CN102394180B - Method for manufacturing chip type organic solid electrolyte electrolytic capacitor - Google Patents
Method for manufacturing chip type organic solid electrolyte electrolytic capacitor Download PDFInfo
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- CN102394180B CN102394180B CN201110199357.3A CN201110199357A CN102394180B CN 102394180 B CN102394180 B CN 102394180B CN 201110199357 A CN201110199357 A CN 201110199357A CN 102394180 B CN102394180 B CN 102394180B
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Abstract
The invention discloses a method for manufacturing a chip type organic solid electrolyte electrolytic capacitor. The method comprises the steps of preparing an anode body; preparing a dielectric oxidation film; and preparing a polymer cathode structure. The method is characterized in that the cathode of the chip type organic solid electrolyte electrolytic capacitor is obtained by employing an electrostatic self-assembling method; and by alternately assembling polyelectrolyte with reverse charges on the surface of the dielectric oxidation film in a solution, an electroconductive polymer composite polyelectrolyte is further stably structured as a cathode film of the chip type organic solid electrolyte electrolytic capacitor. By employing the manufacturing method provided by the invention, the obtained chip type organic solid electrolyte electrolytic capacitor has the characteristics of low equivalent series resistance and favorable voltage withstand property. The method can be used for manufacturing other capacitors or electronic elements.
Description
Technical field
The present invention relates to electronic material and field of electrical components, be specifically related to the preparation method of conducting polymer composite polyelectrolyte as chip capacitor negative electrode.
Background technology
Along with the requirement of electronic product high performance, the high frequency characteristics that an urgent demand improves the performance of sheet type electrolytic capacitor, particularly product is the ESR value of product.Wherein the conductance of solid electrolyte all has a significant impact internal resistance, leakage current and high frequency characteristics.Organic polymer using conducting polymer as representative as solid electrolyte (conductance is at 1 ~ 500s/cm) than traditional chip-type solid tantalum electrolytic capacitor cathode material MnO
2(conductance is 0.1s/cm) has lower resistance, can show good high frequency characteristics.Therefore in recent years, people conduct extensive research as solid electrolyte the conducting polymer such as polypyrrole, polyaniline, in clear 4-56445 patent, deliver take polypyrrole as electrolytical solid aluminum electrolytic capacitor production technology, in clear 62-29124 patent, delivered with polyaniline and form electrolytical solid aluminum electrolytic capacitor production technology after aryl sulfonic acid doping.At present, the company such as external KEMET, AVX has occurred that some prepare chip organic solid electrolytic capacitor by the technique of chemical in-situ deposition conducting polymer thin film.But the method for chemical in-situ deposition is owing to having introduced oxidant, oxidant ion can be in the fault location accumulation of thin dielectric film, the withstand voltage properties of deteriorated thin dielectric film, thus cause the voltage endurance capability of the capacitor obtaining poor, and the rated operational voltage of capacitor cannot improve.
Conductive polymer poly 3,4-vinyl dioxy thiophene/polystyrolsulfon acid (PEDOT/PSS) has higher conductivity, good aqueous solution dispersiveness and photo and thermal stability.Because it is the conducting polymer polyelectrolyte after polymerization, therefore solution state is controlled; In addition, because polyelectrolyte polystyrolsulfon acid (PSS) can ionize and make PEDOT/PSS electronegative in solution, thereby make this material there is stable electrostatic self-assembled ability.For electrolytic capacitor, owing to not needing oxidant just the PEDOT/PSS of good conductivity can be assembled into electrode film, therefore greatly reduce the impact of oxidant on dielectric film, can effectively improve the voltage endurance capability of organic solid electrolytic capacitor, improve the reliability of product; In addition, it is simpler that the technique of employing electrostatic self-assembled is prepared capacitor cathode, and the production cycle is shorter.
Summary of the invention
Technical problem to be solved by this invention is the preparation method how a kind of chip type organic solid electrolyte electrolytic capacitor is provided, the prepared conducting polymer composite polyelectrolyte of the method has overcome existing defect in prior art as chip capacitor negative electrode, eliminate the impact of oxidant ion pair dielectric oxide film, and preparation method is rationally simple, easy operating.
Technical problem proposed by the invention is to solve like this: the anode and the dielectric oxide film that first obtain capacitor by compressing and electrochemical method, then coating conducting polymer composite polyelectrolyte is as negative electrode on dielectric oxide film for the method by electrostatic self-assembled, and finally on conducting polymer composite polyelectrolyte, coating graphite and silver slurry obtain chip type organic solid electrolyte electrolytic capacitor.
Concrete steps are as follows:
1. by metal dust briquet, form capacitor body block;
2. by compressing capacitor body block high temperature sintering in vacuum sintering furnace, obtain the capacitor body block that has some strength;
3. in acid solution, on the capacitor body block 2. obtaining, form dielectric oxide film by electrochemical oxidation method;
4. by cationic polyelectrolyte and the water-soluble solution of conductivity anionic polyelectrolyte difference, 3. the capacitor body block obtaining be impregnated in respectively in said polycation solution and polyanion solution, repeatedly, obtain conducting polymer composite polyelectrolyte as capacitor cathode;
5. by the capacitor body impregnated graphite emulsion 4. obtaining;
6. by the capacitor body impregnated silver pulp 5. obtaining, obtain chip type organic solid electrolyte electrolytic capacitor.
Described metal dust comprises that the specific volume such as tantalum, nickel is the metal of 3000 ~ 70000 μ F.V/g.
Described acid solution is the acid solution after water-soluble such as phosphoric acid, nitric acid, citric acid.
Polycation material be in the aqueous solution ionogenic polyelectrolyte as PDDA (PDDA), polypropylene amine (PAH) etc.
Polyanion material be electric conductive polymer and in the aqueous solution ionogenic polyelectrolyte as poly-3,4-vinyl dioxy thiophene/polystyrolsulfon acid (PEDOT/PSS) etc.
By controlling polycation and the concentration of polyanion and the number of times of dipping, can regulate and control to conducting polymer composite polyelectrolyte the effectively cathode thin film thickness of control capacitor, and then the equivalent series resistance of control capacitor as cathode thin film.
Further, detailed step is as follows:
1. ta powder and tantalum wire are pressed into tantalum piece fuse, tantalum wire insertion depth is 1/3 of tantalum tile height;
2. in the vacuum sintering furnace of 1100-1300 ℃, sinter the tantalum piece fuse 1. obtaining the tantalum piece fuse with some strength into;
3. the tantalum piece fuse 2. obtaining is placed in to 8 ‰ phosphate aqueous solution, adopts electrochemical method to form dielectric oxide film Ta in tantalum piece core surface
2o
5;
4. compound concentration is 1g/ml(A liquid), 5g/ml(B liquid) the PDDA aqueous solution; Configuration concentration is 1.5g/ml(C liquid), 3.5g/ml(D liquid) poly-3,4-vinyl dioxy thiophene/polystyrolsulfon acid;
5. 130 ℃ of oven dry after the tantalum piece fuse 3. obtaining first being flooded to 5min in A liquid, then in B liquid, flood 10min in rear 130 ℃ of oven dry be a circulation, repetitive operation 5-8 time;
6. by 5. obtain tantalum piece fuse in C liquid, flood 5min after 130 ℃ of oven dry, then in D liquid, flood 10min in rear 130 ℃ of oven dry be a circulation, repetitive operation 4-6 time, obtains certain thickness conducting polymer composite polyelectrolyte as capacitor cathode;
7. by the tantalum piece fuse impregnated graphite emulsion 6. obtaining, then 180 ℃ of oven dry;
8. by the tantalum piece fuse impregnated silver pulp 7. obtaining, then 180 ℃ of oven dry, obtain the chip type organic solid electrolyte tantalum electrolytic capacitor of conducting polymer composite polyelectrolyte as capacitor cathode.
The preparation method of chip type organic solid electrolyte electrolytic capacitor provided by the present invention, polycation material used is water-soluble ionogenic polymer dielectric, range of choice is wide.Polyanion material is for having the ionogenic polymer dielectric of electric conductivity, be generally the conducting polymer of polyanion of having adulterated.In the process of assembling chip capacitor cathode thin film, owing to not introducing oxidant and eliminated the impact of oxidant ion pair dielectric oxide film, greatly improve the voltage endurance capability of capacitor.In assembling process, can realize the good control to polymer electrolyte film thickness, the simple easy operating of technique by the state of adjusting poly-yin, yang solion.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that obtains chip type organic solid electrolyte electrolytic capacitor.In figure 6, tantalum wire, 7, deposited the capacitor body of dielectric oxide film, 8, said polycation solution, 9, polyanion solution;
Fig. 2 is the structural representation of chip type organic solid electrolyte electrolytic capacitor obtaining, in figure 1, metal, and 2, dielectric oxide film, 3, conductive poly electrolyte complex film, 4, graphite, 5, silver slurry, 6, tantalum wire.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is further illustrated.
The invention provides a kind of preparation method of chip type organic solid electrolyte electrolytic capacitor, first obtain anode and the dielectric oxide film of capacitor by compressing and electrochemical method, then coating conducting polymer composite polyelectrolyte is as negative electrode on dielectric oxide film for the method by electrostatic self-assembled, and finally on conducting polymer composite polyelectrolyte, coating graphite and silver slurry obtain chip type organic solid electrolyte electrolytic capacitor.Constructing by the statcoulomb active force between polycation material and conductive poly anionic materials of chip-type solid electrolyte electrolytic capacitor negative electrode, using the stable structure conducting polymer composite electrolyte film of the method for alternating deposit as capacitor cathode, because the thickness of dielectric film is controlled, the equivalent series resistance of capacitor also can need to regulate and control according to difference.Conducting polymer composite electrolyte film and dielectric film have good adhesion property.Polycation material is the polymer dielectric that can ionize in the aqueous solution, as PDDA, polypropylene amine etc.Polyanion is to have the conducting polymer doping polyanion material of excellent conductive performance as poly-3,4-vinyl dioxy thiophene/polystyrolsulfon acid.The state of poly-yin, yang ionic material in the aqueous solution can regulate and control by solution concentration, pH value etc., can adjust for the surface state of different medium oxide-film the assembling process of composites polymer electrolytes.
Fig. 1 is the schematic diagram that obtains chip type organic solid electrolyte electrolytic capacitor.In figure 6, tantalum wire, 7, deposited the capacitor body of dielectric oxide film, 8, said polycation solution, 9, polyanion solution;
Fig. 2 is the structural representation of chip type organic solid electrolyte electrolytic capacitor obtaining, in figure 1, metal, and 2, dielectric oxide film, 3, conductive poly electrolyte complex film, 4, graphite, 5, silver slurry, 6, tantalum wire.
Feature of the present invention is to construct the cathode thin film of sheet type electrolytic capacitor by the mode of electrostatic self-assembled, rely on electrostatic interaction between poly-yin, yang ion effectively controlled obtain fine and close, electrolytic thin-membrane uniformly in cavernous capacitor core sub-surface.Owing to having overcome the defect of conventional method, in the process of preparing cathode thin film, do not introduce oxidant, effectively prevent the bad effect of oxidant ion pair condenser dielectric film, greatly improve the withstand voltage properties of capacitor.Meanwhile, the thickness of cathode thin film can be realized by the adjustment to solution state, and then the equivalent series resistance of the chip type organic solid electrolyte electrolytic capacitor obtaining is carried out to Effective Regulation.
The conductive poly anionic polymer of selecting in the present invention need to have higher electric conductivity and good filming performance, and has good photo-thermal and moisture-proof stability, can effectively deposit in cavernous capacitor core sub-surface.
Rely on ripe electrostatic self-assembled method, chip type organic solid electrolyte electrolytic capacitor prepared by the present invention can be realized low ESR, higher withstand voltage properties.
Some capacitors that adopt the present invention to prepare are exemplified below:
1. conducting polymer composite electrolyte sheet type tantalum electrolyte capacitor;
2. conducting polymer composite electrolyte chip nickel electrowinning capacitor;
Below specific embodiments of the invention:
embodiment 1
Tantalum powder is compressed to tantalum piece by certain pressed density, the tantalum piece of acquisition is carried out in vacuum sintering furnace to the tantalum piece fuse of sintering acquisition some strength, now tantalum piece fuse state is spongiform sintered porous state; Then the tantalum piece after sintering is formed to Ta in acidic aqueous solution
2o
5dielectric oxide film, oxide-film is as the dielectric layer of organic sheet type electrolytic capacitor; Flooding in said polycation solution and polyanion solution that the tantalum piece fuse that has formed dielectric oxide film is replaced repeatedly obtains the negative electrode of certain thickness conducting polymer composite polyelectrolyte as sheet type electrolytic capacitor afterwards; Finally by coating the capacitor body of negative electrode respectively impregnated graphite and silver slurry obtain chip type organic solid electrolyte tantalum electrolytic capacitor.
In Fig. 2, the 3rd, the electric conductive polymer dielectric substrate that adopts electrostatic self-assembled method to obtain, it is as the cathode layer of sheet type electrolytic capacitor.
Concrete preparation method is as follows:
1. the tantalum powder that by specific volume is 70000 μ F.V/g is compressed to block fuse, and block fuse is of a size of 1.6mm × 2.3mm × 2.8mm;
2. the tantalum piece fuse 1. obtaining is carried out in 1250 ℃ of vacuum sintering furnaces to the tantalum piece fuse of sintering acquisition some strength.
3. the tantalum piece fuse 2. obtaining is placed in to 8 ‰ phosphate aqueous solution, adopts electrochemical method to form dielectric oxide film Ta in tantalum piece core surface
2o
5, formation voltage is 32V, after forming, the wet survey capacity of capacitor is 470 μ F.
4. compound concentration is 1g/ml(A liquid), 5g/ml(B liquid) PDDA (PDDA) aqueous solution; Configuration concentration is 1.5g/ml(C liquid), 3.5g/ml(D liquid) poly-3,4-vinyl dioxy thiophene/polystyrolsulfon acid (PEDOT/PSS);
5. 130 ℃ of oven dry after the tantalum piece fuse 3. obtaining first being flooded to 5min in A liquid, then in B liquid, flood 10min in rear 130 ℃ of oven dry be a circulation, repetitive operation 5 times;
6. 130 ℃ of oven dry after the tantalum piece fuse 5. obtaining being flooded to 5min in C liquid, then in flooding 10min in D liquid, rear 130 ℃ of oven dry are a circulation, repetitive operation 5 times, obtains certain thickness conducting polymer composite polyelectrolyte (PDDA/PEDOT-PSS) as capacitor cathode;
7. by the tantalum piece fuse impregnated graphite emulsion 6. obtaining, then 180 ℃ of oven dry;
8. by the tantalum piece fuse impregnated silver pulp 7. obtaining, then 180 ℃ of oven dry, obtain the chip type organic solid electrolyte tantalum electrolytic capacitor of conducting polymer composite polyelectrolyte as capacitor cathode.
Obtaining chip type organic solid electrolyte tantalum electrolytic capacitor basic parameter is: rated voltage: 10V; Capacity: 465 μ F; Equivalent series resistance: 36m Ω; Leakage current (12V survey): 28 μ A.
As shown in Figure 1, the preparation flow of capacitor is similar to execution mode one, and the 3. formation voltage in execution mode becomes 38V.
Obtaining chip type organic solid electrolyte tantalum electrolytic capacitor basic parameter is: rated voltage: 10V; Capacity: 337 μ F; Equivalent series resistance: 40m Ω; Leakage current (12V survey): 26 μ A.
embodiment 3
As shown in Figure 1, the preparation flow of capacitor is similar to execution mode one, and the 5. cycle-index in execution mode is 7 times, and the 6. cycle-index in execution mode is 6 times.
Obtaining chip type organic solid electrolyte tantalum electrolytic capacitor basic parameter is: rated voltage: 10V; Capacity: 468 μ F; Equivalent series resistance: 55m Ω; Leakage current (12V survey): 12 μ A.Due to the adjustment of cathode thin film thickness, it is large that capacitor equivalent series resistance becomes.
embodiment 4
As shown in Figure 1, the preparation flow of capacitor is similar to execution mode one, and the 5. cycle-index in execution mode is 5 times, and the 6. cycle-index in execution mode is 4 times.
Obtaining chip type organic solid electrolyte tantalum electrolytic capacitor basic parameter is: rated voltage: 10V; Capacity: 463 μ F; Equivalent series resistance: 30m Ω; Leakage current (12V survey): 32 μ A.Due to the adjustment of cathode thin film thickness, capacitor equivalent series resistance diminishes.
embodiment 5
As shown in Figure 1, the preparation flow of capacitor is similar to execution mode one, and the material 1. in execution mode is niobium powder.Owing to adopting niobium as capacitor matrix metal, what therefore obtain is chip type organic solid electrolyte niobium electrolytic capacitor.
Obtaining chip type organic solid electrolyte niobium electrolytic capacitor basic parameter is: rated voltage: 10V; Capacity: 469 μ F; Equivalent series resistance: 32m Ω; Leakage current (12V survey): 38 μ A.
Claims (1)
1. the preparation method of a chip type organic solid electrolyte electrolytic capacitor, first obtain anode and the dielectric oxide film of capacitor by compressing and electrochemical method, then the method by electrostatic self-assembled on dielectric oxide film coating conducting polymer composite polyelectrolyte as negative electrode, finally on conducting polymer composite polyelectrolyte, coating graphite and silver slurry obtain chip type organic solid electrolyte electrolytic capacitor, it is characterized in that, concrete steps are as follows:
1. by metal dust briquet, form capacitor block fuse;
2. by the capacitor block fuse high temperature sintering in vacuum sintering furnace 1. obtaining, obtain the capacitor block fuse that has some strength;
3. in acid solution, on the capacitor block fuse 2. obtaining, form dielectric oxide film by electrochemical oxidation method;
4. by cationic polyelectrolyte and the water-soluble solution of conductivity anionic polyelectrolyte difference, form said polycation solution and conductive poly anion solutions, 3. the capacitor block fuse obtaining be impregnated in respectively in said polycation solution and conductive poly anion solutions, repeatedly, obtain conducting polymer composite polyelectrolyte as capacitor cathode;
5. by the capacitor block fuse impregnated graphite emulsion 4. obtaining;
6. by the capacitor block fuse impregnated silver pulp 5. obtaining, obtain chip type organic solid electrolyte electrolytic capacitor;
Further, its detailed step is as follows:
1. ta powder and tantalum wire are pressed into tantalum piece fuse, tantalum wire insertion depth is 1/3 of tantalum tile height;
2. in the vacuum sintering furnace of 1100-1300 ℃, sinter the tantalum piece fuse 1. obtaining the tantalum piece fuse with some strength into;
3. the tantalum piece fuse 2. obtaining is placed in to 8 ‰ phosphate aqueous solution, adopts electrochemical method to form dielectric oxide film Ta in tantalum piece core surface
2o
5;
4. compound concentration is the PDDA aqueous solution of 1g/ml, 5g/ml; Configuration concentration is poly-3,4-vinyl dioxy thiophene/polystyrolsulfon acid of 1.5g/ml, 3.5g/ml;
5. 130 ℃ of oven dry after flooding 5min in the PDDA aqueous solution that is first 1g/ml in concentration by the tantalum piece fuse 3. obtaining, then in flooding 10min in the PDDA aqueous solution that is 5g/ml in concentration, rear 130 ℃ of oven dry are a circulation, repetitive operation 5-8 time;
What be 6. 1.5g/ml by the tantalum piece fuse 5. obtaining in concentration gathers 3, in 4-vinyl dioxy thiophene/polystyrolsulfon acid solution, flood 130 ℃ of oven dry after 5min, what be then 3.5g/ml in concentration gathers 3, in 4-vinyl dioxy thiophene/polystyrolsulfon acid solution, flooding rear 130 ℃ of oven dry in 10min is a circulation, repetitive operation 4-6 time, obtains certain thickness conducting polymer composite polyelectrolyte as capacitor cathode;
7. by the tantalum piece fuse impregnated graphite emulsion 6. obtaining, then 180 ℃ of oven dry;
8. by the tantalum piece fuse impregnated silver pulp 7. obtaining, then 180 ℃ of oven dry, obtain the chip type organic solid electrolyte tantalum electrolytic capacitor of conducting polymer composite polyelectrolyte as capacitor cathode.
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| CN102637535B (en) * | 2012-04-16 | 2016-04-27 | 南通江海电容器股份有限公司 | A kind of preparation method of solid electrolytic capacitor of high voltage large capcity |
| CN102709052B (en) * | 2012-06-21 | 2016-08-17 | 电子科技大学 | A kind of method manufacturing nano capacitor |
| WO2019171905A1 (en) * | 2018-03-06 | 2019-09-12 | 住友電気工業株式会社 | Cell structure |
| CN112201482B (en) * | 2020-09-18 | 2021-09-03 | 同济大学 | Super capacitor based on heterojunction polymer gel electrolyte and preparation method thereof |
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| CN101404214A (en) * | 2008-11-18 | 2009-04-08 | 北京七一八友益电子有限责任公司 | Polymer solid sheet type tantalum electrolyte capacitor and its manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101404214A (en) * | 2008-11-18 | 2009-04-08 | 北京七一八友益电子有限责任公司 | Polymer solid sheet type tantalum electrolyte capacitor and its manufacturing method |
Non-Patent Citations (2)
| Title |
|---|
| 《Layer-by-layer assembly of poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)》;Rachel R.Smith et al.;《Macromolecules》;20060815;第39卷(第18期);第6071-6073页 * |
| RachelR.Smithetal..《Layer-by-layerassemblyofpoly(3 4-ethylenedioxythiophene):poly(styrenesulfonate)》.《Macromolecules》.2006 |
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