
(6) And (3) heat treatment: and (3) carrying out high-temperature heat treatment on the boiled tantalum core, wherein the heat treatment temperature is 365 ℃, the heat treatment time is 30 minutes, and the tantalum core is placed to the room temperature after the heat treatment is finished.
(7) Complementary formation (energization): the tantalum core after heat treatment is placed into a forming (energizing) device again for electrification forming, and the constant pressure is kept for 4 hours.
And after the completion of the formation, washing the tantalum core with water to remove the residual formation liquid, wherein the washing time is 90 minutes.
Example 4
Take 50V47 μ F (7.3X 6.0X 4.1) and tantalum powder of 35V23000 μ F.V/g as an example. The energizing process of the tantalum capacitor anode comprises the following steps:
(1) acid washing: 20000g of deionized water and 20000g of nitric acid are uniformly mixed, then poured into a pickling tank, the sintered tantalum core is pickled for 60 minutes, washed with water for 120 minutes after pickling, and then placed into an oven to be dried for 60 minutes at 150 ℃.
(2) Preparing a forming solution: a mixture of 50000g of deionized water and 30g of phosphoric acid was prepared and placed in forming (energized) equipment, and the forming liquor was subjected to water circulation and water heating, at a temperature of 45 ℃.
(3) Forming: and (3) putting the tantalum core after the acid washing into a forming (energizing) device for energizing to form the tantalum core, energizing to form the tantalum core at the rate of 6.5 mA/piece, boosting the voltage for 3 hours to form a voltage of 128V, and performing constant voltage for 4 hours.
(4) Spraying: and (3) putting the tantalum core after the constant pressure is finished into a spraying groove, and spraying the tantalum core by using spraying liquid, wherein the spraying liquid is deionized water, and the spraying time is 10 min.
(5) Boiling and washing: and (3) putting the sprayed tantalum core into a boiling and washing tank, and boiling and washing the tantalum core by using a boiling and washing liquid, wherein the boiling and washing liquid is generally deionized water, the boiling and washing temperature is 25 ℃, and the boiling and washing time is 90 min.
(6) And (3) heat treatment: and (3) carrying out high-temperature heat treatment on the boiled tantalum core, wherein the heat treatment temperature is 255 ℃, the heat treatment time is 30 minutes, and the tantalum core is placed to the room temperature after the heat treatment is finished.
(7) Complementary formation (energization): the tantalum core after heat treatment is placed into a forming (energizing) device again for electrification forming, and the constant pressure is kept for 3 hours.
And after the completion of the formation, washing the tantalum core with water to remove the residual formation liquid, wherein the washing time is 90 minutes.
Example 5
Take 50V47 μ F (7.3X 6.0X 4.1) and tantalum powder of 35V23000 μ F.V/g as an example. The energizing process of the tantalum capacitor anode comprises the following steps:
(1) acid washing: 20000g of deionized water and 20000g of nitric acid are uniformly mixed, then poured into a pickling tank, the sintered tantalum core is pickled for 60 minutes, washed with water for 120 minutes after pickling, and then placed into an oven to be dried for 60 minutes at 150 ℃.
(2) Preparing a forming solution: a mixture of 50000g of deionized water and 30g of phosphoric acid was prepared and placed in forming (energized) equipment, and the forming liquor was subjected to water circulation and water heating, at 65 ℃.
(3) Forming: and (3) putting the tantalum core after the acid washing into a forming (energizing) device for electrification, forming by electrifying at a rate of 4.5 mA/machine, pressing for 7 hours until forming voltage is 128V, and performing constant voltage for 8 hours.
(4) Spraying: and (3) putting the tantalum core after the constant pressure is finished into a spraying groove, and spraying the tantalum core by using a spraying liquid, wherein the spraying liquid is generally deionized water, and the spraying time is 10 min.
(5) Boiling and washing: and (3) putting the sprayed tantalum core into a boiling and washing tank, and boiling and washing the tantalum core by using a boiling and washing liquid, wherein the boiling and washing liquid is generally deionized water, the boiling and washing temperature is 25 ℃, and the boiling and washing time is 90 min.
(6) And (3) heat treatment: and (3) carrying out high-temperature heat treatment on the boiled tantalum core, wherein the heat treatment temperature is 315 ℃, the heat treatment time is 30 minutes, and the tantalum core is placed to the room temperature after the heat treatment is finished.
(7) Complementary formation (energization): the tantalum core after heat treatment is placed into a forming (energizing) device again for electrification forming, and the constant pressure is kept for 3 hours.
And after the completion of the formation, washing the tantalum core with water to remove the residual formation liquid, wherein the washing time is 90 minutes.
Example 6
Take 50V47 μ F (7.3X 6.0X 4.1) and tantalum powder of 35V23000 μ F.V/g as an example. The energizing process of the tantalum capacitor anode comprises the following steps:
(1) acid washing: 20000g of deionized water and 20000g of nitric acid are uniformly mixed, then poured into a pickling tank, the sintered tantalum core is pickled for 60 minutes, washed with water for 120 minutes after pickling, and then placed into an oven to be dried for 30 minutes at 150 ℃.
(2) Preparing a forming solution: a mixture of 50000g of deionized water and 30g of phosphoric acid was prepared and placed in forming (energized) equipment, and the forming liquor was subjected to water circulation and water heating, at 85 ℃.
(3) Forming: and (3) putting the tantalum core after the acid washing into a forming (energizing) device for electrification, forming by electrifying at the rate of 2.5 mA/piece, boosting the pressure for 12 hours to form a voltage of 128V, and carrying out constant voltage for 11 hours.
(4) Spraying: and (3) putting the tantalum core after the constant pressure is finished into a spraying groove, and spraying the tantalum core by using a spraying liquid, wherein the spraying liquid is generally deionized water, and the spraying time is 10 min.
(5) Boiling and washing: and (3) putting the sprayed tantalum core into a boiling and washing tank, and boiling and washing the tantalum core by using a boiling and washing liquid, wherein the boiling and washing liquid is generally deionized water, the boiling and washing temperature is 25 ℃, and the boiling and washing time is 90 min.
(6) And (3) heat treatment: and (3) carrying out high-temperature heat treatment on the boiled tantalum core, wherein the heat treatment temperature is 365 ℃, the heat treatment time is 30 minutes, and the tantalum core is placed to the room temperature after the heat treatment is finished.
(7) Complementary formation (energization): the tantalum core after heat treatment is placed into a forming (energizing) device again for electrification forming, and the constant pressure is kept for 3 hours.
And after the completion of the formation, washing the tantalum core with water to remove the residual formation liquid, wherein the washing time is 90 minutes.
The electrical performance parameters of the tantalum capacitor anodes of examples 1-6 are shown in Table 1 below.
TABLE 1
After the tantalum capacitor anodes in examples 1 to 6 were subjected to polymerization, graphite and silver paste immersion, mold pressing and other processes under the same conditions, the product was subjected to a solder heat resistance test according to a reflow soldering curve having a peak temperature of 265. + -. 5 ℃ and a peak time of 30 sec. + -. 5sec, and a number of times of soldering of 2 times. Test product examples 1 to 6 100 samples were randomly sampled, and the actual U of the samples was 1.2 times that of the samples after the testRThe product was tested for short circuit after charging the product for 30sec (results are shown in table 2 below).
TABLE 2
Comparative example 1
16V220 muF (7.3 multiplied by 4.3 multiplied by 2.8), and the tantalum powder is 16V70000 muF.V/g. The energizing process of the tantalum capacitor anode comprises the following steps:
(1) acid washing: 20000g of deionized water and 20000g of nitric acid are uniformly mixed, then poured into a pickling tank, the sintered tantalum core is pickled for 60 minutes, washed with water for 120 minutes after pickling, and then placed into an oven to be dried for 60 minutes at 150 ℃.
(2) Preparing a forming solution: a mixture of 50000g of deionized water and 30g of phosphoric acid was prepared and placed in forming (energized) equipment, and the forming liquor was subjected to water circulation and water heating, at 25 ℃.
(3) Forming: and (3) putting the tantalum core after acid washing into a forming (energizing) device for electrification, electrifying at a rate of 10 mA/time to form a voltage of 48V, boosting for 2 hours, and then carrying out constant voltage for 3 hours.
(4) Spraying: and (3) putting the tantalum core with the constant pressure into a spraying groove, and spraying the tantalum core by using a spraying liquid, wherein the spraying liquid is generally deionized water, and the spraying time is 10 min.
(5) Boiling and washing: and (3) putting the sprayed tantalum core into a boiling and washing tank, and boiling and washing the tantalum core by using a boiling and washing liquid, wherein the boiling and washing liquid is generally deionized water, the boiling and washing temperature is 25 ℃, and the boiling and washing time is 90 min.
(6) And (3) heat treatment: and (3) carrying out high-temperature heat treatment on the tantalum core after washing, wherein the heat treatment temperature is 315 ℃, the heat treatment time is 30 minutes, and cooling at normal temperature after the heat treatment is finished.
(7) Complementary formation (energization): and putting the tantalum core subjected to the heat treatment into forming (energizing) equipment again for energizing, keeping the constant pressure for 2 hours, and washing the tantalum core with water after the constant pressure is finished for 90 minutes.
The tantalum capacitor formation sintering design, polymerization process, molding process, etc. of comparative example 1 are the same as those of example 3. The leakage current and breakdown voltage after reflow of 10 test products were randomly extracted from the 2 groups of products of example 3 and comparative example 1, respectively, and the peak temperature of the solder curve was 265. + -.5 ℃, the peak time was 30 sec. + -.5 sec, and the number of times of soldering was 2, and the test results thereof are shown in tables 3 and 4.
Table 3 comparison of experimental data for leakage current test after reflow soldering of example 3 and comparative example 1
| Leakage current (μ A) | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Mean value of |
| Before reflow soldering | 16 | 23 | 18 | 19 | 30 | 27 | 25 | 18 | 24 | 23 | 22.3 |
| Comparative example 1 | 46 | 54 | 63 | 69 | 72 | 54 | 68 | 72 | 61 | 72 | 64.1 |
| Example 3 | 24 | 27 | 21 | 25 | 26 | 24 | 28 | 25 | 28 | 24 | 25.2 |
Table 4 comparison of experimental data for breakdown voltage test after reflow soldering of example 3 and comparative example 1
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (10)
1. An energized process for tantalum capacitor anodes, comprising:
pickling the sintered tantalum core, removing the pickling solution on the surface of the tantalum core, and then drying;
electrifying the dried tantalum core to form a tantalum core, wherein the temperature of a forming liquid is 45-90 ℃, boosting the tantalum core to a forming voltage by constant current in the forming process, then performing constant voltage treatment, wherein the current density is 1.5-6.5 mA/piece, and the boosting time is 3-12 hours;
removing residual forming liquid on the surface of the tantalum core, and then carrying out heat treatment, wherein the temperature of the heat treatment is 255-365 ℃;
and (4) cooling the tantalum core after the heat treatment is finished, and then performing compensation formation.
2. The energized process of claim 1, wherein the acid wash solution comprises at least one of an organic acid solution comprising at least one of acetic acid, citric acid, acetic acid, an inorganic acid solution comprising at least one of nitric acid, phosphoric acid, sulfuric acid;
preferably, the concentration of the acid washing solution is 10 wt% to 50 wt%;
preferably, the pickling time is 30-60 min.
3. The energized process of claim 1, wherein the forming liquid comprises at least one of phosphoric acid, nitric acid, and acetic acid;
preferably, the concentration of the forming liquid is 0.5-1 g/L.
4. The energized process of claim 1, wherein the forming voltage is 48-128V.
5. The energized process according to claim 1 or 4, characterized in that the constant pressure treatment time is 3 to 12 hours.
6. The energized process of claim 1, wherein the heat treatment time is 20min to 60 min.
7. The energized process of claim 1, wherein the post-forming conditions are constant pressure for 3 to 4 hours.
8. A tantalum capacitor anode obtained by subjecting a sintered tantalum core to the energizing process of any one of claims 1 to 7.
9. A method of producing a tantalum capacitor comprising the energized process of any one of claims 1 to 7.
10. A tantalum capacitor comprising the tantalum capacitor anode of claim 8.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114050056A (en) * | 2021-11-18 | 2022-02-15 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Tantalum capacitor anode and preparation method thereof, and tantalum capacitor and preparation method thereof |
| CN114334460A (en) * | 2021-12-30 | 2022-04-12 | 贵州师范学院 | Method for improving large ripple current tolerance of tantalum electrolytic capacitor |
| CN115881440A (en) * | 2023-03-01 | 2023-03-31 | 电子科技大学 | Structure for improving high-frequency characteristic of all-tantalum capacitor and manufacturing method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400694A (en) * | 2013-07-10 | 2013-11-20 | 中国振华（集团）新云电子元器件有限责任公司 | Method for manufacturing high-voltage electrolytic capacitor |
| CN103500658A (en) * | 2013-10-17 | 2014-01-08 | 中国振华（集团）新云电子元器件有限责任公司 | Method for reducing leakage current of high-voltage large-capacity tantalum electrolytic capacitor |
| CN103985545A (en) * | 2014-04-28 | 2014-08-13 | 中国振华（集团）新云电子元器件有限责任公司 | Method for heat treatment of high-pressure tantalum electrolytic condenser anode film |
| CN106206029A (en) * | 2016-08-14 | 2016-12-07 | 中国振华（集团）新云电子元器件有限责任公司 | A kind of low temperature forming method of chip tantalum capacitor anode |
-
2019
- 2019-12-31 CN CN201911424328.5A patent/CN111180212A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400694A (en) * | 2013-07-10 | 2013-11-20 | 中国振华（集团）新云电子元器件有限责任公司 | Method for manufacturing high-voltage electrolytic capacitor |
| CN103500658A (en) * | 2013-10-17 | 2014-01-08 | 中国振华（集团）新云电子元器件有限责任公司 | Method for reducing leakage current of high-voltage large-capacity tantalum electrolytic capacitor |
| CN103985545A (en) * | 2014-04-28 | 2014-08-13 | 中国振华（集团）新云电子元器件有限责任公司 | Method for heat treatment of high-pressure tantalum electrolytic condenser anode film |
| CN106206029A (en) * | 2016-08-14 | 2016-12-07 | 中国振华（集团）新云电子元器件有限责任公司 | A kind of low temperature forming method of chip tantalum capacitor anode |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114050056A (en) * | 2021-11-18 | 2022-02-15 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Tantalum capacitor anode and preparation method thereof, and tantalum capacitor and preparation method thereof |
| CN114334460A (en) * | 2021-12-30 | 2022-04-12 | 贵州师范学院 | Method for improving large ripple current tolerance of tantalum electrolytic capacitor |
| CN115881440A (en) * | 2023-03-01 | 2023-03-31 | 电子科技大学 | Structure for improving high-frequency characteristic of all-tantalum capacitor and manufacturing method thereof |
| CN115881440B (en) * | 2023-03-01 | 2023-05-05 | 电子科技大学 | Structure for improving high-frequency characteristic of all-tantalum capacitor and manufacturing method thereof |
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