CN112530707B - Method for reducing leakage current after non-solid electrolyte tantalum capacitor is formed - Google Patents
Method for reducing leakage current after non-solid electrolyte tantalum capacitor is formed Download PDFInfo
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 73
- 239000003990 capacitor Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000001764 infiltration Methods 0.000 claims abstract description 9
- 230000008595 infiltration Effects 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 230000000704 physical effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000009736 wetting Methods 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000035882 stress Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Natural products OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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- 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
-
- 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
-
- 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
- H01G9/0525—Powder therefor
-
- 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
- H01G9/145—Liquid 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G2009/05—Electrodes or formation of dielectric layers thereon characterised by their structure consisting of tantalum, niobium, or sintered material; Combinations of such electrodes with solid semiconductive electrolytes, e.g. manganese dioxide
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- Engineering & Computer Science (AREA)
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- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
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Abstract
The invention belongs to the technical field of manufacturing of non-solid electrolyte tantalum capacitors, and particularly relates to a method for reducing leakage current after a non-solid electrolyte tantalum capacitor is formed, wherein sintered anode tantalum blocks are sequentially subjected to natural infiltration, current application in times, boosting temperature control treatment and heating pressure control treatment; the boosting temperature control treatment comprises the following steps: the anode tantalum block after the current is applied for multiple times is boosted to (T)1+273℃)/(T2The forming voltage is constant for 1.5-2 h at 273 ℃), and the temperature of the forming liquid is controlled at the temperature T during natural infiltration1(ii) a The temperature-rise pressure-control treatment comprises the following steps: the temperature of the formed liquid rises to T2The boosting current is increased to a set voltage by 10% to 50% of the boosting current value. The method provided by the invention effectively reduces the leakage current value after the non-solid electrolyte tantalum capacitor is formed and improves the reliability of the product by changing the wetting mode and time of the anode tantalum block, the flow adding process, the solution temperature control and other modes within the allowable range of the production process of the product.
Description
Technical Field
The invention belongs to the technical field of manufacturing of non-solid electrolyte tantalum capacitors, and particularly relates to a method for reducing leakage current after a non-solid electrolyte tantalum capacitor is formed.
Background
Tantalum electrolytic capacitors are widely used in various civil and military electronic products due to their excellent properties, such as small size, large capacity, low leakage current, low loss, long life, etc. With the development and deepening of industrial revolution, the development mainly faces the direction of miniaturization, light weight, high voltage and large capacity, the specific volume of tantalum powder is higher and higher, and the high specific volume tantalum powder has the physical characteristics of low breakdown voltage, small powder size and the like, so that greater challenges are provided for the technical breakthrough of the tantalum capacitor. Therefore, the reduction of the leakage current value after the tantalum capacitor is formed and the improvement of the quality of the oxide film of the anode tantalum block are the directions of continuous efforts of tantalum capacitor manufacturers.
The patent with the application number of CN201711319318.6 discloses a method for reducing the leakage current value of a non-solid electrolyte tantalum capacitor, which sequentially carries out natural infiltration and current application in times, wherein the first applied current is 5-15% of the total boosted current, and the second applied current is applied at the rate of applying 10-20% of the total boosted current for 5-30 minutes; and reducing the current after applying the current to the rated voltage in multiple times, reducing the current to 50-80% of the total boosted current, and continuing or even increasing the value to form a voltage value. The method can effectively reduce the leakage current value after the non-solid electrolyte tantalum capacitor is formed, and improves the reliability of the product. The technical scheme is a technical scheme of earlier research of the applicant, and the technical scheme is a forming method adopted under a high-temperature part, and has a more obvious effect on medium and high-pressure products; but the effect is not obvious for forming products with higher difficulty, such as products with medium and low pressure, large capacity and small volume.
Patent application No. cn201410834269.x discloses a non-solid tantalum capacitor aging method, comprising the following steps: (1) calculating the multiplying power relation between the applied voltage values at different temperatures and the applied voltage values at room temperature; (2) calculating voltage values to be applied to the product at different temperatures according to the ratio in the step (1); (3) and aging the capacitor. The method can greatly reduce the leakage current of the high-difficulty non-solid tantalum electrolytic capacitor after aging, solve the problems of low finished product qualification rate caused by poor product stability and large leakage current after aging, and improve the stability, reliability and qualification rate of the finished product. The technical scheme is a technical scheme of earlier research of the applicant, and is used for aging the tantalum capacitor to reduce the leakage current of a finished product.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for reducing leakage current after a non-solid electrolyte tantalum capacitor is formed, which can effectively reduce the leakage current value after the non-solid electrolyte tantalum capacitor is formed, in particular to an anode tantalum block formed by pressing high specific capacity tantalum powder, and is realized by the following technical scheme.
A method for reducing leakage current after a non-solid electrolyte tantalum capacitor is formed comprises the steps of sequentially carrying out natural infiltration, current application in times, pressure rise and temperature control treatment and temperature rise and pressure control treatment on a sintered anode tantalum block; the boosting and temperature controlling treatment comprises the following steps: the anode tantalum block after the current is applied for times is boosted to (T)1+273℃)/(T2The forming voltage is constant for 1.5-2 h at 273 ℃), and the temperature of the forming liquid is controlled at the temperature T during natural infiltration1(ii) a The temperature rise and pressure control treatment comprises the following steps: the temperature of the formed liquid rises to T2The current is increased to the formation voltage by 10% to 50% of the boosting current value.
Preferably, the natural infiltration is: and (3) soaking the anode tantalum block formed by sintering the tantalum powder in a forming liquid at 15-35 ℃ for 30-120 min.
Preferably, the divided application currents are: firstly, applying a boosting current value of 5-15% for 30-120 min; the remaining boost current value is then applied.
Preferably, the temperature and pressure raising and controlling treatment is as follows: after the pressure boosting and temperature control treatment, the temperature of the formed liquid is raised to 65-90 ℃, and the current of 10-50% of the pressure boosting current value is raised to the formed voltage.
Preferably, the remaining boost current value is applied at a rate of 10% to 20% of the total current value per 5 to 30 min.
Preferably, the boost current value is calculated according to the number of the anode tantalum block and the single powder weight, and the specific calculation formula is as follows: the boost current value (a) is the anode tantalum block count × single powder weight (g) × K (a/g), where K is a constant, and the specific value is related to the physical properties of the tantalum powder.
Preferably, the anode tantalum block is prepared by sintering tantalum powder with specific volume of 5000-70000 mu F.V/g.
The forming liquid is a forming liquid common in the technical field; is a catalyst containing HNO3、H2SO4、H3PO4And mixed solution of inorganic acid, organic matter such as glycol or citric acid, and other additives.
The technical principle of the invention is as follows: in the process of forming the anode tantalum block, the wettability of the anode tantalum block directly influences the uniformity of the thickness of the formed oxide film, and the anode tantalum block can be sufficiently wetted by adopting natural wetting and electric wetting; the pressure is increased firstly to control the temperature, the original electric stress and the thermal stress jointly act on the anode tantalum block in the forming process to be converted into the electric stress, the electric stress acts on the anode tantalum block, then the temperature and the pressure are increased to control the pressure, the original two stresses can be converted into the thermal stress, and the bearing capacity of the anode tantalum block can be greatly improved, the crystallization (shown as large leakage current) phenomenon of a product is greatly reduced, the leakage current value is reduced, and the quality of the product is improved; the effect is particularly prominent in products with medium and low voltage, large capacity and small volume (the voltage is less than or equal to 75V, the capacity is more than or equal to 470 mu F, and the specific volume of tantalum powder is more than or equal to 15000 mu F.V/g).
The invention has the beneficial effects that:
within the allowable range of the production process of the product, the leakage current value after the non-solid electrolyte tantalum capacitor is formed is effectively reduced by changing the wetting mode and time of the anode tantalum block, the flow adding process, the solution temperature control and other modes, and the reliability of the product is improved; and the production and manufacturing guarantee is provided for the market to meet the high reliability requirement of the products of the type.
Detailed Description
The technical solution of the present invention is further limited by the following specific embodiments, but the scope of the claims is not limited to the description.
Example 1
Raw materials: according to the production principle of the non-solid tantalum capacitor, carbon powder with specific volume of 50000 mu F.V/g is selected and sintered to prepare the anode tantalum block.
A method for reducing leakage current after formation of a non-solid electrolyte tantalum capacitor comprising the steps of:
(1) naturally infiltrating: putting the sintered tantalum block into a forming liquid, and soaking for 60min at the temperature of 25 ℃;
(2) current application for several times: calculating the boost current according to the number of the anode tantalum blocks and the weight of single powder, calculating the boost current to be 10A through a calculation formula (100 pieces multiplied by 5g multiplied by 0.02A/g), and then applying the boost current in times; applying a boosting current of 1A for the first time, wherein the boosting time is 60 min; applying the residual current for the second time at a rate of 1A/15 min;
(3) boosting and controlling temperature: after the voltage is increased to 1.2 times of rated voltage, keeping the voltage constant for 2 hours; controlling the temperature of the formed liquid at 25 ℃;
(4) temperature rise and pressure control treatment: the formation temperature was raised to 85 ℃ and a 3A boost current was applied to boost the formation voltage.
And (3) leakage current experiment: the test was carried out at 10V 10000. mu.F, and the anode tantalum block produced in example 1 was used to produce a tantalum capacitor, and the leakage current value of the anode tantalum block at room temperature of 25 ℃ is shown in Table 1, and the leakage current value is 20 to 23. mu.A.
TABLE 1 leakage current values of anodic tantalum blocks at room temperature (25 ℃ C.)
Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
I(μA)/min | 20 | 20 | 21 | 23 | 22 | 20 | 21 | 21 | 20 | 22 |
Comparative example 1
Raw materials: according to the production principle of the non-solid tantalum capacitor, tantalum powder with specific volume of 50000 mu F.V/g is selected to be sintered into an anode tantalum block.
A method for reducing leakage current after formation of a non-solid electrolyte tantalum capacitor comprising the steps of:
(1) directly putting the sintered tantalum block into forming liquid, wherein the temperature of the forming liquid is 85 ℃;
(2) calculating the boost current density to be 10A; the boosting current of 10A is directly applied to boost the voltage to the formation voltage.
And (3) leakage current experiment: the test was carried out at 10V 10000. mu.F, and the anode tantalum block produced in comparative example 1 was used to produce a tantalum capacitor, and the leakage current value of the anode tantalum block at room temperature of 25 ℃ is shown in Table 2, and the leakage current value is 150-188. mu.A.
TABLE 2 leakage current values of anodic tantalum blocks at room temperature (25 ℃ C.)
Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
I(μA)/min | 165 | 150 | 172 | 188 | 156 | 162 | 176 | 180 | 163 | 170 |
Comparative example 2
Raw materials: according to the production principle of the non-solid tantalum capacitor, tantalum powder with specific volume of 50000 mu F.V/g is selected to be sintered into an anode tantalum block.
The patent with application number CN201711319318.6 discloses a method for reducing leakage current value of tantalum capacitor with non-solid electrolyte:
s1, natural wetting and applying current:
soaking the anode tantalum block in a forming liquid at the temperature of 85 ℃ for 120 minutes; wherein the forming liquid is mixed liquid obtained by mixing phosphoric acid, ethylene glycol and water according to the volume ratio of 1:45: 15;
calculating the total boosting current; the time of the first applied current is 120 minutes, and the first applied current is 5 percent of the total boosted current; the current was applied a second time, which was at a rate of 20% of the total current applied to apply the boost for 30 minutes.
And S2, reducing the current after applying the current to the rated voltage in times, reducing the current to 50% of the total boosted current, and continuing to increase to the forming voltage value.
And (3) leakage current experiment: the test was conducted at 10V 10000. mu.F, and the anode tantalum block produced in comparative example 2 was used to produce a tantalum capacitor, and the values of leakage current of the anode tantalum block at room temperature of 25 ℃ are shown in Table 3.
TABLE 3 leakage current values of anodic tantalum blocks at room temperature (25 ℃ C.)
Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
I(μA)/min | 75 | 65 | 84 | 73 | 69 | 81 | 82 | 75 | 73 | 77 |
It should be noted that the above examples and test examples are only for further illustration and understanding of the technical solutions of the present invention, and are not to be construed as further limitations of the technical solutions of the present invention, and the invention which does not highlight essential features and significant advances made by those skilled in the art still belongs to the protection scope of the present invention.
Claims (5)
1. A method for reducing leakage current after a non-solid electrolyte tantalum capacitor is formed is characterized in that sintered anode tantalum blocks are sequentially subjected to natural infiltration, current application for times, pressure rise and temperature control treatment and temperature rise and pressure control treatment; the boosting and temperature controlling treatment comprises the following steps: the anode tantalum block after the current is applied for times is boosted to (T)1+273℃)/(T2The forming voltage is constant for 1.5-2 h at 273 ℃), and the temperature of the forming liquid is controlled at the temperature T during natural infiltration1(ii) a The temperature rise and pressure control treatment comprises the following steps: after the pressure-increasing temperature-controlling treatment, the temperature of the formed liquid rises to T2Raising the current of 10-50% of the boosted current value to a forming voltage;
the natural infiltration is as follows: soaking the anode tantalum block formed by sintering tantalum powder in a forming liquid at 15-35 ℃ for 30-120 min;
the time-division applied current is as follows: firstly, applying a boosting current value of 5-15% for 30-120 min; then applying the remaining boost current value;
the temperature rise and pressure control treatment comprises the following steps: the temperature of the formed liquid rises to 65-90 ℃, and the current which is 10-50% of the boosting current value rises to the formed voltage.
2. The method of reducing post-formation leakage current in a non-solid electrolyte tantalum capacitor of claim 1, wherein said residual boost current value is applied at a rate of 10% to 20% total current value per 5 to 30 min.
3. The method according to claim 1, wherein the boost current value is calculated based on the number of tantalum blocks and the weight of single powder, and the specific calculation formula is as follows: the boost current value (a) is the anode tantalum block count × single powder weight (g) × K (a/g), where K is a constant, and the specific value is related to the physical properties of the tantalum powder.
4. The method for reducing leakage current after formation of a non-solid electrolyte tantalum capacitor as claimed in claim 1, wherein said anode tantalum block is made by sintering tantalum powder with specific volume of 5000-70000 μ F.V/g.
5. Use of a method according to any of claims 1-4 for reducing leakage current after formation of a non-solid electrolyte tantalum capacitor having a voltage of 75V or less, a capacity of 470 μ F or more, and a tantalum powder having a specific volume of 15000 μ F.V/g or more.
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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 |
CN107958785A (en) * | 2017-11-22 | 2018-04-24 | 贵州振华电子信息产业技术研究有限公司 | High voltage-rated solid electrolyte Ta capacitor anode and preparation method thereof, solid electrolyte Ta capacitor |
CN108091491A (en) * | 2017-12-12 | 2018-05-29 | 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) | The method for reducing the method for non-solid electrolyte tantalum capacity fall off flow valuve and preparing non-solid electrolyte tantalum capacitance |
CN112768260A (en) * | 2020-12-28 | 2021-05-07 | 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) | Capacitor pre-aging device and capacitor pre-aging method |
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CN105428069B (en) * | 2015-08-19 | 2018-02-16 | 中国科学院福建物质结构研究所 | A kind of solid electrolytic capacitor with composite solid electrolyte and preparation method thereof |
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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 |
CN107958785A (en) * | 2017-11-22 | 2018-04-24 | 贵州振华电子信息产业技术研究有限公司 | High voltage-rated solid electrolyte Ta capacitor anode and preparation method thereof, solid electrolyte Ta capacitor |
CN108091491A (en) * | 2017-12-12 | 2018-05-29 | 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) | The method for reducing the method for non-solid electrolyte tantalum capacity fall off flow valuve and preparing non-solid electrolyte tantalum capacitance |
CN112768260A (en) * | 2020-12-28 | 2021-05-07 | 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) | Capacitor pre-aging device and capacitor pre-aging method |
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