CN101894671A - Chemical polymerization process for forming solid electrolyte layer of solid electrolytic capacitor - Google Patents
Chemical polymerization process for forming solid electrolyte layer of solid electrolytic capacitor Download PDFInfo
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- CN101894671A CN101894671A CN 201010207675 CN201010207675A CN101894671A CN 101894671 A CN101894671 A CN 101894671A CN 201010207675 CN201010207675 CN 201010207675 CN 201010207675 A CN201010207675 A CN 201010207675A CN 101894671 A CN101894671 A CN 101894671A
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Abstract
The invention provides a chemical polymerization process for forming a solid electrolyte layer of a solid electrolytic capacitor, which comprises: an oxidation liquid impregnation step of impregnating an anode surface provided with an oxide film medium into oxidation liquid for a certain time, and a monomer solution impregnation step of impregnating the impregnated anode surface into monomer solution for a certain time, wherein the temperature of the monomer solution is controlled to be 10 to 50 DEG C in the monomer solution impregnation step; and the temperature of the oxidation liquid is 5 to 35 DEG C in the oxidation liquid impregnation step. The chemical polymerization process for forming the solid electrolyte layer of the solid electrolytic capacitor has the advantages that: the performance of the electrolytic capacitor produced in the chemical polymerization process is more controllable; moreover, the electrolytic capacitor formed within the temperature range has higher capacitance, lower loss, higher ESR and the like.
Description
[technical field]
The present invention relates to the concrete operation in the solid electrolytic capacitor production process, particularly the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor.
[background technology]
Capacitor belongs to electronics and information industry basic device product, be that a kind of use is the widest, the consumption maximum, and the electronic component of not replacing, its output accounts for 40% of electronic component, along with the development of electronics and information industry, electronics and IT products output, kind constantly increase, and the demand of supporting with it capacitor also constantly increases.The performance of capacitor, kind and quality directly determine or affect the development of electronics and IT products.Adapt to surface mounting technology, chip type, miniaturization in order to solve the traditional liquid electrolytic capacitor, must solve electrolytical solidification.Plurality of advantages such as solid electrolytic capacitor has that volume is littler, performance is better, wide temperature, long-life, anti-high frequency, high reliability and high environmental protection adapt to the development trend and the surface mounting technology requirement of complete electronic set miniaturization, high frequencyization, high speed, highly reliable, high environmental protection.
Solid electrolytic capacitor is to adopt anode oxidation method to generate the skim oxide as dielectric on the surface of oxides such as valve metal such as aluminium, tantalum, niobium, titanium or columbium monoxide, the capacitor that constitutes as negative electrode with solid electrolyte.The solid electrolyte of the solid electrolytic capacitor of the type can be electric conductive polymer, such as polypyrrole, and polythiophene, polyaniline or derivatives thereof.The polymerizing condition of conducting polymer has a significant impact the chemical polymerization process of solid electrolytic capacitor and the character of polymer, the temperature of polymeric solution particularly, and the electric conductivity of the conducting polymer that its reaction speed and polymerization are obtained has material impact.Under different polymeric solution temperature conditions, the electric conductivity difference of the polymerization speed of conducting polymer and conducting polymer is very big, similarly, conductive polymer applications in the polymer solids electrolytic capacitor time, polymerization obtains the solid electrolytic capacitor that conductive polymer membrane is formed into then under different polymeric solution temperature conditions, and the capacity of its solid capacitor, loss and ESR also have than big-difference.
Open day is that on 02 20th, 2008 China Patent No. is 200510041690.6 patent of invention, its name is called " manufacture method of solid sheet type electrolytic capacitor ", the chemical polymerization process of solid electrolytic capacitor is disclosed in this patent documentation, in forming the chemical polymerization process that pre-conductive layer is first solid electrolyte layer, temperature range to polymeric solution does not limit, electric conductivity at the conductive layer that exceeds the formation of suitable temperature scope can not be controlled, thereby cause the performance of solid electrolytic capacitor can not reach its intended purposes.
Open day is that on 07 22nd, 2009 publication number is the Chinese invention patent of CN101486836, its name is called " conductive-polymer solution, the formation method and the solid electrolytic capacitor of conductive polymer coated film conductive-polymer solution ", a kind of chemical polymerization process of coiling type solid capacitor is disclosed in this patent documentation, its chemical polymerization solution is mainly the mixed solution of polymer and solvent formation, polymer can be a polypyrrole, thiophene etc., its be directly with polymer applications in this technology, technical process is that above-mentioned solution is dipped on the valve metal (aluminium foil), then the solvent oven dry is removed.In this patent documentation, the temperature of mixed solution can be controlled at-scope of 30-200 ℃ in.
Open day is that on 09 12nd, 2007 publication number is the Chinese invention patent of CN101034629, its name is called " a kind of manufacture method of coiled solid electrolysis capacitor ", a kind of chemical polymerization process of coiling type solid capacitor is also disclosed in this patent documentation, its chemical polymerization solution is the mixed solution of oxidant and monomer, this technology is that oxidation liquid and reducing solution are mixed, for preventing oxidant and monomer reaction, in this patent documentation, the temperature of mixed solution can be controlled at-scope of 70-60 ℃ in.
Open day is that on 05 17th, 2006 publication number is the Chinese invention patent of CN1773640, its name is called " Solid electrolytic capacitor And Manufacturing approach ", the chemical polymerization process of coiling type solid capacitor (non-chip) is also disclosed in this patent documentation, its chemical polymerization solution also is the mixed solution of oxidant and monomer, the solvent that adopts is an organic solvent, this technology is that oxidation liquid and monomer liquid are mixed, for preventing oxidant and monomer reaction, in this patent documentation, the temperature of mixed solution can be controlled in 20-35 ℃ the scope.
[summary of the invention]
The technical problem to be solved in the present invention, be to provide a kind of chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor, limit by temperature range conducting polymer polymerization solution, the polymerization process that guarantees conducting polymer is controlled, thereby make that the performance that forms the solid electrolytic capacitor that obtains also is controlled, the temperature range that can solve the polymeric solution that exists in the prior art does not limit, can not be controlled at the electric conductivity that exceeds the conductive layer that the suitable temperature scope forms, cause the performance of solid electrolytic capacitor can not reach the problem of its intended purposes.
The present invention is by solving the problems of the technologies described above by the following technical solutions: the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor, described chemical polymerization process comprises the monomer solution immersion liquid step that the anode body surface that will form oxide film dielectric places oxidation liquid to soak the oxidation liquid immersion liquid step of certain hour and place monomer solution immersion certain hour, wherein, in the described monomer solution immersion liquid step, the temperature range of described monomer solution is controlled at 10-50 ℃.
Further, in the described oxidation liquid immersion liquid step, described oxidation liquid temp is 5-35 ℃.
Further, in the described monomer solution immersion liquid step, the temperature range of described monomer solution is controlled at 15-40 ℃.
Further, described monomer solution comprises monomer, dopant and solvent at least.
Further, described monomer can be pyrroles, thiophene, aniline or pyrroles's derivative, the derivative of thiophene, the derivative of aniline.
Further, described dopant can be tosilate, dodecyl benzene sulfonate, dodecane sulfonate, naphthalene sulfonate, alkyl salicylate, benzoate or camsilate.
Further, described oxidation liquid comprises oxidant and solvent at least, and described oxidant is at least a in potassium permanganate, hydrogen peroxide, trivalent iron salt or the persulfate.
Further, comprise the step of cleaning, drying after the described oxidation liquid immersion liquid step, also comprise the step of cleaning, drying after the described monomer solution immersion liquid step.
Further, the production technology of described solid capacitor mainly comprises: the operation that forms oxide film dielectric on the capacitor anode surface; On the oxide film dielectric outer surface, form the operation of solid electrolyte layer; Form the operation of carbon containing cathode layer at the solid electrolyte layer outer surface; Form the operation that contains silver body cathode layer at carbon containing cathode layer outer surface; Make capacitor element,, make the operation of solid electrolytic capacitor, the method that the formation of described solid electrolyte layer adopts chemical polymerization method or chemical polymerization to combine with electrochemical polymerization capacitor element assembling and encapsulation.
Further, the anode bodies of described solid electrolytic capacitor can be valve metal and oxide, and described valve metal can be aluminium, tantalum, niobium or titanium, and described oxide is a columbium monoxide.
The chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor involved in the present invention has following beneficial effect: the temperature range by monomer solution in the control chemical polymerization process is at 10-50 ℃, make that the character of the conductive polymer coating that polymerization obtains is controlled, thereby make that the performance that forms the electrostrictive polymer electrolysis condenser that obtains is controlled, and performances such as the capacitance of the electrolytic capacitor that formation obtains under this solution temperature scope, loss, ESR are better.
[embodiment]
The production technology of solid electrolytic capacitor involved in the present invention mainly comprises: the operation that forms oxide film dielectric on the capacitor anode surface; On the oxide film dielectric outer surface, form the operation of solid electrolyte layer; Form the operation of carbon containing cathode layer at the solid electrolyte layer outer surface; Form the operation that contains silver body cathode layer at carbon containing cathode layer outer surface; Make capacitor element,, make the operation of solid electrolytic capacitor capacitor element assembling and encapsulation.The solid electrolytic capacitor that with the valve metal is aluminium is an example, the operation that forms solid electrolyte layer on the oxide film dielectric outer surface is to form first solid electrolyte layer by the technology that adopts chemical polymerization on aluminium foil surface, and the first solid electrolyte laminar surface forms second solid electrolyte layer by the method for electrochemical polymerization then.Particularly, in the chemical polymerization process, be to place oxidation liquid to soak certain hour on aluminium foil earlier, take out oven dry then, again aluminium foil is placed monomer solution to soak certain hour and take out oven dry, the above-mentioned step of repetitive cycling repeatedly forms solid electrolyte layer at aluminium foil surface in the back, and described oxidation liquid can be the aqueous solution of potassium permanganate, hydrogen peroxide, trivalent iron salt, persulfate, and is first-selected for comprising the solution of potassium permanganate; Described monomer solution can be the mixed aqueous solution of monomer and dopant composition, and described monomer can be pyrroles, thiophene, aniline or pyrroles's derivative, the derivative of thiophene, the derivative of aniline, first-selected pyrroles and azole derivatives; Described dopant can be tosilate, dodecyl benzene sulfonate, dodecane sulfonate, naphthalene sulfonate, alkylsalicylate, benzoate, camsilate, first-selected tosilate.The temperature range of described monomer solution is controlled at 10-50 ℃, and described oxidation liquid temp is 5-35 ℃.
Embodiment 1
In chemical polymerization process, (effective area 3.5mm * 4.0mm) places the KMnO of 0.3M will to comprise aluminium oxide 13VF aluminium foil earlier
4Soaked 1 minute in the aqueous solution, take out oven dry, be 0.5 to contain in the mixed aqueous solution of tosilate of the Py (pyrrole monomer) of 0.4M and 0.5M and soaked 2 minutes in the pH value again, take out oven dry, cleaning, drying after the above step 3 of repetition time promptly forms the first solid electrolyte layer polypyrrole at aluminium foil surface.Wherein, by the water-bath temperature control, keeping the temperature of monomer solution is 20 ℃.The oxidation liquid temp all can in 5-35 ℃ room temperature range.After chemical polymerization process is finished, form the second solid electrolyte layer polypyrrole in the method for the first solid electrolyte laminar surface by electrochemical polymerization then.Form the carbon containing cathode layer successively at the solid electrolyte layer outer surface, contain silver body cathode layer; Make the monolithic capacitor element,, make solid aluminum electrolytic capacitor monolithic capacitor element stack and encapsulation.
Embodiment 2
As different from Example 1, by the water-bath temperature control, keeping the temperature of monomer solution is 30 ℃.
Embodiment 3
As different from Example 1, by the water-bath temperature control, keeping the temperature of monomer solution is 35 ℃.
Embodiment 4
As different from Example 1, by the water-bath temperature control, keeping the temperature of monomer solution is 40 ℃.
Comparative Examples 1
As different from Example 1, by the water-bath temperature control, keeping the temperature of monomer solution is 5 ℃.
Comparative Examples 2
As different from Example 1, by the water-bath temperature control, keeping the temperature of monomer solution is 70 ℃.
By using above-mentioned chemical polymerization process, folded 6 layers at last, be formed into 6.3V/100 μ F capacitor, the average data of the capacitance of 30 capacitors that the various embodiments described above and Comparative Examples are measured, loss, ESR is as shown in table 1.
Table 1 embodiment and Comparative Examples electrical property comparison sheet
| Project | Capacitance (μ F) | Loss (‰) | ESR (mΩ) |
| Embodiment 1 | 100.4 | 10 | 21 |
| Embodiment 2 | 101.2 | 11 | 20 |
| Embodiment 3 | 103.9 | 9 | 22 |
| Embodiment 4 | 103.3 | 10 | 19 |
| Comparative Examples 1 | 63.2 | 42 | 43 |
| Comparative Examples 2 | 54.9 | 64 | 67 |
The data of table 1 show, are controlled in the suitable scope by the monomer solution temperature with the chemical polymerization of forming solid electrolyte layer by solid electrolytic capacitor, and the electrical property of resulting capacitor obviously is better than Comparative Examples.
Claims (10)
1. the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor, described chemical polymerization process comprises the monomer solution immersion liquid step that the anode body surface that will form oxide film dielectric places oxidation liquid to soak the oxidation liquid immersion liquid step of certain hour and place monomer solution immersion certain hour, it is characterized in that: in the described monomer solution immersion liquid step, the temperature range of described monomer solution is controlled at 10-50 ℃.
2. the chemical polymerization solution of forming solid electrolyte layer by solid electrolytic capacitor according to claim 1, it is characterized in that: in the described oxidation liquid immersion liquid step, described oxidation liquid temp is 5-35 ℃.
3. the chemical polymerization solution of forming solid electrolyte layer by solid electrolytic capacitor according to claim 1 and 2 is characterized in that: in the described monomer solution immersion liquid step, the temperature range of described monomer solution is controlled at 15-40 ℃.
4. the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor according to claim 1 and 2, it is characterized in that: described monomer solution comprises monomer, dopant and solvent at least.
5. the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor according to claim 4, it is characterized in that: described monomer can be pyrroles, thiophene, aniline or pyrroles's derivative, the derivative of thiophene, the derivative of aniline.
6. the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor according to claim 4, it is characterized in that: described dopant can be tosilate, dodecyl benzene sulfonate, dodecane sulfonate, naphthalene sulfonate, alkyl salicylate, benzoate or camsilate.
7. the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor according to claim 1 and 2, it is characterized in that: described oxidation liquid comprises oxidant and solvent at least, and described oxidant is at least a in potassium permanganate, hydrogen peroxide, trivalent iron salt or the persulfate.
8. the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor according to claim 1, it is characterized in that: comprise the step of cleaning, drying after the described oxidation liquid immersion liquid step, also comprise the step of cleaning, drying after the described monomer solution immersion liquid step.
9. the chemical polymerization process of forming solid electrolyte layer by solid electrolytic capacitor according to claim 1, it is characterized in that: the production technology of described solid capacitor mainly comprises: the operation that forms oxide film dielectric on the capacitor anode surface; On the oxide film dielectric outer surface, form the operation of solid electrolyte layer; Form the operation of carbon containing cathode layer at the solid electrolyte layer outer surface; Form the operation that contains silver body cathode layer at carbon containing cathode layer outer surface; Make capacitor element,, make the operation of solid electrolytic capacitor, the method that the formation of described solid electrolyte layer adopts chemical polymerization method or chemical polymerization to combine with electrochemical polymerization capacitor element assembling and encapsulation.
10. the chemical polymerization solution of forming solid electrolyte layer by solid electrolytic capacitor according to claim 1, it is characterized in that: the anode bodies of described solid electrolytic capacitor can be valve metal and oxide, described valve metal can be aluminium, tantalum, niobium or titanium, and described oxide is a columbium monoxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059225A (en) * | 2014-06-25 | 2014-09-24 | 福建国光电子科技股份有限公司 | Chemical polymerization process for preparing polypyrrole |
| CN111210995A (en) * | 2013-08-15 | 2020-05-29 | Avx 公司 | Moisture resistant solid electrolytic capacitor assembly |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1369888A (en) * | 2001-02-08 | 2002-09-18 | 松下电器产业株式会社 | Mfg. Method of solid electrolytic capacity and solid electrolytic capacity |
| CN101504887A (en) * | 2009-01-13 | 2009-08-12 | 珠海华冠电容器有限公司 | Manufacturing method for solid aluminum electrolytic capacitor |
-
2010
- 2010-06-23 CN CN 201010207675 patent/CN101894671A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1369888A (en) * | 2001-02-08 | 2002-09-18 | 松下电器产业株式会社 | Mfg. Method of solid electrolytic capacity and solid electrolytic capacity |
| CN101504887A (en) * | 2009-01-13 | 2009-08-12 | 珠海华冠电容器有限公司 | Manufacturing method for solid aluminum electrolytic capacitor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111210995A (en) * | 2013-08-15 | 2020-05-29 | Avx 公司 | Moisture resistant solid electrolytic capacitor assembly |
| CN104059225A (en) * | 2014-06-25 | 2014-09-24 | 福建国光电子科技股份有限公司 | Chemical polymerization process for preparing polypyrrole |
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Application publication date: 20101124 |