CN102496473A - Method for preparing ruthenium oxide coating on inner wall of tantalum shell of electrolytic capacitor - Google Patents
Method for preparing ruthenium oxide coating on inner wall of tantalum shell of electrolytic capacitor Download PDFInfo
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- CN102496473A CN102496473A CN2011104101629A CN201110410162A CN102496473A CN 102496473 A CN102496473 A CN 102496473A CN 2011104101629 A CN2011104101629 A CN 2011104101629A CN 201110410162 A CN201110410162 A CN 201110410162A CN 102496473 A CN102496473 A CN 102496473A
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Abstract
The invention discloses a method for preparing a ruthenium oxide coating on the inner wall of a tantalum shell of an electrolytic capacitor, belonging to capacitor cathode preparation methods. The method comprises the following steps of: mixing a ruthenium compound and valve metal powder to a powder mixture, and mixing the powder mixture and a solvent to obtain a slurry; evenly applying the slurry onto the inner wall of the tantalum shell, and drying; putting the dried tantalum shell into a coating furnace, and introducing steam to carry out thermal decomposition; dissolving ruthenium halide into deionized water to obtain an electrolyte, and adding additives to adjust the pH value to 1-5; and injecting the electrolyte into the tantalum shell, introducing a direct current, of which the current density is 5-50mA/cm<2>, to carry out electroplating for 10-30 minutes, putting the electroplated tantalum shell into the coating furnace, and introducing steam to carry out heat treatment for 1-3 hours. The electrolytic capacitor cathode made by the method disclosed by the invention can increase the capacitance of the liquid tantalum capacitor with the same volume by more than one time, and the equivalent series resistance is smaller; and thus, the invention provides a method for preparing an electrolytic capacitor cathode.
Description
Technical field: the present invention relates to a kind of preparation method of electrolytic capacitor, relate in particular to a kind of preparation method of electrolytic capacitor cathode.
Background technology: along with development of electronic technology, electronic equipment is had higher requirement to the energy density of capacitor.Though tantalum electrolytic capacitor is the capacitor of a kind of big capacity, high voltage and high reliability, its capacity is difficult to drawn fully; This is because when the surface preparation of anode tantalum piece has the manganese dioxide deielectric-coating, and manganese dioxide is difficult to get in the trickle space of tantalum powder formation.Though electrolyte can fully contact capacitor volume (C with anode tantalum piece in theory
Always) equal anode capacity (C
Anode) and cathode capacities (C
Negative electrode) series connection: C
Always=(C
Anode* C
Negative electrode)/(C
Anode+ C
Negative electrode); When cathode capacities and anode capacity equated, capacitor volume had only 50% of anode capacity, and when cathode capacities was ten times of anode capacity, capacitor volume also had only 91% of anode capacity.Therefore, in order to obtain the capacitor of height ratio capacity, not only need improve the specific capacity of anode, and the target capacity is had higher requirement.At present, compacting tantalum powder is one of common method of making on the tantalum electrolytic capacitor negative electrode on the tantalum shell, and its electric weight of negative electrode that this employing tantalum powder is made is stored in the tantalum pentoxide dielectric of tantalum and electrolyte formation, and specific capacity is lower; Be difficult to satisfy the increasingly high requirement of target capacity.
For this reason, publication number is called for the patent of invention of " CN101556869B " discloses name that " a kind of tantalum capacitor is with tantalum shell inwall RuO
2The preparation method of film ", it is to utilize electrochemical method at the cathodic deposition ruthenium-oxide.Its principle is that water power is from the H that goes out
+Become hydrogen by cathodic reduction, the OH in the solution
-With Ru
3+The hydroxide that reaction generates, the hydroxide hydrolysis generates ruthenium-oxide and is deposited on cathode surface; This method is owing to exist the cathode hydrogen evolution reaction, and the ruthenium-oxide of deposition is relatively poor at suprabasil adhesive force.In addition; Publication number contains ruthenium compound for the patent of invention document of " CN101728084A " and " CN101226829A " discloses respectively in the coating of tantalum inner surface of outer cover; At high temperature sintering prepares the method for high power capacity ruthenium-oxide negative electrode then; Though its adhesive force of ruthenium-oxide of this method preparation is higher, ruthenium-oxide can lose the crystallization water and reduce specific capacity.And publication number is called " a kind of electrochemical super-capacitor and manufacturing approach thereof " for the patent of invention document of " CN101271767A " discloses name, and it is to prepare RuO through chemical reaction earlier
2Powder adds binding agent then and conductive agent is processed slurry, is coated in the collector electrode surface again.Its shortcoming is to contain insulation, hydrophobic binding agent in the electrode, so internal resistance is big, power density is low, and adhesive failure rear oxidation ruthenium powder will break away from collector electrode and cause the whole capacitor device to lose efficacy, and the life-span is short, reliability is low.Can find out through above-mentioned analysis: how to prepare big capacity negative electrode and become to hinder the specific capacity of tantalum capacitor and the bottleneck that energy density improves, need a kind of negative electrode of exploitation badly to adapt to the growth requirement of modern electronic equipment with vast capacity.
Summary of the invention: to the above-mentioned defective that exists in the prior art; The purpose of this invention is to provide a kind of method for preparing ruthenium oxide coatings at electrolytic capacitor tantalum outer casing inner wall; This method not only technology is simple, and the specific capacity of the capacitor of making is big, internal resistance is little, output power density is big, the ruthenium oxide coatings strong adhesion.
To achieve these goals, the technical scheme of the present invention's employing is following:
1) will contain ruthenium compound and valve metal powder and mix by 1: 0.5～1.5 weight ratio, mixed powder; The said ruthenium compound that contains is ruthenium halide or one of the mixture of hydration ruthenium halide or ruthenic oxide or hydration ruthenic oxide or ruthenium halide and ruthenic oxide or mixture of ruthenium halide and hydration ruthenic oxide, and said ruthenium halide is ruthenium trichloride or iodate ruthenium; Said valve metal powder is the mixture of conventional tantalum powder or niobium powder or tantalum powder and niobium powder; Perhaps being the mixture of average grain diameter >=150 purpose electrolytic capacitors Ta powder used or niobium powder or tantalum powder and niobium powder, perhaps is the mixture of superfine tantalum powder or niobium powder or tantalum powder and niobium powder;
2) with above-mentioned mixed powder and solvent by 1: 0.5～5 weight ratio hybrid modulation form slurry; Said solvent is the mixture of water or organic solvent or water and organic solvent, and said organic solvent is ethanol or ethylene glycol or acetone;
3) above-mentioned slurry evenly is coated on said tantalum outer casing inner wall, oven dry; Guarantee that oven dry disposed slurry thickness reaches 1 μ m～20 μ m;
4) the tantalum shell after will drying is put into 200～350 ℃ tunicle stove, and the steam heat that feeds 5～90kPa decomposed 2～5 hours;
5) ruthenium halide is dissolved in the deionized water of 25 times of weight is mixed with electrolyte, add additive the pH value of electrolyte is adjusted between 1～5; Said additive is one of boric acid, borax, acetic acid, sodium acetate or salicylic acid;
6) injecting the electrolyte in the tantalum shell of step 4), is anode with this tantalum shell, in electrolyte, inserts the negative electrode that inert metal is made, and electroplates 10～30 minutes, and Control current density is 5～50mA/cm
2
7) will electroplate good tantalum shell and put into 200～350 ℃ tunicle stove, the steam heat that feeds 5～90kPa was handled 1～3 hour.
On the basis of technique scheme; Optimal technical scheme of the present invention is: the weight ratio that contains ruthenium compound and valve metal powder in the step 1) is 1: 0.8～1.2; Step 2) weight ratio of mixed powder and solvent is 1: 1～4 in; The tunicle furnace temperature is that 280 ℃, steam pressure are that 30～70kPa, heating time are 3 hours in step 4) and the step 7), and electroplating time is that 20 minutes, current density are 10～40mA/cm in the step 6)
2
The present invention's optimal technical scheme further is: the weight ratio that contains ruthenium compound and valve metal powder in the step 1) is 1: 1; Step 2) weight ratio of mixed powder and solvent is 1: 2～3 in; The tunicle furnace temperature is that 280 ℃, steam pressure are that 40～50kPa, heating time are 2 hours in step 4) and the step 7), and electroplating time is that 20 minutes, current density are 20～30mA/cm in the step 6)
2
Best-of-breed technology scheme of the present invention is: step 2) weight ratio of mixed powder and solvent is 1: 2.5; The tunicle furnace temperature is that 280 ℃, steam pressure are that 60kPa, heating time are 3 hours in step 4) and the step 7), and electroplating time is that 20 minutes, current density are 20～30mA/cm in the step 6)
2
Compare with prior art, the present invention utilizes electrochemical process to prepare ruthenium-oxide owing to adopted technique scheme, so specific discharge capacity high (greater than 500F/g); Adopt anode oxidation method to prepare ruthenium-oxide, can avoid the evolving hydrogen reaction of cathodic deposition method, improved the adhesive force of ruthenium-oxide; Sintering prepares the ruthenium-oxide precoated shet under the water vapour protection, and it is higher that the ruthenium-oxide of acquisition contains the crystallization water, and the specific capacity of the ruthenium-oxide that therefore obtains is higher; Under the water vapour protection, carry out later stage heat treatment, avoided direct heat to handle the dehydration of the ruthenium-oxide that causes, therefore guaranteed height ratio capacity; In precoated shet, adopt tantalum powder or niobium powder as additive; Not only obtained the precoated shet of high adhesion force; And tantalum compound or niobium compound can be steady in a long-term in the electrolyte (38wt% sulfuric acid) of liquid tantalum electrolytic capacitor, improved life of capacitors and reliability, in addition; Tantalum compound or niobium compound are hydrophilic compounds, have avoided conventional binding agent because hydrophobic and the internal resistance that causes increases.
Embodiment: the embodiment below in conjunction with concrete is described further the present invention:
Embodiment 1
1) will contain ruthenium compound 1 gram and mix, get mixed powder with 0.5 gram valve metal powder;
2) 1.5 above-mentioned mixed powders of gram and 0.75 gram solvent are even, be modulated into slurry;
3) above-mentioned slurry evenly is coated on said tantalum outer casing inner wall (slurry not necessarily all has been coated with), oven dry guarantees that oven dry disposed slurry thickness reaches 1 μ m～20 μ m;
4) the tantalum shell after will drying is put in 200 ℃ the tunicle stove, and the steam heat that feeds 5kPa decomposed 2 hours;
5) ruthenium halide is dissolved in 25 times of weight deionized waters, adding boric acid is adjusted to 1 with the pH value of solution;
6) with electrolyte through implantation step 4) in the tantalum shell handled well, be anode with this tantalum shell, in electrolyte, insert the negative electrode that inert metal is made, electroplated 30 minutes, Control current density is 5mA/cm
2
7) will electroplate good tantalum shell and put into 200 ℃ tunicle stove, the steam heat that feeds 5kPa was handled 1 hour.
Embodiment 2
Each step is with embodiment 1; Wherein, Mixed powder in the step 1) contains ruthenium compound by 1 gram and 1.5 gram valve metal powder mix; Step 2) slurry in is formulated by 2.5 gram mixed powders and 12.5 gram solvents that the present embodiment step 1) makes; The pressure that heating-up temperature in the step 4) is 350 ℃, feed steam is that 90kPa, thermal decomposition time are 5 hours, and the pH value of electrolyte is adjusted to 2 by the borax that adds in the step 5), and the electroplating time in the step 6) is that 10 minutes, current density are 50mA/cm
2, the pressure that the tunicle furnace temperature in the step 7) is 350 ℃, feed steam is that 90kPa, heat treatment time are 3 hours.
Embodiment 3
Each step is with embodiment 1; Wherein, Mixed powder in the step 1) contains ruthenium compound by 1 gram and 0.8 gram valve metal powder mixes; Step 2) slurry in is formulated by 1.8 gram mixed powders and 1.8 gram solvents that the present embodiment step 1) makes; The pressure that heating-up temperature in the step 4) is 280 ℃, feed steam is that 30kPa, thermal decomposition time are 3 hours, and the pH value of electrolyte is adjusted to 3 by the acetic acid that adds in the step 5), and the electroplating time in the step 6) is that 20 minutes, current density are 10mA/cm
2, the pressure that the tunicle furnace temperature in the step 7) is 280 ℃, feed steam is that 30kPa, heat treatment time are 3 hours.
Embodiment 4
Each step is with embodiment 1; Wherein, Mixed powder in the step 1) contains ruthenium compound by 1 gram and 1.2 gram valve metal powder mix; Step 2) slurry in is formulated by 2.2 gram mixed powders and 8.8 gram solvents that the present embodiment step 1) makes; The pressure that heating-up temperature in the step 4) is 280 ℃, feed steam is that 70kPa, thermal decomposition time are 3 hours, and the pH value of electrolyte is adjusted to 4 by the sodium acetate that adds in the step 5), and the electroplating time in the step 6) is that 20 minutes, current density are 40mA/cm
2, the pressure that the tunicle furnace temperature in the step 7) is 280 ℃, feed steam is that 70kPa, heat treatment time are 3 hours.
Embodiment 5
Each step is with embodiment 1; Wherein, Mixed powder in the step 1) contains ruthenium compound by 1 gram and 1 gram valve metal powder mixes; Step 2) slurry in is formulated by 2 gram mixed powders and 4 gram solvents that the present embodiment step 1) makes; The pressure that heating-up temperature in the step 4) is 280 ℃, feed steam is that 40kPa, thermal decomposition time are 2 hours, and the pH value of electrolyte is adjusted to 5 by the salicylic acid that adds in the step 5), and the electroplating time in the step 6) is that 20 minutes, current density are 20mA/cm
2, the pressure that the tunicle furnace temperature in the step 7) is 280 ℃, feed steam is that 40kPa, heat treatment time are 2 hours.
Embodiment 6
Each step is with embodiment 1; Wherein, Mixed powder in the step 1) contains ruthenium compound by 1 gram and 1 gram valve metal powder mixes; Step 2) slurry in is formulated by 2 gram mixed powders and 5 gram solvents that the present embodiment step 1) makes; Heating-up temperature is that 280 ℃, feeding steam pressure are that 60kPa, thermal decomposition time are 3 hours in the step 4), in the step 5) electrolyte by pH value be adjusted to 5 by the salicylic acid that adds, the electroplating time in the step 6) is that 20 minutes, current density are 30mA/cm
2, the pressure that the tunicle furnace temperature in the step 7) is 280 ℃, feed steam is that 60kPa, heat treatment time are 3 hours.
In above-mentioned each embodiment; The said ruthenium compound that contains can be ruthenium halide or hydration ruthenium halide or ruthenic oxide or hydration ruthenic oxide, and mixture that mixture that also can be ruthenium halide and ruthenic oxide form by arbitrary proportion or ruthenium halide and hydration ruthenic oxide are formed by arbitrary proportion or hydration ruthenium halide and hydration ruthenic oxide are by the mixture of arbitrary proportion composition; Said ruthenium halide is ruthenium trichloride or iodate ruthenium, and said hydration ruthenium halide is hydrate ruthenium trichloride or hydration iodate ruthenium.Said valve metal powder can be the mixture of conventional tantalum powder or conventional niobium powder or conventional tantalum powder and conventional niobium powder; Also can be the mixture of average grain diameter >=150 purpose electrolytic capacitors Ta powder used or niobium powder or tantalum powder and niobium powder, can also be the mixture of superfine tantalum powder or ultra-fine niobium powder or superfine tantalum powder and ultra-fine niobium powder.Said solvent is the mixture of water or organic solvent or water and organic solvent, and said organic solvent is ethanol or one of ethylene glycol or acetone.
Claims (4)
1. one kind prepares the method for ruthenium oxide coatings at electrolytic capacitor tantalum outer casing inner wall, it is characterized in that concrete grammar is following:
1) will contain ruthenium compound and valve metal powder and mix by 1: 0.5～1.5 weight ratio, mixed powder; The said ruthenium compound that contains is ruthenium halide or one of the mixture of hydration ruthenium halide or ruthenic oxide or hydration ruthenic oxide or ruthenium halide and ruthenic oxide or mixture of ruthenium halide and hydration ruthenic oxide, and said ruthenium halide is ruthenium trichloride or iodate ruthenium; Said valve metal powder is the mixture of conventional tantalum powder or niobium powder or tantalum powder and niobium powder; Perhaps being the mixture of average grain diameter >=150 purpose electrolytic capacitors Ta powder used or niobium powder or tantalum powder and niobium powder, perhaps is the mixture of superfine tantalum powder or niobium powder or tantalum powder and niobium powder;
2) with above-mentioned mixed powder and solvent by 1: 0.5～5 weight ratio hybrid modulation form slurry; Said solvent is the mixture of water or organic solvent or water and organic solvent, and said organic solvent is ethanol or ethylene glycol or acetone;
3) above-mentioned slurry evenly is coated on said tantalum outer casing inner wall, oven dry; Guarantee that oven dry disposed slurry thickness reaches 1 μ m～20 μ m;
4) the tantalum shell after will drying is put into 200～350 ℃ tunicle stove, and the steam heat that feeds 5～90kPa decomposed 2～5 hours;
5) ruthenium halide is dissolved in the deionized water of 25 times of weight is mixed with electrolyte, add additive the pH value of electrolyte is adjusted between 1～5; Said additive is one of boric acid, borax, acetic acid, sodium acetate or salicylic acid;
6) injecting the electrolyte in the tantalum shell of step 4), is anode with this tantalum shell, in electrolyte, inserts the negative electrode that inert metal is made, and electroplates 10～30 minutes, and Control current density is 5～50mA/cm
2
7) will electroplate good tantalum shell and put into 200～350 ℃ tunicle stove, the steam heat that feeds 5～90kPa was handled 1～3 hour.
2. the method for preparing ruthenium oxide coatings at electrolytic capacitor tantalum outer casing inner wall according to claim 1; It is characterized in that: the weight ratio that contains ruthenium compound and valve metal powder in the step 1) is 1: 0.8～1.2; Step 2) weight ratio of mixed powder and solvent is 1: 1～4 in; The tunicle furnace temperature is that 280 ℃, steam pressure are that 30～70kPa, heating time are 3 hours in step 4) and the step 7), and electroplating time is that 20 minutes, current density are 10～40mA/cm in the step 6)
2
3. the method for preparing ruthenium oxide coatings at electrolytic capacitor tantalum outer casing inner wall according to claim 1; It is characterized in that: the weight ratio that contains ruthenium compound and valve metal powder in the step 1) is 1: 1; Step 2) weight ratio of mixed powder and solvent is 1: 2～3 in; The tunicle furnace temperature is that 280 ℃, steam pressure are that 40～50kPa, heating time are 2 hours in step 4) and the step 7), and electroplating time is that 20 minutes, current density are 20～30mA/cm in the step 6)
2
4. the method for preparing ruthenium oxide coatings at electrolytic capacitor tantalum outer casing inner wall according to claim 1; It is characterized in that: step 2) weight ratio of mixed powder and solvent is 1: 2.5; The tunicle furnace temperature is that 280 ℃, steam pressure are that 60kPa, heating time are 3 hours in step 4) and the step 7), and electroplating time is that 20 minutes, current density are 20～30mA/cm in the step 6)
2
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102891013A (en) * | 2012-09-29 | 2013-01-23 | 上海奥威科技开发有限公司 | Method for preparing ruthenium dioxide combination electrode for energy storage |
| CN103489656A (en) * | 2013-10-17 | 2014-01-01 | 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 |
| CN105405655A (en) * | 2015-12-09 | 2016-03-16 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing non-solid electrolyte tantalum capacitor cathode |
| CN113972073A (en) * | 2021-10-26 | 2022-01-25 | 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 improving inner wall capacity of tantalum shell of non-solid electrolyte tantalum capacitor |
| CN114429870A (en) * | 2022-02-24 | 2022-05-03 | 江苏振华新云电子有限公司 | Steam flow stable output adjusting device for chip tantalum electrolytic capacitor |
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| CN102169759A (en) * | 2010-12-17 | 2011-08-31 | 中国振华（集团）新云电子元器件有限责任公司 | Preparation method of ruthenium oxide electrode material |
| CN102176385A (en) * | 2010-12-17 | 2011-09-07 | 中国振华（集团）新云电子元器件有限责任公司 | Electrochemical preparation method of ruthenium oxide electrode material |
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| US4214971A (en) * | 1978-08-14 | 1980-07-29 | The Dow Chemical Company | Electrode coating process |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102891013A (en) * | 2012-09-29 | 2013-01-23 | 上海奥威科技开发有限公司 | Method for preparing ruthenium dioxide combination electrode for energy storage |
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| CN103489656A (en) * | 2013-10-17 | 2014-01-01 | 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 |
| CN103489656B (en) * | 2013-10-17 | 2016-06-22 | 中国振华（集团）新云电子元器件有限责任公司 | The method preparing solid electrolytic capacitor cathode |
| CN105405655A (en) * | 2015-12-09 | 2016-03-16 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing non-solid electrolyte tantalum capacitor cathode |
| CN105405655B (en) * | 2015-12-09 | 2018-06-29 | 中国振华（集团）新云电子元器件有限责任公司 | A kind of non-solid tantalum electrolytic capacitor cathode preparation method |
| CN113972073A (en) * | 2021-10-26 | 2022-01-25 | 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 improving inner wall capacity of tantalum shell of non-solid electrolyte tantalum capacitor |
| CN114429870A (en) * | 2022-02-24 | 2022-05-03 | 江苏振华新云电子有限公司 | Steam flow stable output adjusting device for chip tantalum electrolytic capacitor |
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Application publication date: 20120613 |