CN102891013A - Method for preparing ruthenium dioxide combination electrode for energy storage - Google Patents
Method for preparing ruthenium dioxide combination electrode for energy storage Download PDFInfo
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Abstract
The invention provides a method for preparing a ruthenium dioxide combination electrode for energy storage. The method is characterized by comprising the following steps of: a) mixing ruthenium dioxide materials with different content, a binder, a thickening agent, carbon and deionized water in shear mixing equipment to prepare a plurality of kinds of slurry with different ruthenium dioxide content and different viscosity; b) coating the slurry with the lowest ruthenium dioxide content on a current collector, drying and forming; and c) coating multi-layer slurry by using the method in the step b). The ruthenium dioxide combination electrode is tightly combined with the current collector, has the characteristics of high capacity and long service life and can be widely applied to the field of energy storage for national defense and civil use.
Description
Technical field
The present invention relates to field of chemical power source, relate to especially the preparation method that the ruthenic oxide combination electrode is used in a kind of energy storage.
Background technology
Ultracapacitor (Super capacitor, Ultra capacitor) claims that again " electrochemical capacitor (Electrochemical Capacitor, EC) " is a kind of new chemical energy storage device between traditional capacitor and battery.Compare traditional capacitor, it has higher energy density, and static capacity can reach hundreds of even thousands of farads; Compare battery, it has higher power density and the cycle life of overlength, so it combines the advantage of traditional capacitor and battery, is a kind of chemical power source that has a extensive future.It has that specific capacity is high, power is large, the life-span is long, the warm limit for width of working, the characteristics such as non-maintaining.
Difference according to energy storage principle, ultracapacitor generally is divided into two large classes: a class is based on the formed electric double layer of electrode/electrolyte interface separation of charge (Double Layer) principle energy storage, another kind ofly is based on fast faraday's " pseudo-capacitance " principle energy storage of producing of redox reaction of electrode surface.Different according to the electrode structure classification, ultracapacitor can be divided into again symmetric form (Symmetric) and asymmetric (Asymmetric; Sometimes claim mixed type, Hybrid) two classes, the former is the most common with activated carbon-activated carbon (CC), most typical example is the product of U.S. Maxwell company, the latter is the most common with activated carbon-metal oxide (CMO), and typical example is activated carbon-nickel oxide (CNiO) and tantalum oxide-ruthenic oxide (TaRuO).Wherein, hydration ruthenic oxide (RuO
2.xH
2O) has high ratio electric capacity (specific activity carbon is large more than 1 times) and the general conductivity of metal, therefore, has important application in the national defence such as military aerospace and specific area, particularly anode is that tantalum pentoxide, negative electrode are the hybrid super capacitor (being commonly referred to " ruthenium tantalum capacitor ") that the hydration ruthenic oxide consists of, and monopolizes the world in the national defence field because it has excellent frequency response characteristic and high low-temperature stability.
Core component as the ruthenium tantalum capacitor, its electrode fabrication is technical barrier always, its reason mainly contains 2 points: the one, because the special surface characteristic of ruthenic oxide material, the electrode surface that causes being made into easily ftractures, cause contacting with collector not good, the final performance that affects the active material chemical property and life-span [Liu Hong, Gan Weiping, Guo Guijin etc. RuO
2.nH
2O thin film technology and phase develop and voltage-current characteristic
. the China YouSe Acta Metallurgica Sinica, 2010,20 (3): 522-527]; The 2nd, because the electrochemical reaction of ruthenic oxide mainly concentrates on the accurate three-dimensional space of two peacekeepings, therefore electrode can not be made too thickly, otherwise can have a strong impact on electrode performance, this just means that prior art has limited it and required application in the occasion of high energy storage density at some.Through retrieval, not yet there is relevant technology open at present.
Summary of the invention
The object of the invention is to overcome above-mentioned technological difficulties, the preparation method of a kind of energy storage with the ruthenic oxide combination electrode is provided, the ruthenic oxide combination electrode is combined tightr with collector, have the characteristics such as high power capacity and long-life.
The present invention proposes a kind of energy storage with the preparation method of ruthenic oxide combination electrode, it is characterized in that comprising the steps:
A) the ruthenic oxide material with different content mixes in shear mixing equipment with binding agent, thickener, carbon and deionized water, makes the multiple slurry that ruthenic oxide content is different, viscosity is different;
B) slurry that ruthenic oxide content is minimum is coated on the collector, drying forming;
C) method coated with multiple layer slurry use step b).
More preferably, the content of the described slurry ruthenic oxide of ground floor is 0-20%.
More preferably, the content of described slurry ruthenic oxide is no more than 85%.
More preferably, the viscosity of described multilayer slurry outwards reduces gradually from inner.
More preferably, the preferred tetrafluoroethene of described binding agent, butadiene-styrene rubber, sodium carboxymethylcellulose.
More preferably, described thickener preferred cellulose ether, polyacrylamide, titanate esters, gum arabic, silicon gel, gelatin and agar etc.
More preferably, the preferred carbon black of described carbon, graphite, Graphene, SuperP, acetylene black, activated carbon, BP2000, VulcanXC-72, VulcanXC-72R, carbon nano-tube and carbon fiber etc.
More preferably, the described methods such as spraying, brushing, coating that are applied to
More preferably, described ruthenic oxide be the hydration ruthenic oxide, without the mixture of the one or both of hydration ruthenic oxide.
More preferably, described collector material is titanium, graphite or stainless steel, and material is shaped as sheet material, foil or bar.
More preferably, described multilayer slurry is greater than 2 layers.
The ruthenic oxide combination electrode that the present invention obtains is combined tightr with collector, have the characteristics such as high power capacity and long-life, can be widely used in national defence and the energy storage field such as civilian.
Embodiment
The below describes specific embodiments of the invention in detail.
The present invention proposes a kind of energy storage with the preparation method of ruthenic oxide combination electrode, comprises the steps:
A) the ruthenic oxide material with different content mixes in shear mixing equipment with binding agent, thickener, carbon and deionized water, makes the multiple slurry that ruthenic oxide content is different, viscosity is different;
B) slurry that ruthenic oxide content is minimum is coated on the collector, drying forming;
C) method coated with multiple layer slurry use step b).
The gradient that is distributed as of ruthenic oxide distributes in the combination electrode of making, and raises gradually away from the content of collector ruthenic oxide.Wherein ruthenic oxide be the hydration ruthenic oxide, without the mixture of the one or both of hydration ruthenic oxide.The content of ground floor slurry ruthenic oxide is 0-20%.The content of ruthenic oxide is no more than 85% in the slurry.The viscosity of each layer slurry is different, and ground floor viscosity is maximum, and viscosity is less more outward.The preferred tetrafluoroethene of binding agent, butadiene-styrene rubber, sodium carboxymethylcellulose.Thickener preferred cellulose ether, polyacrylamide, titanate esters, gum arabic, silicon gel, gelatin and agar etc.The preferred carbon black of carbon, graphite, Graphene, SuperP, acetylene black, activated carbon, BP2000, VulcanXC-72, VulcanXC-72R, carbon nano-tube and carbon fiber etc.Be applied to the methods such as spraying, coating.The collector material is titanium, graphite or stainless steel, and material is shaped as sheet material, foil or bar.
Adopt three-electrode system classical in the electrochemistry, made electrode is carried out capacity and cycle life test (electrolyte is 38% sulfuric acid solution, and potential region is 0-1.0V), to assess its specific capacity and electrochemical stability.
Embodiment 1:
The commercially available hydration ruthenic oxide of 100mg is divided into 4 parts by the 1:2:3:4 mass ratio, become 4 batches in the different slurry of viscosity from SuperP, sodium carboxymethylcellulose, butadiene-styrene rubber and the deionized water shear-mixed of certain content respectively, viscosity is respectively 8000,6000,4000,2800.Wherein, the dry weight of every crowd SuperP, sodium carboxymethylcellulose and butadiene-styrene rubber ratio is 4:1:0.2, and total amount is identical.Employing rock field hand-held spray guns supports the 1st batch of slurry through oil removing, the surperficial slightly titanium foil (thickness is 100 μ m) of good fortune, then on-the-spot the oven dry 5 minutes on the 1000W baking oven.Then, with order 2-4 is criticized slurry and support successively on the electrode surface of last time drying, the combination electrode layer that formation 1-4 layer, ruthenic oxide content increase progressively successively.Be compacting on the roll forming machine of 80mm at last at diameter with combination electrode, oven dry was carried out electrochemistry capacitance and stability experiment after 10 hours in 80 ℃ of air dry ovens.As a comparison, adopt prior art, disposable 100mg ruthenic oxide material is made electrode, test under the same conditions its capacity and stability.Found that, adopt combination electrode of the present invention surface without microcraking, the ratio electric capacity of active ruthenic oxide is 880F/g, and it only is 3.5% that rear its capacity of 5000 weeks of scan round of 50mV/s declines.There is significantly crack splitting in the electrode of contrast, and its capacity only is 600F/g, and under the same sweep speed, the capacity attenuation after 5000 weeks reaches 7.3%.
Embodiment 2
The commercially available hydration ruthenic oxide of 100mg is divided into 4 parts by the 1:2:3:4 mass ratio, become 4 batches in the different slurry of viscosity from SuperP, sodium carboxymethylcellulose, polytetrafluoroethylene and the deionized water shear-mixed of certain content respectively, viscosity is respectively 8000,6000,4000,2800.Wherein, the dry weight of every crowd SuperP, sodium carboxymethylcellulose and polytetrafluoroethylene ratio is 4:1:0.2, and total amount is identical.Adopt manual brushing mode that the 1st batch of slurry supported on the graphite cake that thickness is 300 μ m, then on-the-spot the oven dry 3 minutes on the 1000W baking oven.Then, with order 2-4 is criticized slurry and support successively on the electrode surface of last time drying, the combination electrode layer that formation 1-4 layer, ruthenic oxide content increase progressively successively.Be compacting on the roll forming machine of 80mm at last at diameter with combination electrode, oven dry was carried out electrochemistry capacitance and stability experiment after 10 hours in 80 ℃ of air dry ovens.Found that, adopt combination electrode of the present invention surface without microcraking, the ratio electric capacity of active ruthenic oxide is 950F/g, and it only is 2.8% that rear its capacity of 5000 weeks of scan round of 50mV/s declines.
Embodiment 3
The commercially available hydration ruthenic oxide of 150mg is divided into 3 parts by the 1:2:3 mass ratio, become 3 batches in the different slurry of viscosity from SuperP, sodium carboxymethylcellulose, polytetrafluoroethylene and the deionized water shear-mixed of certain content respectively, viscosity is respectively 6000,5000, and 3500.Wherein, the dry weight of every crowd SuperP, sodium carboxymethylcellulose and polytetrafluoroethylene ratio is 4:1:0.2, and total amount is identical.Adopt the manual brushing method that the 1st batch of slurry supported on the graphite cake (thickness is 300 μ m), then on-the-spot the oven dry 3 minutes on the 1000W baking oven.Then, with order 2-3 is criticized slurry and support successively on the electrode surface of last time drying, the combination electrode layer that formation 1-3 layer, ruthenic oxide content increase progressively successively.Be compacting on the roll forming machine of 80mm at last at diameter with combination electrode, oven dry was carried out electrochemistry capacitance and stability experiment after 10 hours in 80 ℃ of air dry ovens.Found that, adopt combination electrode of the present invention surface without microcraking, the ratio electric capacity of active ruthenic oxide is 1000F/g, and it only is 2.5% that rear its capacity of 5000 weeks of scan round of 50mV/s declines.
Embodiment 4
The commercially available hydration ruthenic oxide of 150mg is divided into 4 parts by the 1:2:3:4 mass ratio, become 4 batches in the different slurry of viscosity from SuperP, sodium carboxymethylcellulose, polytetrafluoroethylene and the deionized water shear-mixed of certain content respectively, viscosity is respectively 6000,5000,3500,2400.Wherein, the dry weight of every crowd SuperP, sodium carboxymethylcellulose and polytetrafluoroethylene ratio is 4:1:0.2, and total amount is identical.Adopt the manual brushing method that the 1st batch of slurry supported on the graphite cake (thickness is 300 μ m), then on-the-spot the oven dry 3 minutes on the 1000W baking oven.Then, with order 2-3 is criticized slurry and support successively on the electrode surface of last time drying, the combination electrode layer that formation 1-4 layer, ruthenic oxide content increase progressively successively.Be compacting on the roll forming machine of 80mm at last at diameter with combination electrode, oven dry was carried out electrochemistry capacitance and stability experiment after 10 hours in 80 ℃ of air dry ovens.Found that, adopt combination electrode of the present invention surface without microcraking, the ratio electric capacity of active ruthenic oxide is 1100F/g, and it only is 2.3% that rear its capacity of 5000 weeks of scan round of 50mV/s declines.
Embodiment 5
The commercially available hydration ruthenic oxide of 100mg is divided into 4 parts by the 1:2:3:4 mass ratio, become 4 batches in the different slurry of viscosity from SuperP, sodium carboxymethylcellulose, polytetrafluoroethylene and the deionized water shear-mixed of certain content respectively, viscosity is respectively 6000,5000,3500,2400.Wherein, the dry weight of every crowd SuperP, sodium carboxymethylcellulose and polytetrafluoroethylene ratio is 4:1:0.2, and total amount is identical.Adopt the manual brushing method that the 1st batch of slurry supported on 316 stainless steels (thickness is 400 μ m), then on-the-spot the oven dry 3 minutes on the 1000W baking oven.Then, with order 2-3 is criticized slurry and support successively on the electrode surface of last time drying, the combination electrode layer that formation 1-4 layer, ruthenic oxide content increase progressively successively.Be compacting on the roll forming machine of 80mm at last at diameter with combination electrode, oven dry was carried out electrochemistry capacitance and stability experiment after 10 hours in 80 ℃ of air dry ovens.Found that, adopt combination electrode of the present invention surface without microcraking, the ratio electric capacity of active ruthenic oxide is 930F/g, and it is 4.7% that rear its capacity of 5000 weeks of scan round of 50mV/s declines.
Embodiment 6
As different from Example 1, when combination electrode prepares, be with 100mg ruthenic oxide material in mass ratio 1:2:3:4:5:6:7:8 be divided into 8 parts, the slurry viscosity of making also changes to respectively 8000:7000:6000:5000:4000:3000:2000:1000.Electrochemical results shows, it is 980F/g than electric capacity, and the capacity attenuation of 5000 all scan rounds is 2.9%.
Described in this specification is preferred embodiment of the present invention, and above embodiment is only in order to illustrate technical scheme of the present invention but not limitation of the present invention.All those skilled in the art all should be within the scope of the present invention under this invention's idea by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (11)
1. the preparation method of an energy storage usefulness ruthenic oxide combination electrode is characterized in that comprising the steps:
A) the ruthenic oxide material with different content mixes in shear mixing equipment with binding agent, thickener, carbon and deionized water, makes the multiple slurry that ruthenic oxide content is different, viscosity is different;
B) slurry that ruthenic oxide content is minimum is coated on the collector, drying forming;
C) method coated with multiple layer slurry use step b).
2. energy storage as claimed in claim 1 is with the preparation method of ruthenic oxide combination electrode, and the content that it is characterized in that the described slurry ruthenic oxide of ground floor is 0-20%.
3. energy storage as claimed in claim 1 is characterized in that with the preparation method of ruthenic oxide combination electrode the content of described slurry ruthenic oxide is no more than 85%.
4. such as the preparation method of the described energy storage of one of claim 1-3 with the ruthenic oxide combination electrode, it is characterized in that the viscosity of described multilayer slurry outwards reduces gradually from inner.
5. energy storage as claimed in claim 1 is characterized in that the preferred tetrafluoroethene of described binding agent, butadiene-styrene rubber, sodium carboxymethylcellulose with the preparation method of ruthenic oxide combination electrode.
6. energy storage as claimed in claim 1 is characterized in that described thickener preferred cellulose ether, polyacrylamide, titanate esters, gum arabic, silicon gel, gelatin and agar etc. with the preparation method of ruthenic oxide combination electrode.
7. energy storage as claimed in claim 1 is characterized in that the preferred carbon black of described carbon, graphite, Graphene, SuperP, acetylene black, activated carbon, BP2000, VulcanXC-72, VulcanXC-72R, carbon nano-tube and carbon fiber etc. with the preparation method of ruthenic oxide combination electrode.
8. energy storage as claimed in claim 1 is characterized in that the described methods such as spraying, brushing, coating that are applied to the preparation method of ruthenic oxide combination electrode.
9. energy storage as claimed in claim 1 is with the preparation method of ruthenic oxide combination electrode, it is characterized in that described ruthenic oxide be the hydration ruthenic oxide, without the mixture of the one or both of hydration ruthenic oxide.
10. energy storage as claimed in claim 1 is characterized in that with the preparation method of ruthenic oxide combination electrode described collector material is titanium, graphite or stainless steel, and material is shaped as sheet material, foil or bar.
11. energy storage as claimed in claim 1 is more than or equal to 2 layers with the preparation method of ruthenic oxide combination electrode, the number of plies that it is characterized in that described multilayer slurry.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400696A (en) * | 2013-07-31 | 2013-11-20 | 株洲宏达电子有限公司 | Conductive polymer ruthenium dioxide membrane electrode and preparation method thereof |
| CN103887077A (en) * | 2014-03-04 | 2014-06-25 | 成都达艾斯电子有限公司 | Super capacitor and method for manufacturing super capacitor |
| CN104021947A (en) * | 2014-06-20 | 2014-09-03 | 贵州中航聚电科技有限公司 | Method for preparing ruthenium oxide electrode with high specific capacitance rate for hybrid super capacitor |
| CN107275568A (en) * | 2017-07-04 | 2017-10-20 | 福州大学 | A kind of ruthenic oxide Quito pore electrod of graphene doping and preparation method thereof |
| CN107633953A (en) * | 2017-09-08 | 2018-01-26 | 西安科技大学 | A kind of multi-layered electrode and its ultracapacitor of preparation |
| CN112670090A (en) * | 2020-12-24 | 2021-04-16 | 电子科技大学 | Electrode plate and preparation method and application thereof |
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| US20080068776A1 (en) * | 2006-09-19 | 2008-03-20 | National Taiwan University Of Science & Technology | Hybrid electrode and method of preparing the same |
| CN102496473A (en) * | 2011-12-12 | 2012-06-13 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing ruthenium oxide coating on inner wall of tantalum shell of electrolytic capacitor |
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Patent Citations (2)
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| US20080068776A1 (en) * | 2006-09-19 | 2008-03-20 | National Taiwan University Of Science & Technology | Hybrid electrode and method of preparing the same |
| CN102496473A (en) * | 2011-12-12 | 2012-06-13 | 中国振华（集团）新云电子元器件有限责任公司 | Method for preparing ruthenium oxide coating on inner wall of tantalum shell of electrolytic capacitor |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400696A (en) * | 2013-07-31 | 2013-11-20 | 株洲宏达电子有限公司 | Conductive polymer ruthenium dioxide membrane electrode and preparation method thereof |
| CN103400696B (en) * | 2013-07-31 | 2016-02-03 | 株洲宏达电子股份有限公司 | A kind of conductive polymer ruthenium dioxide membrane electrode and preparation method thereof |
| CN103887077A (en) * | 2014-03-04 | 2014-06-25 | 成都达艾斯电子有限公司 | Super capacitor and method for manufacturing super capacitor |
| CN103887077B (en) * | 2014-03-04 | 2016-09-14 | 成都达艾斯电子有限公司 | A kind of ultracapacitor and preparation method thereof |
| CN104021947A (en) * | 2014-06-20 | 2014-09-03 | 贵州中航聚电科技有限公司 | Method for preparing ruthenium oxide electrode with high specific capacitance rate for hybrid super capacitor |
| CN104021947B (en) * | 2014-06-20 | 2017-04-12 | 贵州中航聚电科技有限公司 | Method for preparing ruthenium oxide electrode for hybrid super capacitor |
| CN107275568A (en) * | 2017-07-04 | 2017-10-20 | 福州大学 | A kind of ruthenic oxide Quito pore electrod of graphene doping and preparation method thereof |
| CN107275568B (en) * | 2017-07-04 | 2019-08-09 | 福州大学 | A kind of ruthenic oxide Quito pore electrod and preparation method thereof of graphene doping |
| CN107633953A (en) * | 2017-09-08 | 2018-01-26 | 西安科技大学 | A kind of multi-layered electrode and its ultracapacitor of preparation |
| CN107633953B (en) * | 2017-09-08 | 2019-10-15 | 西安科技大学 | A kind of multi-layered electrode and its supercapacitor of preparation |
| CN112670090A (en) * | 2020-12-24 | 2021-04-16 | 电子科技大学 | Electrode plate and preparation method and application thereof |
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