CN110098060A - A method of reducing PEDOT solid tantalum capacitor leakage current - Google Patents
A method of reducing PEDOT solid tantalum capacitor leakage current Download PDFInfo
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- CN110098060A CN110098060A CN201910310664.0A CN201910310664A CN110098060A CN 110098060 A CN110098060 A CN 110098060A CN 201910310664 A CN201910310664 A CN 201910310664A CN 110098060 A CN110098060 A CN 110098060A
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- Prior art keywords
- tantalum
- leakage current
- tantalum capacitor
- capacitor leakage
- purity
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 54
- 239000003990 capacitor Substances 0.000 title claims abstract description 40
- 239000007787 solid Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 title claims abstract 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 4
- 239000011541 reaction mixture Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 2
- 229910052799 carbon Inorganic materials 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000013064 chemical raw material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000010931 ester hydrolysis Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000002791 soaking 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
- H01G9/15—Solid electrolytic capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The present invention discloses a kind of method for reducing PEDOT solid tantalum capacitor leakage current, and this method is that tantalum core is immersed in butyl titanate ethanol solution, forms the TiO of layer in dielectric layer surfaces externally and internally by butyl titanate hydrolysis2Film, then in TiO2Film surface forms PEDOT conductive film using in-situ method.Oxidant, monomer and byproduct of reaction during in-situ polymerization remain in tantalum core inner, cause damage to dielectric layer.The present invention passes through in dielectric layer and Ta2O5TiO is introduced between film2Film improves damage of the situ aggregation method to dielectric layer, prepares the PEDOT solid tantalum capacitor of low-leakage current.
Description
Technical field
The invention belongs to field of energy source materials, in particular to one kind is in poly- 3,4-rthylene dioxythiophene (PEDOT) solid tantalum
Depositing Ti O on the dielectric layer of capacitor2Method of the film to reduce leakage current.
Background technique
Electrolytic capacitor has a wide range of applications in circuit because capacity is big, energy storage, tuning, filtering and rectification etc., knot
Structure is mainly made of anode, dielectric layer and cathode.Common electrolytic capacitor mainly has aluminium electrolutic capacitor and tantalum electrolytic capacitor
Two kinds of device.Relative to aluminium electrolutic capacitor, tantalum electrolytic capacitor because of high reliablity, Aeronautics and Astronautics and in terms of
Using wide.By the Form division of catholyte, tantalum electrolytic capacitor can be divided into solid tantalum electrolytic capacitor and liquid tantalum
Electrolytic capacitor.Electrolytic conductivity lower (10 in liquid tantalum electrolytic capacitor–2~10–3S/cm), there is equivalent series electricity
Hinder the disadvantages of larger, high frequency performance is poor.In addition, the performance of electrolyte is easily influenced by temperature, when high temperature explosive slurry and corrode
Circuit, and solid tantalum electrolytic capacitor can overcome this disadvantage, and be easy to minimize and chip type, thus be tantalum electrolytic capacitor not
Come the direction developed.Currently, the cathode of solid tantalum electrolytic capacitor mainly uses inorganic MnO2, but MnO2Solid tantalum capacitor makes
Used time is found to have following disadvantage: impedance frequency characteristics and capacity-frequency characteristic are poor；Coating MnO2Process needs high temperature, holds
Easily cause Ta2O5Dielectric film damage；Easily cause other elements in burning or explosion or even damaged circuit.
For MnO2The problem of solid tantalum capacitor exists in use, conductive organic polymer tantalum capacitor is because that can overcome
Its disadvantage, therefore be the hot spot of solid tantalum electrolytic capacitor research and the trend of future development.PEDOT is because of conductivity at present
High (about 1~500s/cm), the advantages that thermal stability is good, at low cost, environmentally friendly, be the cathode material of solid tantalum capacitor first choice.
Although PEDOT solid tantalum capacitor has many advantages, such as that high frequency performance is good, capacity is big, there are still leakage current compared with
Big problem influences its further applying in circuit.The present invention is by introducing TiO2Film provides and a kind of prepares low drain
The method of electric current PEDOT solid tantalum capacitor improves damage of the situ aggregation method to deielectric-coating, to efficiently reduce leakage
Electric current.
Summary of the invention
The disadvantage that it is an object of the invention to overcome PEDOT solid tantalum capacitor leakage current larger, provides a kind of reduction
The method of PEDOT solid tantalum capacitor leakage current, this method are that tantalum core is immersed in butyl titanate ethanol solution, pass through metatitanic acid
Butyl ester hydrolysis forms the TiO of layer in dielectric layer surfaces externally and internally2Film, then in TiO2Film surface uses in-situ method shape
At PEDOT conductive film.
The method that the present invention prepares low-leakage current PEDOT solid tantalum capacitor, the specific steps are as follows:
(1) Ti (OC is weighed respectively by 9.5:1 mass ratio4H9)4And water, it is separately added into dehydrated alcohol, and be uniformly mixed；
(2) tantalum core is immersed in step (1) prepared solution about 1~3 minute；
(3) tantalum core is slowly withdrawn, at room temperature naturally dry, it is then dry under 150 DEG C of environment；
(4) step (2) and (3) are repeated 2 times；
(5) Fe (CH is weighed respectively by 8:1 mass ratio3C6H4SO3)3With EDOT (C6H6O2S) monomer is separately added into methanol,
It is uniformly mixed, reaction temperature is 60 DEG C；
(6) tantalum block is immersed in step (5) prepared reaction mixture, dip time is set as 1~5 minute；
(7) after impregnating, tantalum block is taken out, is placed in drying box and is dried；
(8) use EtOH-DI water mixed solvent as cleaning solution under vacuum conditions, dried after cleaning；
(9) step (6)~(8) are repeated 5~10 times；
(10) tantalum block is immersed in 7~8% aquadag solution, is taken out after being dried at 150 DEG C, outside graphite linings again
Coat one layer of silver paste metal layer；
The chemical raw material butyl titanate purity of the step (1) is greater than 98%, and purity of alcohol is that analysis is pure.
Chemical raw material Fe (the CH of the step (5)3C6H4SO3)3Purity be 98%, EDOT monomer purity be 99%, first
Alcohol purity is that analysis is pure.
Beneficial effect
Oxidant, monomer and byproduct of reaction during in-situ polymerization remain in tantalum core inner, cause to dielectric layer
Damage.The present invention passes through in dielectric layer and Ta2O5TiO is introduced between film2Film improves situ aggregation method to dielectric layer
Damage, prepares the PEDOT solid tantalum capacitor of low-leakage current.
Detailed description of the invention
Fig. 1 is PEDOT solid tantalum capacitor preparation flow figure；
Fig. 2 is the internal structure chart of PEDOT solid tantalum capacitor.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated.
Ti (OC is taken first4H9)4Mass ratio with water is 9.5:1, is separately added into dehydrated alcohol, is uniformly mixed.By tantalum core
It impregnates about 2 minutes in the above solution.It is slowly withdrawn tantalum core, at room temperature naturally dry, it is then 30 points dry under 150 DEG C of environment
Clock.Above impregnate is repeated 2 times with drying steps.One layer of TiO has been obtained outside dielectric layer2Film.
Fe (CH is weighed respectively in mass ratio for 8:13C6H4SO3)3It with EDOT monomer, is separately added into methanol, is ultrasonically treated
It is uniformly mixed it, reaction temperature is 60 DEG C.The impregnating speed of tantalum block is controlled and is immersed in reaction mixture for 3mm/s, is soaked
Keep tantalum block and liquid level vertical during stain, soaking time is set as 3 minutes.After immersion, tantalum is taken out with the speed of 3mm/s
Block, while keeping tantalum block and liquid level vertical.Tantalum block after taking-up is placed in drying box, and drying temperature is 60 DEG C, and the time is 10 points
Clock or so.Use EtOH-DI water mixed solvent as cleaning solution, is dried after cleaning, drying temperature 110
DEG C, the time is 5 minutes.Above dipping tantalum block, drying and cleaning step 5 times in reaction mixture are repeated, in TiO2Outside film
Face obtains one layer of PEDOT film.Then tantalum block is immersed in 7~8% aquadag solution, dried at 150 DEG C after taking-up
30 minutes, tantalum block being impregnated in aquadag solution and baking step being repeated 4 times, one layer of silver paste gold is coated with outside graphite linings
Belong to layer convenient for cathode extraction.
Its leakage current at 25 DEG C when different voltages of last test, and with non-depositing Ti O2The PEDOT tantalum capacitor of film
The leakage current of device is compared.
See Table 1 for details for the leakage current test result of the specific embodiment of the invention.
1 leakage current test result of table
When voltage increases, the leakage current of PEDOT solid tantalum capacitor prepared by the present invention is relatively low.At 25 DEG C,
When voltage is 20V, leakage current is 90 μ A, and is not added with TiO under equal conditions2The PEDOT solid tantalum capacitor leakage current of film
For 130 μ A.In conclusion the method step is simple, and it is easily operated, it can effectively reduce leakage current, extend PEDOT solid tantalum capacitor
The service life of device.
Claims (6)
1. a kind of method for reducing PEDOT solid tantalum capacitor leakage current, which is characterized in that specific step is as follows:
(1) Ti (OC is weighed respectively by 9.5:1 mass ratio4H9)4And water, it is separately added into dehydrated alcohol, and be uniformly mixed；
(2) impregnate: tantalum core is immersed in step (1) prepared solution about 1~3 minute；
(3) dry: being slowly withdrawn tantalum core, at room temperature naturally dry, it is then dry under 150 DEG C of environment；
(4) step (2) and (3) are repeated 2 times；
(5) Fe (CH is weighed respectively by 8:1 mass ratio3C6H4SO3)3It with EDOT monomer, is separately added into methanol, is uniformly mixed, reaction
Temperature is 60 DEG C；
(6) impregnate: tantalum block being immersed in step (5) prepared reaction mixture, dip time is set as 1~5 minute；
(7) dry: after dipping, tantalum block being taken out, is placed in drying box and is dried；
(8) use EtOH-DI water mixed solvent as cleaning solution under vacuum conditions, dried after cleaning；
(9) step (6)~(8) are repeated 5~10 times；
(10) tantalum block is immersed in 7~8% aquadag solution, takes out after being dried at 150 DEG C, be coated with outside graphite linings
One layer of silver paste metal layer.
2. a kind of method for reducing PEDOT solid tantalum capacitor leakage current according to claim 1, which is characterized in that institute
State raw material Ti (OC in step (1)4H9)4Purity be greater than 98%, purity of alcohol be analyze it is pure.
3. a kind of method for reducing PEDOT solid tantalum capacitor leakage current according to claim 1, which is characterized in that institute
State raw material Fe (CH in step (5)3C6H4SO3)3Purity be 98%, EDOT monomer purity be 99%, methanol purity be analyze it is pure.
4. a kind of method for reducing PEDOT solid tantalum capacitor leakage current according to claim 1, which is characterized in that institute
Stating in step (6) dipping process keeps tantalum block and liquid level vertical.
5. a kind of method for reducing PEDOT solid tantalum capacitor leakage current according to claim 1, which is characterized in that institute
It states step (7) and takes out tantalum block, while keeping tantalum block and liquid level vertical.
6. a kind of method for reducing PEDOT solid tantalum capacitor leakage current according to claim 1, which is characterized in that institute
It states step (10) dipping and drying is repeated 4 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910310664.0A CN110098060A (en) | 2019-04-17 | 2019-04-17 | A method of reducing PEDOT solid tantalum capacitor leakage current |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910310664.0A CN110098060A (en) | 2019-04-17 | 2019-04-17 | A method of reducing PEDOT solid tantalum capacitor leakage current |
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| Publication Number | Publication Date |
|---|---|
| CN110098060A true CN110098060A (en) | 2019-08-06 |
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| CN201910310664.0A Pending CN110098060A (en) | 2019-04-17 | 2019-04-17 | A method of reducing PEDOT solid tantalum capacitor leakage current |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5812367A (en) * | 1996-04-04 | 1998-09-22 | Matsushita Electric Industrial Co., Ltd. | Solid electrolytic capacitors comprising a conductive layer made of a polymer of pyrrole or its derivative |
| KR20060020148A (en) * | 2004-08-31 | 2006-03-06 | 파츠닉(주) | Method for manufacturing a small size ta capacitor |
| JP2007173454A (en) * | 2005-12-21 | 2007-07-05 | Nec Tokin Corp | Solid electrolytic capacitor |
| CN108475581A (en) * | 2016-01-18 | 2018-08-31 | 阿维科斯公司 | Solid electrolytic capacitor with improved leakage current |
-
2019
- 2019-04-17 CN CN201910310664.0A patent/CN110098060A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5812367A (en) * | 1996-04-04 | 1998-09-22 | Matsushita Electric Industrial Co., Ltd. | Solid electrolytic capacitors comprising a conductive layer made of a polymer of pyrrole or its derivative |
| KR20060020148A (en) * | 2004-08-31 | 2006-03-06 | 파츠닉(주) | Method for manufacturing a small size ta capacitor |
| JP2007173454A (en) * | 2005-12-21 | 2007-07-05 | Nec Tokin Corp | Solid electrolytic capacitor |
| CN108475581A (en) * | 2016-01-18 | 2018-08-31 | 阿维科斯公司 | Solid electrolytic capacitor with improved leakage current |
Non-Patent Citations (1)
| Title |
|---|
| 马小品: "固体钽电容用PEDOT阴极材料的原位合成及力学性能研究", 《工程科技II辑》 * |
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Application publication date: 20190806 |