CN1901113A - Process for preparing conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor - Google Patents
Process for preparing conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor Download PDFInfo
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- CN1901113A CN1901113A CN 200610045344 CN200610045344A CN1901113A CN 1901113 A CN1901113 A CN 1901113A CN 200610045344 CN200610045344 CN 200610045344 CN 200610045344 A CN200610045344 A CN 200610045344A CN 1901113 A CN1901113 A CN 1901113A
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- electrolytic capacitor
- neopelex
- anthraquinone
- cathode material
- aluminum electrolytic
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Abstract
This invention relates to a preparation method for conductive high-molecular cathode materials of solid plate-like Al electrolyte condensers, which takes EDT as the monomer of the conductive high-molecular cathode material to prepare it with a multi-time chemical oxidation method including process of inside film and outside film, which is simple and easy to be applied.
Description
Technical field
The present invention relates to a kind of preparation method of conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor.
Background technology
Solid sheet type aluminum electrolytic capacitor has overcome the drawback that the conventional aluminum electrolytic capacitor uses liquid electrolyte, reduced capacitor equivalent series resistance (ESR), improved capacitance, enlarged the frequency range of using.Conducting high polymers thing material (or conductive plastics) as the high-tech material of a new generation, since being synthesized the seventies, has been the popular object of academia and industrial quarters research and development in decades always.With the solid state cathode material of conducting high polymers thing as aluminium electrolytic capacitor, made aluminium electrolytic capacitor in high stability, long-life, and enlarge aspect such as range of application quantum jump arranged.As the conducting high polymers thing, the conductance of polypyrrole (PPY) can reach 20S/cm, and is higher 10 times than TCNQ, higher more than 100 times than the conductance of the liquid electrolyte in the conventional aluminum electrolytic capacitor.Baytron company is the conductive plastics of new generation of invention in the recent period, and 3,4-polyethylene dioxythiophene (PEDT), conductance can reach 100S/cm, and heat decomposition temperature height (＞245 C).Conducting polymer is applied to also have in the solid sheet type aluminum electrolytic capacitor characteristic of " self-healing " as cathode material, and can not burn.
Summary of the invention
The present invention seeks to provide a kind of preparation method of conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor, this technology not only simply is convenient to implement, and manufactured goods conductance height; Have better thermal stability and moisture resistance.
The preparation method of the conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor of the present invention comprises that inner layer film is made and outer membrane is made two main technique, and concrete steps are as follows:
1), inner layer film is made
(a) aluminium anodes after the anodization being immersed concentration is (in the ethanol of 10～46wt%) EDT, n-butanol or the isopropyl alcohol monomer solution, to take out oven dry;
(b) aluminium anodes after will drying immerses toluene sulfonic acide iron or the ammonium persulfate aqueous solution I that contains anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex, takes out oven dry; Wherein the content of anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex is 0.02～0.15mol/L, and the content of toluene sulfonic acide iron or ammonium persulfate is 0.5～1.5mol/L;
(c) place air to cool off;
(d) repeat (a)-(c) step 3～15 times;
2), outer membrane is made
(e) will finish the aluminium anodes immersion concentration of (d) step for (in the ethanol of 10～46wt%) EDT, n-butanol or the isopropyl alcohol monomer solution, taking out oven dry;
(f) aluminium anodes after will drying immerses and contains in the toluene sulfonic acide iron or ammonium persulfate aqueous solution II of anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex, takes out oven dry; Wherein the content of anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex is 0.05～0.5mol/L, and the content of toluene sulfonic acide iron or ammonium persulfate is 2.0～5.0mol/L;
(g) place air to cool off;
(h) repeat (e) → (g) step 5-20 time;
3), clean
(i) will finish the aluminium anodes washed with de-ionized water of (h) step;
The ethanol of above-mentioned EDT, n-butanol or isopropyl alcohol monomer solution concentration are 24.35wt%.Solution I is preferably 1.0mol/L toluene sulfonic acide iron or the ammonium persulfate aqueous solution that contains 0.1mol/L anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex.Solution II is preferably 3.5mol/L toluene sulfonic acide iron or the ammonium persulfate aqueous solution that contains 0.2mol/L anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex.
As the cathode material of solid sheet type aluminum electrolytic capacitor, the PEDT conducting polymer film needs by " plating " surface at aluminium anodes.Because the surface of aluminium anodes nonconducting deielectric-coating Al that is one deck
2O
3So in fact " plating " film is meant that conducting polymer film is by " plating " Al on aluminium anodes
2O
3The surface.
In technological process of the present invention, aluminium anodes immerses monomer solution earlier, reenters in the oxidant, takes out the reaction film forming, and repeats to obtain required thickness.Wherein cleaning step is to eliminate reactant and the product that remains in conducting polymer film and the aluminium anodes.The PEDT conductive polymer cathode material that this technical matters forms makes solid sheet type aluminum electrolytic capacitor have following good performance:
1, anti-mechanical stress and thermal stress resistance height;
2, form thin and the uniform PEDT film of thickness, greatly reduced the ESR of capacitor;
3, the PEDT film has improved the chemistry and the thermal stability of capacitor not with the impurity of Cl and Fe.
Description of drawings
Fig. 1 is the manufacture craft flow chart of the conducting polymer negative electrode of solid sheet type aluminum electrolytic capacitor.
Embodiment
Aluminium anodes after the anodization was immersed in ethanol, n-butanol or the aqueous isopropanol that EDT concentration is 24.35wt% 5 seconds, take out oven dry; Immersed again in the 1.0mol/L toluene sulfonic acide iron of 0.1mol/L anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex or the ammonium persulfate aqueous solution 5 seconds, and took out oven dry, and place air cooling 2 minutes; Repeat above-mentioned steps 5 times.
The aluminium chip of finishing above-mentioned steps was immersed in ethanol, n-butanol or the aqueous isopropanol that EDT concentration is 24.35wt% 5 seconds, take out oven dry; Immerse the 3.5mol/L toluene sulfonic acide iron of 0.2mol/L anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex or ammonium persulfate aqueous solution again 5 seconds, and took out oven dry, and place air cooling 2 minutes; Repeat above-mentioned steps 9 times.
Use washed with de-ionized water aluminium chip at last, promptly finish whole manufacture craft.
Make 5 capacitor elements with present embodiment, end properties is as shown in table 1
| Capacity (μ F) | Loss | ESR(mΩ) | Leakage current (μ A) | ESR after the Reflow Soldering (m Ω) |
| 9.0 | 0.009 | 45.8 | 0.22 | 55.0 |
| 9.2 | 0.006 | 43.0 | 0.23 | 53.9 |
| 8.9 | 0.007 | 44.6 | 0.20 | 54.6 |
| 9.1 | 0.007 | 45.1 | 0.22 | 55.2 |
| 9.5 | 0.008 | 45.9 | 0.26 | 51.7 |
The present invention is novel, and is reasonable in design, manufactured goods conductance height; Have better thermal stability and moisture resistance, have bigger application value.
Claims (4)
1, a kind of preparation method of conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor is characterized in that: comprise that inner layer film is made and outer membrane is made two main technique, concrete steps are as follows
1), inner layer film is made
(a) aluminium anodes after the anodization being immersed concentration is (in the ethanol of 10～46wt%) EDT, n-butanol or the isopropyl alcohol monomer solution, to take out oven dry;
(b) aluminium anodes after will drying immerses toluene sulfonic acide iron or the ammonium persulfate aqueous solution I that contains anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex, takes out oven dry; Wherein the content of anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex is 0.02～0.15mol/L, and the content of toluene sulfonic acide iron or ammonium persulfate is 0.5～1.5mol/L;
(c) place air to cool off;
(d) repeat (a)-(c) step 3～15 times;
2), outer membrane is made
(e) will finish the aluminium anodes immersion concentration of (d) step for (in the ethanol of 10～46wt%) EDT, n-butanol or the isopropyl alcohol monomer solution, taking out oven dry;
(f) aluminium anodes after will drying immerses and contains in the toluene sulfonic acide iron or ammonium persulfate aqueous solution II of anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex, takes out oven dry; Wherein the content of anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex is 0.05～0.5mol/L, and the content of toluene sulfonic acide iron or ammonium persulfate is 2.0～5.0mol/L;
(g) place air to cool off;
(h) repeat (e) → (g) step 5-20 time;
3), clean
(i) will finish the aluminium anodes washed with de-ionized water of (h) step.
2, the preparation method of the conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor according to claim 1 is characterized in that: the ethanol of EDT, n-butanol or isopropyl alcohol monomer solution concentration are 24.35wt%.
3, the preparation method of the conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor according to claim 1 is characterized in that: solution I is preferably 1.0mol/L toluene sulfonic acide iron or the ammonium persulfate aqueous solution that contains 0.1mol/L anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex.
4, the preparation method of the conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor according to claim 1 is characterized in that: solution II is preferably 3.5mol/L toluene sulfonic acide iron or the ammonium persulfate aqueous solution that contains 0.2mol/L anthraquinone-2-sodium, paratoluenesulfonic acid sodium salt or neopelex.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610045344A CN100576389C (en) | 2006-07-11 | 2006-07-11 | The preparation method of the conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor |
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|---|---|---|---|
| CN200610045344A CN100576389C (en) | 2006-07-11 | 2006-07-11 | The preparation method of the conductive polymer cathode material of solid sheet type aluminum electrolytic capacitor |
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| CN1901113A true CN1901113A (en) | 2007-01-24 |
| CN100576389C CN100576389C (en) | 2009-12-30 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101866748A (en) * | 2010-06-23 | 2010-10-20 | 福建国光电子科技股份有限公司 | Chemical polymerization process for forming solid electrolyte layer on solid electrolytic capacitor |
| CN101866750A (en) * | 2010-06-23 | 2010-10-20 | 福建国光电子科技股份有限公司 | Electrochemical polymerization process for forming solid electrolyte layer on solid electrolytic capacitor |
| CN101871115A (en) * | 2010-05-31 | 2010-10-27 | 福建国光电子科技股份有限公司 | Electrolyte used for treating aluminium foil in aluminium electrolytic capacitor |
| CN101894672A (en) * | 2010-06-23 | 2010-11-24 | 福建国光电子科技股份有限公司 | Chemical polymerization process for forming solid electrolyte layer by solid electrolytic capacitor |
| CN102543491A (en) * | 2012-02-29 | 2012-07-04 | 万星光电子(东莞)有限公司 | Manufacturing method for laminated solid aluminium electrolytic capacitor |
| CN107039184A (en) * | 2017-04-01 | 2017-08-11 | 中南大学 | A kind of solid-state aluminum electrolytic capacitor and preparation method thereof |
| CN113990665A (en) * | 2020-07-27 | 2022-01-28 | 深圳市柏瑞凯电子科技股份有限公司 | Method for manufacturing conductive polymer cathode material of laminated solid aluminum electrolytic capacitor |
-
2006
- 2006-07-11 CN CN200610045344A patent/CN100576389C/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101871115A (en) * | 2010-05-31 | 2010-10-27 | 福建国光电子科技股份有限公司 | Electrolyte used for treating aluminium foil in aluminium electrolytic capacitor |
| CN101866748A (en) * | 2010-06-23 | 2010-10-20 | 福建国光电子科技股份有限公司 | Chemical polymerization process for forming solid electrolyte layer on solid electrolytic capacitor |
| CN101866750A (en) * | 2010-06-23 | 2010-10-20 | 福建国光电子科技股份有限公司 | Electrochemical polymerization process for forming solid electrolyte layer on solid electrolytic capacitor |
| CN101894672A (en) * | 2010-06-23 | 2010-11-24 | 福建国光电子科技股份有限公司 | Chemical polymerization process for forming solid electrolyte layer by solid electrolytic capacitor |
| CN102543491A (en) * | 2012-02-29 | 2012-07-04 | 万星光电子(东莞)有限公司 | Manufacturing method for laminated solid aluminium electrolytic capacitor |
| CN107039184A (en) * | 2017-04-01 | 2017-08-11 | 中南大学 | A kind of solid-state aluminum electrolytic capacitor and preparation method thereof |
| CN107039184B (en) * | 2017-04-01 | 2019-10-22 | 中南大学 | A kind of solid-state aluminum electrolytic capacitor and preparation method thereof |
| CN113990665A (en) * | 2020-07-27 | 2022-01-28 | 深圳市柏瑞凯电子科技股份有限公司 | Method for manufacturing conductive polymer cathode material of laminated solid aluminum electrolytic capacitor |
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| Publication number | Publication date |
|---|---|
| CN100576389C (en) | 2009-12-30 |
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