CN104538181A - Compacting method for manganese dioxide layer forming of tantalum capacitor - Google Patents
Compacting method for manganese dioxide layer forming of tantalum capacitor Download PDFInfo
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- CN104538181A CN104538181A CN201410836826.1A CN201410836826A CN104538181A CN 104538181 A CN104538181 A CN 104538181A CN 201410836826 A CN201410836826 A CN 201410836826A CN 104538181 A CN104538181 A CN 104538181A
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- tunicle
- nitrate solution
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Abstract
The invention provides a compacting method for manganese dioxide layer forming of a tantalum capacitor. The method includes the following steps that (1) a tantalum block subjected to reinforcement treatment is dipped in a manganous nitrate solution; (2) the tantalum block dipped with the manganous nitrate solution is placed in a metal box, and the tantalum block together with the metal box is placed in a manganese dioxide layer forming oven to be subjected to thermal decomposition; (3) the step (1) and the step (2) are repeated one to two times; (4) after the previous steps are completed, the tantalum block is dipped in the manganous nitrate solution; (5) the step (2) is repeated; (6) the step (4) and the step (5) are repeated one to two times; (7) the tantalum block is placed in a forming solution and charged with electricity. The decomposition rate of Mn(NO3)2 is controlled through the method, the quality of a formed manganese dioxide layer is guaranteed, and therefore the tantalum capacitor is stable in electrical performance parameter. The prepared manganese dioxide layer of the tantalum capacitor is uniform in density and compact, and equivalent series resistance is good in consistency and is reduced by more than 25% compared with that of an existing process.
Description
Technical field
The invention belongs to capacitor manufacturing technology field, be specifically related to a kind of dense method of tantalum capacitor tunicle.
Background technology
Tantalum capacitor volume is little, capacity is large, larger than the capacitance of other capacitors of same volume more than 2 times, miniaturization of electronic products development and performance boost are played an important role, be widely used in the field such as computer, mobile communication network and terminal equipment, intelligent appliance, Internet of Things, due to the electronic technology fast development of the industries such as consumer electronics, automotive electronics and high-tech Aero-Space, the demand of electrolytic capacitor is increased considerably, more and more higher requirement be there has also been to its reliability simultaneously.
The high reliability request tantalum electric capacity of tantalum electric capacity has excellent unit for electrical property parameters, as everyone knows, is one of key factor affecting solid electrolyte Ta capacitor performance by membrane process.So-called by membrane process, be exactly that the anode substrate after being formed is immersed Mn (NO
3)
2in solution, infiltration is taken out, and decomposes and produce electronic conductance type MnO in the high-temperature atmosphere containing steam
2.As the MnO of electrolytic capacitor electrolyte
2layer, multiple physics, chemistry and electric property must be had, the requirement of capacitor could be met, and these all with Mn (NO
3)
2thermal decomposition relevant.
By the MnO that thermal decomposition is formed
2the stability of layer to tantalum capacitor leakage current, loss angle tangent, equivalent series resistance and capacitance, all plays decisive role.And Mn (NO during thermal decomposition
3)
2decomposition rate directly affect MnO
2the size of layer crystal grain, the compactness of structure and flat appearance rule degree.Under existing technology state, we are difficult to control Mn (NO
3)
2decomposition rate, adding tunicle furnace interior has certain space, like this stove interior space each point on temperature, steam air pressure, wind speed etc. be uneven, these have impact on MnO to a great extent
2the quality of layer, tantalum electric capacity unit for electrical property parameters also becomes uneven thereupon.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of dense method of tantalum capacitor tunicle.
The present invention is achieved by the following technical programs.
The dense method of a kind of tantalum capacitor tunicle provided by the invention, comprises the following steps:
(1), the tantalum core crossed through intensive treatment being immersed proportion is 1.60g/cm
3~ 1.90g/cm
3manganese nitrate solution in, impregnating depth is 2/5 ~ 4/5 of tantalum core, and the temperature of manganese nitrate solution is 20 DEG C ~ 60 DEG C, and dip time is 5min ~ 15min;
(2), by the tantalum core of dipping pernitric acid manganese solution put into can, and put into tunicle stove with can and carry out thermal decomposition;
(3), step (1), step (2) 1 ~ 2 times are repeated;
(4), complete above step after, by tantalum core immerse proportion be 1.30g/cm
3~ 1.60g/cm
3manganese nitrate solution in, impregnating depth is 1/4 ~ 3/4 of tantalum core, and the temperature of manganese nitrate solution is 20 DEG C ~ 60 DEG C, and dip time is 5min ~ 15min;
(5), step (2) is repeated;
(6), step (4), step (5) 1 ~ 2 times are repeated;
(7), by tantalum core put into formed liquid, conduction time 10min ~ 60min, power-on voltage is 1.5 ~ 3 times of tantalum capacitor rated voltage.
Temperature in described tunicle stove is 200 DEG C ~ 300 DEG C, and steam oxygen content is 8% ~ 18%, and the resolving time is 5min ~ 15min.
Described formation liquid is 0.1% ~ 1%v/v acetic acid aqueous solution.
Can in described step (2) is uncovered cuboid, and all large than the tunicle stove framework 10mm ~ 30mm of the length, width and height of described can.
The material of described can is stainless steel, aluminium alloy.
The wall thickness of described can is 0.5mm ~ 2.0mm.
The bottom part of described can is furnished with aperture, and the aperture of described aperture is Φ 3mm ~ Φ 10mm, and pitch of holes is 15mm ~ 50mm.
Beneficial effect of the present invention is: adopt the method control Mn (NO
3)
2decomposition rate, by tantalum core is put into can, and put into tunicle stove with can and carry out thermal decomposition, make the temperature on each point of stove interior space, steam air pressure, wind speed more even like this, further ensure the MnO of formation
2the quality of layer, improve the stability of tantalum capacitor leakage current, loss angle tangent, equivalent series resistance and capacitance, the tantalum capacitor dioxy manganese layer even density that present invention process obtains, densification, equivalent series resistance consistency is good, reduces by more than 25% than existing technique.
Accompanying drawing explanation
Fig. 1 is the structural representation of uncovered tetragonal body can in the present invention.
Embodiment
Further describe technical scheme of the present invention below, but described in claimed scope is not limited to.
The invention provides a kind of dense method of tantalum capacitor tunicle, tunicle is dense the stage, product is put into the uncovered tetragonal body can of a bottom of which has holes, as shown in Figure 1, then carries out thermal decomposition.Manganese nitrate solution its chemical reaction equation when thermal decomposition is as follows:
First stage
Second stage
For the first stage, due to the existence of steam, chemical balance can be allowed to move to the left side, during thermal decomposition, after adding can, steam can rest in can the long period, and the water molecule number namely overflowed in the unit interval will reduce, chemical balance is moved to the left side, and this is just equivalent to the Mn (NO that slowed down
3)
26H
2the thermal decomposition process of O, contributes to fine and close MnO
2the generation of layer.Due to the good conductor that metal is heat, at the uniform velocity rise through tunicle stove temperature after heating, and in can, temperature is comparatively even, the MnO therefore generated
2layer is very fine and close, even.
When forming tunicle, porous anode matrix is flooded to high concentration repeatedly by low concentration, thermal decomposition manganese nitrate solution, when repeatedly carrying out after 6 ~ 20 times, in order to ensure MnO
2the thickness of layer and hardness, just need dipping to be added with MnO
2the high concentration manganese nitrate suspension-turbid liquid of powder, then oven dry, thermal decomposition, industry slang is referred to as strengthening.After having strengthened, MnO
2surface layer is less, in order to increase MnO
2surface layer, and then increase MnO
2layer and next operation apply the contact area of carbon-coating and silver slurry layer, reduce contact resistance, and need again dipping, thermal decomposition manganese nitrate solution repeatedly, this process industry term is referred to as dense.The manganese dioxide that dense process generates mainly is attached to fuse outmost surface, carbon-coating will be applied with next operation directly to contact with silver slurry layer, the quality of the manganese dioxide layer quality now generated is very large on the impact of tantalum capacitor equivalent series resistance, so in the tunicle dense stage, the present invention will add that can carries out thermal decomposition.
Embodiment 1
Choose the tantalum powder that CV value is 32000 μ FV/g, compacting specification is the tantalum capacitor anodes matrix of 10V470 μ F, and porousness anode substrate is sintered in 1450 DEG C of high vacuum, anode substrate after sintering is anodizing to 40V in the phosphoric acid,diluted aqueous solution, form dielectric layer, again the tantalum fuse after formation dielectric layer is flooded manganese nitrate solution repeatedly, thermal decomposition, manganese dioxide cathodes layer is formed in tantalum core surface, when preparing manganese dioxide cathodes layer, the dense stage carries out according to the following steps:
(1) the tantalum core crossed through intensive treatment being immersed proportion is 1.78g/cm
3manganese nitrate solution in, impregnating depth is 2/3 of tantalum core, and the temperature of manganese nitrate solution is 45 DEG C, and dip time is 10min.
(2) the tantalum core having flooded manganese nitrate solution is put into can, and put into tunicle stove with can and carry out thermal decomposition, the temperature in described tunicle stove is 280 DEG C, and steam oxygen content is 13%, and the resolving time is 6min.
(3) step (1), step (2) 1 times are repeated.
(4), after completing above step, it is 1.55g/cm that tantalum core is immersed proportion
3manganese nitrate solution in, impregnating depth is 2/3 of tantalum core, and the temperature of manganese nitrate solution is 45 DEG C, and dip time is 10min.
(5) again the tantalum core having flooded manganese nitrate solution is put into can, and put into tunicle stove with can and carry out thermal decomposition, the temperature in described tunicle stove is 280 DEG C, and steam oxygen content is 13%, and the resolving time is 6min.
(6) step (4), step (5) 2 times are repeated.
(7) tantalum core is put into formed liquid, formed liquid be 0.3%v/v acetic acid aqueous solution, conduction time 50min, power-on voltage is 2 times of tantalum capacitor rated voltage.
The material of the can in above-mentioned steps (2) and step (5) is stainless steel, and the thickness of can is 1.0mm, all large than the tunicle stove framework 20mm of length, width and height; The aperture of can small hole at bottom part is Φ 10mm, and pitch of holes is 30mm, is uniformly distributed in bottom can.
Embodiment 2
Choose the tantalum powder that CV value is 10000 μ FV/g, compacting specification is the tantalum capacitor anodes matrix of 16V100 μ F, and porousness anode substrate is sintered in 1700 DEG C of high vacuum, anode substrate after sintering is anodizing to 64V in the phosphoric acid,diluted aqueous solution, forms dielectric layer, then the tantalum fuse after forming dielectric layer is flooded manganese nitrate solution repeatedly, thermal decomposition, form manganese dioxide cathodes layer in tantalum core surface, when preparing manganese dioxide cathodes layer, the dense stage carries out according to the following steps:
(1) the tantalum core crossed through intensive treatment being immersed proportion is 1.80g/cm
3manganese nitrate solution in, impregnating depth is 2/3 of tantalum core, and the temperature of manganese nitrate solution is 50 DEG C, and dip time is 6min.
(2) the tantalum core having flooded manganese nitrate solution is put into can, and put into tunicle stove with can and carry out thermal decomposition, the temperature in described tunicle stove is 260 DEG C, and steam oxygen content is 14%, and the resolving time is 10min.
(3) step (1), step (2) 2 times are repeated.
(4), after completing above step, it is 1.50g/cm that tantalum core is immersed proportion
3manganese nitrate solution in, impregnating depth is 2/3 of tantalum core, and the temperature of manganese nitrate solution is 45 DEG C, and dip time is 6min.
(5) again the tantalum core having flooded manganese nitrate solution is put into can, and put into tunicle stove with can and carry out thermal decomposition, the temperature in described tunicle stove is 260 DEG C, and steam oxygen content is 14%, and the resolving time is 10min.
(6) step (4), step (5) 1 times are repeated.
(7) tantalum core is put into formed liquid, formed liquid be 0.5%v/v acetic acid aqueous solution, conduction time 40min, power-on voltage is 2 times of tantalum capacitor rated voltage.
The material of the can in above-mentioned steps (2) and step (5) is aluminium alloy, and the thickness of can is 1.5mm, all large than the tunicle stove framework 30mm of length, width and height; The aperture of can small hole at bottom part is Φ 8mm, and pitch of holes is 25mm, is uniformly distributed in bottom can.
Embodiment 3
Choose the tantalum powder that CV value is 15000 μ FV/g, compacting specification is the tantalum capacitor anodes matrix of 25V100 μ F, and at 1600 DEG C of high-vacuum sintering porousness anode substrates, anode substrate after sintering is anodizing to 100V in the phosphoric acid,diluted aqueous solution, forms dielectric layer, then the tantalum fuse after forming dielectric layer is flooded manganese nitrate solution repeatedly, thermal decomposition, form manganese dioxide cathodes layer in tantalum core surface, when preparing manganese dioxide cathodes layer, the dense stage carries out according to the following steps:
(1) the tantalum core crossed through intensive treatment being immersed proportion is 1.85g/cm
3manganese nitrate solution in, impregnating depth is 2/3 of tantalum core, and the temperature of manganese nitrate solution is 45 DEG C, and dip time is 7min.
(2) the tantalum core having flooded manganese nitrate solution is put into can, and put into tunicle stove with can and carry out thermal decomposition, the temperature in described tunicle stove is 270 DEG C, and steam oxygen content is 14%, and the resolving time is 7min.
(3) step (1), step (2) 2 times are repeated.
(4), after completing above step, it is 1.45g/cm that tantalum core is immersed proportion
3manganese nitrate solution in, impregnating depth is 2/3 of tantalum core, and the temperature of manganese nitrate solution is 55 DEG C, and dip time is 7min.
(5) again the tantalum core having flooded manganese nitrate solution is put into can, and put into tunicle stove with can and carry out thermal decomposition, the temperature in described tunicle stove is 270 DEG C, and steam oxygen content is 14%, and the resolving time is 7min.
(6) step (4), step (5) 2 times are repeated.
(7) tantalum core is put into formed liquid, formed liquid be 0.4%v/v acetic acid aqueous solution, conduction time 20min, power-on voltage is 2 times of tantalum capacitor rated voltage.
The material of the can in above-mentioned steps (2) and step (5) is aluminium alloy, and the thickness of can is 2.0mm, all large than the tunicle stove framework 20mm of length, width and height; The aperture of can small hole at bottom part is Φ 10mm, and pitch of holes is 40mm, is uniformly distributed in bottom can.
Complete the preparation of solid electrolyte negative electrode according to embodiment 1,2,3, separately get the preparation executed and complete solid electrolyte negative electrode in example 1,2,3 with batch tantalum fuse by existing technique respectively.By tantalum fuse coating carbon-coating and silver slurry layer, respectively randomly draw the ESR of 10 tantalum fuses test capacitors under frequency is 100KHz condition, in table 1,2,3.
Table 1 10V470 μ F
Table 2 16V100 μ F
Table 3 25V100 μ F
Utilize the negative electrode dioxy manganese layer even density that present invention process is obtained, as can be seen from table 1, table 2, table 3, adopt the equivalent series resistance of tantalum electric capacity prepared by present invention process little, and consistency is good, reduces by more than 25% than existing technique.
Claims (7)
1. a dense method for tantalum capacitor tunicle, is characterized in that: comprise the following steps:
(1), the tantalum core crossed through intensive treatment being immersed proportion is 1.60g/cm
3~ 1.90g/cm
3manganese nitrate solution in, impregnating depth is 2/5 ~ 4/5 of tantalum core, and the temperature of manganese nitrate solution is 20 DEG C ~ 60 DEG C, and dip time is 5min ~ 15min;
(2), by the tantalum core of dipping pernitric acid manganese solution put into can, and put into tunicle stove with can and carry out thermal decomposition;
(3), step (1), step (2) 1 ~ 2 times are repeated;
(4), complete above step after, by tantalum core immerse proportion be 1.30g/cm
3~ 1.60g/cm
3manganese nitrate solution in, impregnating depth is 1/4 ~ 3/4 of tantalum core, and the temperature of manganese nitrate solution is 20 DEG C ~ 60 DEG C, and dip time is 5min ~ 15min;
(5), step (2) is repeated;
(6), step (4), step (5) 1 ~ 2 times are repeated;
(7), by tantalum core put into formed liquid, conduction time 10min ~ 60min, power-on voltage is 1.5 ~ 3 times of tantalum capacitor rated voltage, dries 5min ~ 15min after taking-up in the baking oven of 120 DEG C ~ 150 DEG C.
2. the dense method of tantalum capacitor tunicle as claimed in claim 1, is characterized in that: the temperature in described tunicle stove is 200 DEG C ~ 300 DEG C, and steam oxygen content is 8% ~ 18%, and the resolving time is 5min ~ 15min.
3. the dense method of tantalum capacitor tunicle as claimed in claim 1, is characterized in that: described formation liquid is 0.1% ~ 1%v/v acetic acid aqueous solution.
4. the dense method of tantalum capacitor tunicle as claimed in claim 1, is characterized in that: the can in described step (2) is uncovered cuboid, and all large than the tunicle stove framework 10mm ~ 30mm of the length, width and height of described can.
5. the dense method of tantalum capacitor tunicle as claimed in claim 4, is characterized in that: the material of described can is stainless steel, aluminium alloy.
6. the dense method of the tantalum capacitor tunicle as described in claim 4 or 5, is characterized in that: the wall thickness of described can is 0.5mm ~ 2.0mm.
7. the dense method of the tantalum capacitor tunicle as described in claim 4 or 5, is characterized in that: the bottom part of described can is furnished with aperture, and the aperture of described aperture is Φ 3mm ~ Φ 10mm, and pitch of holes is 15mm ~ 50mm.
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| CN104538181B CN104538181B (en) | 2017-06-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113628886A (en) * | 2021-08-16 | 2021-11-09 | 标瑞新能源技术(重庆)有限公司 | Method and material for coating cathode of tantalum electrolytic capacitor |
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| CN1776847A (en) * | 2005-11-18 | 2006-05-24 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing solid electrolytic capacitor cathode |
| CN201530851U (en) * | 2009-11-13 | 2010-07-21 | 宁波盛事达磁业有限公司 | Boat group for sintering Al-Ni-Co permanent magnetic alloy |
| CN102039206A (en) * | 2010-12-20 | 2011-05-04 | 成都东方凯特瑞环保催化剂有限责任公司 | Catalyst calcining box |
| CN102800480A (en) * | 2012-08-24 | 2012-11-28 | 中国振华（集团）新云电子元器件有限责任公司 | Preparation method for cathode of Nb capacitor |
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- 2014-12-29 CN CN201410836826.1A patent/CN104538181B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1776847A (en) * | 2005-11-18 | 2006-05-24 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing solid electrolytic capacitor cathode |
| CN201530851U (en) * | 2009-11-13 | 2010-07-21 | 宁波盛事达磁业有限公司 | Boat group for sintering Al-Ni-Co permanent magnetic alloy |
| CN102039206A (en) * | 2010-12-20 | 2011-05-04 | 成都东方凯特瑞环保催化剂有限责任公司 | Catalyst calcining box |
| CN102800480A (en) * | 2012-08-24 | 2012-11-28 | 中国振华（集团）新云电子元器件有限责任公司 | Preparation method for cathode of Nb capacitor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113628886A (en) * | 2021-08-16 | 2021-11-09 | 标瑞新能源技术(重庆)有限公司 | Method and material for coating cathode of tantalum electrolytic capacitor |
| CN113628886B (en) * | 2021-08-16 | 2023-03-14 | 标瑞新能源技术(重庆)有限公司 | Method and material for cathode coating of tantalum electrolytic capacitor |
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