CN106548870B - It is a kind of improve tantalum capacitor breakdown voltage by film method - Google Patents
It is a kind of improve tantalum capacitor breakdown voltage by film method Download PDFInfo
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- CN106548870B CN106548870B CN201510602954.4A CN201510602954A CN106548870B CN 106548870 B CN106548870 B CN 106548870B CN 201510602954 A CN201510602954 A CN 201510602954A CN 106548870 B CN106548870 B CN 106548870B
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Abstract
The present invention provides it is a kind of improve tantalum capacitor breakdown voltage by film method, include the following steps：It will thermally decompose and complete, treat that benefit forms tantalum fuse immersion temperature and washed to be boiled in 80~100 DEG C of deionized water；Tantalum fuse is put into the baking oven that temperature is 125~150 DEG C and is dried；Tantalum fuse is immersed in electrolytic cell in a concentration of 0.01~0.1 ‰ acid solution, applies voltage and tantalum fuse is mended to be formed；The tantalum fuse mended after being formed is put into the baking oven that temperature is 125~150 DEG C and is dried.The present invention takes dipping alkaline solution method before tantalum fuse is mended and to be formed and high-temperature boiling washing method cleans tantalum fuse, removes the soluble M n not decomposed thoroughly in tantalum fuse2+, improve the breakdown voltage of tantalum fuse；Improve mend form voltage, can fully will because thermally decompose Ta2O5The MnO at the fault position that deielectric-coating generates2It is converted to the higher Mn of specific resistance2O3, reduce the leakage current of product and improve the reliability of capacitor.
Description
Technical field
The present invention relates to it is a kind of improve tantalum capacitor breakdown voltage by film method, belong to tantalum capacitor technology of preparing neck
Domain.
Background technology
Tantalum capacitor has many superiority such as small, capacitance is big, leakage current is small, long lifespan, excellent storage stability
Can and be widely used in that various aerospace, space flight, aviation, weapons, ship, communication, instrument and meter etc. be military and civilian electricity
In subdomains.In recent years, with the continuous development of microelectronic industry technology, the volume that complete electronic set requires is less and less.At present,
Tantalum capacitor just develops towards small size, high reliability direction.
Tantalum capacitor it is highly reliable not only with anode manufacture, deielectric-coating manufacture it is related, also with the cathode of tantalum capacitor manufacture
Technology is closely related, the size of tantalum capacitor loss angle tangent, the quality of high frequency characteristics, the size of leakage current, reliability height
It is low all with cathode MnO2Depositing operation it is inseparable.Existing tantalum capacitor cathode manufacturing process is all by thermally decomposing nitric acid
Manganese solution deposits MnO2As the electrolyte of capacitor, in order to solve capacitor pyrolytic MnO2Lead to the leakage current of capacitor
And integrity problem, generally benefit will be taken to form measure in pyrolytic tantalum fuse 2~5 times, i.e., in phosphoric acid, nitric acid, second
The benefits such as acid are formed in solution, apply certain voltage to tantalum fuse, and effects of ion electric current and electronic current are formed by mending
Effect, by Ta2O5Deielectric-coating fault position MnO2Be converted to the higher Mn of specific resistance2O3, with reduce the leakage current of capacitor and
Improve the reliability of capacitor.
In existing tantalum capacitor cathode preparation process, tantalum fuse, which is mended to be formed, in order to prevent there is punch-through, adopts
The method for being greatly reduced and mending and forming voltage is taken to mend to be formed, it is general mend to form voltage and be no more than form the 65% of voltage.It is especially specified
Voltage is greater than or equal to the high pressure tantalum capacitor of 63V, and benefit forms voltage no more than forming the 50% of voltage, benefit is caused to form effect
It is undesirable, influence the leakage current and reliability of capacitor.
In existing tantalum capacitor cathode preparation process, no matter how to Mn2(NO)3It is mixed in solution, how to change heat
Resolution parameter condition, Mn2(NO)3Solution thermally decomposes to generate MnO2Conversion ratio be impossible to up to 100%, more or less exist and remove
MnO2Outer other manganese salt residual impurities.The research born et al. according to Japanese outlying islets, there are Mn2+Solution in mend formed, tantalum
The flash over voltage of fuse declines 25.0~33.3%.
Invention content
In order to solve the above technical problems, the present invention provides it is a kind of improve tantalum capacitor breakdown voltage by film method, should
To be thermally decomposed by film method for tantalum capacitor breakdown voltage is improved to complete, wait that the tantalum fuse for mending formation immerses the alkaline ring of PH ＞ 7
In the solution of border, make soluble M n in tantalum fuse2+With the OH in alkaline solution-Generate chemical reaction, generation Mn (OH)2Or MnO
(OH)2Precipitation cleans tantalum fuse by the method that high-temperature boiling is washed, and is not formed to benefit and brings Mn in solution into2+, so as to carry
High tantalum fuse mends the breakdown voltage to be formed.
The present invention is achieved by the following technical programs.
It is provided by the invention it is a kind of improve tantalum capacitor breakdown voltage by film method, include the following steps：
(1) will thermally decompose complete, wait to mend formed tantalum fuse immerse temperature be boiled in 80~100 DEG C of deionized water wash 40~
90min, and tantalum block there is not under upstream face completely；
(2) tantalum fuse is put into the baking oven that temperature is 125~150 DEG C and dries 10~15min；
(3) tantalum fuse is immersed in electrolytic cell in a concentration of 0.01~0.1 ‰ acidic aqueous solution, and by the tantalum of tantalum fuse
Silk is connect with positive pole, and electrolytic cell connection power cathode applies voltage and tantalum fuse is mended to be formed, and the time is 20~60min；
(4) the tantalum fuse mended after being formed is put into the baking oven that temperature is 125~150 DEG C and dries 10~15min.
The step (1) first takes thermal decomposition to complete, waits to mend 5 in the alkaline solution of tantalum fuse immersion PH ＞ 7 formed before
~30min, and tantalum block immersion depth is submerges under liquid level completely.
The solute of the alkaline solution is one kind in alkali or strong base-weak acid salt.
The solute of the alkaline solution is potassium hydroxide, sodium hydroxide, ammonium hydroxide, potassium carbonate, sodium carbonate, sodium bicarbonate, carbon
Potassium hydrogen phthalate, potassium phosphate, sodium phosphate, potassium acetate, sodium acetate.
The alkaline solution a concentration of 0.1%~10%.
The alkaline solution a concentration of 1%~10%.
Acid solution in the step (3) is phosphoric acid, nitric acid or acetic acid aqueous solution.
The voltage applied in the step (3) is 50%~70% formation voltage.
The beneficial effects of the present invention are：It improves existing envelope and mends formation process, taken before tantalum fuse is mended and to be formed
Dipping alkaline solution method and high-temperature boiling washing method clean tantalum fuse, remove do not decompose thoroughly in tantalum fuse can
Dissolubility Mn2+, improve the breakdown voltage of tantalum fuse；Improve mend form voltage, can fully will because thermally decompose Ta2O5Deielectric-coating generates
Fault position MnO2It is converted to the higher Mn of specific resistance2O3, reduce the leakage current of product and improve the reliability of capacitor；
This method technological operation is simple, easy to control, is suitble to industrial mass production.
Specific embodiment
Be described further below technical scheme of the present invention, but claimed range be not limited to it is described.
Embodiment 1
It is a kind of improve tantalum capacitor breakdown voltage by film method, with 3500 μ FV/g than CAK45 types that capacitance tantalum powder designs
For chip tantalum capacitor 75V4.7 μ F, it is comprised the steps of：
(1) thermal decomposition is taken to complete, waits to mend the tantalum fuse formed, immerses 20min in a concentration of 5% sodium hydroxide solution,
And tantalum block immersion depth is submerges under liquid level completely；
(2) the tantalum fuse for impregnating sodium hydroxide solution is immersed in the deionized water that temperature is 80~100 DEG C to boil and is washed
40min carries out tantalum fuse HIGH TEMPERATURE PURGE, and tantalum block immersion depth is submerges underwater completely；
(3) tantalum fuse is put into the baking oven that temperature is 125 DEG C and dries 15min；
(4) tantalum fuse is immersed in electrolytic cell in a concentration of 0.1 ‰ aqueous solution of nitric acid, by the tantalum wire and power supply of tantalum fuse
Anode connects, and electrolytic cell connection power cathode applies 130V voltages and tantalum fuse is mended to be formed, time 40min；
(5) the tantalum fuse mended after being formed is put into the baking oven that temperature is 125 DEG C and dries 15min.
Capacitor cathode is completed by prior art step and draws layer coating graphite and silver paste, is completed capacitor cathode and is drawn layer
Manufacture.
Embodiment 2
It is a kind of improve tantalum capacitor breakdown voltage by film method, with 2500 μ FV/g than CAK45 types that capacitance tantalum powder designs
For chip tantalum capacitor 100V10 μ F, it is comprised the steps of：
(1) thermal decomposition is taken to complete, waits to mend the tantalum fuse formed, immerses 10min in a concentration of 20% ammonia spirit, and tantalum
Block immersion depth is submerges under liquid level completely；
(2) the tantalum fuse for impregnating ammonia spirit is immersed in the deionized water that temperature is 80~100 DEG C to boil and washes 90min,
HIGH TEMPERATURE PURGE is carried out to tantalum fuse, tantalum block immersion depth is submerges underwater completely；
(3) tantalum fuse is put into the baking oven that temperature is 150 DEG C and dries 10min；
(4) tantalum fuse is immersed in electrolytic cell in a concentration of 0.05 ‰ acetic acid aqueous solution, tantalum wire and positive pole is connected
It connects, electrolytic cell connection power cathode applies 160V voltages and tantalum fuse is mended to be formed, time 20min；
(5) the tantalum fuse mended after being formed is put into the baking oven that temperature is 150 DEG C and dries 10min.
Capacitor cathode is completed by prior art step and draws layer coating graphite and silver paste, is completed capacitor cathode and is drawn layer
Manufacture.
By CAK45 type chip tantalum capacitor 75V4.7 μ F, two specification products of 100V10 μ F according to embodiment 1, embodiment 2
Method makes 100, tantalum fuse, then the leakage current of tantalum fuse is tested, test result is shown in Table 1, table 2.
The 75V4.7 μ F leakage current test cases that table 1 makes according to embodiment 1
The 100V10 μ F leakage current test cases that table 2 makes according to embodiment 1
Meanwhile with the leakage current test case of the 75V4.7 μ F of prior art production, two specification tantalum capacitors of 100V10 μ F
It is shown in Table 3, table 4.
The 75V4.7 μ F electric leakage current test test cases of 3 prior art of table production
The 100V10 μ F electric leakage current test test cases of 4 prior art of table production
As can be seen that prior art produced in test result from table 1, table 2 with tantalum capacitor leakage current in table 3, table 4
Two 75V4.7 μ F, 100V10 μ F specification tantalum capacitor breakdown are apparent, and tantalum capacitor envelope produced by the invention is used to mend shape
Occur into no punch-through, in other words, method using the present invention can significantly improve the breakdown voltage of tantalum capacitor, so as to improve
The reliability of product.
Claims (7)
1. it is a kind of improve tantalum capacitor breakdown voltage by film method, include the following steps：
(1) thermal decomposition is taken to complete, waits to mend 5~30min in the alkaline solution of tantalum fuse immersion PH ＞ 7 formed, and tantalum block immerses
Depth is submerges under liquid level completely；
(2) the tantalum fuse for impregnating parlkaline solution is immersed in the deionized water that temperature is 80~100 DEG C to boil and washes 40~90min,
And tantalum block there is not under upstream face completely；
(3) tantalum fuse is put into the baking oven that temperature is 125~150 DEG C and dries 10~15min；
(4) by tantalum fuse immerse electrolytic cell in a concentration of 0.01~0.1 ‰ acidic aqueous solution in, and by the tantalum wire of tantalum fuse with
Positive pole connects, and electrolytic cell connection power cathode applies voltage and tantalum fuse is mended to be formed, and the time is 20~60min；
(5) the tantalum fuse mended after being formed is put into the baking oven that temperature is 125~150 DEG C and dries 10~15min.
2. as described in claim 1 improve tantalum capacitor breakdown voltage by film method, it is characterised in that：The alkaline solution
Solute be one kind in alkali or strong base-weak acid salt.
3. as described in claim 1 improve tantalum capacitor breakdown voltage by film method, it is characterised in that：The alkaline solution
Solute for potassium hydroxide, sodium hydroxide, ammonium hydroxide, potassium carbonate, sodium carbonate, sodium bicarbonate, saleratus, potassium phosphate, sodium phosphate,
Potassium acetate, sodium acetate.
4. as described in any in claims 1 to 3 raising tantalum capacitor breakdown voltage by film method, it is characterised in that：Institute
State alkaline solution a concentration of 0.1%~10%.
5. as described in any in claims 1 to 3 raising tantalum capacitor breakdown voltage by film method, it is characterised in that：Institute
State alkaline solution a concentration of 1%~10%.
6. as described in claim 1 improve tantalum capacitor breakdown voltage by film method, it is characterised in that：The step (4)
In acid solution be phosphoric acid, nitric acid or acetic acid aqueous solution.
7. as described in claim 1 improve tantalum capacitor breakdown voltage by film method, it is characterised in that：The step (4)
The voltage of middle application is 50%~70% formation voltage.
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| CN201510602954.4A CN106548870B (en) | 2015-09-21 | 2015-09-21 | It is a kind of improve tantalum capacitor breakdown voltage by film method |
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| CN201510602954.4A CN106548870B (en) | 2015-09-21 | 2015-09-21 | It is a kind of improve tantalum capacitor breakdown voltage by film method |
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| CN106548870B true CN106548870B (en) | 2018-07-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107958785B (en) * | 2017-11-22 | 2019-08-27 | 贵州振华电子信息产业技术研究有限公司 | Tantalum capacitor anodes and preparation method thereof, solid electrolyte Ta capacitor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3496075A (en) * | 1967-08-09 | 1970-02-17 | Mallory & Co Inc P R | Surface treatment for improved dry electrolytic capacitors |
| CN1614726A (en) * | 2004-09-28 | 2005-05-11 | 宁夏星日电子股份有限公司 | Producing method for solid electrolytic capacitor |
| CN104021940A (en) * | 2014-05-29 | 2014-09-03 | 中国振华（集团）新云电子元器件有限责任公司 | Cathode preparation process for reducing niobium oxide capacitor equivalent series resistance |
| CN104538180A (en) * | 2014-12-24 | 2015-04-22 | 中国振华（集团）新云电子元器件有限责任公司 | Method for manufacturing solid organic electrolytic capacitor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63268232A (en) * | 1987-04-27 | 1988-11-04 | Matsushita Electric Ind Co Ltd | Manufacture of solid electrolytic capacitor |
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2015
- 2015-09-21 CN CN201510602954.4A patent/CN106548870B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3496075A (en) * | 1967-08-09 | 1970-02-17 | Mallory & Co Inc P R | Surface treatment for improved dry electrolytic capacitors |
| CN1614726A (en) * | 2004-09-28 | 2005-05-11 | 宁夏星日电子股份有限公司 | Producing method for solid electrolytic capacitor |
| CN104021940A (en) * | 2014-05-29 | 2014-09-03 | 中国振华（集团）新云电子元器件有限责任公司 | Cathode preparation process for reducing niobium oxide capacitor equivalent series resistance |
| CN104538180A (en) * | 2014-12-24 | 2015-04-22 | 中国振华（集团）新云电子元器件有限责任公司 | Method for manufacturing solid organic electrolytic capacitor |
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