CN102800484B - A kind of method making anode pellet of niobium capacitor - Google Patents
A kind of method making anode pellet of niobium capacitor Download PDFInfo
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- CN102800484B CN102800484B CN201210292935.2A CN201210292935A CN102800484B CN 102800484 B CN102800484 B CN 102800484B CN 201210292935 A CN201210292935 A CN 201210292935A CN 102800484 B CN102800484 B CN 102800484B
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Abstract
A kind of method making anode pellet of niobium capacitor of the present invention, belong to fabrication of electronic components technical field, it is that niobium oxide powder is mixed with binding agent ethyl benzoate and adhesive polyethylene alcohol respectively, and by the mesh screen of 0.2mm～1.0mm, the anode pellet of niobium capacitor needed for powder pressing being become by existing technique after naturally drying.The present invention adopts twice binding agent to mix powder for twice, and mixed powder body 100% sieves, and makes mixed powder particles size basically identical, anode block compacted density is uniform, the problems such as crack-free, fracture, unfilled corner, thus make the equivalent series resistance ESR of Niobiuim solid electrolytic capacitor little, leakage current value is little.
Description
Technical field
The present invention relates to the Technology solving anode pellet of niobium capacitor Density inhomogeneity, niobium monoxide powder poor fluidity, a kind of specifically method making anode pellet of niobium capacitor.
Background technology: in the development process of niobium capacitor, niobium suboxide (NbOx, wherein X is 0.5～1.7) high conductivity, non-flammability, ceramic characteristics cause concern in the industry, use the exploitation of electrolysis condenser manufacturing technology that niobium suboxide makes capacitor anode pellet to instead of the development of niobium capacitor gradually.The electrolysis condenser made of low valence niobium oxide powder has the advantage identical with tantalum capacitor, also has that the use voltage range of decrease is little, not burning feature, and its Technology, technological process are similar to tantalum capacitor.
The technology making solid electrolytic capacitor of low valence niobium oxide powder is conducted in-depth research by the research worker of the country such as Japan, the U.S., Germany, as all referred to the manufacture method of niobium electrolytic capacitor in patents such as CN200980129545.X, CN02807111.5, CN200710140391.7, CN01818013.2, CN200980151003.2.Main method is by niobium powder or the extruded anode pellet of low valence niobium oxide powder, then under a high vacuum through the calcining of 1000 DEG C～1500 DEG C, by electrochemical oxidation at anode pellet Surface Creation niobium pentaoxide deielectric-coating, again by thermally decomposing prepared manganese dioxide solid state cathode layer or polymeric conductive polymeric solid cathode layer on deielectric-coating, finally it is encapsulated in metal shell or epoxy resin material.But it is not exclusively niobium pentaoxide composition due to deielectric-coating, more or less contains part low valence niobium oxide, and NbO is a kind of brittle oxide ceramics, there will be micro-crack during anode molding, can not so as to repair completely even across calcining.In above-mentioned patent document, for how improving the density CONSENSUS of the mobility of niobium oxide powder, anode pellet, reducing the breaking of anode pellet, rupture, the problem proposition solution such as unfilled corner.
For the widely used columned or traditional rectangle chip capacitor of existing market, the making of its anode pellet is compressing by the mode extruded with niobium oxide powder, although in Deutsche Bundespatent CN200980151003.2 " capacitor anode ", refer to the manufacture method of anode pellet: (1) niobium oxide powder is suspended in inert fluid, fill or extrude in the mould of boat shape, tubbiness or cochlear；(2) niobium oxide powder is configured to paste together with organic bond, in modes such as screen printing, mould printing, ink jet printings at tantalum or niobate substrate Shangyang polar body.Both anode pellet moulding processs, for the making of chip capacitor anode pellet of columned or rectangle inapplicable.
Tantalum powder is also processed the binding agent such as stearic acid, Camphora, polyvinyl alcohol etc. that use in technique and is applied in the process of niobium oxide powder by research worker of the present invention, but change the proportioning of binding agent and powder in any case, solve only powder mobility, the density CONSENSUS of anode pellet, the breaking of anode pellet, rupture, in the problem such as unfilled corner one or several.By experimental study, the present invention, it was discovered by researchers that niobium oxide powder is carried out different adhesive treatment, can efficiently solve the problems referred to above existed in anode pellet molding.
Summary of the invention: for the defect existed in prior art, the object of the invention aims to provide the manufacturing technology that a kind of niobium monoxide powder system makes the anode pellet of Niobiuim solid electrolytic capacitor, be for anode pellet molding before the treatment technology of niobium oxide powder body, concrete grammar is the process using binding agent two kinds different that niobium oxide powder is processed.
To achieve these goals, a kind of method making anode pellet of niobium capacitor of the present invention, it is characterized in that following these steps to processing successively: container is put in the water-bath that water temperature is 40 DEG C～90 DEG C by (1), the niobium oxide powder weighing 1 part of adhesive A and 1～5 part of (weight ratio) solvent joins in container, and is continuously agitated and makes binding agent and niobium oxide powder be sufficiently mixed；
(2) joining in container by 0.2～1 part relative to the binding agent B of niobium oxide grain weight, stirring makes binding agent and niobium oxide powder be sufficiently mixed；
(3) take out mixed niobium oxide powder, be run through the mesh screen of 0.2mm～1.0mm.By the powder ball of mesh screen, after mesh screen after pulverizing, all can not pass through until all powder balls；
(4) will be laid in enamel tray by the powder of mesh screen, be collected in reservoir bottle after the 1h～4h that naturally dries in the air standby；
(5) anode pellet of niobium capacitor needed for powder pressing being become according to existing technique, and complete medium oxidizing film preparation, catholyte is coated with, and graphite silver slurry auxiliary is drawn layer and processed.
Described adhesive A: be that 1 part of binding agent is dissolved in 5～20 parts of weight ratio solvents, wherein binding agent is the one in benzoic acid, sodium benzoate, phenylacetic acid, sodium phenylacetate, essence of Niobe, ethyl benzoate, and solvent is the one in ethanol, ether, dichloromethane, chloroform, acetone, terpineol, propylene glycol, n-butyl alcohol, butanediol；
Described binding agent B: be that 1 part of binding agent is dissolved in 1～5 part of weight ratio solvent, wherein binding agent Camphora, stearic acid, polyvinyl alcohol, acrylate, cellulose, one in polysaccharide, solvent is the one in ethanol, ether, dichloromethane, chloroform, acetone, terpineol, propylene glycol, n-butyl alcohol, butanediol.
The preferred ethyl benzoate of binding agent of adhesive A, solvent is the weight ratio of terpineol, binding agent and solvent is 1:8；
The binding agent preferably polyethylene alcohol of binding agent B, solvent is the weight ratio of terpineol, binding agent and solvent is 1:3.
The order that adhesive A and binding agent B use can be exchanged, and namely first uses binding agent B in step (1), then uses adhesive A in step (2).
Adopting the anode pellet compacted density uniformity that this method manufactures, the problem such as anode pellet crack-free, fracture, unfilled corner, equivalent series resistance (ESR) value of the niobium oxide solid electrolyte capacitor produced and leakage current value are little.
Compare with existing tantalum capacitor blending processes of powders, present invention employs the process technique adopting heating in water bath, mixed powder body 100% to sieve when two kinds of binding agents mix powder, mixed powder for twice, additive is made to be uniformly coated on niobium oxide powder particles surface, improve the mobile performance of niobium oxide powder, it is ensured that the anode block of molding occurs without fracture, breaks, unfilled corner；100% sieves process, makes the niobium oxide powder particles size after mixed powder basically identical, it is ensured that the anode block compacted density of molding is uniform.
Below in conjunction with specific embodiment, the present invention is further illustrated:
Embodiment 1
The proportioning of adhesive A is: the benzoic acid of 1 part of weight is dissolved in the dichloromethane of 10 parts of weight.
The proportioning of binding agent B is: the Camphora of 1 part of weight is dissolved in the dichloromethane of 3.5 parts of weight.
Weighing the niobium oxide powder that 4Kg specific volume is 80000 μ F V/g to pour in the container being positioned over the water-bath that temperature is 60 DEG C, the adhesive A weighing 1Kg is poured in container, stirs 10min；The binding agent B weighing 1.2Kg again pours in container, stirs 15min.Stirring is sieved with the mesh screen of 0.6mm after terminating, and is laid in enamel tray by niobium oxide powder naturally cool 1h, by standby in the niobium oxide powder loading bottle that dries.
Embodiment 2:
The proportioning of adhesive A is: the ethyl benzoate of 1 part of weight is dissolved in the terpineol of 8 parts of weight.
The proportioning of binding agent B is: the polyvinyl alcohol of 1 part of weight is dissolved in the terpineol of 3 parts of weight.
Weighing the niobium oxide powder that 5Kg specific volume is 120000 μ F V/g to pour in the container being positioned over the water-bath that temperature is 60 DEG C, the binding agent B weighing 1.5Kg pours in container, stirs 20min；The adhesive A weighing 1.8Kg again is poured in container, stirs 15min.Stirring is sieved with the mesh screen of 0.6mm after terminating, and is laid in enamel tray by niobium oxide powder naturally cool 2h, by standby in the niobium oxide powder loading bottle that dries.
With above-mentioned tantalum powder respectively by the niobium oxide solid electrochemical capacitor of existing explained hereafter 4V330 μ F and 4V,470 two specifications of μ F, wherein the anode block specific volume of 4V330 μ F is the powder molding of 80000 μ F V/g, and the anode block specific volume of 4V470 μ F is the powder molding of 120000 μ F V/g.The capacitance of two specification products, loss angle tangent, leakage current, ESR parameter testing value respectively in Table 1 and table 2, and the niobium oxide powder used in Table 3 and two specification products of table 4(by the electric parameters testing value of 4V330 μ F and 4V470 μ F two specification product of existing explained hereafter, product design with and subsequent technique all identical).
Product Contrast of Electrical Parameter from table 1～4 it can be seen that adopt the present invention produce the leakage current value of niobium oxide solid electrolyte capacitor, equivalent series resistance (ESR) value be existing explained hereafter product 50% within, loss angle tangent parameter also has certain reduction.
Claims (1)
1. the method making anode pellet of niobium capacitor, it is characterized in that following these steps to processing successively: container is put in the water-bath that water temperature is 40 DEG C～90 DEG C by (1), weigh adhesive A and niobium oxide powder joins in container, and ceaselessly stirring makes adhesive A and niobium oxide powder be sufficiently mixed, the weight ratio of niobium oxide powder and adhesive A is 1-5:1, the binding agent of adhesive A is ethyl benzoate, and solvent is the weight ratio of terpineol, binding agent and solvent is 1:8；
(2) joining in container by binding agent B, stirring makes binding agent B and niobium oxide powder be sufficiently mixed, and the weight ratio of niobium oxide powder and binding agent B is 1-5:1, and the binding agent of binding agent B is polyvinyl alcohol, and solvent is the weight ratio of terpineol, binding agent and solvent is 1:3；
(3) take out mixed niobium oxide powder, be run through the mesh screen of 0.2mm～1.0mm, it is impossible to by the powder ball of mesh screen, after mesh screen after pulverizing, until all powder balls all pass through；
(4) will be laid in enamel tray by the powder of mesh screen, be collected in reservoir bottle after the 1h～4h that naturally dries in the air standby；
(5) anode pellet of niobium capacitor needed for powder pressing being become according to existing technique.
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| CN201210292935.2A CN102800484B (en) | 2012-08-17 | 2012-08-17 | A kind of method making anode pellet of niobium capacitor |
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| CN201210292935.2A CN102800484B (en) | 2012-08-17 | 2012-08-17 | A kind of method making anode pellet of niobium capacitor |
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| CN102800484B true CN102800484B (en) | 2016-07-20 |
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| 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 |
| 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 |
Citations (4)
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4307146B2 (en) * | 2003-05-06 | 2009-08-05 | ニチコン株式会社 | Method for producing solid electrolytic capacitor anode body |
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Patent Citations (4)
| 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 |
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