CN103295787B - The processing method of electrolytic capacitor manufacture process medium oxide-film - Google Patents
The processing method of electrolytic capacitor manufacture process medium oxide-film Download PDFInfo
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Abstract
The present invention relates to the processing method of electrolytic capacitor manufacture process medium oxide-film, in particular to traditional with valve metals such as tantalum, niobium, titanium, aluminium for anode, with conductive polymer polymer for catholyte manufactures the pretreated method to dielectric oxide film increased in electrolytic capacitor process, it comprises the following steps: valve metal powder is become the leaded anodic porous sintered body of band through mold pressing and vacuum-sintering; Electrochemical method is adopted to form dielectric oxide film on anodic porous sintered body surface; The preliminary treatment of anode pellet dielectric oxide film; Conducting high polymers layer is formed on the anodic porous sintered body surface with dielectric oxide film; At conducting high polymers nitride layer outer coated graphite layer and silver slurry layer successively; Finished product is formed by moulded package.The electrolytic capacitor of the method manufacture has the advantages such as equivalent series resistance (ESR) is low, leakage current is little.
Description
Technical field
The present invention relates to the processing method of electrolytic capacitor manufacture process medium oxide-film, in particular to traditional with valve metals such as tantalum, niobium, titanium, aluminium for anode, with conductive polymer polymer for catholyte manufactures the pretreated method to dielectric oxide film increased in electrolytic capacitor process.
Background technology
Usually, the Chief manufacturing process of solid electrolytic capacitor comprises: use the valve metal powder compacting sinterings such as tantalum, niobium, titanium, aluminium to become porous anode body, the surface of this anode bodies is formed dielectric oxide film by the method for electrochemical oxidation, this dielectric oxide rete forms dielectric substrate, then forms cathode layer thereon.We know, the key technical indexes of capacitor has capacitance, withstand voltage, resistance to temperature value, leakage current, loss.Except these three important indicators, for Low ESR series electrolytic capacitor, it also has a very important index to be exactly that equivalent series resistance (ESR), and ESR is lower, and loss is less, and output current is larger, and the quality of capacitor is higher.In recent years, in order to make capacitor obtain more low ESR (ESR), as dielectric substrate many employings electroconductive polymer layer.Simultaneously in order to meet hyundai electronics information equipment to demand that is miniaturized, high speed development, a series of new requirement being proposed to capacitor, particularly small-size high-capacity tight demand is proposed to the electrolytic capacitor of switch power filter.
Describe by 3 in European patent EP-A-340512 specification, the solid electrolyte poly-3 that 4 ethyldioxythiophene are made, the production method of 4 ethyldioxythiophene (PEDT), and by oxidation polymerization effect, PEDT is used for the purposes of the solid electrolyte in electrolytic capacitor.PEDT, as the substitute of manganese dioxide in solid electrolytic capacitor or charge transfer complex, because it has higher conductivity, therefore can reduce the equivalent series resistance of capacitor and improve frequency performance.In addition at Unexamined Patent 2-130906, U.S.Pat.Nos.5,729,428; 5,968,417; 6,001,281; The manufacture of electrostrictive polymer electrolysis condenser is all related in many patents such as 6,059,999 and 6,674,635.
But the electrolytic capacitor involved by these patents has a common feature, namely leakage current is large, which greatly limits the range of application of conductive polymer thing electrolytic capacitor.
Summary of the invention
In order to overcome the large shortcoming of existing conductive polymer polymer solid electrolyte condenser leakage current, the present invention aims to provide a kind of processing method of electrolytic capacitor manufacture process medium oxide-film, produces the electrolytic capacitor that equivalent series resistance (ESR) is low, leakage current is little.Its technical scheme taked is as follows:
A processing method for electrolytic capacitor manufacture process medium oxide-film, adds anode pellet dielectric oxide film preprocessing process, comprises the following steps:
Step 1: valve metal powder is become the leaded anodic porous sintered body of band through mold pressing and vacuum-sintering, and described valve metal powder specific volume >50000 μ F/g, sintered density is 5.2 ~ 5.8g.cm
3, thickness is 0.6 ~ 1.2mm;
Step 2: adopt electrochemical method to form dielectric oxide film on anodic porous sintered body surface;
Step 3: anode pellet dielectric oxide film preliminary treatment;
Step 4: form conducting high polymers layer on the anodic porous sintered body surface with dielectric oxide film;
Step 5: at conducting high polymers nitride layer outer coated graphite layer and silver slurry layer successively, cathode conductive layer graphite used is the low temperature graphite of tool high conduction performance, its electric conductivity < 30 Ω .m-2, curing temperature < 100 DEG C;
Step 6: form finished product by moulded package.
Anode pellet dielectric oxide film preliminary treatment described in described step 3, comprises the following steps:
3.1: by volume proportions pretreatment fluid, in pretreatment fluid, include that concentration is 0.001mol/l ~ 1mol/l, the Ester that comprises the straight or branched of 1 to 10 carbon atom, saturated or undersaturated polymeric anion group, the organic sulfonic acid of concentration <5%, all the other solution are solvent;
3.2: pretreatment fluid is placed in water bath with thermostatic control, bath temperature is 25 DEG C ~ 50 DEG C;
3.3: the capacitor anode pellet making oxidation film layer is completely infused in pretreatment fluid, adopt D.C. regulated power supply to add the DC offset voltage of 5V at capacitor anode pellet two ends simultaneously, this direct voltage is generally 10% ~ 20% of anode pellet oxide-film coating-forming voltage, and dip time is 10 ~ 15min;
3.4: first the capacitor after dipping is good is placed in the dry 10min of baking oven of 50 DEG C, be then placed in the dry 15 ~ 20min of baking oven of 150 DEG C;
Ester described in described step 3-3.1 is carbomethoxy, ethoxycarbonyl, propyl ester base, polyglycidyl base, isopropyl esters, epoxyisopropyl ester, butyl ester base, pentyl ester base and one or more in ester group.
The concentration of polymeric anion group described in described step 3-3.1 is 0.01mol/l ~ 0.1mol/l.
In described step 3-3.1, organic sulfonic acid is 1% ~ 3%.
Solvent described in described step 3-3.1 is water and ethanol.
The content <50% of water described in described step 3-3.1.
The content of water described in described step 3-3.1 is 20 ~ 40%.
In described step 3-3.1, bath temperature is 30 ~ 35 DEG C.
Compared with prior art, the invention provides a kind of processing method of electrolytic capacitor manufacture process medium oxide-film, especially be the preparation technique of dielectric surface treatment liquid with valve metal oxides such as tantalum, niobium, titanium, aluminium, prepared surface treatment liquid is used for the manufacture of conductive polymer polymer solid electrolyte capacitor, intrinsic contaminant defect in capacitor anode valve metal oxides dielectric layer is isolated, thus reduce the leakage current of capacitor, thus produce the electrolytic capacitor that equivalent series resistance (ESR) is low, leakage current is little.
Embodiment
The manufacture method of general solid electrolytic capacitor, comprises the following steps: successively
A, valve metal powder is become the leaded anodic porous sintered body of band through mold pressing and vacuum-sintering;
B, electrochemical method is adopted to form dielectric oxide film on anodic porous sintered body surface;
C, form conducting high polymers layer on the anodic porous sintered body surface with dielectric oxide film;
D, at conducting high polymers nitride layer outer coated graphite layer and silver slurry layer successively;
E, form final products by moulded package.
Wherein a, valve metal refer to metal tantalum, niobium, titanium or aluminium, and by the anodic porous agglomerate (abbreviation agglomerate) that valve metal powder (specific volume 50000 more than μ F/g) is formed after mold pressing and vacuum-sintering, its sintered density is 5.2 ~ 5.8g.cm
-3, thickness is 0.6 ~ 1.2mm.
Wherein b, to adopt electrochemical method to form dielectric oxide film on anodic porous agglomerate surface be immersed in dilute phosphoric acid solution by agglomerate, through medium oxidizing rete that electrochemical reaction is formed under certain voltage condition.
The graphite that wherein d, negative electrode conducting shell are used is the low temperature graphite of tool high conduction performance, the electric conductivity < 30 Ω .m of this graphite
-2, curing temperature < 100 DEG C.
Silver used is starched as the low-temperature silver of tool high conduction performance is starched, the electric conductivity < 0.015 Ω .m of this silver slurry
-2, curing temperature < 150 DEG C.
Wherein e, by press mold encapsulation formed final products.
Maximum feature of the present invention is to increase a dielectric oxide film preprocessing process, the especially compound method of dielectric oxide film surface treatment liquid between step b and step c.
A processing method for electrolytic capacitor manufacture process medium oxide-film, adds anode pellet dielectric oxide film preprocessing process, comprises the following steps:
Step 1: valve metal powder is become the leaded anodic porous sintered body of band through mold pressing and vacuum-sintering, and described valve metal powder specific volume >50000 μ F/g, sintered density is 5.2 ~ 5.8g.cm
-3, thickness is 0.6 ~ 1.2mm;
Step 2: adopt electrochemical method to form dielectric oxide film on anodic porous sintered body surface;
Step 3: the preliminary treatment of anode pellet dielectric oxide film, comprises the following steps;
3.1: by volume proportions pretreatment fluid, in pretreatment fluid, including concentration is 0.001mol/L ~ 1mol/L, comprise the straight or branched of 1 to 10 carbon atom, the carbomethoxy of saturated or undersaturated polymeric anion group, ethoxycarbonyl, propyl ester base, polyglycidyl base, isopropyl esters, epoxyisopropyl ester, butyl ester base, one or more Esters in pentyl ester base and ester group, the organic sulfonic acid of concentration <5%, preferred concentration is 1% ~ 3% organic sulfonic acid, all the other solution are solvent, solvent preferred water and ethanol, wherein, the content <50% of water, the content of preferred water is 20 ~ 40%, preferred 0.01mol/L ~ the 0.1mol/L of concentration of polymeric anion group,
3.2: pretreatment fluid is placed in water bath with thermostatic control, bath temperature is 25 DEG C ~ 50 DEG C, and preferred water bath temperature is 30 ~ 35 DEG C;
3.3: the capacitor anode pellet making oxidation film layer is completely infused in pretreatment fluid, adopt D.C. regulated power supply to add the DC offset voltage of 5V at capacitor anode pellet two ends simultaneously, this direct voltage is generally 10% ~ 20% of anode pellet oxide-film coating-forming voltage, and dip time is 10 ~ 15min;
3.4: first the capacitor after dipping is good is placed in the dry 10min of baking oven of 50 DEG C, be then placed in the dry 15 ~ 20min of baking oven of 150 DEG C;
Step 4: forming conducting high polymers layer with dielectric oxide film anodic porous sintered body surface;
Step 5: at conducting high polymers nitride layer outer coated graphite layer and silver slurry layer successively, cathode conductive layer graphite used is the low temperature graphite of tool high conduction performance, its electric conductivity < 30 Ω .m-2, curing temperature < 100 DEG C;
Step 6: form finished product by moulded package.
Usually, the working centre of solid electrolytic capacitor is the dielectric oxide film adopting electrochemical method to be formed on anodic porous sintered body surface, optimal state is that requirement this layer of oxidation film layer exists with amorphous form completely, but in the manufacture process of solid electrolytic capacitor, the valve metal powder that anode uses always also exists various (such as iron, carbon, calcium, magnesium etc.) trace impurity, although some volatile impurity can be got rid of by high-temperature vacuum sintering, but this effect is limited, most impurity element is solidificated in formed anodic porous agglomerate by high temperature sintering, when adopting electrochemical method to form dielectric oxide rete by certain voltage on valve metal surface, these impurity elements will become the crystallization center in dielectric oxide rete, if do not processed these crystallization centers, then when making conductive polymer polymer cathode dielectric substrate, in the crystallization at these impurity places, cardioelectric field will be concentrated, dielectric layer is generated heat, conductive polymer coating Yin Gaore can be made and directly evaporate on the one hand, the graphite of post-production can be made on the other hand to draw layer directly contact with dielectric oxide layer, condenser leakage current is caused to increase, thus finally cause puncturing of whole capacitor.
Found in the process formed at electrolytic capacitor anode dielectric oxide rete by a large amount of experiments, mostly the crystallization center formed for micro-transition metal impurity defect is the center of positive charge be positive, in the capacitor course of work, the a large amount of electronics of gathering causes electric stress to concentrate by these center of positive charge, in order to stop concentrating of conduction electrons stream, the crystallization center formed impurity defect adopts the weakly conducting with anionic functional group or non-conductive polymer polymerization plasma to carry out preliminary treatment, these have anionic functional group high molecular polymerization ion in the solution by be gathered in positively charged impurity defect around.The polymeric anion group used in the present invention mainly comprises the straight or branched of 1 to 10 carbon atom, saturated or unsaturated alkyl ester group, and alternative embodiment attached bag draws together carbomethoxy, ethoxycarbonyl, propyl ester base, polyglycidyl base, isopropyl esters, epoxyisopropyl ester, butyl ester base, pentyl ester base and ester group.But the invention is not restricted to these examples.
With the solid electrolytic capacitor that the inventive method is produced, there is ultra-low equivalent series resistance ERS value, under the test frequency of 100KHz, its ESR value <50m Ω.Product leakage current is low to moderate 0.01CV, be starkly lower than the leakage current 0.1CV of conventional polymer electrolyte capacitor product, its impedance frequency characteristic is good, its ESR value can keep stable within the scope of 10KHz ~ 1000KHz, rate of change < 10%, can meet the particular/special requirement of modern high frequency Switching Power Supply to filter capacitor completely.
Embodiment 1: choosing CV value is 32, the tantalum powder of 000 μ Fv/g, tabletted, and high temperature high-vacuum sintering becomes containing tantalum lead-in wire at 1450 DEG C, be of a size of the anode porosity agglomerate (abbreviation agglomerate) of 4.3mm × 3.1mm × 0.9mm, agglomerate is changed into 53V at phosphoric acid,diluted aqueous solution Anodic, forms dielectric oxide rete, then there is the teflon gasket of insulation property on anode tap is altered.Then prepare oxidation film layer surface preparation liquid in the steps below, carry out surface preparation:
Prepare pretreatment fluid in proportion, pretreatment fluid composition is: methyl methacrylate 5%, camphorsulfonic acid 2%, water 30%, ethanol 63%;
Pretreatment fluid is placed in water bath with thermostatic control, and bath temperature remains on 30 DEG C;
The capacitor anode pellet making oxidation film layer is completely infused in pretreatment fluid, adopt D.C. regulated power supply to add the DC offset voltage of 5V at capacitor anode pellet two ends simultaneously, this direct voltage is generally 10% ~ 20% of anode pellet oxide-film coating-forming voltage, and dip time is 10min ~ 15min;
First capacitor after dipping is good is placed in the dry 10min of baking oven of 50 DEG C, is then placed in the dry 15min ~ 20min of baking oven of 150 DEG C.
Then will through pretreated anode pellet under 0 ~ 10 DEG C of low temperature, immerse the first polymer fluid, first polymer fluid is containing the conducting polymer monomer 3 of 2wt%, 4-ethylenedioxythiophene, containing the oxidant p-methyl benzenesulfonic acid iron of 40wt%, containing the silane coupler of 0.3%, all the other are solvent, n-butanol and isopropyl alcohol, n-butanol and isopropyl alcohol weight proportion 1:1, soak after 6 ~ 10 minutes, take out agglomerate, at room temperature place 10 minutes, be placed in 50 DEG C of constant temperature ovens and react 20min, then be warmed up to 120 DEG C of insulation 15min and complete polymerization reaction, then repeatedly clean with ethanol and deionized water, and 40min is changed into again in the benefit formation liquid p-methyl benzenesulfonic acid aqueous solution of 0.1wt% concentration, cleaning is also dry in deionized water afterwards, repeat above-mentioned dipping, polymerization, change into again and cleaning-drying process 6 times, obtain the first dielectric substrate, then the agglomerate with the first dielectric substrate is immersed the second polymer fluid, second polymer fluid batching is added with 0.3wt% polyvinylpyrrolidone organic adhesive on the first polymer fluid batching basis, the amount of polymer monomer increases to 4wt%, all the other batchings are with the first polymer fluid, it operates dipping, polymerization, cleaning, change into again and the operation of cleaning-drying with the first dielectric substrate, 5 times repeatedly, obtain the second dielectric substrate, thickness 15 ~ 20 μm, then on conducting polymer skin, low-temperature conductive graphite linings is applied, conductive silver slurry layer, complete the preparation of conductive cathode.Then the anode of lead frame and cathode weld, complete the encapsulation of resin bed, forms solid electrolytic capacitor.
Comparative example 1:
Make capacitor pellet according to embodiment 1, just change the formula of pretreatment fluid into following composition: 3-methyl epoxyisopropyl silane 3%, camphorsulfonic acid 2%, water 30%, ethanol 65%; Then on conducting polymer skin, apply low-temperature conductive graphite linings, conductive silver slurry layer, complete the preparation of conductive cathode.
Comparative example 2:
Capacitor pellet is made according to embodiment 1, just after product formation oxidation film layer, do not carry out surface preparation, directly in anode pellet, make conductive polymer coating by process described in embodiment 1, then on conducting polymer skin, apply low-temperature conductive graphite linings, conductive silver slurry layer, complete the preparation of conductive cathode.
It is 16V47 μ F that tantalum anode in the embodiment of the present invention forms dielectric oxide film product specification after dilute phosphoric acid solution changes into, and complete all processes in embodiment, capacitance is tested at 120 hz, and average size extraction rate reaches 98%.Equivalent series resistance is tested respectively under 10KHz, 100KHz, 1000KHz, 2000KHz, and leakage current tests 30 seconds readings under 1.2 times of rated voltages (i.e. 19.2V).Following table 1 is the mean value of each enforcement 20 samples:
Table 1
Can be found out by the data of upper table; the electrostrictive polymer electrolysis condenser that technical scheme of the present invention is produced has lower ESR value; adopt pretreatment fluid of the present invention and preconditioning technique; impurity defect in electrolytic capacitor anodized film forming process can be played a very good protection; thus significantly reduce the leakage current of product; make the ESR value of product reduce with the change of frequency simultaneously; improve the high frequency characteristics of product, the particular/special requirement of high frequency switch power filter circuit of new generation can be met well.
Claims (6)
1. the processing method of electrolytic capacitor manufacture process medium oxide-film, is characterized in that: add anode pellet dielectric oxide film preprocessing process, comprise the following steps:
Step 1: valve metal powder is become the leaded anodic porous sintered body of band through mold pressing and vacuum-sintering, and described valve metal powder specific volume >50000 μ F/g, sintered density is 5.2 ~ 5.8g.cm
3, thickness is 0.6 ~ 1.2mm;
Step 2: adopt electrochemical method to form dielectric oxide film on anodic porous sintered body surface;
Step 3: anode pellet dielectric oxide film preliminary treatment;
Step 4: form conducting high polymers layer on the anodic porous sintered body surface with dielectric oxide film;
Step 5: at conducting high polymers nitride layer outer coated graphite layer and silver slurry layer successively, cathode conductive layer graphite used is the low temperature graphite of tool high conduction performance, its electric conductivity < 30 Ω .m-2, curing temperature < 100 DEG C;
Step 6: form finished product by moulded package;
Anode pellet dielectric oxide film preliminary treatment described in described step 3, comprises the following steps:
3.1: by volume proportions pretreatment fluid, in pretreatment fluid, include that concentration is 0.001mol/L ~ 1mol/L, the Ester that comprises the straight or branched of 1 to 10 carbon atom, saturated or undersaturated polymeric anion group, the organic sulfonic acid of concentration <5%, all the other solution are solvent;
3.2: pretreatment fluid is placed in water bath with thermostatic control, bath temperature is 25 DEG C ~ 50 DEG C;
3.3: the capacitor anode pellet making oxidation film layer is completely infused in pretreatment fluid, adopt D.C. regulated power supply to add the DC offset voltage of 5V at capacitor anode pellet two ends simultaneously, this direct voltage is generally 10% ~ 20% of anode pellet oxide-film coating-forming voltage, and dip time is 10 ~ 15min;
3.4: first the capacitor after dipping is good is placed in the dry 10min of baking oven of 50 DEG C, be then placed in the dry 15 ~ 20min of baking oven of 150 DEG C.
2. the processing method of a kind of electrolytic capacitor manufacture process medium oxide-film according to claim 1, is characterized in that: Ester described in described step 3.1 is carbomethoxy, ethoxycarbonyl, propyl ester base, polyglycidyl base, isopropyl esters, epoxyisopropyl ester, butyl ester base, pentyl ester base and one or more in ester group.
3. the manufacture method of electrolytic capacitor according to claim 1, is characterized in that: the concentration of polymeric anion group described in described step 3.1 is 0.01mol/l ~ 0.1mol/l.
4. the manufacture method of electrolytic capacitor according to claim 1, is characterized in that: in described step 3.1, the concentration of organic sulfonic acid is 1% ~ 3%.
5. the manufacture method of electrolytic capacitor according to claim 1, is characterized in that: solvent described in described step 3.1 is water and ethanol.
6. the manufacture method of electrolytic capacitor according to claim 1, is characterized in that: aqueous phase described in described step 3.1 is 30% for the content of pretreatment fluid.
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| CN109994318B (en) * | 2019-03-06 | 2021-01-26 | 湖南艾华集团股份有限公司 | Aluminum electrolytic capacitor and preparation method thereof |
| CN112490004B (en) * | 2020-11-23 | 2022-08-19 | 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) | Method for manufacturing electrolytic capacitor |
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| CN101350253A (en) * | 2008-09-17 | 2009-01-21 | 中国振华（集团）新云电子元器件有限责任公司 | Solid electrolyte capacitor with ultra-low equivalent series resistance and manufacturing method thereof |
| CN101692412A (en) * | 2009-08-06 | 2010-04-07 | 中国振华（集团）新云电子元器件有限责任公司 | New type solid electrolytic capacitor and manufacturing method thereof |
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| CN101350253A (en) * | 2008-09-17 | 2009-01-21 | 中国振华（集团）新云电子元器件有限责任公司 | Solid electrolyte capacitor with ultra-low equivalent series resistance and manufacturing method thereof |
| CN101692412A (en) * | 2009-08-06 | 2010-04-07 | 中国振华（集团）新云电子元器件有限责任公司 | New type solid electrolytic capacitor and manufacturing method thereof |
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