CN103500657B - The method reducing tantalum capacitor volume - Google Patents
The method reducing tantalum capacitor volume Download PDFInfo
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- CN103500657B CN103500657B CN201310484449.5A CN201310484449A CN103500657B CN 103500657 B CN103500657 B CN 103500657B CN 201310484449 A CN201310484449 A CN 201310484449A CN 103500657 B CN103500657 B CN 103500657B
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Abstract
The invention discloses a kind of method reducing tantalum capacitor volume, it is desirable to provide a kind of volume reducing tantalum capacitor。Prepare dielectric oxide film including by electrochemical means on anode tantalum block surface: anode tantalum block is dipped in mass percentage concentration be 40～70%, temperature be in the aqueous slkali of 5～20 DEG C, in 20～140 minutes, 3.5～5 times of rated capacitor voltage are boosted to, constant voltage 10～30 minutes by the electric current density of 0.5～12A/g；Clean be dipped in after drying mass percentage concentration be 0.01～0.1%, temperature be, in the phosphoric acid solution of 85 ± 5 DEG C, rise to 1.5～3 times of rated capacitor voltage by the electric current density of 10～50mA/g by forming voltage, constant voltage 90～180 minutes；Clean and prepare cathode layer by normal technique after drying and be assembled into tantalum capacitor。By the tantalum capacitor that the present invention makes, its volume can reduce more than 25%。
Description
Technical field
The present invention relates to the manufacture method of a kind of electrolysis condenser, particularly relate to a kind of method reducing tantalum capacitor volume。
Background technology
It is known that tantalum capacitor mainly by tantalum powder after compressing through the anode tantalum block of vacuum-sintering, the Ta being coated on this anode tantalum block surface2O5Dielectric oxide film, it is coated on this Ta2O5The manganese dioxide deielectric-coating on dielectric oxide film surface and be encapsulated in the working electrolyte in metal shell and constitute。In order to reduce the volume of tantalum capacitor, the tantalum powder of Fabrication of High Specific Capacitance is generally adopted to make capacitor at present；However as the raising of tantalum powder specific volume, the particle diameter of tantalum powder is more and more less, and breakdown voltage also can decrease。For the tantalum capacitor of same size, when its rated voltage is identical with capability value, also limit the high specific capacitance of adopted tantalum powder, thus limiting the minimum volume of tantalum capacitor。In order to reduce the volume of tantalum capacitor further, many producers take to reduce and form voltage multiplying power, improve pressed density, cancel the measures such as strengthening layer；Although the volume of tantalum capacitor can be reduced to a certain extent, but add again control difficulty and the production cost of production process simultaneously。
At present, generally adopting in the phosphoric acid solution that anode tantalum block immerses concentration 0.01～1%, boost to the rated operational voltage of 3.5～5 times by the electric current density of 10～50mA/g, the constant voltage method of 1.5～3 hours prepares Ta on anode tantalum block surface2O5Dielectric oxide film forms capacitor anode。To Ta2O5Dielectric oxide film carries out 120～450V pressure test, retouches the position finding breakdown point less all at the superficies of tantalum anode block through Electronic Speculum, and any breakdown point does not occur in internal layer。If the Ta of the rated operational voltage that can bear 3.5～5 times quickly can be formed at the outer layer of tantalum anode block2O5Medium oxidizing rete, the internal layer at tantalum anode block reduces and forms voltage, thinning Ta2O5The thickness of dielectric oxide film, can improve capability value, thus reaching not only to ensure tantalum capacitor rated operational voltage and capability value, but also reducing the purpose of volume of tantalum capacitor。
Summary of the invention
For the drawbacks described above existed in prior art, it is desirable to provide a kind of method reducing tantalum capacitor volume, utilize capacitor prepared by the method not only can ensure tantalum capacitor rated operational voltage and capability value, but also the volume of tantalum capacitor can have been reduced。
To achieve these goals, the technical solution used in the present invention includes preparing dielectric oxide film by electrochemical mode on anode tantalum block surface, and concrete grammar is as follows:
1) described anode tantalum block is dipped in mass percentage concentration be 40～70%, temperature be, in the aqueous slkali of 5～20 DEG C, in 20～140 minutes, rise to rated capacitor voltage 3.5～5 times by forming voltage by the electric current density of 0.5～12A/g, constant voltage 10～30 minutes；Described aqueous slkali is formulated by Lithium hydrate or sodium hydroxide or potassium hydroxide and water；
2) surface preparation there is Ta2O5The anode tantalum block of dielectric oxide film is taken out, and cleans with the deionized waters of 85 ± 5 DEG C, dries；
3) anode tantalum block through drying is dipped in mass percentage concentration be 0.01～0.1%, temperature be, in the phosphoric acid solution of 85 ± 5 DEG C, rise to 1.5～3 times of rated capacitor voltage by the electric current density of 10～50mA/g by forming voltage, constant voltage 90～180 minutes；
4) anode tantalum block through second time electrochemical treatments is taken out, clean with the deionized waters of 85 ± 5 DEG C, dry。
In technique scheme, the technological parameter of each step is preferably: the aqueous slkali mass percentage concentration in step 1) is 45～65%, and boost current density is 1.1～10A/g, pressure rising time is 40～120 minutes, constant voltage time is 15～25 minutes；Phosphoric acid solution mass percentage concentration in step 3) is 0.03～0.07%, boost current density is 15～45mA/g, constant voltage 120～150 minutes。
In technique scheme, the technological parameter of each step is more preferably: the aqueous slkali mass percentage concentration in step 1) is 50～60%, and boost current density is 4～7A/g, pressure rising time is 60～100 minutes, constant voltage time is 20 minutes；Phosphoric acid solution mass percentage concentration in step 3) is 0.05%, boost current density is 20～40mA/g, constant voltage 130 minutes。
In technique scheme, the technological parameter of each step is further preferably: the aqueous slkali mass percentage concentration in step 1) is 55%, and boost current density is 5.5A/g, pressure rising time be 80 clocks, constant voltage time is 20 minutes；Phosphoric acid solution mass percentage concentration in step 3) is 0.05%, boost current density is 30mA/g, constant voltage 130 minutes。
Compared with the prior art, due to the fact that first with aqueous slkali for forming liquid, therefore, it is possible to quickly form the Ta of the rated operational voltage that can bear 3.5～5 times at anode tantalum block outer layer2O5Medium oxidizing rete；Then again with phosphoric acid solution for forming liquid and reducing formation voltage, Ta therefore it is thinned2O5The thickness of dielectric oxide film, improve capability value such that it is able to when ensureing tantalum capacitor rated operational voltage and capability value, reduce the volume of tantalum capacitor。
The following is two groups of data that the anode tantalum block of the three kinds of specifications (4000 μ FV/g, 50000 μ FV/g, 100000 μ FV/g) respectively prepared by the inventive method and traditional method is tested:
Table 1:4000 μ FV/g, 50000 μ FV/g, 100000 μ FV/g anode tantalum block performance parameters
It is seen from the above data that adopt the tantalum capacitor that the inventive method produces due to outer layer Ta2O5The breakdown voltage of dielectric oxide film does not change, and the leakage current value of tantalum capacitor does not increase；But owing to reducing internal layer Ta2O5The formation voltage of medium oxidizing rete and be thinned internal layer Ta2O5Dielectric oxide film, so that the volume-diminished more than 25% of tantalum capacitor。
Detailed description of the invention
Separately below to prepare specification be 4000 μ FV/g, the invention will be further described for specific embodiment for the anode tantalum block of 50000 μ FV/g, 100000 μ FV/g:
Embodiment 1, the tantalum capacitor that tantalum powder manufacturing specification is 50V10 μ F with specific volume is 4000 μ FV/g:
1) tantalum powder makes 5 × 3.8 × 2.6 according to a conventional method, pressed density is 7.5g/cm3Tantalum briquet, this tantalum briquet vacuum-sintering according to a conventional method is become anode tantalum block；
2) described anode tantalum block is dipped in mass percentage concentration be 40%, temperature be in the aqueous slkali of 20 DEG C, voltage will be formed rise to 3.5 times (175V) of rated capacitor voltage by the electric current density of 0.5A/g in 140 minutes, constant voltage 30 minutes；Described aqueous slkali is sodium hydroxide solution；
3) surface preparation there is Ta2O5The anode tantalum block of dielectric oxide film is taken out, and cleans with the deionized water of 85 ± 5 DEG C, is then fed in the baking oven of 150 ± 5 DEG C and dry；
4) anode tantalum block through drying is dipped in mass percentage concentration be 0.01%, temperature be in the phosphoric acid solution of 85 ± 5 DEG C, voltage will be formed rise to 1.5 times (75V) of rated capacitor voltage by the electric current density of 50mA/g, constant voltage 180 minutes；
5) anode tantalum block through second time electrochemical treatments is taken out, clean with the deionized water of 85 ± 5 DEG C, be then fed in the baking oven of 150 ± 5 DEG C and dry；
6) preparation is had internal layer and outer layer Ta2O5The anode tantalum block of dielectric oxide film is prepared cathode layer by normal technique and is assembled into tantalum capacitor。
Embodiment 2, the tantalum capacitor that tantalum powder manufacturing specification is 50V10 μ F with specific volume is 4000 μ FV/g:
Each step is with embodiment 1；Wherein, step 2) in the concentration of sodium hydroxide solution be 70%, temperature be 5 DEG C, electric current density is 12A/g, pressure rising time is 20 minutes, forms 5 times (250V) that voltage is rated capacitor voltage, constant voltage time is 10 minutes；In step 4), the concentration of phosphoric acid solution is 0.1%, and electric current density is 10mA/g, forms 3 times (150V) that voltage is rated capacitor voltage, constant voltage 90 minutes。
Embodiment 3, the tantalum capacitor that tantalum powder manufacturing specification is 16V33 μ F with specific volume is 50000 μ FV/g:
Each step is with embodiment 1；Wherein, step 2) in the aqueous slkali lithium hydroxide solution that to be concentration be 45%, temperature is 8 DEG C, boost current density is 10A/g, pressure rising time is 40 minutes, forms 4 times (56V) that voltage is rated capacitor voltage, constant voltage time is 25 minutes；Phosphoric acid solution concentration in step 4) is 0.03%, boost current density is 45mA/g, form voltage is 2 times (320V) of rated capacitor voltage, constant voltage 120 minutes。
Embodiment 4, the tantalum capacitor that tantalum powder manufacturing specification is 16V33 μ F with specific volume is 50000 μ FV/g:
Each step is with embodiment 3；Wherein, step 2) in lithium hydroxide solution concentration be 65%, temperature be 13 DEG C, boost current density is 1.1A/g, pressure rising time is 120 minutes, forms 4.5 times (72V) that voltage is rated capacitor voltage, constant voltage time is 15 minutes；Phosphoric acid solution concentration in step 4) is 0.07%, boost current density is 15mA/g, form 2.5 times (40V) that voltage is rated capacitor voltage, constant voltage 150 minutes。
Embodiment 5, the tantalum capacitor that tantalum powder manufacturing specification is 6V100 μ F with specific volume is 100000 μ FV/g:
Each step is with embodiment 1；Wherein, step 2) in the aqueous slkali potassium hydroxide solution that to be concentration be 50%, temperature is 10 DEG C, boost current density is 7A/g, pressure rising time is 60 minutes, forms 4.2 times (25V) that voltage is rated capacitor voltage, constant voltage time is 20 minutes；Phosphoric acid solution concentration in step 4) is 0.05%, boost current density is 20mA/g, form 1.8 times (11V) that voltage is rated capacitor voltage, constant voltage 130 minutes。
Embodiment 6, the tantalum capacitor that tantalum powder manufacturing specification is 6V100 μ F with specific volume is 100000 μ FV/g:
Each step is with embodiment 5；Wherein, step 2) in the potassium hydroxide potassium hydroxide solution that to be concentration be 60%, temperature is 18 DEG C, boost current density is 4A/g, pressure rising time be 100 minutes, form 4.8 times (25V) that voltage is rated capacitor voltage；Boost current density in step 4) is 40mA/g。
Embodiment 7, the tantalum capacitor that tantalum powder manufacturing specification is 6V100 μ F with specific volume is 100000 μ FV/g:
Each step is with embodiment 6；Wherein, step 2) in potassium hydroxide be concentration be 55%, boost current density is 5.5A/g, pressure rising time be 80 minutes, form 3.8 times (23V) that voltage is rated capacitor voltage；Boost current density in step 4) is 30mA/g。
Claims (4)
1. the method reducing tantalum capacitor volume, prepares dielectric oxide film including by electrochemical means on anode tantalum block surface, it is characterised in that concrete grammar is as follows:
1) described anode tantalum block is dipped in mass percentage concentration be 40～70%, temperature be, in the aqueous slkali of 5～20 DEG C, in 20～140 minutes, rise to rated capacitor voltage 3.5～5 times by forming voltage by the electric current density of 0.5～12A/g, constant voltage 10～30 minutes；Described aqueous slkali is formulated by Lithium hydrate or sodium hydroxide or potassium hydroxide and water；
2) surface preparation there is Ta2O5The anode tantalum block of dielectric oxide film is taken out, and cleans with the deionized waters of 85 ± 5 DEG C, dries；
3) anode tantalum block through drying is dipped in mass percentage concentration be 0.01～0.1%, temperature be, in the phosphoric acid solution of 85 ± 5 DEG C, rise to 1.5～3 times of rated capacitor voltage by the electric current density of 10～50mA/g by forming voltage, constant voltage 90～180 minutes；
4) anode tantalum block through second time electrochemical treatments is taken out, clean with the deionized waters of 85 ± 5 DEG C, dry。
2. the method reducing tantalum capacitor volume according to claim 1, it is characterized in that: the aqueous slkali mass percentage concentration in step 1) is 45～65%, boost current density is 1.1～10A/g, pressure rising time is 40～120 minutes, constant voltage time is 15～25 minutes；Phosphoric acid solution mass percentage concentration in step 3) is 0.03～0.07%, boost current density is 15～45mA/g, constant voltage 120～150 minutes。
3. the method reducing tantalum capacitor volume according to claim 1, it is characterised in that: the aqueous slkali mass percentage concentration in step 1) is 50～60%, and boost current density is 4～7A/g, pressure rising time is 60～100 minutes, constant voltage time is 20 minutes；Phosphoric acid solution mass percentage concentration in step 3) is 0.05%, boost current density is 20～40mA/g, constant voltage 130 minutes。
4. the method reducing tantalum capacitor volume according to claim 1, it is characterised in that: the aqueous slkali mass percentage concentration in step 1) is 55%, and boost current density is 5.5A/g, pressure rising time be 80 clocks, constant voltage time is 20 minutes；Phosphoric acid solution mass percentage concentration in step 3) is 0.05%, boost current density is 30mA/g, constant voltage 130 minutes。
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| CN109285703A (en) * | 2018-10-26 | 2019-01-29 | 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) | The method for improving the method for tantalum capacitor voltage endurance capability and making tantalum capacitor |
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| CN1374414A (en) * | 2001-03-13 | 2002-10-16 | 上海南汇新海印染机械配件厂 | Formation of chemical protecting film for tantalum device |
| CN101354965A (en) * | 2008-09-16 | 2009-01-28 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing high-temperature electrolytic capacitor anodized film |
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| JPH0661104A (en) * | 1992-07-27 | 1994-03-04 | Nippon Steel Corp | Treatment method of electrode material for capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374414A (en) * | 2001-03-13 | 2002-10-16 | 上海南汇新海印染机械配件厂 | Formation of chemical protecting film for tantalum device |
| CN101354965A (en) * | 2008-09-16 | 2009-01-28 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing high-temperature electrolytic capacitor anodized film |
Non-Patent Citations (1)
| Title |
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| 镍在碱溶液中阳极氧化膜的拉曼光谱;翟大程;《复旦学报》;19941231;第33卷(第6期);全文 * |
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