CN101269851A - Method for preparing ruthenium oxide electrode material - Google Patents
Method for preparing ruthenium oxide electrode material Download PDFInfo
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- CN101269851A CN101269851A CNA2008100239657A CN200810023965A CN101269851A CN 101269851 A CN101269851 A CN 101269851A CN A2008100239657 A CNA2008100239657 A CN A2008100239657A CN 200810023965 A CN200810023965 A CN 200810023965A CN 101269851 A CN101269851 A CN 101269851A
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Abstract
The invention relates to a preparation method of ruthenium oxide electrode material, which has the procedures that polyvinyl alcohol is added into RuCl3 water solution, then ammonium hydrogen carbonate NH4HCO3 or sodium bicarbonate NaHCO3 is added, thereby reacting to obtain the Ru(HCO3)3; the Ru(HCO3)3 prepared by washing fully by using deionized water is utilized to remove the polyvinyl alcohol, and the Ru(HCO3)3 is heated and decomposed and dehydrated under the condition of 200-220 DEG C to obtain RuO2; conductive acetylene black or carbon nanometer pipe with the weight being 10-40 percent of the RuO2 is added in the prepared RuO2, after being mixed fully, the ruthenium oxide electrode material can be prepared. The preparation method has the advantages of simple production process, high ruthenium oxide yield, and large output, the prepared electrode material has the characteristics of large capacity, low essential resistance, high crystallization temperature, and stable performance.
Description
One, technical field
The present invention relates to a kind of preparation method of ruthenium oxide electrode material, relate in particular to a kind of preparation method of electrochemical super-capacitor ruthenium oxide electrode material.
Two, background technology
Ultra-capacitor is meant and adopts high-specific surface area carbon material or RuO
2Make electrode Deng metal oxide containing precious metals, the electrochemical capacitor of the Senior Three to four of a volume ratio traditional capacitor order of magnitude.From the mechanism of store electrical energy, adopt the energy storage mechanism of the ultra-capacitor of material with carbon element to be based on the electric double layer capacitance that separation of charge produces on carbon electrode/electrolyte interface; Adopt RuO
2Ultra-capacitor electric capacity be on the oxide electrode surface and the redox reaction that takes place mutually of body and the adsorption capacitance that produces, because the generation mechanism of such electric capacity is different from electric double layer capacitance and follow the generation of charge transfer process, this electric capacity is called as pseudo capacitance.Under the situation of identical electrode area, the latter's ratio electric capacity is the former 10～100 times, but the former power characteristic of transient large current discharge is better than the latter.The preparation method of capacitance characteristic ruthenium oxide is varied at present, and method one is the ruthenium oxide film that forms on the titanium matrix by the pyrolysated method.Method two is to prepare ruthenium-oxide by electrochemistry anodic oxidation at the ruthenium matrix.Method three is to adopt the method for cathodic deposition to prepare the ruthenium oxide film on various metallic matrixes.Also having a kind of method is to adopt the standby unformed ruthenium-oxide of method legal system of ruthenic chloride and NaOH reaction.Though the ruthenium oxide of above-mentioned preparation method preparation all in various degree have a capacitance characteristic, but ubiquity preparation with the equipment complexity, the ruthenium oxide yield is low, output is little and the electrode materials capacity is on the low side and at 170 ℃ shortcomings such as crystallization and capacity reduction just take place, and is not suitable for the manufacturing in enormous quantities use of ultra-capacitor.
Three, technology contents
At above-mentioned shortcoming, the object of the present invention is to provide that a kind of production technique is simple, the ruthenium oxide yield high and preparation method that can mass-produced ruthenium oxide electrode material.
Technology contents of the present invention is, a kind of preparation method of ruthenium oxide electrode material, and its step is
(1), in 150～250ml concentration is the RuCl of 0.3～0.8mol/L
3The polyvinyl alcohol that adds 45～55g in the aqueous solution;
(2), in mentioned solution, add the carbonic hydroammonium NH that 150～250ml concentration is 1.0～2.0mol/L concentration
4HCO
3Or sodium acid carbonate NaHCO
3Solution, reaction makes Ru (HCO
3)
3
(3), fully wash the Ru (HCO that makes with deionized water
3)
3To remove polyvinyl alcohol wherein, again with Ru (HCO
3)
3Under 200～220 ℃ of conditions, add the thermal decomposition dehydration and obtain RuO
2
(4), at prepared RuO
2The middle RuO that adds
2Black or the CNT of 10%～40% conductive acetylene of weight namely makes ruthenium oxide electrode material after fully mixing.
The advantage that the present invention is compared with prior art had:
The present invention adopts and utilizes ruthenium chloride and sodium bicarbonate and bicarbonate of ammonia to be the reaction precursor body, and sol-gel method has prepared the ultra-fine ruthenium oxide electrode material of particle diameter less than 70nm.After 200～220 ℃ of lower heat-agglomeratings were processed, material had good surface characteristic and excellent electrochemistry capacitance characteristic and impedance operator with ruthenium oxide electrode material.When going into additive such as the black or carbon nanotube of an amount of conductive acetylene when the admixture in the above-mentioned ruthenium oxide material, the electrochemical properties of combination electrode material be improved significantly.Advantages such as aforesaid method has that technology is simple, ruthenium oxide yield height, output are big, prepared electrode materials have that capacity is big, and internal resistance is low, the crystallization temperature height, and characteristics such as stable performance are suitable as the electrode materials of ultra-capacitor very much.
Four, specific embodiment
Example 1, be the RuCl of 0.5mol/L in concentration
3The pure polyvinyl alcohol of Additive analysis that adds 50g among the aqueous solution 200ml; Adding 200ml concentration in mentioned solution is the carbonic hydroammonium NH of 1.5mol/L
4HCO
3Solution, question response make Ru (HCO
3)
3Adopt deionized water fully to wash Ru (HCO
3)
3To remove polyvinyl alcohol wherein; With gained Ru (HCO
3)
3Under 210 ℃ of conditions, add the thermal decomposition dehydration and obtain RuO
2At prepared RuO
2Add RuO in the material
2The black additive of the conductive acetylene of weight 20% also fully namely makes ruthenium oxide electrode material after the mixing.
Example 2, be the RuCl of 0.5mol/L in concentration
3The pure polyvinyl alcohol of Additive analysis that adds 50g among the aqueous solution 200ml; Adding 200ml concentration in mentioned solution is the sodium acid carbonate NaHCO of 1.5mol/L
3Solution, question response make Ru (HCO
3)
3Adopt deionized water fully to wash Ru (HCO
3)
3To remove polyvinyl alcohol wherein; With gained Ru (HCO
3)
3Under 210 ℃ of conditions, add the thermal decomposition dehydration and obtain RuO
2At prepared RuO
2Add RuO in the material
2The CNT additive of weight 25% also fully namely makes ruthenium oxide electrode material after the mixing.
Claims (1)
1, a kind of preparation method of ruthenium oxide electrode material, its step is
(1), in 150～250ml concentration is the RuCl of 0.3～0.8mol/L
3The polyvinyl alcohol that adds 45～55g in the aqueous solution;
(2), in mentioned solution, add the carbonic hydroammonium NH that 150～250ml concentration is 1.0～2.0mol/L concentration
4HCO
3Or sodium acid carbonate NaHCO
3Solution, reaction makes Ru (HCO
3)
3
(3), fully wash the Ru (HCO that makes with deionized water
3)
3To remove polyvinyl alcohol wherein, again with Ru (HCO
3)
3Under 200～220 ℃ of conditions, add the thermal decomposition dehydration and obtain RuO
2
(4), at the above-mentioned RuO that makes
2The middle RuO that adds
2Black or the CNT of 10～40% conductive acetylenes of weight namely makes ruthenium oxide electrode material after fully mixing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100239657A CN101269851A (en) | 2008-04-23 | 2008-04-23 | Method for preparing ruthenium oxide electrode material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100239657A CN101269851A (en) | 2008-04-23 | 2008-04-23 | Method for preparing ruthenium oxide electrode material |
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| Publication Number | Publication Date |
|---|---|
| CN101269851A true CN101269851A (en) | 2008-09-24 |
Family
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|---|---|---|---|
| CNA2008100239657A Pending CN101269851A (en) | 2008-04-23 | 2008-04-23 | Method for preparing ruthenium oxide electrode material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923797A (en) * | 2012-11-06 | 2013-02-13 | 上海奥威科技开发有限公司 | Method for preparing high-dispersion high-activity hydration ruthenium dioxide electrode material |
| CN103887078A (en) * | 2014-03-04 | 2014-06-25 | 成都达艾斯科技有限公司 | Preparation method for ruthenium-oxide-based electrode material |
| CN105632789A (en) * | 2016-03-21 | 2016-06-01 | 贵州理工学院 | Preparation method of composite electrode material for super capacitor |
| CN106395922A (en) * | 2016-08-30 | 2017-02-15 | 昆明贵容电子材料有限公司 | Preparation method of high purity ultrafine ruthenium oxide |
| CN106587180A (en) * | 2016-11-22 | 2017-04-26 | 昆明理工大学 | Method for preparing ruthenium dioxide for resistance paste |
| CN106952745A (en) * | 2017-03-14 | 2017-07-14 | 苏州海凌达电子科技有限公司 | A kind of preparation method of ultracapacitor ruthenium-oxide based combined electrode material |
| CN107758751A (en) * | 2017-10-27 | 2018-03-06 | 潮州三环（集团）股份有限公司 | A kind of preparation method of resistance slurry ruthenic oxide |
| CN109659163A (en) * | 2018-12-18 | 2019-04-19 | 清华大学 | Laminated structure supercapacitor and preparation method with resistance to high acceleration shock |
| CN110117797A (en) * | 2018-02-07 | 2019-08-13 | 中国科学院福建物质结构研究所 | A kind of electrolytic cell and its application in water electrolysis hydrogen production |
-
2008
- 2008-04-23 CN CNA2008100239657A patent/CN101269851A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923797A (en) * | 2012-11-06 | 2013-02-13 | 上海奥威科技开发有限公司 | Method for preparing high-dispersion high-activity hydration ruthenium dioxide electrode material |
| CN103887078A (en) * | 2014-03-04 | 2014-06-25 | 成都达艾斯科技有限公司 | Preparation method for ruthenium-oxide-based electrode material |
| CN105632789B (en) * | 2016-03-21 | 2018-07-10 | 贵州理工学院 | The preparation method of composite electrode material for super capacitor |
| CN105632789A (en) * | 2016-03-21 | 2016-06-01 | 贵州理工学院 | Preparation method of composite electrode material for super capacitor |
| CN106395922A (en) * | 2016-08-30 | 2017-02-15 | 昆明贵容电子材料有限公司 | Preparation method of high purity ultrafine ruthenium oxide |
| CN106395922B (en) * | 2016-08-30 | 2017-09-19 | 昆明贵容电子材料有限公司 | A kind of preparation method of high pure and ultra-fine ruthenium-oxide |
| CN106587180B (en) * | 2016-11-22 | 2018-05-11 | 昆明理工大学 | A kind of resistance slurry ruthenic oxide preparation method |
| CN106587180A (en) * | 2016-11-22 | 2017-04-26 | 昆明理工大学 | Method for preparing ruthenium dioxide for resistance paste |
| CN106952745A (en) * | 2017-03-14 | 2017-07-14 | 苏州海凌达电子科技有限公司 | A kind of preparation method of ultracapacitor ruthenium-oxide based combined electrode material |
| CN107758751A (en) * | 2017-10-27 | 2018-03-06 | 潮州三环（集团）股份有限公司 | A kind of preparation method of resistance slurry ruthenic oxide |
| CN110117797A (en) * | 2018-02-07 | 2019-08-13 | 中国科学院福建物质结构研究所 | A kind of electrolytic cell and its application in water electrolysis hydrogen production |
| CN110117797B (en) * | 2018-02-07 | 2020-10-02 | 中国科学院福建物质结构研究所 | Electrolytic cell and application thereof in hydrogen production by electrolyzing water |
| CN109659163A (en) * | 2018-12-18 | 2019-04-19 | 清华大学 | Laminated structure supercapacitor and preparation method with resistance to high acceleration shock |
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Open date: 20080924 |