CN102842434A - Preparation method for cathode of electrolytic capacitor - Google Patents
Preparation method for cathode of electrolytic capacitor Download PDFInfo
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- CN102842434A CN102842434A CN201210326942XA CN201210326942A CN102842434A CN 102842434 A CN102842434 A CN 102842434A CN 201210326942X A CN201210326942X A CN 201210326942XA CN 201210326942 A CN201210326942 A CN 201210326942A CN 102842434 A CN102842434 A CN 102842434A
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- manganese nitrate
- electrolytic capacitor
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- nitrate solution
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Abstract
The invention discloses a preparation method for a cathode of an electrolytic capacitor. The preparation method comprises the following steps of: impregnating a metal block, which is used as an anode, in a manganese nitrate solution with different specific gravities for a plurality of times, wherein the specific gravity of the manganese nitrate solution is 1.10-1.90 and increased with the increasing of the number of times; and during each impregnation, generating manganese dioxide at a temperature of 200-270 DEG C by the manganese nitrate so as to form a metal block containing the manganese dioxide in the outer layer; the preparation method further comprises a manganese nitrate mixed solution preparing step as follows: adding powdery filling material, which accounts for 30-70% of the weight of the manganese nitrate solution, and graphite, which accounts for 30-70% of the weight of the manganese nitrate solution, to the manganese nitrate solution with the specific gravity of 1.10-1.30, wherein the filling material is obtained by mixing nanoscale carbon powder and a resin according to a weight ratio of 1:(1-5); and the preparation method comprises an impregnating and decomposing step as follows: impregnating the metal block in the prepared manganese nitrate mixed solution for a plurality of times; generating the manganese dioxide at a temperature 200-270 DEG C by the manganese nitrate; and mixing the powdery filling material and the graphite in the manganese dioxide so as to form a cathode.
Description
Technical field
The present invention relates to the preparation of electrolytic capacitor, particularly relate to a kind of cathode preparation method of electrolytic capacitor.
Background technology
Along with a large amount of of intelligent portable electronic equipment popularize; In these equipment, power supply is provided and as the capacitor of power filter (the Equivalent Series Resistance that requires to have littler equivalent series resistance to IC; ESR), thus electric capacity must adapt to new requirement.The approach that improves product E SR at present mainly contains following several kinds: 1, change product structure: the multianode design; 2, change cathode material: use the higher conducting polymer of conductivity; 3, improve the product negative electrode and draw associativity and compatibility between the material.Yet no matter which kind of approach to improve ESR through, the 3rd kind of approach all is suitable for, and is absolutely necessary.
With the tantalum electrolytic capacitor is example, and Fig. 1 is its negative electrode deriving structure sketch map, its ESR=R
Be situated between+ R
Separate+ R
Gold, R wherein
Be situated betweenThe resistance of expression dielectric oxide film, R
GoldThe expression negative electrode is drawn the resistance of layer, R
SeparateContact resistance, graphite linings self-resistance, graphite linings and the silver layer contact resistance, the silver layer resistance that comprise manganese dioxide self-resistance, manganese dioxide layer and graphite linings; In these several kinds of resistance; Contact resistance is more important with respect to the resistance of each material self; On the one hand it reduce can make the ESR of whole capacitor device obviously reduce, it also affects the stability of properties of product to a great extent on the other hand.
Summary of the invention
Technical problem to be solved by this invention is: remedy the deficiency of above-mentioned prior art, propose a kind of cathode preparation method of electrolytic capacitor, can effectively reduce the ESR of electrolytic capacitor.
Technical problem of the present invention solves through following technical scheme:
A kind of cathode preparation method of electrolytic capacitor; Contain the manganese dioxide solid in the negative electrode of said electrolytic capacitor, comprise the steps: the metal derby as anode is contained several in the manganese nitrate solution that is immersed in different specific weight, the proportion of said manganese nitrate solution is 1.10 ~ 1.90; And increase with the impregnation number of times; The proportion of manganese nitrate solution is ascending, and during each impregnation, manganese nitrate all decomposes down at 200 ℃ ~ 270 ℃ and generates manganese dioxide; To form the metal derby that skin contains manganese dioxide, also comprise the steps:
Preparation manganese nitrate mixed solution step: in proportion is 1.10 ~ 1.30 manganese nitrate solution; Add the Powdered inserts of this manganese nitrate solution weight 30% ~ 70% and the graphite of this manganese nitrate solution weight 30% ~ 70%, said Powdered inserts is to be that the nanoscale carbon dust and the mixed with resin of 1:1 ~ 5 forms by weight ratio;
The impregnation decomposition step: the metal derby that said skin is contained manganese dioxide contains several in the manganese nitrate mixed solution that is immersed in above-mentioned preparation; Decompose generation manganese dioxide at 200 ~ 270 ℃ of following manganese nitrates; Said Powdered inserts and graphite are blended in the manganese dioxide, accomplish the manufacturing of said negative electrode.
Preferably, the particle diameter of said Powdered inserts is 100 ~ 200nm, and thus, corresponding, the particle diameter of nanoscale carbon dust is 100 ~ 200nm, and the particle diameter of toner also is 100 ~ 200nm.
Preferably, the addition of said Powdered inserts is 60% ~ 70% of a manganese nitrate solution weight.
Preferably, said resin is a polyvinyl alcohol, and its molecular weight is 150 ~ 250D.
Preferably, said electrolytic capacitor is tantalum electrolytic capacitor or niobium electrolytic capacitor.
A kind of inserts that is used for mixing electrolytic capacitor cathode is that the nanoscale carbon dust and the mixed with resin of 1:1 ~ 5 forms by weight ratio.
Preferably, said resin is a polyvinyl alcohol, and its molecular weight is 150 ~ 250D.
Preferably, the particle diameter of said nanoscale carbon dust is 100 ~ 200nm.
A kind of negative electrode of electrolytic capacitor is made by above-mentioned any described preparation method.
A kind of electrolytic capacitor comprises above-mentioned negative electrode.
The beneficial effect of the present invention and prior art contrast is: in manganese nitrate solution, add the evenness that Powdered inserts can improve the manganese dioxide cathodes layer, thereby improve the contact of manganese dioxide layer and graphite linings, reduce ESR.
Description of drawings
Fig. 1 is the negative electrode deriving structure sketch map of tantalum electrolytic capacitor in the prior art.
Embodiment
Below in conjunction with preferred embodiment the present invention is carried out detailed elaboration.
The present invention provides a kind of cathode preparation method of electrolytic capacitor; Contain the manganese dioxide solid in the negative electrode of said electrolytic capacitor; In one embodiment, comprise the steps: the metal derby as anode is contained several in the manganese nitrate solution that is immersed in different specific weight, the proportion of said manganese nitrate solution is 1.10 ~ 1.90; And increase with the impregnation number of times; The proportion of manganese nitrate solution is ascending, and during each impregnation, manganese nitrate all decomposes down at 200 ℃ ~ 270 ℃ and generates manganese dioxide; To form the metal derby that skin contains manganese dioxide; Also comprise the steps: to prepare manganese nitrate mixed solution step: in proportion is 1.10 ~ 1.30 manganese nitrate solution, add the Powdered inserts of this manganese nitrate solution weight 30% ~ 70% and the graphite of this manganese nitrate solution weight 30% ~ 70%, said Powdered inserts is to be that the nanoscale carbon dust and the mixed with resin of 1:1 ~ 5 forms by weight ratio; The impregnation decomposition step: the metal derby that said skin is contained manganese dioxide contains several in the manganese nitrate mixed solution that is immersed in above-mentioned preparation; Decompose generation manganese dioxide at 200 ~ 270 ℃ of following manganese nitrates; Said Powdered inserts and graphite are blended in the manganese dioxide of impregnation decomposition step generation, accomplish the manufacturing of said negative electrode.
After the manganese dioxide capacity of manganese nitrate decomposition generation in early stage was enough, along with later stage manganese nitrate proportion improves, the content of inner manganese dioxide can increase; Also can form rough surface state during reaction, improve proportion gradually at manganese nitrate solution and decompose the back and (also promptly contain and be immersed in the manganese nitrate solution for several times, with the increase of number of times as the metal derby of anode; Manganese nitrate is from thin to thick), form the outer metal derby that contains manganese dioxide, at this moment; The number of times of impregnation is good with the thickness of the cathode layer of formation with 0.07-0.08mm, and then in the manganese nitrate solution of proportion less (proportion is 1.10 ~ 1.30), adds a certain amount of Powdered inserts and graphite; And will before the skin that the forms metal derby that contains manganese dioxide contain and be immersed in this solution for several times; The number of times of impregnation is good with the thickness that increases by 0.04 ~ 0.05mm, and it is good that the thickness of the cathode layer that also promptly finally forms is no more than 0.12 ~ 0.13mm, the experiment proof; Impregnation is advisable for 2 ~ 3 times; Manganese nitrate resolves into manganese dioxide during each impregnation, and Powdered inserts and graphite are blended in the manganese dioxide cathodes layer, and inserts can be filled concavo-convex place; Make it form fine and close relatively and smooth surface state; Improve the evenness of manganese dioxide cathodes layer, thereby reduced the contact resistance of manganese dioxide, thereby the area of the manganese dioxide of opposed flattened can increase the contact that has improved between manganese dioxide layer and the graphite linings.
After experiment showed, this inserts of interpolation, the ESR of product can reduce by 10%～30%.
In a preferred embodiment, the particle diameter of Powdered inserts is 100 ~ 200nm, and thus, corresponding, the particle diameter of nanoscale carbon dust is 100 ~ 200nm, and the particle diameter of toner also is 100 ~ 200nm.
In a preferred embodiment, the addition of Powdered inserts is 60% ~ 70% of a manganese nitrate solution weight.
In a preferred embodiment, said resin is a polyvinyl alcohol, and its molecular weight is 150 ~ 250D.
Preferably, said electrolytic capacitor is tantalum electrolytic capacitor or niobium electrolytic capacitor.
The present invention also provides a kind of inserts that is used for mixing electrolytic capacitor cathode, is that the nanoscale carbon dust and the mixed with resin of 1:1 ~ 5 forms by weight ratio, preferably; Said resin is a polyvinyl alcohol; Its molecular weight is 150 ~ 250D, and preferably, the particle diameter of said nanoscale carbon dust is 100 ~ 200nm.
Below through embodiment more specifically the present invention is set forth in detail.
Embodiment one
To contain several in the manganese nitrate solution that is immersed in different specific weight as the tantalum piece of anode; The proportion of manganese nitrate solution is 1.10 ~ 1.90, and with the increase of impregnation number of times, the proportion of manganese nitrate solution is ascending; During each impregnation; Manganese nitrate all decomposes generation manganese dioxide down at 200 ℃ ~ 270 ℃, to form the metal derby that skin contains manganese dioxide, carries out following steps then:
Preparation manganese nitrate mixed solution step: in proportion is 1.10 manganese nitrate solution; (addition of graphite can also be other values in 30% ~ 70% certainly with the graphite of this manganese nitrate solution weight 30% to add the Powdered inserts of this manganese nitrate solution weight 30%; The factor that influences the ESR of product among the present invention mainly is Powdered inserts and addition thereof); Powdered inserts is to be that nanoscale carbon dust and the polyvinyl alcohol of 1:1 mixes and form by weight ratio, and the molecular weight of polyvinyl alcohol is 250D.
The impregnation decomposition step: the metal derby that above-mentioned skin is contained manganese dioxide contains in the manganese nitrate mixed solution that is immersed in above-mentioned preparation 2 ~ 3 times; During each impregnation; All decompose and generate manganese dioxide at 200 ~ 270 ℃ of following manganese nitrates; Powdered inserts and graphite are blended in the manganese dioxide, accomplish the negative electrode manufacturing thus.The negative electrode that makes in the present embodiment is further made tantalum electrolytic capacitor by the method for routine, and recording its ESR is 1.0 Ω.
Embodiment two
Be with the difference of embodiment one: in the preparation manganese nitrate mixed solution step; The proportion of manganese nitrate solution is 1.30; The addition of Powdered inserts is 40% of this manganese nitrate solution weight; The addition of graphite is 40% (with embodiment one, the addition of graphite can also be other values in 30% ~ 70%, and the factor that influences the ESR of product among the present invention mainly is Powdered inserts and addition thereof) of this manganese nitrate solution weight; Powdered inserts is to be that nanoscale carbon dust and the polyvinyl alcohol of 1:2 mixes and form by weight ratio, and the molecular weight of polyvinyl alcohol is 170D.The negative electrode that makes in the present embodiment is further made tantalum electrolytic capacitor by the method for routine, and recording its ESR is 0.8 Ω.
Embodiment three
Be with the difference of embodiment one: in the preparation manganese nitrate mixed solution step; The proportion of manganese nitrate solution is 1.20; The addition of Powdered inserts is 50% of this manganese nitrate solution weight; The addition of graphite is 50% (with embodiment one, the addition of graphite can also be other values in 30% ~ 70%, and the factor that influences the ESR of product among the present invention mainly is Powdered inserts and addition thereof) of this manganese nitrate solution weight; Powdered inserts is to be that nanoscale carbon dust and the polyvinyl alcohol of 1:3 mixes and form by weight ratio, and the molecular weight of polyvinyl alcohol is 150D.The negative electrode that makes in the present embodiment is further made tantalum electrolytic capacitor by the method for routine, and recording its ESR is 0.7 Ω.
Embodiment four
Be with the difference of embodiment one: in the preparation manganese nitrate mixed solution step; The proportion of manganese nitrate solution is 1.20; The addition of Powdered inserts is 60% of this manganese nitrate solution weight; The addition of graphite is 60% (with embodiment one, the addition of graphite can also be other values in 30% ~ 70%, and the factor that influences the ESR of product among the present invention mainly is Powdered inserts and addition thereof) of this manganese nitrate solution weight; Powdered inserts is to be that nanoscale carbon dust and the polyvinyl alcohol of 1:5 mixes and form by weight ratio, and the molecular weight of polyvinyl alcohol is 150D.The negative electrode that makes in the present embodiment is further made tantalum electrolytic capacitor by the method for routine, and recording its ESR is 0.6 Ω.
Embodiment five
Be with the difference of embodiment one: in the preparation manganese nitrate mixed solution step; The proportion of manganese nitrate solution is 1.20; The addition of Powdered inserts is 70% of this manganese nitrate solution weight; The addition of graphite is 70% (with embodiment one, the addition of graphite can also be other values in 30% ~ 70%, and the factor that influences the ESR of product among the present invention mainly is Powdered inserts and addition thereof) of this manganese nitrate solution weight; Powdered inserts is to be that nanoscale carbon dust and the polyvinyl alcohol of 1:5 mixes and form by weight ratio, and the molecular weight of polyvinyl alcohol is 150D.The negative electrode that makes in the present embodiment is further made tantalum electrolytic capacitor by the method for routine, and recording its ESR is 0.4 ~ 0.5 Ω.
Comparative example
To contain several in the manganese nitrate solution that is immersed in different specific weight as the tantalum piece of anode, and also be added with graphite in the manganese nitrate solution, the proportion of manganese nitrate solution is 1.10 ~ 1.90; And increase with the impregnation number of times; The proportion of manganese nitrate solution is ascending, and during each impregnation, manganese nitrate solution all decomposes down at 200 ℃ ~ 270 ℃ and generates manganese dioxide; It is outer that manganese dioxide and graphite mix the metal derby that is formed on anode, as negative electrode.The negative electrode that makes in this comparative example is further made tantalum electrolytic capacitor by the method for routine, and recording its ESR is 1.5 Ω.
The present invention also provides a kind of negative electrode of electrolytic capacitor, is made by the preparation method of above-mentioned any embodiment.
The present invention also provides a kind of electrolytic capacitor, comprises above-mentioned negative electrode.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, do not breaking away under the prerequisite of the present invention design, make some being equal to substitute or obvious modification, and performance or purposes are identical, all should be regarded as belonging to protection scope of the present invention.
Claims (10)
1. the cathode preparation method of an electrolytic capacitor contains the manganese dioxide solid in the negative electrode of said electrolytic capacitor, comprises the steps: the metal derby as anode is contained several in the manganese nitrate solution that is immersed in different specific weight; The proportion of said manganese nitrate solution is 1.10 ~ 1.90; And with the increase of impregnation number of times, the proportion of manganese nitrate solution is ascending, during each impregnation; Manganese nitrate all decomposes generation manganese dioxide down at 200 ℃ ~ 270 ℃; To form the metal derby that skin contains manganese dioxide, it is characterized in that, also comprise the steps:
Preparation manganese nitrate mixed solution step: in proportion is 1.10 ~ 1.30 manganese nitrate solution; Add the Powdered inserts of this manganese nitrate solution weight 30% ~ 70% and the graphite of this manganese nitrate solution weight 30% ~ 70%, said Powdered inserts is to be that the nanoscale carbon dust and the mixed with resin of 1:1 ~ 5 forms by weight ratio;
The impregnation decomposition step: the metal derby that said skin is contained manganese dioxide contains several in the manganese nitrate mixed solution that is immersed in above-mentioned preparation; Decompose generation manganese dioxide at 200 ~ 270 ℃ of following manganese nitrates; Said Powdered inserts and graphite are blended in the manganese dioxide, accomplish the manufacturing of said negative electrode.
2. the cathode preparation method of electrolytic capacitor as claimed in claim 1, it is characterized in that: the particle diameter of said Powdered inserts is 100 ~ 200nm.
3. the cathode preparation method of electrolytic capacitor as claimed in claim 1, it is characterized in that: the addition of said Powdered inserts is 60% ~ 70% of a manganese nitrate solution weight.
4. the cathode preparation method of electrolytic capacitor as claimed in claim 1, it is characterized in that: said resin is a polyvinyl alcohol, its molecular weight is 150 ~ 250D.
5. the cathode preparation method of electrolytic capacitor as claimed in claim 1, it is characterized in that: said electrolytic capacitor is tantalum electrolytic capacitor or niobium electrolytic capacitor.
6. inserts that is used for mixing electrolytic capacitor cathode is characterized in that: by weight ratio is that the nanoscale carbon dust and the mixed with resin of 1:1 ~ 5 forms.
7. inserts as claimed in claim 6 is characterized in that: said resin is a polyvinyl alcohol, and its molecular weight is 150 ~ 250D.
8. inserts as claimed in claim 6 is characterized in that: the particle diameter of said nanoscale carbon dust is 100 ~ 200nm.
9. the negative electrode of an electrolytic capacitor is characterized in that: made by any described preparation method of claim 1-5.
10. an electrolytic capacitor is characterized in that: comprise the described negative electrode of claim 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109300695A (en) * | 2018-11-06 | 2019-02-01 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | A kind of cathode and preparation method thereof of low ESR tantalum electrolytic capacitor |
| CN114974901A (en) * | 2022-06-07 | 2022-08-30 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Coating method for improving capacitance extraction rate of tantalum capacitor |
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| US4945452A (en) * | 1989-11-30 | 1990-07-31 | Avx Corporation | Tantalum capacitor and method of making same |
| EP0633583A1 (en) * | 1993-07-05 | 1995-01-11 | Nec Corporation | Low impedance solid electrolytic capacitor and method for fabricating the same |
| JPH11274009A (en) * | 1998-03-26 | 1999-10-08 | Hitachi Chem Co Ltd | Solid electrolytic capacitor and manufacture thereof |
| 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 |
| CN101404212A (en) * | 2008-11-13 | 2009-04-08 | 北京七一八友益电子有限责任公司 | Sheet type niobium oxide solid electrolyte capacitor and its manufacturing method |
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Patent Citations (5)
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| US4945452A (en) * | 1989-11-30 | 1990-07-31 | Avx Corporation | Tantalum capacitor and method of making same |
| EP0633583A1 (en) * | 1993-07-05 | 1995-01-11 | Nec Corporation | Low impedance solid electrolytic capacitor and method for fabricating the same |
| JPH11274009A (en) * | 1998-03-26 | 1999-10-08 | Hitachi Chem Co Ltd | Solid electrolytic capacitor and manufacture thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109300695A (en) * | 2018-11-06 | 2019-02-01 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | A kind of cathode and preparation method thereof of low ESR tantalum electrolytic capacitor |
| CN109300695B (en) * | 2018-11-06 | 2020-10-16 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Cathode of low ESR tantalum electrolytic capacitor and preparation method thereof |
| CN114974901A (en) * | 2022-06-07 | 2022-08-30 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Coating method for improving capacitance extraction rate of tantalum capacitor |
| CN114974901B (en) * | 2022-06-07 | 2023-05-23 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Coating method for improving capacitance extraction rate of tantalum capacitor |
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