CN104538181B - A kind of dense method of tantalum capacitor envelope - Google Patents
A kind of dense method of tantalum capacitor envelope Download PDFInfo
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- CN104538181B CN104538181B CN201410836826.1A CN201410836826A CN104538181B CN 104538181 B CN104538181 B CN 104538181B CN 201410836826 A CN201410836826 A CN 201410836826A CN 104538181 B CN104538181 B CN 104538181B
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Abstract
The invention provides a kind of dense method of tantalum capacitor envelope, comprise the following steps：(1) in the tantalum core immersion manganese nitrate solution that will be crossed through intensive treatment；(2) the tantalum core for impregnating pernitric acid manganese solution is put into can, and is put into envelope stove with can and is thermally decomposed；(3) repeat step (1), step (2) 1~2 times；(4) after completing above step, tantalum core is immersed in manganese nitrate solution, (5) repeat step (2)；(6) repeat step (4), step (5) 1~2 times；(7) tantalum core is put into forming liquid, is powered.The present invention controls the decomposition rate of Mn (NO3) 2 using the method, it is ensured that the quality of MnO2 layers of formation, so that tantalum electric capacity unit for electrical property parameters stabilization；Tantalum capacitor dioxy manganese layer even density, densification obtained in present invention process, equivalent series resistance uniformity are good, than existing process reduction by more than 25%.
Description
Technical field
The invention belongs to capacitor manufacturing technology field, and in particular to a kind of dense method of tantalum capacitor envelope.
Background technology
Tantalum capacitor small volume, capacity are big, bigger than the capacitance of other capacitors of same volume more than 2 times, and electronics is produced
Product miniaturization and performance boost play an important role, and are widely used in computer, mobile communication network and terminal device, intelligence
The fields such as energy household electrical appliances, Internet of Things, due to the electronic technology of the industries such as consumer electronics, automotive electronics and high-tech Aero-Space
Fast development, the demand to electrolytic capacitor is increased considerably, while there has also been higher and higher requirement to its reliability.
The high reliability request tantalum electric capacity of tantalum electric capacity has excellent unit for electrical property parameters, it is well known that by membrane process be shadow
Ring one of key factor of solid electrolyte Ta capacitor performance.It is so-called by membrane process, be exactly by the anode substrate leaching after formation
Enter Mn (NO3)2In solution, infiltration is taken out, and is decomposed in the high-temperature atmosphere containing steam and is produced electronic conductance type MnO2.As electrolysis
The MnO of capacitor electrolyte2Layer, it is necessary to have various physics, chemically and electrically performance, could meet the requirement of capacitor,
And these all with Mn (NO3)2Thermal decomposition it is relevant.
By the MnO being decomposed thermally to form2Layer is to tantalum capacitor leakage current, loss angle tangent, equivalent series resistance and electric capacity
The stability of amount, all plays decisive role.And Mn (NO when thermally decomposing3)2Decomposition rate directly affect MnO2Layer crystal grain it is big
Small, structure compactness and flat appearance rule degree.Under existing technology state, we are difficult control Mn (NO3)2's
Decomposition rate, along with envelope furnace interior has certain space, the temperature, water so on each point of stove interior space are steamed
Gas air pressure, wind speed etc. are uneven, and these largely have impact on MnO2The quality of layer, tantalum electric capacity unit for electrical property parameters
Become therewith uneven.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of dense method of tantalum capacitor envelope.
The present invention is achieved by the following technical programs.
A kind of dense method of tantalum capacitor envelope that the present invention is provided, comprises the following steps：
(1) the tantalum core immersion proportion that, will be crossed through intensive treatment is 1.60g/cm3~1.90g/cm3Manganese nitrate solution in,
Impregnating depth is the 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), the tantalum core for impregnating pernitric acid manganese solution is put into can, and is put into envelope stove with can and is carried out heat
Decompose；
(3), repeat step (1), step (2) 1~2 times；
(4) it is 1.30g/cm by tantalum core immersion proportion after, completing above step3~1.60g/cm3Manganese nitrate solution in,
Impregnating depth is the 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), repeat step (2)；
(6), repeat step (4), step (5) 1~2 times；
(7), tantalum core is put into forming liquid, conduction time 10min~60min, power-on voltage is the specified electricity of tantalum capacitor
1.5~3 times of pressure.
Temperature in the envelope stove is 200 DEG C~300 DEG C, and vapor oxygen content is the percent by volume of percent by volume
8%~18%, the resolving time be 5min~15min.
The formation liquid is 0.1%~1%v/v acetic acid aqueous solutions.
Can in the step (2) is uncovered cuboid, and the can length, width and height than envelope stove frame
Big 10mm~the 30mm of frame.
The material of described can is stainless steel, aluminium alloy.
The wall thickness of the can is 0.5mm~2.0mm.
The bottom of the can is distributed with aperture, and the aperture of the aperture is Φ 3mm~Φ 10mm, and pitch of holes is 15mm
~50mm.
The beneficial effects of the present invention are：Using the method control Mn (NO3)2Decomposition rate, be put into gold by by tantalum core
In category box, and it is put into envelope stove with can and is thermally decomposed, so makes temperature, the water on each point of stove interior space
Steam air pressure, wind speed are more uniform, further ensure the MnO to be formed2The quality of layer, improves tantalum capacitor leakage current, damages
The stability of consumption angle tangent, equivalent series resistance and capacitance, tantalum capacitor dioxy manganese layer density is equal obtained in present invention process
Even, densification, equivalent series resistance uniformity is good, than existing process reduction by more than 25%.
Brief description of the drawings
Fig. 1 is the structural representation of uncovered tetragonal body can in the present invention.
Specific embodiment
Be described further below technical scheme, but claimed scope be not limited to it is described.
The present invention provides a kind of dense method of tantalum capacitor envelope, and envelope is dense the stage, and product is put into a bottom
In uncovered tetragonal body can with holes, as shown in figure 1, being thermally decomposed again.Manganese nitrate solution its chemistry in thermal decomposition is anti-
Answer equation as follows：
First stageSecond stage
For the first stage, due to the presence of vapor, chemical balance can be allowed to be moved to the left side, during thermal decomposition, add gold
After category box, vapor can be rested in can the long period, i.e., the moisture subnumber for being overflowed in the unit interval will be reduced, chemistry
Balance and moved to the left side, this is equivalent to slow down Mn (NO3)26H2The thermal decomposition process of O, contributes to fine and close MnO2The life of layer
Into.Due to the good conductor that metal is heat, temperature at the uniform velocity rises after envelope stove heat, and temperature is more uniform in can, therefore
The MnO of generation2Layer is very fine and close, uniform.
When forming envelope, porous anode matrix is impregnated, thermally decomposes manganese nitrate solution repeatedly by low concentration to high concentration, when anti-
Carry out after 6~20 times again, in order to ensure MnO2The thickness and hardness of layer, it is necessary to which dipping is added with MnO2The high concentration of powder
Manganese nitrate suspension, then dries, thermally decomposes, and industry slang is referred to as reinforcing.After the completion of reinforcing, MnO2Surface layer compared with
It is small, in order to increase MnO2Surface layer, and then increase MnO2Layer coats the contact area of carbon-coating and silver slurry layer with next operation,
Contact resistance is reduced, it is necessary to impregnate repeatedly again, thermally decompose manganese nitrate solution, this process industry term is referred to as dense.It is close
The manganese dioxide of cause process generation is mainly attached to fuse outmost surface, will be direct with next operation coating carbon-coating and silver slurry layer
Contact, the quality of the manganese dioxide layer quality for now generating is very big on the influence of tantalum capacitor equivalent series resistance, so of the invention
To be thermally decomposed plus can in the envelope dense stage.
Embodiment 1
It is the tantalum powder of 32000 μ FV/g to choose CV values, and compacting specification is the tantalum capacitor anodes matrix of 10V470 μ F, and
Porous anode substrate is sintered into 1450 DEG C of high vacuum, the anode substrate after sintering is entered in the phosphoric acid,diluted aqueous solution with 40V
Row is anodizing to, and forms dielectric layer, then the tantalum fuse after formation dielectric layer is impregnated manganese nitrate solution repeatedly, is thermally decomposed,
Manganese dioxide cathodes layer is formed in tantalum core surface, when manganese dioxide cathodes layer is prepared, the dense stage is carried out according to the following steps：
(1) the tantalum core immersion proportion that will be crossed through intensive treatment is 1.78g/cm3Manganese nitrate solution in, impregnating depth is tantalum
The 2/3 of core, the temperature of manganese nitrate solution is 45 DEG C, and dip time is 10min.
(2) the tantalum core that will impregnate manganese nitrate solution is put into can, and is put into envelope stove with can and is carried out heat
Decompose, the temperature in the envelope stove is 280 DEG C, and vapor oxygen content is the 13% of percent by volume, and the resolving time is 6min.
(3) repeat step (1), step (2) 1 times.
(4) it is 1.55g/cm by tantalum core immersion proportion after completing above step3Manganese nitrate solution in, impregnating depth is
The 2/3 of tantalum core, the temperature of manganese nitrate solution is 45 DEG C, and dip time is 10min.
(5) the tantalum core that will impregnate manganese nitrate solution again is put into can, and is put into envelope stove with can and is carried out
Thermal decomposition, temperature in the envelope stove is 280 DEG C, and vapor oxygen content is the 13% of percent by volume, and the resolving time is
6min。
(6) repeat step (4), step (5) 2 times.
(7) tantalum core is put into forming liquid, forms liquid for 0.3%v/v acetic acid aqueous solutions, conduction time 50min, be powered electricity
Press 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, length and width
Height is than the big 20mm of envelope stove framework；The aperture of can small hole at bottom part is Φ 10mm, and pitch of holes is 30mm, is uniformly distributed in gold
Category cassette bottom portion.
Embodiment 2
It is the tantalum powder of 10000 μ FV/g to choose CV values, and compacting specification is the tantalum capacitor anodes matrix of 16V100 μ F, and
Porous anode substrate is sintered into 1700 DEG C of high vacuum, anode substrate after sintering is carried out in the phosphoric acid,diluted aqueous solution with 64V
It is anodizing to, forms dielectric layer, then the tantalum fuse after formation dielectric layer is impregnated manganese nitrate solution repeatedly, thermally decomposes,
Tantalum core surface forms manganese dioxide cathodes layer, and when manganese dioxide cathodes layer is prepared, the dense stage is carried out according to the following steps：
(1) the tantalum core immersion proportion that will be crossed through intensive treatment is 1.80g/cm3Manganese nitrate solution in, impregnating depth is tantalum
The 2/3 of core, the temperature of manganese nitrate solution is 50 DEG C, and dip time is 6min.
(2) the tantalum core that will impregnate manganese nitrate solution is put into can, and is put into envelope stove with can and is carried out heat
Decompose, temperature in the envelope stove is 260 DEG C, and vapor oxygen content is the 14% of percent by volume, the resolving time is
10min。
(3) repeat step (1), step (2) 2 times.
(4) it is 1.50g/cm by tantalum core immersion proportion after completing above step3Manganese nitrate solution in, impregnating depth is
The 2/3 of tantalum core, the temperature of manganese nitrate solution is 45 DEG C, and dip time is 6min.
(5) the tantalum core that will impregnate manganese nitrate solution again is put into can, and is put into envelope stove with can and is carried out
Thermal decomposition, temperature in the envelope stove is 260 DEG C, and vapor oxygen content is the 14% of percent by volume, and the resolving time is
10min。
(6) repeat step (4), step (5) 1 times.
(7) tantalum core is put into forming liquid, forms liquid for 0.5%v/v acetic acid aqueous solutions, conduction time 40min, be powered electricity
Press 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, length and width
Height is than the big 30mm of envelope stove framework；The aperture of can small hole at bottom part is Φ 8mm, and pitch of holes is 25mm, is uniformly distributed in gold
Category cassette bottom portion.
Embodiment 3
It is the tantalum powder of 15000 μ FV/g to choose CV values, and compacting specification is the tantalum capacitor anodes matrix of 25V100 μ F, and
1600 DEG C of high-vacuum sintering porous anode substrates, sun is carried out by the anode substrate after sintering in the phosphoric acid,diluted aqueous solution with 100V
It is polarized to, forms dielectric layer, then the tantalum fuse after formation dielectric layer is impregnated manganese nitrate solution repeatedly, thermally decomposes, in tantalum
Core surface forms manganese dioxide cathodes layer, and when manganese dioxide cathodes layer is prepared, the dense stage is carried out according to the following steps：
(1) the tantalum core immersion proportion that will be crossed through intensive treatment is 1.85g/cm3Manganese nitrate solution in, impregnating depth is tantalum
The 2/3 of core, the temperature of manganese nitrate solution is 45 DEG C, and dip time is 7min.
(2) the tantalum core that will impregnate manganese nitrate solution is put into can, and is put into envelope stove with can and is carried out heat
Decompose, the temperature in the envelope stove is 270 DEG C, and vapor oxygen content is the 14% of percent by volume, and the resolving time is 7min.
(3) repeat step (1), step (2) 2 times.
(4) it is 1.45g/cm by tantalum core immersion proportion after completing above step3Manganese nitrate solution in, impregnating depth is
The 2/3 of tantalum core, the temperature of manganese nitrate solution is 55 DEG C, and dip time is 7min.
(5) the tantalum core that will impregnate manganese nitrate solution again is put into can, and is put into envelope stove with can and is carried out
Thermal decomposition, temperature in the envelope stove is 270 DEG C, and vapor oxygen content is the 14% of percent by volume, and the resolving time is
7min。
(6) repeat step (4), step (5) 2 times.
(7) tantalum core is put into forming liquid, forms liquid for 0.4%v/v acetic acid aqueous solutions, conduction time 20min, be powered electricity
Press 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, length and width
Height is than the big 20mm of envelope stove framework；The aperture of can small hole at bottom part is Φ 10mm, and pitch of holes is 40mm, is uniformly distributed in gold
Category cassette bottom portion.
The preparation of solid electrolyte negative electrode is completed according to embodiment 1,2,3, is separately taken respectively and is applied in example 1,2,3 with batch tantalum core
Son is completed the preparation of solid electrolyte negative electrode by existing process.Tantalum fuse is coated into carbon-coating and silver slurry layer, 10 are respectively randomly selected
The ESR of tantalum fuse test capacitors under the conditions of frequency is 100KHz, is shown in Table 1,2,3.
The 10V470 μ F of table 1
The 16V100 μ F of table 2
The 25V100 μ F of table 3
Using negative electrode dioxy manganese layer even density obtained in present invention process, from table 1, table 2, table 3 as can be seen that using this
The equivalent series resistance of tantalum electric capacity is small prepared by invented technology, and uniformity is good, than existing process reduction by more than 25%.
Claims (7)
1. a kind of dense method of tantalum capacitor envelope, it is characterised in that：Comprise the following steps：
(1) the tantalum core immersion proportion that, will be crossed through intensive treatment is 1.60g/cm3~1.90g/cm3Manganese nitrate solution in, dipping
Depth is the 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 impregnate pernitric acid manganese solution tantalum core be put into can, and be put into envelope stove with can carry out heat point
Solution；
(3), repeat step (1), step (2) 1~2 times；
(4) it is 1.30g/cm by tantalum core immersion proportion after, completing above step3~1.60g/cm3Manganese nitrate solution in, dipping
Depth is the 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), repeat step (2)；
(6), repeat step (4), step (5) 1~2 times；
(7), tantalum core is put into forming liquid, conduction time 10min~60min, power-on voltage is tantalum capacitor rated voltage
1.5~3 times, 5min~15min is dried after taking-up in 120 DEG C~150 DEG C of baking oven.
2. the dense method of tantalum capacitor envelope as claimed in claim 1, it is characterised in that：Temperature in the envelope stove is
200 DEG C~300 DEG C, vapor oxygen content is the 8%~18% of percent by volume, and the resolving time is 5min~15min.
3. the dense method of tantalum capacitor envelope as claimed in claim 1, it is characterised in that：It is described formation liquid be 0.1%~
1%v/v acetic acid aqueous solutions.
4. the dense method of tantalum capacitor envelope as claimed in claim 1, it is characterised in that：Metal in the step (2)
Box be uncovered cuboid, and the can length, width and height than the big 10mm~30mm of envelope stove framework.
5. the dense method of tantalum capacitor envelope as claimed in claim 4, it is characterised in that：The material of described can is
Stainless steel, aluminium alloy.
6. the dense method of the tantalum capacitor envelope as described in claim 4 or 5, it is characterised in that：The wall thickness of the can
It is 0.5mm~2.0mm.
7. the dense method of the tantalum capacitor envelope as described in claim 4 or 5, it is characterised in that：The bottom of the can
Aperture is distributed with, the aperture of the aperture is Φ 3mm~Φ 10mm, and pitch of holes is 15mm~50mm.
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| CN104538181B true CN104538181B (en) | 2017-06-16 |
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| 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 |
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 |
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2014
- 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 |
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