CN102394180A - 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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- CN102394180A CN102394180A CN2011101993573A CN201110199357A CN102394180A CN 102394180 A CN102394180 A CN 102394180A CN 2011101993573 A CN2011101993573 A CN 2011101993573A CN 201110199357 A CN201110199357 A CN 201110199357A CN 102394180 A CN102394180 A CN 102394180A
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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 the compound polyelectrolyte of conducting polymer as the 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 very big influence to internal resistance, leakage current and high frequency characteristics.With the conducting polymer be representative organic polymer as solid electrolyte (conductance 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 have carried out extensive studies to conducting polymers such as polypyrrole, polyanilines as solid electrolyte; Having delivered with polypyrrole in the clear 4-56445 patent is electrolytical solid aluminum electrolytic capacitor production technology, in clear 62-29124 patent, has delivered with polyaniline and after aryl sulfonic acid mixes, has formed electrolytical solid aluminum electrolytic capacitor production technology.At present, companies such as external KEMET, AVX some technologies through chemical in-situ deposition conducting polymer thin film occurred and have prepared chip organic solid electrolytic capacitor.But the method for chemical in-situ deposition is owing to introduced oxidant; The oxidant ion can be in the fault location accumulation of thin dielectric film; The withstand voltage properties of deterioration thin dielectric film, thus the voltage endurance capability of the capacitor that causes obtaining is relatively poor, and the rated operational voltage of capacitor can't improve.
Conductive polymer poly 3,4-vinyl dioxy thiophene/polystyrolsulfon acid (PEDOT/PSS) have higher conductivity, good aqueous solution dispersiveness and photo and thermal stability.Because it is the conducting polymer polyelectrolyte after the polymerization, so solution state is controlled; In addition, because polyelectrolyte polystyrolsulfon acid (PSS) can ionization make PEDOT/PSS electronegative in solution, thereby make this material have stable static self assembly ability.For electrolytic capacitor; Owing to do not need oxidant just can the PEDOT/PSS of good conductivity be assembled into electrode film; Therefore greatly reduce the influence of oxidant, can effectively improve the voltage endurance capability of organic solid electrolytic capacitor, improve reliability of products dielectric film; In addition, it is simpler that the technology of employing static self assembly prepares 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 organic solid electrolyte based electrolytic capacitor is provided; The prepared compound polyelectrolyte of conducting polymer of this method has overcome existing defective in the prior art as the chip capacitor negative electrode; Eliminated the influence of oxidant ion pair dielectric oxide film; And the 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 at first obtain capacitor through compression moulding and electrochemical method; Method through the static self assembly is covered the compound polyelectrolyte of conducting polymer as negative electrode on dielectric oxide film then, and lining graphite obtains chip organic solid electrolyte based electrolytic capacitor with the silver slurry on the compound polyelectrolyte of conducting polymer at last.
Concrete steps are following:
1. with the metal dust briquet, form the capacitor body block;
2. with capacitor body block high temperature sintering in vacuum sintering furnace of compression moulding, obtain to have the capacitor body block of certain intensity;
3. in acid solution, on the capacitor body block that 2. obtains, form dielectric oxide film through electrochemical oxidation method;
4. with in cationic polyelectrolyte and the water-soluble solution of conductivity anionic polyelectrolyte difference; 3. the capacitor body block that obtains impregnated in respectively in said polycation solution and the polyanion solution; Repeat repeatedly, obtain the compound polyelectrolyte of conducting polymer as capacitor cathode;
The capacitor body impregnated graphite emulsion that 5. will 4. obtain;
The capacitor body impregnated silver pulp that 6. will 5. obtain obtains chip organic solid electrolyte based electrolytic capacitor.
Said metal dust comprises that specific volumes such as tantalum, nickel are the metal of 3000 ~ 70000 μ F.V/g.
Said acid solution is the acid solution after water-soluble such as phosphoric acid, nitric acid, citric acid.
The polycation material be in the aqueous solution ionogenic polyelectrolyte like PDDA (PDDA), polypropylene amine (PAH) etc.
The polyanion material be electric conductive polymer and in the aqueous solution ionogenic polyelectrolyte as: gather 3,4-vinyl dioxy thiophene/polystyrolsulfon acid (PEDOT/PSS) etc.
Through control polycation and the concentration of polyanion and the number of times of dipping, can regulate and control the effectively cathode thin film thickness of control capacitance device, and then the equivalent series resistance of control capacitance device as cathode thin film to the compound polyelectrolyte of conducting polymer.
Further, detailed step is following:
1. ta powder and tantalum wire are pressed into tantalum piece fuse, the tantalum wire insertion depth is 1/3 of a tantalum tile height;
The tantalum piece fuse that 2. will 1. obtain sinters the tantalum piece fuse with certain intensity in 1100-1300 ℃ vacuum sintering furnace;
The tantalum piece fuse that 3. will 2. obtain places 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 (A liquid), 5g/ml (B liquid); Configuration concentration be 1.5g/ml (C liquid), 3.5g/ml (D liquid) gather 3,4-vinyl dioxy thiophene/polystyrolsulfon acid;
The tantalum piece fuse that 5. will 3. obtain 130 ℃ of oven dry behind the dipping 5min in A liquid earlier, then in B liquid among the dipping 10min back 130 ℃ of oven dry be a circulation, repetitive operation 5-8 time;
The tantalum piece fuse that 6. will 5. obtain floods 130 ℃ of oven dry behind the 5min in C liquid, then in D liquid among the dipping 10min back 130 ℃ of oven dry be a circulation, repetitive operation 4-6 time obtains the compound polyelectrolyte of certain thickness conducting polymer as capacitor cathode;
The tantalum piece fuse impregnated graphite emulsion that 7. will 6. obtain is then 180 ℃ of oven dry;
The tantalum piece fuse impregnated silver pulp that 8. will 7. obtain then 180 ℃ of oven dry, obtains the chip organic solid electrolyte based tantalum electrolytic capacitor of the compound polyelectrolyte of conducting polymer as capacitor cathode.
The preparation method of chip organic solid electrolyte based electrolytic capacitor provided by the present invention, used polycation material is water-soluble ionogenic polymer dielectric, range of choice is wide.The polyanion material is for having the ionogenic polymer dielectric of electric conductivity, be generally the conducting polymer of polyanion of having mixed.In the process of assembling chip capacitor cathode thin film, do not eliminated the influence of oxidant ion pair dielectric oxide film owing to introducing oxidant, improved the voltage endurance capability of capacitor greatly.Can realize excellent control, the simple easy operating of technology through the state that adjustment gathers the yin, yang solion in the assembling process to polymer electrolyte film thickness.
Description of drawings
Fig. 1 is the schematic diagram that obtains chip organic solid electrolyte based electrolytic capacitor.Among the 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 the chip organic solid electrolyte based electrolytic capacitor that obtains, among the figure 1, metal, and 2, dielectric oxide film, 3, the conductive poly electrolyte complex film, 4, graphite, 5, the silver slurry, 6, tantalum wire.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
The invention provides a kind of preparation method of chip organic solid electrolyte based electrolytic capacitor; At first obtain the anode and the dielectric oxide film of capacitor through compression moulding and electrochemical method; Method through the static self assembly is covered the compound polyelectrolyte of conducting polymer as negative electrode on dielectric oxide film then, and lining graphite obtains chip organic solid electrolyte based electrolytic capacitor with the silver slurry on the compound polyelectrolyte of conducting polymer at last.Constructing of chip-type solid electrolyte electrolytic capacitor cathode through the statcoulomb active force between polycation material and the conductive poly anionic materials; With the stable structure conducting polymer composite electrolyte film of the method for alternating deposit as capacitor cathode; Because the controllable thickness of dielectric film, the equivalent series resistance of capacitor also can be regulated and control according to different needs.Conducting polymer composite electrolyte film and dielectric film have good adhesion property.The polycation material be can ionization in the aqueous solution polymer dielectric, like PDDA, polypropylene amine etc.Polyanion is to have the conducting polymer doping polyanion material of excellent conductive performance as gathering 3,4-vinyl dioxy thiophene/polystyrolsulfon acid.Gathering the state of yin, yang ionic material in the aqueous solution can wait through solution concentration, pH value, can adjust the assembling process of polymer composite electrolyte to the surface state of different medium oxide-film.
Fig. 1 is the schematic diagram that obtains chip organic solid electrolyte based electrolytic capacitor.Among the 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 the chip organic solid electrolyte based electrolytic capacitor that obtains, among the figure 1, metal, and 2, dielectric oxide film, 3, the conductive poly electrolyte complex film, 4, graphite, 5, the silver slurry, 6, tantalum wire.
Characteristics of the present invention are to construct the cathode thin film of sheet type electrolytic capacitor through the mode of static self assembly, rely on the electrostatic interaction gather between the yin, yang ion effectively controlled obtain fine and close, electrolytic thin-membrane uniformly in cavernous capacitor core sub-surface.Owing to overcome the defective of conventional method, in the process of preparation cathode thin film, do not introduce oxidant, effectively prevented the deterioration effect of oxidant ion pair condenser dielectric film, improved the withstand voltage properties of capacitor greatly.Simultaneously, the thickness of cathode thin film can realize through the adjustment to solution state, and then the equivalent series resistance of the chip organic solid electrolyte based electrolytic capacitor that obtains is effectively regulated and control.
The conductive poly anionic polymer of selecting among the present invention needs higher electric conductivity and filming performance preferably, and has good photo-thermal and moisture-proof stability, can effectively deposit in cavernous capacitor core sub-surface.
Rely on ripe static self-assembling method, the chip organic solid electrolyte based electrolytic capacitor of the present invention's preparation can be realized low ESR, higher withstand voltage properties.
Adopt some capacitors of the present invention's preparation to be exemplified below:
1. conducting polymer composite electrolyte sheet type tantalum electrolyte capacitor;
2. conducting polymer composite electrolyte chip nickel electrowinning capacitor;
Below be specific embodiment of the present invention:
Embodiment 1
The tantalum powder is compressed to the tantalum piece by certain pressed density, the tantalum piece that obtains is carried out the tantalum piece fuse that sintering obtains certain intensity in vacuum sintering furnace, this moment, tantalum piece fuse state was spongiform sintered porous state; Then the tantalum piece behind the sintering is formed Ta in acidic aqueous solution
2O
5Dielectric oxide film, oxide-film is as the dielectric layer of organic sheet type electrolytic capacitor; The back of in said polycation solution and polyanion solution, flooding repeatedly that the tantalum piece fuse that has formed dielectric oxide film is replaced obtains the negative electrode of the compound polyelectrolyte of certain thickness conducting polymer as sheet type electrolytic capacitor; To be covered at last negative electrode capacitor body respectively impregnated graphite obtain chip organic solid electrolyte based tantalum electrolytic capacitor with the silver slurry.
In Fig. 2, the 3rd, the electric conductive polymer dielectric substrate that adopts the static self-assembling method to obtain, it is as the cathode layer of sheet type electrolytic capacitor.
Concrete preparation method is following:
1. be that the tantalum powder of 70000 μ F.V/g is compressed to block fuse with specific volume, the block fuse is of a size of 1.6mm * 2.3mm * 2.8mm;
The tantalum piece fuse that 2. will 1. obtain carries out the tantalum piece fuse that sintering obtains certain intensity in 1250 ℃ of vacuum sintering furnaces.
The tantalum piece fuse that 3. will 2. obtain places 8 ‰ phosphate aqueous solution, adopts electrochemical method to form dielectric oxide film Ta in tantalum piece core surface
2O
5, formation voltage is 32V, forming the wet survey capacity of back capacitor is 470 μ F.
4. compound concentration is PDDA (PDDA) aqueous solution of 1g/ml (A liquid), 5g/ml (B liquid); Configuration concentration be 1.5g/ml (C liquid), 3.5g/ml (D liquid) gather 3,4-vinyl dioxy thiophene/polystyrolsulfon acid (PEDOT/PSS);
The tantalum piece fuse that 5. will 3. obtain 130 ℃ of oven dry behind the dipping 5min in A liquid earlier, then in B liquid among the dipping 10min back 130 ℃ of oven dry be a circulation, repetitive operation 5 times;
The tantalum piece fuse that 6. will 5. obtain floods 130 ℃ of oven dry behind the 5min in C liquid; Then in D liquid the dipping 10min in back 130 ℃ of oven dry be a circulation; Repetitive operation 5 times obtains the compound polyelectrolyte of certain thickness conducting polymer (PDDA/PEDOT-PSS) as capacitor cathode;
The tantalum piece fuse impregnated graphite emulsion that 7. will 6. obtain is then 180 ℃ of oven dry;
The tantalum piece fuse impregnated silver pulp that 8. will 7. obtain then 180 ℃ of oven dry, obtains the chip organic solid electrolyte based tantalum electrolytic capacitor of the compound polyelectrolyte of conducting polymer as capacitor cathode.
Obtaining chip organic solid electrolyte based 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 with execution mode one, and the 3. formation voltage in the execution mode becomes 38V.
Obtaining chip organic solid electrolyte based 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 with execution mode one, and the 5. cycle-index in the execution mode is 7 times, and the 6. cycle-index in the execution mode is 6 times.
Obtaining chip organic solid electrolyte based 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.Because the adjustment of cathode thin film thickness, capacitor equivalent series resistance become big.
Embodiment 4
As shown in Figure 1, the preparation flow of capacitor is similar with execution mode one, and the 5. cycle-index in the execution mode is 5 times, and the 6. cycle-index in the execution mode is 4 times.
Obtaining chip organic solid electrolyte based 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.Because the adjustment of cathode thin film thickness, the capacitor equivalent series resistance diminishes.
Embodiment 5
As shown in Figure 1, the preparation flow of capacitor is similar with execution mode one, and the material 1. in the execution mode is the niobium powder.Because adopt niobium as the capacitor matrix metal, what therefore obtain is chip organic solid electrolyte based niobium electrolytic capacitor.
Obtaining chip organic solid electrolyte based 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 (10)
1. the preparation method of a chip organic solid electrolyte based electrolytic capacitor; It is characterized in that: the anode and the dielectric oxide film that at first obtain capacitor through compression moulding and electrochemical method; Method through the static self assembly is covered the compound polyelectrolyte of conducting polymer as negative electrode on dielectric oxide film then, and lining graphite obtains chip organic solid electrolyte based electrolytic capacitor with the silver slurry on the compound polyelectrolyte of conducting polymer at last.
2. the preparation method of chip organic solid electrolyte based electrolytic capacitor according to claim 1 is characterized in that concrete steps are following:
1. with the metal dust briquet, form capacitor block fuse;
Capacitor block fuse high temperature sintering in vacuum sintering furnace that 2. will 1. obtain, acquisition has the capacitor block fuse of certain intensity;
3. in acid solution, on the capacitor block fuse that 2. obtains, form dielectric oxide film through electrochemical oxidation method;
4. with in cationic polyelectrolyte and the water-soluble solution of conductivity anionic polyelectrolyte difference; 3. the capacitor block fuse that obtains impregnated in respectively in said polycation solution and the conductive poly anion solutions; Repeat repeatedly, obtain the compound polyelectrolyte of conducting polymer as capacitor cathode;
The capacitor block fuse impregnated graphite emulsion that 5. will 4. obtain;
The capacitor block fuse impregnated silver pulp that 6. will 5. obtain obtains chip organic solid electrolyte based electrolytic capacitor.
3. the preparation method of chip organic solid electrolyte based electrolytic capacitor according to claim 1 and 2 is characterized in that detailed step is following:
1. ta powder and tantalum wire are pressed into tantalum piece fuse, the tantalum wire insertion depth is 1/3 of a tantalum tile height;
The tantalum piece fuse that 2. will 1. obtain sinters the tantalum piece fuse with certain intensity in 1100-1300 ℃ vacuum sintering furnace;
The tantalum piece fuse that 3. will 2. obtain places 8 ‰ phosphate aqueous solution, adopts electrochemical method to form dielectric oxide film Ta2O5 in tantalum piece core surface;
4. compound concentration is the PDDA aqueous solution of 1g/ml (A liquid), 5g/ml (B liquid); Configuration concentration be 1.5g/ml (C liquid), 3.5g/ml (D liquid) gather 3,4-vinyl dioxy thiophene/polystyrolsulfon acid;
The tantalum piece fuse that 5. will 3. obtain 130 ℃ of oven dry behind the dipping 5min in A liquid earlier, then in B liquid among the dipping 10min back 130 ℃ of oven dry be a circulation, repetitive operation 5-8 time;
The tantalum piece fuse that 6. will 5. obtain floods 130 ℃ of oven dry behind the 5min in C liquid, then in D liquid among the dipping 10min back 130 ℃ of oven dry be a circulation, repetitive operation 4-6 time obtains the compound polyelectrolyte of certain thickness conducting polymer as capacitor cathode;
The tantalum piece fuse impregnated graphite emulsion that 7. will 6. obtain is then 180 ℃ of oven dry;
The tantalum piece fuse impregnated silver pulp that 8. will 7. obtain then 180 ℃ of oven dry, obtains the chip organic solid electrolyte based tantalum electrolytic capacitor of the compound polyelectrolyte of conducting polymer as capacitor cathode.
4. according to the preparation method of claim 2 or 3 described chip organic solid electrolyte based electrolytic capacitors, it is characterized in that: said metal dust comprises that specific volumes such as tantalum, nickel are the metal of 3000 ~ 70000 μ F.V/g.
5. according to the preparation method of claim 2 or 3 described chip organic solid electrolyte based electrolytic capacitors, it is characterized in that said acid solution is phosphoric acid, nitric acid or the citric acid acid solution after water-soluble.
6. according to the preparation method of claim 2 or 3 described chip organic solid electrolyte based electrolytic capacitors, it is characterized in that: the polycation material is ionogenic polyelectrolyte in the aqueous solution.
7. the preparation method of chip organic solid electrolyte based electrolytic capacitor according to claim 6 is characterized in that: the polycation material is PDDA (PDDA) or polypropylene amine (PAH).
8. according to the preparation method of claim 2 or 3 described chip organic solid electrolyte based electrolytic capacitors, it is characterized in that: the polyanion material be electric conductive polymer and in the aqueous solution ionogenic polyelectrolyte.
9. the preparation method of chip organic solid electrolyte based electrolytic capacitor according to claim 8 is characterized in that: the polyanion material is for gathering 3,4-vinyl dioxy thiophene/polystyrolsulfon acid (PEDOT/PSS).
10. according to the preparation method of claim 2 or 3 described chip organic solid electrolyte based electrolytic capacitors; It is characterized in that; Through control polycation and the concentration of polyanion and the number of times of dipping; Can regulate and control the effectively cathode thin film thickness of control capacitance device, and then the equivalent series resistance of control capacitance device to the compound polyelectrolyte of conducting polymer as cathode thin film.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102637535A (en) * | 2012-04-16 | 2012-08-15 | 南通江海电容器股份有限公司 | Preparation method of solid electrolytic capacitor with high voltage and large capacity |
| CN102709052A (en) * | 2012-06-21 | 2012-10-03 | 电子科技大学 | Method for manufacturing nano capacitor |
| CN111801826A (en) * | 2018-03-06 | 2020-10-20 | 住友电气工业株式会社 | Battery structure |
| CN112201482A (en) * | 2020-09-18 | 2021-01-08 | 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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| 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102637535A (en) * | 2012-04-16 | 2012-08-15 | 南通江海电容器股份有限公司 | Preparation method of solid electrolytic capacitor with high voltage and large capacity |
| 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 |
| CN102709052A (en) * | 2012-06-21 | 2012-10-03 | 电子科技大学 | Method for manufacturing nano capacitor |
| CN102709052B (en) * | 2012-06-21 | 2016-08-17 | 电子科技大学 | A kind of method manufacturing nano capacitor |
| CN111801826A (en) * | 2018-03-06 | 2020-10-20 | 住友电气工业株式会社 | Battery structure |
| CN112201482A (en) * | 2020-09-18 | 2021-01-08 | 同济大学 | Super capacitor based on heterojunction polymer gel electrolyte and preparation method thereof |
| 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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