CN1332406C - Electrolyte for liquid Ta electrolytic condenser and producing method thereof - Google Patents
Electrolyte for liquid Ta electrolytic condenser and producing method thereof Download PDFInfo
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- CN1332406C CN1332406C CNB2005100142696A CN200510014269A CN1332406C CN 1332406 C CN1332406 C CN 1332406C CN B2005100142696 A CNB2005100142696 A CN B2005100142696A CN 200510014269 A CN200510014269 A CN 200510014269A CN 1332406 C CN1332406 C CN 1332406C
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Abstract
The invention discloses a kind of electrolyte applying in the condenser that has high voltage (160V) and large capacity (more than 47 muf) and is used to electrolyze the liquid of tantalum. The electrolyte is made up of the electrolyte of dipping and gel. The electrolyte is made up of 26-34% sulfuric acid, 14-25%ethanediol-butyl aether by weight and de-ionized water. In the electrolyte of gel, the capacity rate of silicon sol and sulfuric acid is 2.4-3.2 and the weight rate of ethanediol-butyl aether is 12-22%. The tantalum electrolyzing condenser made of this kind of electrolyte meets completely the special need of electrical source filter circuit in communication engineering. Its flash voltage is up to 210V.
Description
Technical field
The present invention relates to a kind of electrolyte of electrolytic capacitor, electrolyte that particularly a kind of highly pressurised liquid tantalum electrolytic capacitor is used and preparation method thereof.
Background technology
The power unit of a new generation's communication engineering workbench requires to adopt the high-voltage capacitor of 160V to carry out filtering, so require capacitor must possess larger capacity and high voltage product (CU), filtering performance is better.Though the performance of ceramic capacitor is good, capacitance too little (pf level), and solid tantalum electrolytic capacitor is compared leakage current with liquid tantalum electrolytic capacitor bigger, so all can not be fit to the instructions for use of communication engineering electric source filter circuit.
Full seal type liquid tantalum electrolytic capacitor capacity is big, good reliability, function admirable, is first-selected capacity type.All select the important components and parts of the capacitor of this type at present both at home and abroad for use as active power filtering.But the maximum operating voltage of China existing C A35 type series liquid tantalum electrolytic capacitor only is 125V (referring to the GJB733A-96 closed specification), does not reach 160V.The rated voltage that improves capacitor is except energize technology and the sintering process that improve capacitor, the character that also depends on capacitor electrolysis matter, electrolyte is the actual negative electrode of electrolytic capacitor, it is one of key structure material of electrolytic capacitor, therefore, electrolytical performance is not improved raising, just is difficult to produce the high pressure of specific (special) requirements and purposes, jumbo liquid tantalum electrolytic capacitor.
The manufacturer of China CA35 type liquid tantalum electrolytic capacitor, its used electrolyte mostly is the single concentrated sulfuric acid, silicon dioxide and Ludox system, capacitor with this system electrolyte, its flash over voltage is lower than 200V, and when subzero temperature (55 ℃), easily condense, and more volatile during high temperature, as the electrolyte for liquid Ta electrolytic condenser of high pressure (greater than 160V), yet there are no open report both at home and abroad.
Summary of the invention
Technical problem to be solved by this invention provides a kind of electrolyte that high voltage, jumbo liquid tantalum electrolytic capacitor are used that is suitable for making, with this electrolytical capacitor, its flash over voltage will reach the instructions for use of the high-voltage filtering capacitor device that could satisfy the 160V rated voltage more than the 200V.
For achieving the above object, the technical solution used in the present invention is: prepared the electrolyte that a kind of highly pressurised liquid tantalum electrolytic capacitor is used, it is made of dipping electrolyte and gel electrolyte, consisting of of its dipping electrolyte: by weight percentage, sulfuric acid 26%～34%, ethylene glycol-ether 14%～25%, all the other are deionized water; Consisting of of its gel electrolyte: the volume ratio of Ludox and sulfuric acid is: 2.4: 1～3.2: 1, the content of ethylene glycol-methyl ether accounted for 12%～22% of this gel electrolyte weight; The weight concentration of sulfuric acid described in two kinds of electrolyte is 〉=and 97%.
In above-mentioned electrolyte, preferably consist of: flood electrolyte by weight percentage, sulfuric acid 26%～30%, ethylene glycol-ether 18%～25%, all the other are deionized water; Gel electrolyte is 2.8: 1～3.2: 1 by the volume ratio of Ludox and sulfuric acid, and the content of ethylene glycol-methyl ether accounts for 16%～22% of this gel electrolyte weight.
The percentage composition of sulfuric acid is the acidity of dipping electrolyte in the dipping electrolyte; The acidity of gel electrolyte should be revised when calculating, and promptly the electrolyte component total weight should deduct the quality of silicon dioxide in the Ludox, calculates its acidity then, and this acidity should be consistent with the acidity of dipping electrolyte.
By electrolyte provided by the present invention, the specification requirement of its each component is as follows: deionization resistivity of water 〉=15 * 10
6M Ω cm; Ethylene glycol-ether, ethylene glycol-methyl ether are analytical reagent; Sodium ions content≤1000mg/L in the Ludox, potassium content≤30mg/L.
A kind of preparation method of electrolyte for liquid Ta electrolytic condenser of the present invention, it comprises following two steps:
(1) by weight percentage, sulfuric acid 26%～34%, ethylene glycol-ether 14%～25%, all the other are the proportioning of deionized water, and sulfuric acid is added in the deionized water, stir, add ethylene glycol-ether then, and water-bath in 20 ℃ of cold water, promptly make dipping electrolyte after continuing to be stirred to evenly;
(2) Ludox is filtered earlier, make its sodium ions content≤1000mg/L, potassium content≤30mg/L, volume ratio by Ludox and sulfuric acid is 2.4: 1～3.2: 1 then, ethylene glycol-methyl ether content accounts for 12%～22% proportioning of this gel electrolyte weight, in the Ludox after ethylene glycol-methyl ether adding is filtered, water-bath in 20 ℃ cold water, and stir, at last sulfuric acid is dripped in the above-mentioned Ludox that contains ethylene glycol-methyl ether, the limit adds sour limit stirs, and promptly makes gel electrolyte after evenly.
The weight concentration of sulfuric acid described in two kinds of electrolyte is 〉=and 97%.
By electrolyte preparation method provided by the present invention, preferred proportioning is in the step (1): by weight percentage, sulfuric acid 26%～30%, ethylene glycol-ether 18%～25%, all the other are deionized water; Preferred proportioning is in the described step (2): the volume ratio of Ludox and sulfuric acid is 2.8: 1～3.2: 1, and the content of ethylene glycol-methyl ether accounts for 16%～22% of this gel electrolyte weight.
By electrolyte preparation method provided by the present invention, the acidity of its gel electrolyte should be consistent the weight concentration of used sulfuric acid 〉=97%, used deionization resistivity of water 〉=15 * 10 with the acidity of dipping electrolyte
6M Ω cm, used ethylene glycol-ether, ethylene glycol-methyl ether are for analyzing pure or capacitor pure reagent.
Beneficial effect of the present invention is summarized as follows:
Highly pressurised liquid tantalum electrolytic capacitor electrolyte of the present invention, its dipping used for electrolyte is in soaking into the dielectric micropore of sintering tantalum core, its gel electrolyte is used for the filling between tantalum core and the shell, because it adds ethylene glycol-ether and these two kinds of polarity organic macromolecule materials of ethylene glycol-methyl ether of certain content respectively, but their antianode dielectric interfaces form electric field shielding, particularly the former, therefore significantly reduced the anion concentration of capacitor anode near interface, prevented that harmful substance is to capacitor Ta
2O
5The infringement of deielectric-coating, just near the anion concentration the anodic interface reduce just to have suppressed effectively the oxonium ion discharge, thereby improved the withstand voltage properties of working electrolyte.Usually, the flash over voltage of capacitor should be higher than 1.25 times of rated voltage (160V) of capacitor, promptly be higher than 200V, electrolyte of the present invention is containing 18%～25% ethylene glycol-ether and 16%～22% ethylene glycol-methyl ether, its acidity is 26～30 o'clock, the flash over voltage average out to 211.5V (seeing Table 2) that the capacitor that is assembled records.
In the process of preparation gel electrolyte, because contained SiO in the Ludox
2Only constitute the frame structure of gel, do not participate in form electrolyte ingredient and effect in the frame structure, therefore when the acidity of calculated for gel electrolyte, its component total amount should deduct the quality of silicon dioxide in the Ludox, the acidity that makes its calculating is consistent with the acidity of dipping electrolyte, can prevent the difference of electrolyte acidity like this and the ion concentration gradient that produces influences whole electrolytical performance.
Embodiment
The present invention will be further described below in conjunction with embodiment:
Table 1 shows the electrolytical several composition examples of the present invention, and table 2 shows the test result of forming the capacitor flash over voltage of example assembling with electrolyte of the present invention.As shown in Table 2, with the electrolyte of example 1～example 4, the average flash over voltage of capacitor can reach 211.5V; Therefore the example 1～example 4 in the table 1 is preferred the composition; The weight percentage of its ethylene glycol-ether is best (acidity is 26～30) 18%～25%; The weight percentage of ethylene glycol-methyl ether is best (acidity is 26～30) 16%～22%.In the example shown in the table 1 was formed, the technical parameter of its each component: the deionization resistivity of water was 15 * 10
6M Ω cm; Ethylene glycol-ether, ethylene glycol-methyl ether are analytical reagent; The weight concentration of sulfuric acid is 98% (dipping electrolyte in example 1～example 6) and 97% (gel electrolyte in example 1～example 6); Sodium ions content in the Ludox and potassium content (mg/L): example 1 is 995 and 30, example 2 is 998 and 28, example 3 is 1000 and 30, example 4 is 992 and 29, example 5 is 991 and 30, example 6 is 1000 and 29.
Electrolyte of the present invention is formed the preparation method of example, comprises two steps:
1) pressing the composition proportioning of example 1～example 6, is that to add resistivity be 15 * 10 for 98% sulfuric acid with concentration expressed in percentage by weight
6In the deionized water of M Ω cm, stir, add the analytical reagent ethylene glycol-ether then, and water-bath in 20 ℃ cold water, promptly make the dipping electrolyte of example 1～example 6 after continuing to be stirred to evenly, wherein preferred proportioning is example 1～example 4;
2) Ludox is filtered earlier, survey its sodium ions content and potassium content (mg/L): example 1 is 995 and 30, example 2 is 998 and 28, example 3 is 1000 and 30, example 4 is 992 and 29, example 5 is 991 and 30, example 6 is 1000 and 29; Press the composition proportioning of example 1～example 6 then, in the high-purity silicasol after analytical reagent ethylene glycol-methyl ether adding is filtered, water-bath in 20 ℃ cold water, and stir, be that 97% sulfuric acid slowly drips in the Ludox that contains ethylene glycol-methyl ether at last with weight concentration, the limit adds sour limit stirs, and promptly makes the gel electrolyte of example 1～example 6 after evenly, and wherein preferred proportioning is example 1～example 4.
In above-mentioned preparation process, the calculating of the gel electrolyte acidity of example 1～example 6 should be revised, and (referring to the remarks in the table 1), the acidity of its correction should be consistent with the acidity of dipping electrolyte.
Table 1 highly pressurised liquid tantalum electrolytic capacitor is formed example with electrolytical several prescriptions
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Table 2 table 1 is formed the test result of the capacitor flash over voltage of example assembling
| Example | 1 | 2 | 3 | 4 | Mean value |
| Flash over voltage (v) | 220 | 213 | 210 | 208 | 211.5 |
| Remarks | Test condition :-25 ℃ ± 2 ℃ | ||||
With composite gel system electrolyte provided by the present invention, good pressure-resistant performance not only, and the capacitor that is assembled has passed through 2000 hours endurance test, this electrolyte can be made the liquid tantalum electrolytic capacitor of big capacity (greater than 47 μ f) high voltage (160V), can satisfy the special instructions for use of the communications field to the high-voltage filtering capacitor device fully.
Claims (9)
1. electrolyte for liquid Ta electrolytic condenser, it is characterized in that it is made of dipping electrolyte and gel electrolyte, the consisting of of described dipping electrolyte: by weight percentage, sulfuric acid 26%～34%, all the other are deionized water for ethylene glycol-ether 14%～25%; Consisting of of described gel electrolyte: the volume ratio of Ludox and sulfuric acid is: 2.4: 1～3.2: 1, the content of ethylene glycol-methyl ether accounted for 12%～22% of this gel electrolyte weight; The weight concentration of sulfuric acid described in two kinds of electrolyte is 〉=and 97%.
2. electrolyte for liquid Ta electrolytic condenser according to claim 1 is characterized in that, the consisting of of described dipping electrolyte: by weight percentage, sulfuric acid 26%～30%, ethylene glycol-ether 18%～25%, all the other are deionized water; Consisting of of described gel electrolyte: the volume ratio of Ludox and sulfuric acid 2.8: 1～3.2: 1, the content of ethylene glycol-methyl ether accounts for 16%～22% of this gel electrolyte weight.
3. electrolyte for liquid Ta electrolytic condenser according to claim 1 and 2 is characterized in that, the acidity of described gel electrolyte is consistent with the acidity of dipping electrolyte.
4. electrolyte for liquid Ta electrolytic condenser according to claim 1 and 2 is characterized in that described deionization resistivity of water 〉=15 * 10
6M Ω cm, described ethylene glycol-ether, ethylene glycol-methyl ether are analytical reagent.
5. electrolyte for liquid Ta electrolytic condenser according to claim 1 and 2 is characterized in that, the sodium ions content≤1000mg/L of described Ludox, potassium content≤30mg/L.
6. the preparation method of the electrolyte for liquid Ta electrolytic condenser of a claim 1 is characterized in that, it comprises the following steps:
(1) by weight percentage, sulfuric acid 26%～34%, ethylene glycol-ether 14%～25%, all the other are the proportioning of deionized water, and sulfuric acid is added in the deionized water, stir, add ethylene glycol-ether then, and water-bath in 20 ℃ of cold water, promptly make dipping electrolyte after continuing to be stirred to evenly;
(2) Ludox is filtered earlier, make its sodium ions content≤1000mg/L, potassium content≤30mg/L, volume ratio by Ludox and sulfuric acid is 2.4: 1～3.2: 1 then, ethylene glycol-methyl ether content accounts for 12%～22% proportioning of this gel electrolyte weight, in the Ludox after ethylene glycol-methyl ether adding is filtered, water-bath in 20 ℃ cold water, and stir, at last sulfuric acid is dripped in the above-mentioned Ludox that contains ethylene glycol-methyl ether, the limit adds sour limit stirs, and promptly makes gel electrolyte after evenly;
The weight concentration of sulfuric acid described in two kinds of electrolyte is 〉=and 97%.
7. the preparation method of electrolyte for liquid Ta electrolytic condenser according to claim 6. it is characterized in that the proportioning in the described step (1) is: by weight percentage, and sulfuric acid 26%～30%, ethylene glycol-ether 18%～25%, all the other are deionized water; Described step 2) proportioning in is: the volume ratio of Ludox and sulfuric acid is 2.8: 1～3.2: 1, and the content of ethylene glycol-methyl ether accounts for 16%～22% of this gel electrolyte weight.
8. according to the preparation method of claim 6 or 7 described electrolyte for liquid Ta electrolytic condenser, it is characterized in that the acidity of described gel electrolyte is consistent with the acidity of dipping electrolyte.
9. according to the preparation method of claim 6 or 7 described electrolyte for liquid Ta electrolytic condenser, it is characterized in that described deionization resistivity of water 〉=15 * 10
6M Ω cm, described ethylene glycol-ether, ethylene glycol-methyl ether are analytical reagent.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100142696A CN1332406C (en) | 2005-06-30 | 2005-06-30 | Electrolyte for liquid Ta electrolytic condenser and producing method thereof |
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| CNB2005100142696A CN1332406C (en) | 2005-06-30 | 2005-06-30 | Electrolyte for liquid Ta electrolytic condenser and producing method thereof |
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| CN1332406C true CN1332406C (en) | 2007-08-15 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103700506B (en) * | 2013-12-25 | 2016-06-29 | 佛山市高明区利明电子有限公司 | A kind of 160V electrolysis condenser and production technology thereof |
| CN103887085B (en) * | 2014-03-28 | 2016-07-27 | 贵州中航聚电科技有限公司 | Hybrid super tantalum capacitor high-pressure electrolysis matter and preparation method thereof |
| CN105070509A (en) * | 2015-07-15 | 2015-11-18 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing middle-and-high-frequency non-solid electrolytic tantalum capacitor |
| CN109887750B (en) * | 2019-02-20 | 2020-10-16 | 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) | Working electrolyte of non-solid electrolyte tantalum capacitor, preparation method of working electrolyte and non-solid electrolyte tantalum capacitor |
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| CN1046818A (en) * | 1989-04-21 | 1990-11-07 | 马渊马达株式会社 | Carbon brush for miniature motors and manufacture method thereof |
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| JP2001167797A (en) * | 1999-09-30 | 2001-06-22 | Sony Corp | Gel phase electrolyte and gel phase electrolyte cell |
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Patent Citations (5)
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| CN1046818A (en) * | 1989-04-21 | 1990-11-07 | 马渊马达株式会社 | Carbon brush for miniature motors and manufacture method thereof |
| CN1230001A (en) * | 1998-03-23 | 1999-09-29 | 松下电器产业株式会社 | Aluminium electrolysis capacitor |
| CN1293461A (en) * | 1999-09-30 | 2001-05-02 | 索尼株式会社 | Gel electrolyte and gel electrolyte battery |
| JP2001167797A (en) * | 1999-09-30 | 2001-06-22 | Sony Corp | Gel phase electrolyte and gel phase electrolyte cell |
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Non-Patent Citations (3)
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| 电解质对液体钽电容器闪火电压影响的研究 刘仲娥，孙石光，压电与声光，第24卷第6期 2002 * |
| 电解质对液体钽电容器高频电性能影响的研究 刘仲娥，桂娟，陈晓靜，宋金荣，电子元件与材料，第22卷第10期 2003 * |
| 电解质对液体钽电容器高频电性能影响的研究 刘仲娥，桂娟，陈晓靜，宋金荣，电子元件与材料，第22卷第10期 2003;电解质对液体钽电容器闪火电压影响的研究 刘仲娥，孙石光，压电与声光，第24卷第6期 2002 * |
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