CN102800484A - Method for making anode pellet of niobium capacitor - Google Patents
Method for making anode pellet of niobium capacitor Download PDFInfo
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- CN102800484A CN102800484A CN2012102929352A CN201210292935A CN102800484A CN 102800484 A CN102800484 A CN 102800484A CN 2012102929352 A CN2012102929352 A CN 2012102929352A CN 201210292935 A CN201210292935 A CN 201210292935A CN 102800484 A CN102800484 A CN 102800484A
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Abstract
The invention relates to a method for making an anode pellet of a niobium capacitor, and belongs to the technical field of electronic element manufacturing. The steps are as follows: mixing niobium oxide powder with the adhesive of ethyl benzenecarboxylate and the adhesive of polyvinyl accohol, sieving the mixed powder with a screen of 0.2mm to 1.0mm, naturally drying out the mixed powder, and then pressing the mixed powder to produce the required anode pellet of the niobium capacitor according to the prior art. According to the invention, the niobium oxide powder is mixed with two adhesives for two times and the mixed powder is sieved for 100%, so that the granules of the mixed powder are basically of the same size, and the anode block has uniform compacted density but no crack, fracture, corner missing, and other problems. Therefore, the equivalent series resistance (ESR) of the niobium solid electrolytic condenser is low and the value of the leaking current is small.
Description
Technical field
The present invention relates to solve that niobium capacitor anode pellet density unevenness is even, the technology of the mobile difference of niobium monoxide powder, specifically a kind of method of making niobium capacitor anode pellet.
Background technology: in the development process of niobium capacitor, niobium suboxide (NbO
x, wherein X is 0.5~1.7) high conductivity, non-flammability, ceramic characteristics cause concern in the industry, the exploitation of using niobium oxide at a low price to make the electrolytic capacitor manufacturing technology of capacitor anode pellet has replaced the development of niobium capacitor gradually.The electrolytic capacitor made from the low valence niobium oxide powder has the advantage identical with tantalum capacitor, also has little, the burning feature not of the working voltage range of decrease, and its technology, technological process are similar with tantalum capacitor.
The researcher of countries such as Japan, the U.S., Germany has carried out deep research to the technology of making solid electrolytic capacitor with the low valence niobium oxide powder, as all relate to the manufacturing approach of niobium electrolytic capacitor in patents such as CN200980129545.X, CN02807111.5, CN200710140391.7, CN01818013.2, CN200980151003.2.Main method is with niobium powder or low valence niobium oxide powder extrusion modling anode pellet; Then under high vacuum through 1000 ℃~1500 ℃ calcining; Generating the niobium pentaoxide deielectric-coating through electrochemical oxidation on anode pellet surface; On deielectric-coating, make manganese dioxide solid state cathode layer or polymerization conductive solid polymer cathode layer again, be encapsulated at last in metal shell or the epoxy resin material through thermal decomposition.But because deielectric-coating not exclusively is the niobium pentaoxide composition, more or less contain the part low valence niobium oxide, and NbO is a kind of crisp oxide ceramics that is prone to, micro-crack can occurs during the anode moulding, even can not make it to repair fully through calcining.In above-mentioned patent document,, reduce problems such as the breaking of anode pellet, fracture, unfilled corner and propose solution for the consistent in density property of the flowability that how to improve the niobium oxide powder, anode pellet.
For the widely used columned or traditional rectangular chip capacitor of existing market; The making of its anode pellet is with the mode compression moulding of niobium oxide powder through extruding; Though in Deutsche Bundespatent CN200980151003.2 " capacitor anode "; Mentioned the manufacture method of anode pellet: (1) niobium oxide powder is suspended in the inert fluid, fills or extrudes in the mould of boat shape, tubbiness or cochlear; (2) the niobium oxide powder is configured to paste with organic bond, with mode anode bodies on tantalum or niobate substrate such as screen printing, mould printing, ink jet printings.These two kinds of anode pellet moulding processs are for the making of the chip capacitor anode pellet of columned or rectangle and inapplicable.
Researcher of the present invention also is applied to the adhesive that uses in the tantalum powder treatment process such as stearic acid, camphor, polyvinyl alcohol etc. in the processing of niobium oxide powder; But change the proportioning of adhesive and powder in any case, only solved that powder is mobile, in the problems such as the breaking of the consistent in density property of anode pellet, anode pellet, fracture, unfilled corner one or several.Through experimental study, researcher of the present invention finds, the niobium oxide powder is carried out different adhesive treatment, can solve the problems referred to above that exist in the moulding of anode pellet effectively.
Summary of the invention: to the defective that exists in the prior art; The object of the invention aims to provide a kind of manufacturing technology of making the anode pellet of Niobiuim solid electrolytic capacitor with the niobium monoxide powder system; Be treatment technology to the niobium oxide powder before the moulding of anode pellet, the process that concrete grammar is to use two kinds of different adhesives that the niobium oxide powder is handled.
To achieve these goals; A kind of method of making niobium capacitor anode pellet of the present invention; It is characterized in that following these steps to successively processing: (1) is put into water temperature with container is in 40 ℃~90 ℃ the water-bath; The niobium oxide powder that takes by weighing 1 part of adhesive A and 1~5 part of (weight ratio) solvent joins in the container, and ceaselessly stirring makes adhesive fully mix with the niobium oxide powder;
(2) 0.2~1 part of adhesive B with respect to the niobium oxide grain weight is joined in the container, stirring makes adhesive fully mix with the niobium oxide powder;
(3) take out mixed niobium oxide powder, make it mesh screen through 0.2mm~1.0mm.Can not pulverize the back after mesh screen through the powder ball of mesh screen, all pass through up to all powder balls;
(4) will be tiled in through the powder of mesh screen in the enamel tray, collect in the reservoir bottle subsequent use behind the 1h~4h that dries in the air naturally;
(5) according to existing technology powder is pressed into required niobium capacitor anode pellet, and accomplishes the dielectric oxide film preparation, catholyte coats, and graphite silver is starched the auxiliary layer processing of drawing.
Said adhesive A: be that 1 part of adhesive is dissolved in 5~20 parts of weight ratio solvents; Wherein adhesive is a kind of in benzoic acid, Sodium Benzoate, phenylacetic acid, sodium phenylacetate, methyl benzoate, the ethyl benzoate, and solvent is a kind of in ethanol, ether, carrene, chloroform, acetone, terpinol, propane diols, n-butanol, the butanediol;
Said adhesive B: be that 1 part of adhesive is dissolved in 1~5 part of weight ratio solvent; A kind of in adhesive camphor, stearic acid, polyvinyl alcohol, acrylic acid ester, cellulose, the polysaccharide wherein, solvent is a kind of in ethanol, ether, carrene, chloroform, acetone, terpinol, propane diols, n-butanol, the butanediol.
The preferred ethyl benzoate of the adhesive of adhesive A, solvent are terpinol, and the weight ratio of adhesive and solvent is 1:8;
The adhesive preferably polyethylene alcohol of adhesive B, solvent is a terpinol, the weight ratio of adhesive and solvent is 1:3.
The order that adhesive A and adhesive B use can be exchanged, and promptly in step (1), uses adhesive B earlier, in step (2), uses adhesive A again.
The anode pellet compacted density uniformity that adopts this method to make, problems such as anode pellet crack-free, fracture, unfilled corner, the equivalent series resistance of the niobium oxide solid electrolyte capacitor of being produced (ESR) value and leakage current value are little.
Mix powder craft relatively with existing tantalum capacitor; The present invention has adopted two kinds of treatment process that adhesive mixes powder for twice, adopts water-bath heating, mixed powder 100% to sieve when mixing powder; Make additive be coated on niobium oxide powder particles surface equably; Improved the mobile performance of niobium oxide powder, guaranteed that rupturing does not appear in the anode block of moulding, break, unfilled corner; 100% processing of sieving makes the niobium oxide powder particles size basically identical that mixes behind the powder, has guaranteed that the anode block compacted density of moulding is even.
Embodiment below in conjunction with concrete is further described the present invention:
Embodiment 1
The proportioning of adhesive A is: the benzoic acid of 1 part of weight is dissolved in the carrene of 10 parts of weight.
The proportioning of adhesive B is: the camphor of 1 part of weight is dissolved in the carrene of 3.5 parts of weight.
The niobium oxide powder that takes by weighing the 4Kg specific volume and be 80000 μ FV/g is poured into and is positioned over temperature is that the adhesive A that takes by weighing 1Kg is poured in the container, stirs 10min in 60 ℃ the container of water-bath; The adhesive B that takes by weighing 1.2Kg again pours in the container, stirs 15min.After stir finishing, sieve with the mesh screen of 0.6mm, the niobium oxide powder is tiled in cool naturally 1h in the enamel tray, the niobium oxide powder that will dry is packed into subsequent use in the bottle.
Embodiment 2:
The proportioning of adhesive A is: the ethyl benzoate of 1 part of weight is dissolved in the terpinol of 8 parts of weight.
The proportioning of adhesive B is: the polyvinyl alcohol of 1 part of weight is dissolved in the terpinol of 3 parts of weight.
The niobium oxide powder that takes by weighing the 5Kg specific volume and be 120000 μ FV/g is poured into and is positioned over temperature is that the adhesive B that takes by weighing 1.5Kg pours in the container, stirs 20min in 60 ℃ the container of water-bath; The adhesive A that takes by weighing 1.8Kg is again poured in the container, stirs 15min.After stir finishing, sieve with the mesh screen of 0.6mm, the niobium oxide powder is tiled in cool naturally 2h in the enamel tray, the niobium oxide powder that will dry is packed into subsequent use in the bottle.
Press the niobium oxide solid electrolytic condenser of existing explained hereafter 4V330 μ F and two specifications of 4V470 μ F respectively with above-mentioned tantalum powder; Wherein the anode block of 4V330 μ F use specific volume is the powder moulding of 80000 μ FV/g, and it is the powder moulding of 120000 μ FV/g that the anode block of 4V470 μ F uses specific volume.The capacitance of two products, loss angle tangent, leakage current, ESR parameter testing value are seen table 1 and table 2 respectively, and see table 3 and table 4 (the niobium oxide powder of two products uses, product design with and subsequent technology all identical) by the 4V330 μ F of existing explained hereafter and the electric parameters testing value of 4V470 μ F two products.
The contrast of product electrical quantity can be found out from table 1~4; Leakage current value, equivalent series resistance (ESR) value that adopts the niobium oxide solid electrolyte capacitor that the present invention produces be have now the explained hereafter product 50% in, the loss angle tangent parameter also has certain reduction.
Claims (4)
1. method of making niobium capacitor anode pellet; It is characterized in that following these steps to successively processing: (1) is put into water temperature with container is in 40 ℃~90 ℃ the water-bath; The niobium oxide powder that takes by weighing 1 part of adhesive A and 1~5 part of weight ratio solvent joins in the container, and ceaselessly stirring makes adhesive fully mix with the niobium oxide powder;
(2) 0.2~1 part of adhesive B with respect to the niobium oxide grain weight is joined in the container, stirring makes adhesive fully mix with the niobium oxide powder;
(3) take out mixed niobium oxide powder, make it mesh screen, can not pulverize the back after mesh screen, all pass through up to all powder balls through the powder ball of mesh screen through 0.2mm~1.0mm;
(4) will be tiled in through the powder of mesh screen in the enamel tray, collect in the reservoir bottle subsequent use behind the 1h~4h that dries in the air naturally;
(5) according to existing technology powder is pressed into required niobium capacitor anode pellet.
2. a kind of method of making niobium capacitor anode pellet according to claim 1; It is characterized in that said adhesive A: 1 part of adhesive is dissolved in 5~20 parts of weight ratio solvents; Wherein adhesive is a kind of in benzoic acid, Sodium Benzoate, phenylacetic acid, sodium phenylacetate, methyl benzoate, the ethyl benzoate, and solvent is a kind of in ethanol, ether, carrene, chloroform, acetone, terpinol, propane diols, n-butanol, the butanediol;
Said adhesive B: 1 part of adhesive is dissolved in 1~5 part of weight ratio solvent; A kind of in adhesive camphor, stearic acid, polyvinyl alcohol, acrylic acid ester, cellulose, the polysaccharide wherein, solvent is a kind of in ethanol, ether, carrene, chloroform, acetone, terpinol, propane diols, n-butanol, the butanediol.
3. a kind of method of making niobium capacitor anode pellet according to claim 2, the adhesive that it is characterized in that adhesive A is an ethyl benzoate, and solvent is a terpinol, and the weight ratio of adhesive and solvent is 1:8;
The adhesive of adhesive B is a polyvinyl alcohol, and solvent is a terpinol, and the weight ratio of adhesive and solvent is 1:3.
4. a kind of method of making niobium capacitor anode pellet according to claim 1 is characterized in that the order of adhesive A and adhesive B use can be exchanged, and promptly in step (1), uses adhesive B earlier, in step (2), uses adhesive A again.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103065797A (en) * | 2013-01-15 | 2013-04-24 | 中国振华(集团)新云电子元器件有限责任公司 | Powder mixing craft of niobium oxide capacitor |
CN105428071A (en) * | 2016-01-12 | 2016-03-23 | 深圳顺络电子股份有限公司 | Manufacturing method of anode |
CN106128763A (en) * | 2016-06-14 | 2016-11-16 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of Large Copacity novel high-energy solid electrolyte niobium capacitor |
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CN1243464A (en) * | 1997-01-13 | 2000-02-02 | Avx有限公司 | Binder removal method |
CN1427996A (en) * | 2000-03-23 | 2003-07-02 | 卡伯特公司 | Oxygen reduced niobium oxides |
CN1471717A (en) * | 2000-10-26 | 2004-01-28 | �Ѻ͵繤��ʽ���� | Powder for capacitor, sintered body and capacitor using the sintered body |
JP2004335630A (en) * | 2003-05-06 | 2004-11-25 | Nichicon Corp | Solid electrolytic capacitor anode and manufacturing method thereof |
CN1813323A (en) * | 2003-04-28 | 2006-08-02 | 昭和电工株式会社 | Valve acting metal sintered body, production method therefor and solid electrolytic capacitor |
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2012
- 2012-08-17 CN CN201210292935.2A patent/CN102800484B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1243464A (en) * | 1997-01-13 | 2000-02-02 | Avx有限公司 | Binder removal method |
CN1427996A (en) * | 2000-03-23 | 2003-07-02 | 卡伯特公司 | Oxygen reduced niobium oxides |
CN1471717A (en) * | 2000-10-26 | 2004-01-28 | �Ѻ͵繤��ʽ���� | Powder for capacitor, sintered body and capacitor using the sintered body |
CN1813323A (en) * | 2003-04-28 | 2006-08-02 | 昭和电工株式会社 | Valve acting metal sintered body, production method therefor and solid electrolytic capacitor |
JP2004335630A (en) * | 2003-05-06 | 2004-11-25 | Nichicon Corp | Solid electrolytic capacitor anode and manufacturing method thereof |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103065797A (en) * | 2013-01-15 | 2013-04-24 | 中国振华(集团)新云电子元器件有限责任公司 | Powder mixing craft of niobium oxide capacitor |
CN105428071A (en) * | 2016-01-12 | 2016-03-23 | 深圳顺络电子股份有限公司 | Manufacturing method of anode |
CN105428071B (en) * | 2016-01-12 | 2019-01-18 | 深圳顺络电子股份有限公司 | A kind of manufacturing method of anode |
CN106128763A (en) * | 2016-06-14 | 2016-11-16 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of Large Copacity novel high-energy solid electrolyte niobium capacitor |
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