CN103325570B - The preparation method of high temperature resistant capacitor - Google Patents
The preparation method of high temperature resistant capacitor Download PDFInfo
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- CN103325570B CN103325570B CN201310276707.0A CN201310276707A CN103325570B CN 103325570 B CN103325570 B CN 103325570B CN 201310276707 A CN201310276707 A CN 201310276707A CN 103325570 B CN103325570 B CN 103325570B
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Abstract
The preparation method who the invention discloses a kind of high temperature resistant capacitor, belongs to capacitor manufacture method; Aim to provide a kind of capacitor manufacture method that tolerates 230 DEG C of following temperature. Its method is according to a conventional method anode tantalum piece to be immersed in phosphoric acid and carries out electrochemical treatments, then the anode tantalum piece that is prepared with dielectric oxide film is carried out soaking with sulfuric acid after vacuum heat, anode tantalum piece that will soak through persulfuric acid immerses in electrolyte and carries out electrochemical treatments for the second time, will clean dry for standby through the anode tantalum piece of electrochemical treatments for the second time; Deionized water, sulfuric acid, property-modifying additive, the hydrogen agent that disappears are hybridly prepared into electrolyte in proportion, this electrolyte and anode tantalum piece for subsequent use are packaged in shell according to a conventional method, make capacitor. Adopting the electrolytic capacitor that the inventive method is manufactured in the hot environment of 200～230 DEG C, normally to work 500 hours continuously, is indispensable electronic component in electric source filter circuit.
Description
Technical field
The present invention relates to a kind of manufacture method of electrolytic capacitor, relate in particular to a kind of preparation method of high temperature resistant capacitor.
Background technology
Electrolytic capacitor is one of electronic component being most widely used. At present, the manufacture method of tantalum electrolytic capacitor is: the anode tantalum piece through high-temperature vacuum sintering is immersed in acidic aqueous solution and carries out electrochemical treatments, make the surface of this anode tantalum piece form one deck tantalum pentoxide dielectric oxide film, then by welding encapsulation in packaged this anode tantalum metal shell that enters to fill liquid state or gel working electrolyte, finally weld Anodic lead-out wire. Its operating temperature of the tantalum electrolytic capacitor of this conventional method manufacture is usually less than 125 DEG C, and in the industries such as oil drilling, geological prospecting, spacecraft, equipment operating ambient temperature is often far away higher than 125 DEG C, therefore capacitor usually lost efficacy because environment temperature is too high, thereby cause output waveform distortion, circuit normally to work, even cause device damage. For this reason, in the patent of invention that applicant is " ZL200810068913.1 " in the patent No., propose a kind of " preparation method of high-temperature electrolytic capacitor anodized film ", although the operating temperature of the capacitor of preparing by the method has increased significantly (can normally working under the environment of 200 DEG C); But when operating temperature is during higher than 200 DEG C (200～230 DEG C), the leakage current of capacitor sharply rises, can not ensure that circuit normally works.
Summary of the invention
For the above-mentioned defect existing in prior art, the present invention aims to provide a kind of preparation method of high temperature resistant capacitor, utilizes capacitor prepared by the method in 200～230 DEG C of environment, normally to work continuously.
To achieve these goals, the technical solution used in the present invention is included in anode tantalum piece surface and prepares the preparation of dielectric oxide film, electrolyte, capacitor assembling; Concrete steps are as follows:
1) in the phosphoric acid that is 0.1～1% by 70～90 DEG C of anode tantalum piece immersions, concentration expressed in percentage by volume, carry out electrochemical treatments, by the boost current density of 0.06～0.65mA/CV, voltage is risen to 1.5～1.9 times of capacitor rated voltage;
2) the anode tantalum piece through electrochemical treatments is cleaned, dried, putting into vacuum is 2x10-3Torr is above, temperature is heat treatment 20～60 minutes in the vacuum drying oven of 320～380 DEG C;
3) be that 38% sulfuric acid soaks 30 minutes by be placed in mass percent concentration through heat treated anode tantalum piece;
4) in the electrolyte that the anode tantalum piece that soaks through persulfuric acid to be immersed to temperature be 160～180 DEG C, mixed by phosphoric acid and ethylene glycol, carry out electrochemical treatments 1～2 hour, apply voltage and be 1.1～1.4 times of capacitor rated voltage; In described electrolyte, the concentration of volume percent of phosphoric acid is 1～15%, the concentration of volume percent of ethylene glycol solution is 50～70%, and all the other are water;
5) the anode tantalum piece through electrochemical treatments is for the second time cleaned to dry for standby;
6) sulfuric acid that is 98% by deionized water with mass percent concentration mixes by the volume ratio of 4:1～2:1, is mixed with aqueous sulfuric acid;
7) to the property-modifying additive that adds 1/10～1/7 times of weight deionized water in described aqueous sulfuric acid, be mixed with mixed solution; Described property-modifying additive is the one in ethylene glycol, EGME, sweet mellow wine, succinic acid, or formulated by two kinds of volume ratios of pressing 1:1～1:1.5 in ethylene glycol, EGME, sweet mellow wine, succinic acid;
8) to the hydrogen agent that disappears that adds 1/15～1/9 times of weight deionized water in above-mentioned mixed solution, make electrolyte; The described hydrogen agent that disappears is the one in paranitrobenzoic acid ammonium, p-nitrophenol, p-nitrophenyl methyl alcohol, or formulated by two kinds of volume ratios of pressing 1:1～1:1.5 in paranitrobenzoic acid ammonium, p-nitrophenol, p-nitrophenyl methyl alcohol;
9) described electrolyte and anode tantalum piece for subsequent use are packaged in shell, make capacitor.
On the basis of technique scheme, the present invention can also adopt following preferred version: in step 1), phosphoric acid temperature is that 80 DEG C, phosphoric acid concentration are 0.5%, boost current density is that 0.35mA/CV, voltage are 1.7 times of capacitor rated voltage; Step 2) in heat treatment temperature be that 360 DEG C, heat treatment time are 45 minutes, in step 4), the temperature of electrolyte is that in 175 DEG C, electrolyte, the concentration of phosphoric acid is 8.5%, the concentration of ethylene glycol is 62%, the electrochemistry time is that 1.5 hours, voltage are 1.2 times of capacitor rated voltage.
On the basis of technique scheme, the present invention can also adopt following preferred version: in step 6), the ratio of deionized water and sulfuric acid is 3:1, in step 7), the addition of property-modifying additive is 1/8 times of deionized water, and the addition of the hydrogen agent that disappears in step 8) is 1/11 times of deionized water.
In technique scheme, adopt sulfuric acid to soak and can remove the foreign ion adhering in oxide-film; The effect of property-modifying additive is the boiling point that improves electrolyte, prevents aquation, and the hydrogen agent that disappears can reduce the hydrogen producing in capacitor ageing and use procedure.
Compared with the prior art, the present invention has not only adopted twice dielectric oxide film to form technique, but also has increased vacuum heat treatment process, sulfuric acid soaking technology; Electrolyte is carried out to modification simultaneously, therefore adopted the ability of its dielectric oxide film withstand high temperatures of capacitor product that the present invention manufactures significantly to be strengthened, thereby effectively improved the reliability and stability of electrolytic capacitor in hot environment. Make a concrete analysis of as follows:
1,, owing to having selected the electrolyte of phosphoric acid and ethylene glycol preparation, therefore not only can ensure that electrolyte had higher flash over voltage, but also can effectively prevent dielectric oxide film crystallization, thereby can improve the electrical property of capacitor product;
2, owing to having adopted electrochemical treatments technique twice, therefore electrochemical treatments can be at the dielectric oxide film of the surface of former dielectric oxide film formation one deck densification for the second time, thickness, intensity and the commutating character of anode tantalum piece surface dielectric film are not only improved, but also the blemish that can repair former dielectric oxide film, dielectric oxide film is more uniform and smooth, has improved the resistance to elevated temperatures of capacitor product;
3, because Technology for Heating Processing has been destroyed the defective dielectric oxide film in close anode substrate surface, therefore can make anode substrate be oxidized and generate oxide, thereby make dielectric oxide film finer and close evenly, improve the unit for electrical property parameters of capacitor product;
4, adopt sulfuric acid soaking technology can remove the foreign ion adhering in oxide-film;
5, use property-modifying additive can improve the boiling point of electrolyte, prevent aquation, therefore can improve capacitor resistance to elevated temperatures; The hydrogen producing in capacitor ageing and use procedure can be eliminated or reduce to the use of hydrogen agent of disappearing, and therefore can reduce interiors of products air pressure, improve reliability.
Be below adopt the specification of the inventive method manufacture be the tantalum electrolytic capacitor of 50V160 μ F, 75V180 μ F under 230 DEG C of conditions after 500 hours performance tests, the electrical performance test parameter recording at normal temperatures:
The electrical quantity of table 1:50V160 μ F at 230 DEG C, after 240h performance test
| Exemplar sequence number | 1 | 2 | 3 | 4 | 5 |
| Capacitance (μ F) | 170 | 171.5 | 170.6 | 169.6 | 170.7 |
| Loss (%) | 5.5 | 6.4 | 5.5 | 6.9 | 6.4 |
| Leakage current (μ A) | 5.2 | 7.6 | 6.5 | 8.0 | 11.0 |
The electrical quantity of table 2:50V160 μ F at 230 DEG C, after 500h performance test
| Exemplar sequence number | 1 | 2 | 3 | 4 | 5 |
| Capacitance (μ F) | 174.6 | 177.5 | 174.7 | 163.3 | 171.7 |
| Loss (%) | 6.6 | 10.8 | 8.1 | 4.8 | 7.7 |
| Leakage current (μ A) | 2.1 | 4.3 | 3.6 | 5.7 | 9.0 |
The electrical quantity of table 3:75V180 μ F at 230 DEG C, after 240h performance test
| Exemplar sequence number | 1 | 2 | 3 | 4 | 5 |
| Capacitance (μ F) | 185.5 | 182.6 | 184.8 | 186.4 | 185.1 |
| Loss (%) | 23.6 | 28.6 | 18.1 | 10.8 | 12.1 |
| Leakage current (μ A) | 2.0 | 2.2 | 2.3 | 2.1 | 2.4 |
The electrical quantity of table 4:75V180 μ F at 230 DEG C, after 500h performance test
| Exemplar sequence number | 1 | 2 | 3 | 4 | 5 |
| Capacitance (μ F) | 180.7 | 169.9 | 172.6 | 159.3 | 177.7 |
| Loss (%) | 45.5 | 75.3 | 78.1 | 76.6 | 49.2 |
| Leakage current (μ A) | 1.5 | 1.6 | 1.4 | 1.4 | 1.2 |
Can find out from above-mentioned test data, adopt the electrolytic capacitor of the inventive method manufacture still can normally work in the hot environment of 230 DEG C, and the unit for electrical property parameters such as loss, leakage current of capacitance all be controlled in allowed limits.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
1) in the phosphoric acid that is 1% by 70 DEG C of anode tantalum piece immersions, concentration expressed in percentage by volume, carry out electrochemical treatments, by the boost current density of 0.06mA/CV, voltage is risen to 1.9 times of capacitor rated voltage;
2) water of putting into 60～80 DEG C through the anode tantalum piece of electrochemical treatments is boiled and washes 100～120 minutes, it is 2x10 that taking-up is put into vacuum after drying-3Torr is above, temperature is heat treatment 60 minutes in the vacuum drying oven of 320 DEG C;
3) be that 38% sulfuric acid soaks 30 minutes by be placed in mass percent concentration through heat treated anode tantalum piece;
4) in the electrolyte that the anode tantalum piece that soaks through persulfuric acid to be immersed to temperature be 160 DEG C, mixed by phosphoric acid and ethylene glycol, carry out electrochemical treatments 2 hours, apply voltage and be 1.1 times of capacitor rated voltage; In described electrolyte, the concentration of volume percent of phosphoric acid is 15%, the concentration of volume percent of ethylene glycol solution is 50%, and all the other are water;
5) boil and wash 100～120 minutes put into 60～80 DEG C of water through the anode tantalum piece of electrochemical treatments for the second time, take out dry for standby;
6) sulfuric acid that is 98% by deionized water with mass percent concentration mixes by the volume ratio of 4:1, is mixed with sulfuric acid solution;
7) to the property-modifying additive that adds 1/7 times of weight deionized water in described sulfuric acid solution, be mixed with mixed solution; Described property-modifying additive is the one in ethylene glycol, EGME, sweet mellow wine, succinic acid;
8) to the hydrogen agent that disappears that adds 1/15 times of weight deionized water in above-mentioned mixed solution, make electrolyte; The described hydrogen agent that disappears is the one in paranitrobenzoic acid ammonium, p-nitrophenol, p-nitrophenyl methyl alcohol;
9) described electrolyte and anode tantalum piece for subsequent use are packaged in shell according to a conventional method, make capacitor.
Embodiment 2
Each step is with embodiment 1; Wherein, in step 1), the temperature of phosphoric acid is that 90 DEG C, phosphoric acid concentration are 0.1%, boost current density 0.65mA/CV, voltage are capacitor rated voltage 1.5 times; Step 2) in heat treatment temperature be 380 DEG C, heat treatment time 20 minutes; In step 4), the temperature of electrolyte is that 180 DEG C, electrochemical treatments time are 1 hour, and voltage is 1.4 times of capacitor rated voltage, and in electrolyte, phosphoric acid concentration is 1%, ethylene glycol solution concentration is 70% in electrolyte, and all the other are water; In step 6), the volume ratio of deionized water and sulfuric acid is 2:1; In step 7), the addition of property-modifying additive is 1/10 times of described deionized water weight; The addition of hydrogen agent of disappearing in step 8) is 1/9 times of deionized water weight.
Embodiment 3
Each step is with embodiment 1; Wherein, in step 1), the temperature of phosphoric acid is that 80 DEG C, phosphoric acid concentration are 0.5%, boost current density 0.35mA/CV, voltage are capacitor rated voltage 1.7 times; Step 2) in heat treatment temperature be 360 DEG C, heat treatment time 45 minutes; In step 4), the temperature of electrolyte is that 175 DEG C, electrochemical treatments time are that 1.5 hours, voltage are 1.2 times of capacitor rated voltage, and in electrolyte, phosphoric acid concentration is 8.5%, ethylene glycol solution concentration is 62% in electrolyte, and all the other are water; In step 6), the volume ratio of deionized water and sulfuric acid is 3:1; In step 7), the addition of property-modifying additive is 1/8 times of deionized water weight; The addition of hydrogen agent of disappearing in step 8) is 1/11 times of deionized water weight.
Embodiment 4
Each step is with embodiment 1; Wherein, in step 1), the temperature of phosphoric acid is that 75 DEG C, phosphoric acid concentration are 0.8%, boost current density 0.15mA/CV, voltage are capacitor rated voltage 1.8 times; Step 2) in heat treatment temperature be 340 DEG C, heat treatment time 50 minutes; In step 4), the temperature of electrolyte is that 170 DEG C, electrochemical treatments time are that 1.8 hours, voltage are 1.2 times of capacitor rated voltage, and in electrolyte, phosphoric acid concentration is 13%, glycol concentration is 58% in electrolyte, and all the other are water; In step 7), the addition of property-modifying additive is that 1/9 times of deionized water weight, property-modifying additive are formulated by two kinds in ethylene glycol, EGME, sweet mellow wine, the succinic acid volume ratios by 1:1; The addition of hydrogen agent of disappearing in step 8) is that 1/10 times of deionized water weight, the hydrogen agent that disappears are formulated by two kinds in paranitrobenzoic acid ammonium, p-nitrophenol, the p-nitrophenyl methyl alcohol volume ratios by 1:1.5.
Embodiment 5
Each step is with embodiment 1; Wherein, the phosphoric acid temperature in step 1) is that 85 DEG C, phosphoric acid concentration are 0.3%, boost current density is that 0.5mA/CV, voltage are 1.6 times of capacitor rated voltage; Step 2) in heat treatment temperature be 370 DEG C, heat treatment time 30 minutes; In step 4), the temperature of electrolyte is that 175 DEG C, electrochemical treatments time are that 1.2 hours, voltage are 1.3 times of capacitor rated voltage, and in electrolyte, phosphoric acid concentration is 4%, glycol concentration is 66% in electrolyte, and all the other are water; In step 7), the addition of property-modifying additive is that 1/8 times of deionized water weight, property-modifying additive are formulated by two kinds in ethylene glycol, EGME, sweet mellow wine, the succinic acid volume ratios by 1:1.5; The addition of hydrogen agent of disappearing in step 8) is that 1/14 times of deionized water weight, the hydrogen agent that disappears are formulated by two kinds in paranitrobenzoic acid ammonium, p-nitrophenol, the p-nitrophenyl methyl alcohol volume ratios by 1:1.
Embodiment 6
Each step is with embodiment 4; Wherein, the property-modifying additive in step 7) is the one in ethylene glycol, EGME, sweet mellow wine, succinic acid; The addition of hydrogen agent of disappearing in step 8) is 1/13 times of deionized water weight, and the hydrogen agent that disappears is formulated by 1:1.2 volume ratio by two kinds in paranitrobenzoic acid ammonium, p-nitrophenol, p-nitrophenyl methyl alcohol.
Embodiment 7
Each step is with embodiment 4; Wherein, it is formulated that the property-modifying additive in step 7) is pressed 1:1.3 volume ratio by two kinds in ethylene glycol, EGME, sweet mellow wine, succinic acid, and the hydrogen agent that disappears in step 8) is the one in paranitrobenzoic acid ammonium, p-nitrophenol, p-nitrophenyl methyl alcohol.
Claims (3)
1. a preparation method for high temperature resistant capacitor, is included in anode tantalum piece surface and prepares dielectric oxide film, electrolyte preparation, capacitor assembling; It is characterized in that concrete steps are as follows:
1) in the phosphoric acid that is 0.1～1% by 70～90 DEG C of anode tantalum piece immersions, concentration expressed in percentage by volume, carry out electrochemical treatments, by the boost current density of 0.06～0.65mA/CV, voltage is risen to 1.5～1.9 times of capacitor rated voltage;
2) the anode tantalum piece through electrochemical treatments is cleaned, dried, putting into vacuum is 2x10-3Torr is above, temperature is heat treatment 20～60 minutes in the vacuum drying oven of 320～380 DEG C;
3) be that 38% sulfuric acid soaks 30 minutes by be placed in mass percent concentration through heat treated anode tantalum piece;
4) in the electrolyte that the anode tantalum piece that soaks through persulfuric acid to be immersed to temperature be 160～180 DEG C, mixed by phosphoric acid and ethylene glycol, carry out electrochemical treatments 1～2 hour, apply voltage and be 1.1～1.4 times of capacitor rated voltage; In described electrolyte, the concentration of volume percent of phosphoric acid is 1～15%, the concentration of volume percent of ethylene glycol solution is 50～70%, and all the other are water;
5) the anode tantalum piece through electrochemical treatments is for the second time cleaned to dry for standby;
6) sulfuric acid that is 98% by deionized water with mass percent concentration mixes by the volume ratio of 4:1～2:1, is mixed with aqueous sulfuric acid;
7) to the property-modifying additive that adds 1/10～1/7 times of weight deionized water in described aqueous sulfuric acid, be mixed with mixed solution; Described property-modifying additive is the one in ethylene glycol, EGME, sweet mellow wine, succinic acid, or formulated by two kinds of volume ratios of pressing 1:1～1:1.5 in ethylene glycol, EGME, sweet mellow wine, succinic acid;
8) to the hydrogen agent that disappears that adds 1/15～1/9 times of weight deionized water in above-mentioned mixed solution, make electrolyte; The described hydrogen agent that disappears is the one in paranitrobenzoic acid ammonium, p-nitrophenol, p-nitrophenyl methyl alcohol, or formulated by two kinds of volume ratios of pressing 1:1～1:1.5 in paranitrobenzoic acid ammonium, p-nitrophenol, p-nitrophenyl methyl alcohol;
9) described electrolyte and anode tantalum piece for subsequent use are packaged in shell, make capacitor.
2. the preparation method of high temperature resistant capacitor according to claim 1, is characterized in that: in step 1), phosphoric acid temperature is that 80 DEG C, phosphoric acid concentration are 0.5%, boost current density is that 0.35mA/CV, voltage are 1.7 times of capacitor rated voltage; Step 2) in heat treatment temperature be that 360 DEG C, heat treatment time are 45 minutes, in step 4), the temperature of electrolyte is that in 175 DEG C, electrolyte, the concentration of phosphoric acid is 8.5%, the concentration of ethylene glycol is 62%, the electrochemistry time is that 1.5 hours, voltage are 1.2 times of capacitor rated voltage.
3. the preparation method of high temperature resistant capacitor according to claim 1, it is characterized in that: in step 6), the ratio of deionized water and sulfuric acid is 3:1, in step 7), the addition of property-modifying additive is 1/8 times of deionized water, and the addition of the hydrogen agent that disappears in step 8) is 1/11 times of deionized water.
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| CN103985545B (en) * | 2014-04-28 | 2017-02-15 | 中国振华（集团）新云电子元器件有限责任公司 | Method for heat treatment of high-pressure tantalum electrolytic condenser anode film |
| CN104008899B (en) * | 2014-05-12 | 2016-09-07 | 中国振华（集团）新云电子元器件有限责任公司 | A kind of high energy width temperature tantalum capacitor preparation method |
| CN104517734A (en) * | 2014-12-01 | 2015-04-15 | 益阳家鑫电子科技有限公司 | Working electrolyte and preparation method thereof of high-temperature resistant aluminum electrolytic capacitor |
| CN105304330A (en) * | 2015-11-03 | 2016-02-03 | 铜陵市科峰电子有限责任公司 | Heat-resisting aluminum electrolytic capacitor and preparation method thereof |
| CN106206018B (en) * | 2016-06-27 | 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 electrolytic capacitor is electrochemically formed device systems |
| CN107665773A (en) * | 2017-07-27 | 2018-02-06 | 李勇 | A kind of high pressure resistant resistant to elevated temperatures electrolyte |
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| CN101373665A (en) * | 2007-08-23 | 2009-02-25 | 南通瑞达电子材料有限公司 | Long-life working electrolyte for electrolytic capacitor |
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| JPS6015304A (en) * | 1983-07-04 | 1985-01-26 | Sumitomo Electric Ind Ltd | Supply chute for legged parts of unusual shape |
| JPH11150041A (en) * | 1997-11-19 | 1999-06-02 | Hitachi Aic Inc | Manufacture of solid electrolytic capacitor |
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| CN101243212A (en) * | 2005-08-18 | 2008-08-13 | 昭和电工株式会社 | Method for chemical conversion treatment of valve action metal material |
| CN101373665A (en) * | 2007-08-23 | 2009-02-25 | 南通瑞达电子材料有限公司 | Long-life working electrolyte for electrolytic capacitor |
| 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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