CN101901690B - Miniature super capacitor and manufacturing method thereof - Google Patents
Miniature super capacitor and manufacturing method thereof Download PDFInfo
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- CN101901690B CN101901690B CN2010102436322A CN201010243632A CN101901690B CN 101901690 B CN101901690 B CN 101901690B CN 2010102436322 A CN2010102436322 A CN 2010102436322A CN 201010243632 A CN201010243632 A CN 201010243632A CN 101901690 B CN101901690 B CN 101901690B
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- super capacitor
- microelectrode
- polyimides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a miniature super capacitor and a manufacturing method thereof, and belongs to the technical field of micro-electronic machines. The miniature super capacitor consists of a polyimide supporting body, microelectrodes, a gel-like electrolyte and a sliver seal cover, and has a winding structure, wherein each microelectrode comprises an energy storage material, a conducting material and an adhesive, and is prepared by a screen printing method; and the gel-like electrolyte is prepared by mixing polyvinyl alcohol, sodium carboxymethyl cellulose, potassium hydroxide and water, and is coated among the microelectrodes by a spin coating method. The manufacturing method can reduce the internal resistance of the miniature super capacitor and improve the energy storage property of the miniature super capacitor. The miniature super capacitor is widely used in fields of sensor network node power supplies, fuze power supplies and the like.
Description
Technical field
The invention belongs to the micro-electronic mechanical skill field, particularly a kind of micro super capacitor and manufacturing approach thereof.
Background technology
Miniaturization of electronic products, microminiaturization, integrated be the trend of the times of world today's technical development.Microelectromechanical systems (Micro Electro Mechanical Systems is called for short MEMS) has mobility, automatic control property, characteristics such as integrated, is one of most important technological innovation in recent years.When a sub-systems can be integrated on the chip piece, power supply also must be accomplished the revolution of miniaturization, microminiaturization.The MEMS micro-energy resource system is meant the technology based on MEMS; It is that micron order, overall dimension are the micro-system of Centimeter Level that one or more electric energy feedwaies are integrated into a characteristic size; Can realize long-time, high-effect, multi-mode power supply, be specially adapted to some particular surroundings that conventional power source can't be used.The miniature energy of excellent performance is to the development of MEMS system and improve and just have special meaning.At present the patent in external this field mainly concentrates on fields such as miniature lithium ion battery, micro zinc-nickel battery, like the patent (US.6610440BS) of the relevant micro zinc-nickel battery of the patent (US.5567210) of the relevant miniature lithium ion battery of U.S. oak ridge National Laboratory and U.S. Bipolar technologies company.Preparation method in the involved little energy device of above-mentioned related patent U.S. Patent No. technology is through the small microelectrode of prepared in various methods yardstick; Receive the restriction of factors such as electrode area is limited; Indexs such as the internal resistance of prepared miniature energy device, capacity can not satisfy device requirement, have seriously restricted the application of miniature energy device.Compare with minicell, micro super capacitor requires to have lower internal resistance to satisfy its instantaneous high power discharge ability.And up to the present,, effective solution is not proposed as yet to the internal resistance that how effectively to reduce micro super capacitor.
Summary of the invention
The purpose of this invention is to provide a kind of micro super capacitor and manufacturing approach thereof, it is higher to micro super capacitor internal resistance in the prior art, can't satisfy device energy storage requirement and propose.
A kind of micro super capacitor; It is characterized in that; The structure of this micro super capacitor is on a slice polyimides supporter, to arrange microelectrode, gel-like electrolyte and microelectrode according to this, on combination surface, covers identical a slice polyimides supporter again and forms a unit, interconnects the back with the polyimides supporter of a plurality of unit and reels and become the coin structure; In coin shape structure both sides is silver-colored capping, and silver-colored capping plays collector as electrode terminal simultaneously.
Said microelectrode is for admixture partially conductive material and adhesive in energy storage material and add the electrode slurry that deionized water forms good fluidity, and the electrode slurry composition is Ru
2O
3, acetylene black, adhesive, water ratio of quality and the number of copies be 8: 1: 1: 40.
Said electric conducting material is an acetylene black, and adhesive is that butadiene-styrene rubber and sodium carboxymethylcellulose are 3: 1 mixture by ratio of quality and the number of copies.
Said energy storage material is a ruthenium-oxide, uses ruthenic chloride RuCl
3Give birth to hydroxide ruthenium Ru (OH) with NaOH NaOH reaction
3And carry out heat treated and generate ruthenium-oxide Ru
2O
3Specifically be with RuCl
3Add in the deionized water, be mixed with the RuCl that concentration range is 0.001-0.01mol/L
3Solution; The compound concentration scope is the NaOH solution of 0.001-0.03mol/L; Continuing under the stirring condition NaOH solution dropwise to be added RuCl
3In the solution, it is reacted completely, filtration and washing obtain black Ru (OH)
3, be placed on that heat treated obtains black electrode energy storage material Ru under the 120-160 ℃ of condition after 1 hour
2O
3Perhaps use the reaction of ruthenic chloride and carbonic hydroammonium to generate bicarbonate ruthenium Ru (HCO
3)
3And then heat treated generates ruthenium-oxide Ru
2O
3,Specifically be with RuCl
3The compound concentration scope is the RuCl of 0.001-0.01mol/L in deionized water
3Solution, compound concentration scope are the NH of 0.001-0.03mol/L
4HCO
3Solution.Continuing under the stirring condition, NH
4HCO
3Dropwise add RuCl
3It is reacted completely, and filtration and washing obtain black Ru (HCO
3)
3, be placed on that heating and decomposition treatment obtains black electrode energy storage material Ru under the 200-250 ℃ of condition after 1 hour
2O
3
Said gel-like electrolyte is made up of polyvinyl alcohol, sodium carboxymethylcellulose, potassium hydroxide, deionized water; Four mass percent example is 8-15: 2-5: 30-40: 30-50.Compare with independent use polyvinyl alcohol, polyvinyl alcohol and sodium carboxymethylcellulose blend can improve the moisture retention and the mechanical performance of gel-like electrolyte film; The content of potassium hydroxide and water is the key factor of restriction electrolyte performance in the gel-like electrolyte.The two mass ratio sum is 60%-90%.。
A kind of manufacturing approach of micro super capacitor; It is characterized in that, prepare microelectrode array, on microelectrode array, get rid of and be coated with the gel-like electrolyte layer in the polyimides supporting body surface; Lid layer polyimides supporter then; Large tracts of land polyimides supporter microelectrode array is cut into a plurality of unit, interconnect the back with the polyimides supporter of a plurality of unit and reel and become the coin structure, coin shape structure both sides adopt magnetron sputtering method and galvanoplastic to prepare silver-colored capping with the completion capacitor package; The silver capping plays collector as electrode terminal,
The preparation of said microelectrode array is to adopt silk screen print method that electrode slurry is coated in the polyimides supporting body surface, forms equidistant strip microelectrode array,
It is with strip microelectrode five equilibrium that said microelectrode array cuts into a plurality of unit, forms to comprise the unit of arranging by microelectrode, gel-like electrolyte, microelectrode.
The invention has the beneficial effects as follows that this micro super capacitor adopts the microstructure of polyimides supporter, microelectrode, gel-like electrolyte and silver-colored capping; Silver capping technology can reduce the micro super capacitor internal resistance, and then reaches the effect of improving the micro super capacitor energy storage characteristic.The operating voltage of micro super capacitor of the present invention is 1V, and capacity is 0.4 farad, and internal resistance is merely 2 ohm, and nominal discharge current reaches 20 milliamperes, and volume is merely 50mm
3, have good energy storage characteristic.
Description of drawings
Fig. 1 is the micro super capacitor structural representation.
Fig. 2 is the micro super capacitor schematic diagram of fabrication technology.
Embodiment
The present invention provides a kind of micro super capacitor and manufacturing approach thereof, and it is higher to micro super capacitor internal resistance in the prior art, can't satisfy device energy storage requirement and propose.
Need to prove that under the situation of not conflicting, embodiment and the characteristic among the embodiment among the application can make up each other.Below with reference to accompanying drawing and combine embodiment to specify the present invention.
Fig. 1 is that the micro super capacitor structure is formed sketch map.Shown in Figure 1; The structure of this micro super capacitor is on a slice polyimides supporter 1, to arrange microelectrode 2, gel-like electrolyte 3 and microelectrode 2 according to this; On combination surface, cover identical a slice polyimides supporter 1 again and form a unit 11; The polyimides supporter 1 of a plurality of unit 11 interconnects the back coiling becomes the coin structure, is silver-colored capping 4 in coin shape structure both sides, plays collector as electrode terminal simultaneously.The structure of this micro super capacitor is passed through effectively to contact with microelectrode 2 in large-area silver-colored capping 4, thereby has reduced the micro super capacitor internal resistance, and then improves the energy storage characteristic of microelectrode and even micro super capacitor effectively.
Fig. 2 is the microelectrode schematic diagram of fabrication technology; Shown in Fig. 2 (a), adopt silk screen print method at polyimide matrix surface preparation microelectrode array, the preparation of said microelectrode array is to adopt silk screen print method that electrode slurry is coated in polyimides supporter 1 surface; Form equidistant strip electrode 7; A plurality of strip electrodes 7 form microelectrode array array 6 on large tracts of land polyimides supporter, 500 microns-3000 microns of strip electrode widths, preferred 2000 microns.500 microns-1000 microns of electrode spacings, preferred 500 microns.200 microns-2000 microns of thickness of electrode, preferred 1000 microns.With data by MoM and MEI, method for printing screen can prepare the trickle clearly figure of figure on supporter.
Being prepared as in the electrode energy storage material admixture partially conductive material and adhesive and adding the slurry that deionized water forms good fluidity of above-mentioned electrode slurry.Conductive material is an acetylene black.Adhesive is the mixture of butadiene-styrene rubber and sodium carboxymethylcellulose.The ratio of quality and the number of copies of butadiene-styrene rubber and sodium carboxymethylcellulose is 3: 1.The electrode slurry composition is Ru
2O
3, acetylene black, adhesive, water, its best in quality portion rate is 8: 1: 1: 40.Said components is mixed and carries out ball-milling treatment.Adhesive is to guarantee that slurry had both had good fluidity, and by having the key factor of good cohesive strength with matrix, its mass percent in slurry should not be lower than 1%, should not be higher than 5%, preferred 2%.Binder content is low excessively, and then electrode structure intensity is relatively poor, and binder content is too high then to cause the electrode internal resistance to raise.
Above-mentioned electrode energy storage material is ultra-fine ruthenium-oxide, can use ruthenic chloride RuCl
3Give birth to hydroxide ruthenium Ru (OH) with NaOH NaOH reaction
3And carry out heat treated and generate ruthenium-oxide Ru
2O
3Concrete grammar is with RuCl
3In deionized water, compound concentration is the RuCl of 0.005mol/L
3Solution, compound concentration scope are the NaOH solution of 0.02mol/L.Continuing under the stirring condition NaOH dropwise to be added RuCl
3It is reacted completely, and filtration and washing obtain black Ru (OH)
3, be placed on that heat treated obtains black electrode energy storage material Ru under 140 ℃ of conditions after 1 hour
2O
3Heating-up temperature is a key influence factor, and it is thorough inadequately that temperature is crossed low then dehydration, the too high then Ru of temperature
2O
3Crystallization occurs, the direct performance of the two all is that material capacity reduces.Perhaps ultra-fine ruthenium-oxide can use ruthenic chloride and carbonic hydroammonium reaction to generate bicarbonate ruthenium Ru (HCO
3)
3And then heat treated generates ruthenium-oxide Ru
2O
3Be specially RuCl
3The compound concentration scope is the RuCl of 0.005mol/L in deionized water
3Solution, compound concentration scope are the NH of 0.02mol/L
4HCO
3Solution.Continuing under the stirring condition, NH
4HCO
3Dropwise add RuCl
3It is reacted completely, and filtration and washing obtain black Ru (HCO
3)
3, be placed on that heating and decomposition treatment obtains black electrode energy storage material Ru under 230 ℃ of conditions after 1 hour
2O
3
Gel-like electrolyte 3 between above-mentioned microelectrode adopts lacquering technique to coat.Gel-like electrolyte is made up of polyvinyl alcohol, sodium carboxymethylcellulose, potassium hydroxide, deionized water.Four best in quality percentages are 15: 5: 35: 45.Compare with independent use polyvinyl alcohol, polyvinyl alcohol and sodium carboxymethylcellulose blend can improve moisture retention and the mechanical performance of covering polymer dielectric film.The content of potassium hydroxide and water is the key factor of restriction electrolyte performance in the gel-like electrolyte.The two mass ratio sum should not be lower than 60%, should not be higher than 90%.Too high levels can cause electrolyte rare excessively, be prone to take place flows, and causes the subsequent technique difficulty, and is prone to cause leakage after the capacitor package.Content is crossed to hang down and is then caused the electrolyte internal resistance too big, and is prone to cause condenser capacity to reduce.
It is that the polyimides supporter is fixed on the photoresist spinner platform that the getting rid of of gel-like electrolyte is coated with technology; On supporter 1, drip an amount of above-mentioned gel-like electrolyte; The supporter rotating speed is evenly accelerated to necessarily than the slow-speed of revolution from static; Range of speeds 800-1200 rev/min, preferred 1000 rev/mins, and kept 10 seconds; Evenly accelerate to higher rotation speed then, range of speeds 1500-2000 rev/min, preferred 1800 change, and keep 25 seconds, evenly are decelerated to static then.The supporter of brush accomplishing in 25 ℃ of room temperature environments horizontal positioned 10-30 minute, preferred 30 minutes, so that gel-like electrolyte oneself leveling.After accomplishing, above-mentioned technology filled gel-like electrolyte 3 between the strip electrode 7, shown in Fig. 2 (b).
Electrolyte is placed one deck and the identical polyimides supporter of polyimides supporter after getting rid of and being coated with completion again above microelectrode array 6, shown in Fig. 2 (c).Because gel-like electrolyte has big viscosity, this strata acid imide supporter can adhere to each other with substructure.
Cut into a plurality of unit 11 with forming microelectrode array array 6 on the large tracts of land polyimides supporter, it is with strip microelectrode 7 five equilibriums, forms to comprise the unit of arranging by microelectrode 2, gel-like electrolyte 3, microelectrode 2 11 (shown in Fig. 2 (d)).The polyimides supporter 1 of a plurality of then unit 11 interconnects the back coiling becomes coin structure (shown in Fig. 2 (e)), and microelectrode 2 is positioned at the two sides of coin structure and exposes at this moment.
The magnetron sputtering technique process of silver capping is that the coin structure simultaneously upwards is fixed on the specimen holder of magnetron sputtering apparatus, adopts silver (99.99wt%) as target, and at first being evacuated to reative cell air pressure is 5 * 10
-4Pa, charging into high-purity argon gas to air pressure then is 3Pa, the beginning sputtering technology, keeping sputtering power in the sputter procedure is 100-150W, preferred 120W, sedimentation time 240 minutes, the preparation silver thickness is greater than 10 microns.The coin structure simultaneously deposits after the completion its upset, the deposition another side.Silver capping thickness should be controlled and be not less than 10 microns, and encapsulation is accomplished in silver-colored capping, like Fig. 2 (f).Silver capping thickness is crossed to hang down and is prone to cause the microelectrode covering imperfect, is prone to cause electrolyte to reveal.Silver capping thickness can not satisfy the requirement of capacitor well packaged far away, therefore adopts electro-plating method to prepare silver layer surface at magnetron sputtering and continues thickness and the structural strength of plated metal silver to strengthen silver-colored capping.The technology of electrosilvering is that the coin structure of accomplishing magnetron sputtering deposition technology is immersed in the electroplate liquid as negative electrode, adopts argent as anode, contains silver nitrate AgNO in the plating bath
3(concentration range 8-15g/L, preferred 10g/L), thiomalic acid (concentration range 30-60g/L, preferred 45g/L), glucose (concentration range 50-100g/L, preferred 60g/L), the plating bath pH value is 1, current range is 5-30mA/cm
2, preferred 10mA/cm
2, reaction temperature is 20-35 ℃, preferred 30 ℃.Thickness of coating scope 100-500 micron, the too small then silver-colored capping intensity of thickness of coating is too low, and thickness is excessive to cause the capsule stress excessive and phenomenon such as cracking occurs easily.Electroplating technology can be with carrying out simultaneously behind the capacitor two-stage parallel connection.Silver is sealed on the function of also bearing the microelectrode outside terminal when realizing the micro super capacitor sealing, and electric charge flows into or the outflow microelectrode through silver-colored capping 4 in the charge and discharge process.Magnetron sputtering silver capping technology can realize that microelectrode contact with large tracts of land between the electrode terminal, has realized effective reduction of contact resistance between microelectrode and the silver-colored capping, and then reduction capacitor electronics, improves the heavy-current discharge characteristic of capacitor.Magnetron sputtering technique can also be guaranteed effective sealing of micro super capacitor, has avoided ultracapacitor actual effect phenomenon in the course of the work.
The present invention proposes a kind of micro super capacitor structure and manufacturing approach thereof; Can reduce the capacitor internal resistance effectively; Improve the energy storage characteristic of micro super capacitor, be widely used in fields such as sensor network nodes power supply, fuze power supplies based on micro super capacitor described in the invention.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. micro super capacitor; It is characterized in that; The structure of this micro super capacitor is on a slice polyimides supporter, to arrange microelectrode, gel-like electrolyte and microelectrode according to this, on combination surface, covers identical a slice polyimides supporter again and forms a unit, interconnects the back with the polyimides supporter of a plurality of unit and reels and become the coin structure; In coin shape structure both sides is silver-colored capping, and silver-colored capping plays collector as electrode terminal simultaneously.
2. according to the said micro super capacitor of claim 1, it is characterized in that said microelectrode is at Ru
2O
3Middle admixture acetylene black and adhesive, and add the electrode slurry that deionized water forms good fluidity, the ratio of quality and the number of copies of this electrode slurry composition is Ru
2O
3: acetylene black: adhesive: deionized water=8: 1: 1: 40.
3. according to the said micro super capacitor of claim 2, it is characterized in that said adhesive is that butadiene-styrene rubber and sodium carboxymethylcellulose are 3: 1 mixture by ratio of quality and the number of copies.
4. according to the said micro super capacitor of claim 1, it is characterized in that said energy storage material is a ruthenium-oxide, use ruthenic chloride RuCl
3Give birth to hydroxide ruthenium Ru (OH) with NaOH NaOH reaction
3And carry out heat treated and generate ruthenium-oxide Ru
2O
3Specifically be with RuCl
3Add in the deionized water, be mixed with the RuCl that concentration range is 0.001～0.01mol/L
3Solution; The compound concentration scope is the NaOH solution of 0.001～0.03mol/L; Continuing under the stirring condition NaOH solution dropwise to be added RuCl
3In the solution, it is reacted completely, filtration and washing obtain black Ru (OH)
3, be placed on that heat treated obtains black electrode energy storage material Ru under 120～160 ℃ of conditions after 1 hour
2O
3Perhaps use the reaction of ruthenic chloride and carbonic hydroammonium to generate bicarbonate ruthenium Ru (HCO
3)
3And then heat treated generates ruthenium-oxide Ru
2O
3Specifically be with RuCl
3The compound concentration scope is the RuCl of 0.001～0.01mol/L in deionized water
3Solution, compound concentration scope are the NH of 0.001～0.03mol/L
4HCO
3Solution; Continuing under the stirring condition, NH
4HCO
3Dropwise add RuCl
3It is reacted completely, and filtration and washing obtain black Ru (HCO
3)
3, be placed on that heating and decomposition treatment obtains black electrode energy storage material Ru under 200～250 ℃ of conditions after 1 hour
2O
3
5. according to the said micro super capacitor of claim 1, it is characterized in that said gel-like electrolyte is made up of polyvinyl alcohol, sodium carboxymethylcellulose, potassium hydroxide, deionized water; Four mass percent example is 8-15: 2-5: 30-40: 30-50; Compare with independent use polyvinyl alcohol, polyvinyl alcohol and sodium carboxymethylcellulose blend can improve the moisture retention and the mechanical performance of gel-like electrolyte film.
6. the manufacturing approach of a micro super capacitor; It is characterized in that, prepare microelectrode array, on microelectrode array, get rid of and be coated with the gel-like electrolyte layer in the polyimides supporting body surface; Lid layer polyimides supporter then; Large tracts of land polyimides supporter microelectrode array is cut into a plurality of unit, interconnect the back with the polyimides supporter of a plurality of unit and reel and become the coin structure, coin shape structure both sides adopt magnetron sputtering method and galvanoplastic to prepare silver-colored capping with the completion capacitor package; The silver capping plays collector as electrode terminal.
7. according to the manufacturing approach of the said micro super capacitor of claim 6, it is characterized in that the preparation of said microelectrode array is to adopt silk screen print method that electrode slurry is coated in the polyimides supporting body surface, forms equidistant strip microelectrode array.
8. according to the manufacturing approach of the said micro super capacitor of claim 6, it is characterized in that it is with strip microelectrode five equilibrium that said microelectrode array cuts into a plurality of unit, form the unit that comprises by microelectrode, gel-like electrolyte, microelectrode arrangement.
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|---|---|---|---|
| CN2010102436322A CN101901690B (en) | 2010-08-03 | 2010-08-03 | Miniature super capacitor and manufacturing method thereof |
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| CN101901690B true CN101901690B (en) | 2012-05-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103198933A (en) * | 2012-07-05 | 2013-07-10 | 吴凯明 | Liquid flow type double electrode layer capacitor of electrolyte comprising conducting carbon particles |
| CN104332327A (en) * | 2014-09-04 | 2015-02-04 | 湖南中大新能源科技有限公司 | Preparation method of laminated minisize energy storage device |
| CN105845460B (en) * | 2016-03-18 | 2018-11-13 | 复旦大学 | A kind of ultra-thin ultracapacitor and preparation method thereof based on microtomy |
| CN106158411A (en) * | 2016-08-17 | 2016-11-23 | 武汉理工大学 | A kind of high-performance symmetrical expression metal-oxide base micro super capacitor and preparation method thereof |
| CN109585940A (en) * | 2018-12-19 | 2019-04-05 | 苏州柔能纳米科技有限公司 | A kind of alkalinity flexible solid electrolytic thin-membrane and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1145348B1 (en) * | 1998-10-22 | 2002-09-18 | Ramot University Authority For Applied Research & Industrial Development Ltd. | Micro-electrochemical energy storage cells |
| CN101325130A (en) * | 2008-05-22 | 2008-12-17 | 清华大学 | Poly-pyrrole minisize super capacitor based on MEMS technique and method for manufacturing the same |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6610440B1 (en) * | 1998-03-10 | 2003-08-26 | Bipolar Technologies, Inc | Microscopic batteries for MEMS systems |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1145348B1 (en) * | 1998-10-22 | 2002-09-18 | Ramot University Authority For Applied Research & Industrial Development Ltd. | Micro-electrochemical energy storage cells |
| CN101325130A (en) * | 2008-05-22 | 2008-12-17 | 清华大学 | Poly-pyrrole minisize super capacitor based on MEMS technique and method for manufacturing the same |
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