CN102903528B - Method for rapidly preparing conducting carbon and ruthenium oxide combination electrode material - Google Patents
Method for rapidly preparing conducting carbon and ruthenium oxide combination electrode material Download PDFInfo
- Publication number
- CN102903528B CN102903528B CN201210321459.2A CN201210321459A CN102903528B CN 102903528 B CN102903528 B CN 102903528B CN 201210321459 A CN201210321459 A CN 201210321459A CN 102903528 B CN102903528 B CN 102903528B
- Authority
- CN
- China
- Prior art keywords
- ruthenium
- electrode material
- conducting carbon
- ruthenium oxide
- conductive carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention provides a method for rapidly preparing a conducting carbon and ruthenium oxide combined electrode material. The method comprises (1) adding a conducting carbon material into distilled water, and performing ultrasonic dispersion to prepare dispersed liquid of the conducting carbon material; (2) adding a ruthenium-containing precursor into the dispersed liquid obtained in the step (1), and mixing to enable the ruthenium-containing precursor to be dissolved totally; (3) performing heating treatment on the obtained mixed liquid, and obtaining black precipitates; (4) filtering and washing the black precipitates obtained in the step (3), and obtaining the conducting carbon and ruthenium oxide combined electrode material after vacuum drying. The preparation method for rapidly preparing the conducting carbon and ruthenium oxide combined electrode material is simple in process, simple and convenient to operate, low in cost, rapid, energy-saving and enables mass production to be achieved. The prepared material not only has good electrical conductivity, but also enables ruthenium oxide to be highly dispersed on the surface of the conducting carbon in a nanoscale ion mode, and the electrochemical utilization rate of ruthenium oxide is remarkably improved.
Description
Technical field
That the present invention relates to is a kind of preparation method of nano-electrode material.Be specifically related to a kind of quick method preparing conductive carbon/ruthenium-oxide combination electrode material.
Background technology
21 century, energy problem is unquestionable is the huge challenge that countries in the world face.Day by day exhausted along with the increasingly serious of the Climatic issues such as global warming and conventional fossil fuel, the demand of people to clean traffic and clean energy resource becomes particularly urgent.Ultracapacitor is a kind of novel novel energy-storing device between storage battery and conventional dielectric capacitor, is widely used in the every field such as automobile, electronics, communication, by countries in the world institute extensive concern.According to the difference of energy storage mechnism, ultracapacitor can be divided into two types: double electric layer capacitor and Faraday pseudo-capacitance device.The former is the electric double layer produced based on electrode (active carbon with high specific surface area)/electrolyte interface separation of charge, the latter be the surface of electrode or body mutually in two dimension or accurate two-dimensional space on, electroactive material carries out underpotential deposition, there is chemical adsorption desorption or the redox reaction of high reversible, produce the electric capacity relevant with electrode charge current potential.When identical electrodes area, its capacity is tens times of electric double layer capacitance.In various electrode material, ruthenium oxide electrode material not only has high theoretical specific capacity (> 1000F/g) and high conductivity, and there is wider electrochemical window and excellent electrochemical cycle stability, therefore, a kind of electrode material for super capacitor of excellent performance is acknowledged as.But ruthenium-oxide is not only expensive, and the aggregate that as easy as rolling off a log formation is larger in preparation process, significantly reduce the electrochemical utilization rate of ruthenium-oxide, cause its chemical property to be deteriorated, thus suppress its large-scale commercial applications.In order to make full use of ruthenium-oxide electrochemical utilization rate, reduce costs, with various conductive carbon (carbon nano-tube, Graphene etc.) for basis material, prepare the extensive concern that homodisperse ruthenium-oxide nano composite material receives people.At present, the preparation method of carbon/ruthenium-oxide mainly contains following several: (1) adopts conventional method, join in ruthenium trichloride solution by material with carbon element, then adopt alkali lye to precipitate ruthenium trichloride, then carry out hydro-thermal reaction and prepare carbon load ruthenium-oxide (Chinese Patent Application No.: 201010295214.8); (2) adopt oxidant direct oxidation ruthenium trichloride, join in ruthenium trichloride solution by material with carbon element, then adopt oxidant eremacausis ruthenium trichloride to prepare the ruthenium-oxide (Chinese Patent Application No.: 200610033782.4) of carbon load.But, above-mentioned two kinds of methods not only complex process, and consuming time, energy resource consumption is large, is difficult to realize suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide that a kind of technique is relatively simple, easy and simple to handle, with low cost, fast energy-saving and the quick method preparing conductive carbon and ruthenium-oxide combination electrode material that can be mass-produced.
The object of the present invention is achieved like this:
(1) join in distilled water by conductive carbon material, ultrasonic disperse prepares the dispersion liquid of conductive carbon material;
(2) will join in the dispersion liquid of step (1) gained containing ruthenium predecessor, and stir and make it to dissolve completely;
(3) mixed liquor of step (2) gained is carried out heat treated, obtain black precipitate;
(4) black precipitate of step (3) gained filtered, wash, namely vacuumize obtain conductive carbon and ruthenium-oxide combination electrode material.
The present invention can also comprise:
1, described conductive carbon material is one or more the arbitrary proportion mixture in conductive black, carbon nano-tube, carbon fiber or Graphene.
The concentration of the dispersion liquid of 2, described conductive carbon material is 0.001-0.1g/mL, and the time of described ultrasonic disperse is 0.1-20h.
3, described ruthenium predecessor is KRuO
4.
4, conductive carbon material and KRuO
4weight ratio be 1:0.1-1:200.
5, described heat treated is microwave heating, and power is 400-2000W, and microwave heating time is 1-30min.
6, described vacuum drying baking temperature is 60-150 DEG C, and drying time is 2-48h.
For with Problems existing in current techique, the present invention proposes that a kind of technique is relatively simple, easy and simple to handle, with low cost, fast energy-saving and the preparation method of the conductive carbon that can be mass-produced/ruthenium-oxide combination electrode material.Conductive carbon/ruthenium-oxide composite material prepared by this method, not only has good conductivity, and makes ruthenium-oxide be highly dispersed at the surface of conductive carbon with nano level ion, significantly improve the electrochemical utilization rate of ruthenium-oxide.It can be used as electrode material for super capacitor, not only there is high specific capacity, good power characteristic, and there is good electrochemical cycle stability.
Compared with prior art, tool of the present invention has the following advantages:
The preparation method of conductive carbon/ruthenium-oxide combination electrode material that the present invention proposes has that technique is simple, easy and simple to handle, with low cost, preparation process environmental friendliness, fast energy-saving and the advantage that can be mass-produced.Compared with traditional handicraft, the complicated technology of reprocessing after the preparation method that the present invention proposes precipitates without traditional ruthenium trichloride and alkaline matter, prepared ruthenium-oxide particle is more tiny, more even at the Dispersion on surface of conductive carbon material, and the productive rate of ruthenium-oxide is higher.The features such as prepared electrode material has that specific capacity is high, internal resistance is low, energy density and power density is high, good cycling stability, therefore this electrode material is expected to be applied to the fields such as hybrid-electric car as the high performance electrode material for super capacitor of one, will have wide prospects for commercial application.
Accompanying drawing explanation
The specific capacity curve of Fig. 1 conductive carbon prepared by the embodiment of the present invention 6/ruthenium-oxide combination electrode material.
The cycle life curve of Fig. 2 conductive carbon prepared by the embodiment of the present invention 6/ruthenium-oxide combination electrode material.
Embodiment
The present invention is described further in citing below:
Conductive carbon material and KRuO
4weight ratio generally at 5:1-1:200.
Embodiment 1
(A) preparation of conductive carbon/ruthenium oxide electrode material
First, 0.1g carbon nano-tube is joined in 100mL distilled water, ultrasonic 1h, then take 20g KRuO
4, join in above-mentioned mixed liquor, stir and make it fully dissolve, being placed in power is until completely dissolved that the microwave heating equipment of 1000W heats 1min; The black precipitate obtained is filtered, fully washed, 60 DEG C of vacuumize 48h, obtains conductive carbon/ruthenium-oxide combination electrode material.
(B) the preparation and property test of electrode
Obtained combination electrode material, conductive black, polytetrafluoroethylene (5wt%), ethanol are mixed according to the ratio of 80:10:5:5 and makes slurry, evenly be coated on stainless steel collector, 110 DEG C of vacuumize 10h, with 1mol/L sulfuric acid solution for electrolyte, adopt three-electrode system, the specific capacity of cyclic voltammetry composite material.
Embodiment 2
By 0.5g carbon nano-tube and 0.5g conductive black, join in 10mL distilled water, ultrasonic 10h, then take 0.1g KRuO
4, join in above-mentioned mixed liquor, stir and make it fully dissolve, being placed in power is until completely dissolved that the microwave heating equipment of 400W heats 30min; The black precipitate obtained is filtered, fully washed, 120 DEG C of vacuumize 2h, obtains conductive carbon/ruthenium-oxide combination electrode material.The preparation of electrode and method of testing are with embodiment 1.
Embodiment 3
By 0.1g conductive black, join in 50mL distilled water, ultrasonic 6h, then take 1g KRuO
4, join in above-mentioned mixed liquor, stir and make it fully dissolve, being placed in power is until completely dissolved that the microwave heating equipment of 600W heats 10min; The black precipitate obtained is filtered, fully washed, 80 DEG C of vacuumize 10h, obtains conductive carbon/ruthenium-oxide combination electrode material.The preparation of electrode and method of testing are with embodiment 1.
Embodiment 4
By 0.08g conductive carbon fibres peacekeeping 0.02g Graphene, join in 50mL distilled water, ultrasonic 15h, then take 2g KRuO
4, join in above-mentioned mixed liquor, stir and make it fully dissolve, being placed in power is until completely dissolved that the microwave heating equipment of 1000W heats 4min; The black precipitate obtained is filtered, fully washed, 120 DEG C of vacuumize 6h, obtains conductive carbon/ruthenium-oxide combination electrode material.The preparation of electrode and method of testing are with embodiment 1.
Embodiment 5
By 0.1g conductive carbon fibre, join in 50mL distilled water, ultrasonic 0.1h, then take 1.5g KRuO
4, join in above-mentioned mixed liquor, stir and make it fully dissolve, being placed in power is until completely dissolved that the microwave heating equipment of 2000W heats 6min; The black precipitate obtained is filtered, fully washed, 150 DEG C of vacuumize 8h, obtains conductive carbon/ruthenium-oxide combination electrode material.The preparation of electrode and method of testing are with embodiment 1.
Embodiment 6
By 0.1g Graphene, join in 100mL distilled water, ultrasonic 20h, then take 10g KRuO
4, join in above-mentioned mixed liquor, stir and make it fully dissolve, being placed in power is until completely dissolved that the microwave heating equipment of 700W heats 5min; The black precipitate obtained is filtered, fully washed, 100 DEG C of vacuumize 12h, obtains conductive carbon/ruthenium-oxide combination electrode material.The preparation of electrode and method of testing are with embodiment 1.
Claims (1)
1. prepare a method for conductive carbon and ruthenium-oxide combination electrode material fast, it is characterized in that: by 0.1g Graphene, join in 100mL distilled water, ultrasonic 20h, then take 10g KRuO
4, join in above-mentioned mixed liquor, stir and make it fully dissolve, being placed in power is until completely dissolved that the microwave heating equipment of 700W heats 5min; The black precipitate obtained is filtered, fully washed, 100 DEG C of vacuumize 12h, obtains conductive carbon/ruthenium-oxide combination electrode material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210321459.2A CN102903528B (en) | 2012-04-25 | 2012-09-03 | Method for rapidly preparing conducting carbon and ruthenium oxide combination electrode material |
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210124375.X | 2012-04-25 | ||
| CN201210124375 | 2012-04-25 | ||
| CN201210124375X | 2012-04-25 | ||
| CN201210321459.2A CN102903528B (en) | 2012-04-25 | 2012-09-03 | Method for rapidly preparing conducting carbon and ruthenium oxide combination electrode material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102903528A CN102903528A (en) | 2013-01-30 |
| CN102903528B true CN102903528B (en) | 2015-05-27 |
Family
ID=47575722
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210321459.2A Expired - Fee Related CN102903528B (en) | 2012-04-25 | 2012-09-03 | Method for rapidly preparing conducting carbon and ruthenium oxide combination electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102903528B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103996546A (en) * | 2013-02-20 | 2014-08-20 | 海洋王照明科技股份有限公司 | Graphene composite material and preparation method thereof, electrochemical capacitor and electrode thereof |
| CN105655133A (en) * | 2016-03-30 | 2016-06-08 | 电子科技大学 | Cathode material of composite tantalum capacitor and preparation method of cathode material |
| CN109110793A (en) * | 2018-03-22 | 2019-01-01 | 云南大学 | A kind of preparation method of alumina load nano-cerium oxide compound gold and ru oxide |
| CN110057486B (en) * | 2019-04-15 | 2020-12-18 | 绍兴文理学院元培学院 | Preparation process of ceramic thick film pressure sensor |
| CN113077998B (en) * | 2021-03-22 | 2022-07-12 | 西安交通大学 | Ruthenium dioxide/graphene composite electrode for supercapacitor and preparation method thereof |
| CN114121336B (en) * | 2022-01-27 | 2022-04-19 | 西安宏星电子浆料科技股份有限公司 | High-wear-resistance paste |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5797971A (en) * | 1994-12-09 | 1998-08-25 | The United States Of America As Represented By The Secretary Of The Army | Method of making composite electrode materials for high energy and high power density energy storage devices |
| CN101599370A (en) * | 2009-04-23 | 2009-12-09 | 哈尔滨工程大学 | A kind of quick method for preparing conductive carbon/manganese dioxide composite electrode material |
-
2012
- 2012-09-03 CN CN201210321459.2A patent/CN102903528B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5797971A (en) * | 1994-12-09 | 1998-08-25 | The United States Of America As Represented By The Secretary Of The Army | Method of making composite electrode materials for high energy and high power density energy storage devices |
| CN101599370A (en) * | 2009-04-23 | 2009-12-09 | 哈尔滨工程大学 | A kind of quick method for preparing conductive carbon/manganese dioxide composite electrode material |
Non-Patent Citations (1)
| Title |
|---|
| "Ru oxide/carbon nanotube composites for supercapacitors prepared by spontaneous reduction of Ru(VI) and Ru(VII)";Xiaorong Liu et al.;《Electrochimica Acta》;20090723;第54卷(第27期);第7141–7147页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102903528A (en) | 2013-01-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101527202B (en) | Oxidized grapheme/polyaniline super capacitor composite electrode material and preparation method | |
| CN102903528B (en) | Method for rapidly preparing conducting carbon and ruthenium oxide combination electrode material | |
| CN102543464B (en) | ZnO/reduced graphene oxide/polypyrrole ternary composite material preparation method, and application of the ternary composite material | |
| CN101599370B (en) | Method for fast preparing conductive carbon/manganese dioxide composite electrode material | |
| CN101800131B (en) | Active carbon-based material and preparation method thereof | |
| CN103326007B (en) | The preparation method of three-dimensional graphite thiazolinyl tin dioxide composite material and application thereof | |
| CN103723721B (en) | A kind of preparation method of graphene oxide modification activated carbon for super capacitors | |
| CN103594254A (en) | Method for preparing manganese dioxide/mesoporous carbon nanometer graded composite electrode material | |
| CN103788646B (en) | Nitrogen-doped graphene/cobalt ferrite/polyaniline nano-composite material and preparation method thereof | |
| CN103787320B (en) | The Synthesis and applications of the carbon nanosheet material of one kind graphene sheet layer structure | |
| CN104176783B (en) | The preparations and applicatio method of the coated manganese dioxide nanowire of a kind of nitrogen carbon material | |
| CN102915844B (en) | A kind of method and application thereof preparing the hierarchical composite material of carbon plate/manganese dioxide nano-plates | |
| CN106207279A (en) | A kind of preparation method of lead crystalline substance carbon accumulator | |
| CN105206430B (en) | Polyaniline nanotube array/graphene composite material electrode and its preparation method and application | |
| CN106345501B (en) | A kind of method that iron phosphide is prepared based on the carbon nano-tube modified composite material of magnetic ionic liquids and products thereof and application | |
| CN103680993A (en) | Preparation method for 3D Ni-Co bimetallic hydroxide hollow microsphere and application in super capacitor | |
| CN103871755A (en) | N-doped graphene/nickel ferrite nanometer compound material and preparation thereof | |
| CN101696323A (en) | Method for preparing polyaniline/manganese dioxide composite material for super capacitor | |
| CN104681300B (en) | Polyaniline-sulfonated graphene composite electrode material and preparation method thereof | |
| CN103887080B (en) | Nanocomposite material of nitrogen doped with graphene/copper ferrite and preparation method thereof | |
| CN103214845B (en) | Boron doped graphene-polyaniline nanocomposite and preparation method thereof | |
| CN105788881B (en) | A kind of preparation method of nitrogen doped corrugated carbon nanotube | |
| CN103366972B (en) | The preparation method of a kind of multi-walled carbon nano-tubes/polyaniline nano fiber composite supercapacitor electrode | |
| CN104078247B (en) | Composite electrode material vanadium trioxide or carbon for super capacitor and preparation method thereof | |
| CN103723720B (en) | A kind of preparation method being applicable to the Graphene modified activated carbon of ultracapacitor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150527 Termination date: 20210903 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |