CN102294239A - Metal nano electro-catalyst for redox reaction of fuel cell, and preparation method and application thereof - Google Patents
Metal nano electro-catalyst for redox reaction of fuel cell, and preparation method and application thereof Download PDFInfo
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Abstract
A preparation method of a metal nano electro-catalyst for a redox reaction of a fuel cell. A complexing agent of EDTA and a reducing agent of NaBH4 are employed to reduce a mixed solution of H2PtCl6 and powdered carbon or a mixed solution of H2PtCl6 and CoCl2 and NiCl2 and powdered carbon to carbon-loaded metal nano catalyst particles through a one-step hydrothermal method. The catalyst particles are separated, washed, added with absolute ethyl alcohol and a Nafion solution and dispersed by ultrasonic to a paste, which is pasted on a titanium sheet surface to prepare a corresponding carbon-loaded nano platinum electrode (Pt/C) and a carbon-loaded nano platinum-cobalt-nickel electrode (PtCoNi/C). The ternary platinum-cobalt-nickel metal nano electro-catalyst of the invention has an obviously decreased platinum content, but an initial potential and a current density of a redox reaction much higher than those of a crystal platinum electrode and a Pt/C electrode. The electrode material of the present invention not only has excellent catalytic activity to the redox reaction, but also substantially reduces a usage amount of the precious metal platinum; besides the electrode material is simply prepared, has a stable structure and can be widely used in fuel cells.
Description
Technical field
The invention belongs to fuel cell technology and new energy materials technical field, be specifically related to a kind of carbon and carry platinum-cobalt-nickel ternary metal nanometer electrical catalyst particle and its production and application.
Background technology
Fuel cell is one of direction of giving priority to of new energy field, and advantage such as it has efficiently, cleaning and low noise has been subjected to national governments and scientist's great attention.The oxidant that fuel cell adopts is generally oxygen, so oxygen reduction reaction has just constituted a very important reaction in the fuel cell operation process.The metal that oxygen reduction reaction is had excellent electro catalytic activity is metal platinum (Pt), but platinum is a kind of expensive metal, thereby has greatly limited its practical application in fuel cell.Therefore with platinum and other low price and common metal composition metal alloy or compound, use it for the eelctro-catalyst of oxygen reduction reaction, not only greatly reduce the consumption of platinum, but also the electro catalytic activity of enhancing platinum, this is a main direction of fuel cell oxygen reduction reaction eelctro-catalyst exploitation, and the practical application of fuel cell is had great importance.The present invention adopts hydro-thermal method, in the presence of reducing agent, be deposited on metal platinum, cobalt and nickel on the carbon dust together, form platinum-cobalt-nickel ternary nano metal catalyst particles that carbon carries, this catalyst granules not only greatly reduces the consumption of metal platinum, and they increase significantly with respect to pure nano-platinum particle for the electro catalytic activity of oxygen reduction reaction.
Summary of the invention
The purpose of this invention is to provide a kind of carbon that is used for the fuel cell oxygen reduction reaction and carry platinum-cobalt-nickel ternary metal nanometer electrical catalyst, its take-off potential to oxygen reduction reaction is significantly increased (shuffling), the oxygen reduction reaction current density is significantly increased, and the consumption of metal platinum descends greatly in this ternary metal nanometer electrical catalyst.
The objective of the invention is also to have supplied a kind of carbon that is used for the fuel cell oxygen reduction reaction to carry the preparation method of platinum-cobalt-nickel ternary metal nanometer electrical catalyst.
For achieving the above object, embodiment of the present invention are: a kind of preparation method who is used for the metal nano eelctro-catalyst of fuel cell oxygen reduction reaction, make complexing agent with EDTA, NaBH
4Make reducing agent, adopt one step of hydro-thermal method H
2PtCl
6+ carbon dust mixed solution is reduced into the carbon-supported metal nanocatalyst; Below the concrete steps:
(1) with H
2PtCl
6Solution places hydrothermal reaction kettle, adds complexing agent EDTA and Vulcan XC-72 carbon dust successively, carries out ultrasonic processing at normal temperatures, drips NaBH
4Solution; The amount of described Vulcan XC-72 carbon dust is 40 ~ 60% of a metal catalyst particles Pt quality;
(2) reactor is heated to 140 ~ 200
oKept behind the C 6 ~ 12 hours;
(3) after reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle are washed with absolute ethyl alcohol with pure water successively and are washed, and promptly obtain carbon-supported nano Pt metal nano eelctro-catalyst;
Described H
2PtCl
6The concentration of solution is 2 ~ 10 mM, and the concentration of complexing agent EDTA is 40 ~ 200 mM, and the time of ultrasonic processing is 5 ~ 20 min, NaBH
4The mass percentage concentration of solution is 3 ~ 10%.
A kind of preparation method who is used for the metal nano eelctro-catalyst of fuel cell oxygen reduction reaction makes complexing agent with EDTA, NaBH
4Make reducing agent, adopt one step of hydro-thermal method H
2PtCl
6+ CoCl
2+ NiCl
2+ carbon dust mixed solution is reduced into the carbon-supported metal nanocatalyst; Below the concrete steps:
(1) with H
2PtCl
6+ CoCl
2+ NiCl
2Solution places hydrothermal reaction kettle, adds complexing agent EDTA and Vulcan XC-72 carbon dust successively, carries out ultrasonic processing at normal temperatures, drips NaBH
4Solution; The amount of described Vulcan XC-72 carbon dust is 40 ~ 60% of a metal catalyst particles Pt+Co+Ni gross mass;
(2) reactor is heated to 140 ~ 200
oKept behind the C 6 ~ 12 hours;
(3) after reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle are washed with absolute ethyl alcohol with pure water successively and are washed, and promptly obtain carbon-supported nano Pt+Co+Ni metal nano eelctro-catalyst;
Described H
2PtCl
6The concentration of solution is 2 ~ 10 mM, CoCl
2Concentration be 0.8 ~ 4 mM, NiCl
2Concentration be 0.8 ~ 4 mM, the concentration of complexing agent EDTA is 40 ~ 200 mM, the time of ultrasonic processing is 5 ~ 20 min, NaBH
4The mass percentage concentration of solution is 3 ~ 10%.
Described pure water is washed and is: wash twice with pure water, each 1mL; Described absolute ethyl alcohol is washed and is: wash twice with absolute ethyl alcohol, each 1mL.
A kind of metal nano eelctro-catalyst for preparing according to the preparation method of the above-mentioned metal nano eelctro-catalyst that is used for the fuel cell oxygen reduction reaction.
The metal nano eelctro-catalyst is as the application of carbon-supported nano platinum electrode (Pt/C) and carbon-supported nano platinum-cobalt-nickel electrode (PtCoNi/C), concrete grammar is: described carbon-supported nano Pt or carbon are carried platinum-cobalt-nickel ternary metal nanometer electrical catalyst mix with absolute ethyl alcohol, add Nafion(mass percent 5%) solution, then the ultrasonic processing of mixture back is formed pastel, at last this pastel is dripped in titanium plate surface, dry back is as working electrode.
The present invention adopts hydro-thermal method, in the presence of reducing agent, be deposited on metal platinum, cobalt and nickel on the carbon dust together, form platinum-cobalt-nickel ternary nano metal catalyst particles that carbon carries, the platinum content of this three-way catalyst particle has only 70% ~ 83% of pure nano-platinum particle, and they the take-off potential of oxygen reduction reaction has been shifted to an earlier date 60 ~ 70mV, oxygen reduction reaction current density with respect to pure nano-platinum particle is 2 ~ 2.5 times of pure nano-platinum particle.
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Description of drawings
Fig. 1 is the linear scan curve of the prepared carbon-supported nano Pt catalyst of embodiment 1 to oxygen reduction reaction;
Fig. 2 is the linear scan curve of the prepared carbon-supported nano Pt catalyst of embodiment 2 to oxygen reduction reaction;
Fig. 3 is the linear scan curve of the prepared carbon-supported nano Pt catalyst of embodiment 3 to oxygen reduction reaction;
Fig. 4 is the linear scan curve of the prepared carbon-supported nano Pt-Co-Ni catalyst of embodiment 4 to oxygen reduction reaction;
Fig. 5 is the linear scan curve of the prepared carbon-supported nano Pt-Co-Ni catalyst of embodiment 5 to oxygen reduction reaction;
Fig. 6 is the linear scan curve of the prepared carbon-supported nano Pt-Co-Ni catalyst of embodiment 6 to oxygen reduction reaction.
The specific embodiment
With concentration is the H of 2 mM
2PtCl
6Solution 20 mL place hydrothermal reaction kettle, and adding concentration successively is 40 mM complexing agent EDTA 1 mL and Vulcan XC-72 carbon dust 5 mg, carries out ultrasonic processing 5 min then at normal temperatures, drip mass percentage concentration afterwards and be 3% NaBH
4Solution 2 ml; Then reactor is heated to 140
o Kept 6 hours behind the C; After reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle washes twice with pure water and absolute ethyl alcohol successively, promptly obtains carbon-supported nano Pt eelctro-catalyst; 5 mg mix with 1 mL absolute ethyl alcohol with this carbon-supported nano Pt eelctro-catalyst, add Nafion(mass percent 5%) solution 50 mL, to form pastel behind the ultrasonic processing of the mixture 30min then, at last this pastel is dripped in titanium plate surface, its electro catalytic activity to oxygen reduction reaction is measured as working electrode in dry back in 0.5 M sulfuric acid solution.Constantly aerating oxygen, sweep speed 1 mV/s, corresponding linear scanning curve are seen Fig. 1 in 0.5 M sulfuric acid solution.The oxygen reduction reaction take-off potential is 0.6 V..
With concentration is the H of 5 mM
2PtCl
6Solution 20 mL place hydrothermal reaction kettle, and adding concentration successively is 100 mM complexing agent EDTA 1 mL and Vulcan XC-72 carbon dust 8 mg, carries out ultrasonic processing 10 min then at normal temperatures, drip mass percentage concentration afterwards and be 6% NaBH
4Solution 2 ml; Then reactor is heated to 180
o Kept 8 hours behind the C; After reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle washes twice with pure water and absolute ethyl alcohol successively, promptly obtains carbon-supported nano Pt eelctro-catalyst; 5 mg mix with 1 mL absolute ethyl alcohol with this carbon-supported nano Pt eelctro-catalyst, add Nafion(mass percent 5%) solution 50 mL, to form pastel behind the ultrasonic processing of the mixture 30min then, at last this pastel is dripped in titanium plate surface, its electro catalytic activity to oxygen reduction reaction is measured as working electrode in dry back in 0.5 M sulfuric acid solution.Constantly aerating oxygen, sweep speed 1 mV/s, corresponding linear scanning curve are seen Fig. 2 in 0.5 M sulfuric acid solution.The oxygen reduction reaction take-off potential is 0.6 V.
With concentration is the H of 10 mM
2PtCl
6Solution 20 mL place hydrothermal reaction kettle, and adding concentration successively is 200 mM complexing agent EDTA 1 mL and Vulcan XC-72 carbon dust 12 mg, carries out ultrasonic processing 20 min then at normal temperatures, drip mass percentage concentration afterwards and be 10% NaBH
4Solution 2 ml; Then reactor is heated to 200
o Kept 12 hours behind the C; After reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle washes twice with pure water and absolute ethyl alcohol successively, promptly obtains carbon-supported nano Pt eelctro-catalyst; 5 mg mix with 1 mL absolute ethyl alcohol with this carbon-supported nano Pt eelctro-catalyst, add Nafion(mass percent 5%) solution 50 mL, to form pastel behind the ultrasonic processing of the mixture 30min then, at last this pastel is dripped in titanium plate surface, its electro catalytic activity to oxygen reduction reaction is measured as working electrode in dry back in 0.5 M sulfuric acid solution.Constantly aerating oxygen, sweep speed 1 mV/s, corresponding linear scanning curve are seen Fig. 3 in 0.5 M sulfuric acid solution.The oxygen reduction reaction take-off potential is 0.6 V.
Embodiment 4:
With concentration is the H of 2 mM
2PtCl
6Solution 20 mL, 0.8 mM CoCl
2Solution 30mL and 0.8 mM NiCl
2Solution 30mL places hydrothermal reaction kettle, and adding concentration successively is 40 mM complexing agent EDTA 2.2 mL and Vulcan XC-72 carbon dust 5 mg, carries out ultrasonic processing 5 min then at normal temperatures, drips mass percentage concentration afterwards and be 3% NaBH
4Solution 3 ml; Then reactor is heated to 140
o Kept 6 hours behind the C; After reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle washes twice with pure water and absolute ethyl alcohol successively, promptly obtains carbon-supported nano Pt-Co-Ni eelctro-catalyst; 5 mg mix with 1 mL absolute ethyl alcohol with this carbon-supported nano Pt-Co-Ni eelctro-catalyst, add Nafion(mass percent 5%) solution 50 mL, to form pastel behind the ultrasonic processing of the mixture 30min then, at last this pastel is dripped in titanium plate surface, its electro catalytic activity to oxygen reduction reaction is measured as working electrode in dry back in 0.5 M sulfuric acid solution.Constantly aerating oxygen, sweep speed 1 mV/s, corresponding linear scanning curve are seen Fig. 4 in 0.5 M sulfuric acid solution.The oxygen reduction reaction take-off potential is 0.6 V, and the current density when current potential is 0.2V is 2 times among Fig. 1-3.
With concentration is the H of 5 mM
2PtCl
6Solution 20 mL, 2 mM CoCl
2Solution 15 mL and 2 mM NiCl
2Solution 15mL places hydrothermal reaction kettle, and adding concentration successively is 100 mM complexing agent EDTA 1.6 mL and Vulcan XC-72 carbon dust 8 mg, carries out ultrasonic processing 10 min then at normal temperatures, drips mass percentage concentration afterwards and be 6% NaBH
4Solution 3 ml; Then reactor is heated to 180
o Kept 8 hours behind the C; After reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle washes twice with pure water and absolute ethyl alcohol successively, promptly obtains carbon-supported nano Pt-Co-Ni eelctro-catalyst; 5 mg mix with 1 mL absolute ethyl alcohol with this carbon-supported nano Pt-Co-Ni eelctro-catalyst, add Nafion(mass percent 5%) solution 50 mL, to form pastel behind the ultrasonic processing of the mixture 30min then, at last this pastel is dripped in titanium plate surface, its electro catalytic activity to oxygen reduction reaction is measured as working electrode in dry back in 0.5 M sulfuric acid solution.Constantly aerating oxygen, sweep speed 1 mV/s, corresponding linear scanning curve are seen Fig. 5 in 0.5 M sulfuric acid solution.The oxygen reduction reaction take-off potential is 0.66 V, and the current density when current potential is 0.2V is 2.2 times among Fig. 1-3.
With concentration is the H of 10 mM
2PtCl
6Solution 20 mL, 4 mM CoCl
2Solution 25 mL and 4 mM NiCl
2Solution 25mL places hydrothermal reaction kettle, and adding concentration successively is 200 mM complexing agent EDTA 2 mL and Vulcan XC-72 carbon dust 12 mg, carries out ultrasonic processing 20 min then at normal temperatures, drips mass percentage concentration afterwards and be 10% NaBH
4Solution 3 ml; Then reactor is heated to 200
o Kept 12 hours behind the C; After reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle washes twice with pure water and absolute ethyl alcohol successively, promptly obtains carbon-supported nano Pt-Co-Ni eelctro-catalyst; 5 mg mix with 1 mL absolute ethyl alcohol with this carbon-supported nano Pt-Co-Ni eelctro-catalyst, add Nafion(mass percent 5%) solution 50 mL, to form pastel behind the ultrasonic processing of the mixture 30min then, at last this pastel is dripped in titanium plate surface, its electro catalytic activity to oxygen reduction reaction is measured as working electrode in dry back in 0.5 M sulfuric acid solution.Constantly aerating oxygen, sweep speed 1 mV/s, corresponding linear scanning curve are seen Fig. 6 in 0.5 M sulfuric acid solution.The oxygen reduction reaction take-off potential is 0.67 V, and the current density when current potential is 0.2V is 2.5 times among Fig. 1-3.
Claims (5)
1. a preparation method who is used for the metal nano eelctro-catalyst of fuel cell oxygen reduction reaction is characterized in that, makes complexing agent with EDTA, NaBH
4Make reducing agent, adopt one step of hydro-thermal method H
2PtCl
6+ carbon dust mixed solution is reduced into the carbon-supported metal nanocatalyst; Below the concrete steps:
(1) with H
2PtCl
6Solution places hydrothermal reaction kettle, adds complexing agent EDTA and Vulcan XC-72 carbon dust successively, carries out ultrasonic processing at normal temperatures, drips NaBH
4Solution; The amount of described Vulcan XC-72 carbon dust is 40 ~ 60% of a metal catalyst particles Pt quality;
(2) reactor is heated to 140 ~ 200
oKept behind the C 6 ~ 12 hours;
(3) after reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle are washed with absolute ethyl alcohol with pure water successively and are washed, and promptly obtain carbon-supported nano Pt metal nano eelctro-catalyst;
Described H
2PtCl
6The concentration of solution is 2 ~ 10 mM, and the concentration of complexing agent EDTA is 40 ~ 200 mM, and the time of ultrasonic processing is 5 ~ 20 min, NaBH
4The mass percentage concentration of solution is 3 ~ 10%.
2. a preparation method who is used for the metal nano eelctro-catalyst of fuel cell oxygen reduction reaction is characterized in that, makes complexing agent with EDTA, NaBH
4Make reducing agent, adopt one step of hydro-thermal method H
2PtCl
6+ CoCl
2+ NiCl
2+ carbon dust mixed solution is reduced into the carbon-supported metal nanocatalyst; Below the concrete steps:
(1) with H
2PtCl
6+ CoCl
2+ NiCl
2Solution places hydrothermal reaction kettle, adds complexing agent EDTA and Vulcan XC-72 carbon dust successively, carries out ultrasonic processing at normal temperatures, drips NaBH
4Solution; The amount of described Vulcan XC-72 carbon dust is 40 ~ 60% of a metal catalyst particles Pt+Co+Ni gross mass;
(2) reactor is heated to 140 ~ 200
oKept behind the C 6 ~ 12 hours;
(3) after reaction is finished reactor is cooled to room temperature, reacting liquid filtering, gained nanocatalyst particle are washed with absolute ethyl alcohol with pure water successively and are washed, and promptly obtain carbon-supported nano Pt+Co+Ni metal nano eelctro-catalyst;
Described H
2PtCl
6The concentration of solution is 2 ~ 10 mM, CoCl
2Concentration be 0.8 ~ 4 mM, NiCl
2Concentration be 0.8 ~ 4 mM, the concentration of complexing agent EDTA is 40 ~ 200 mM, the time of ultrasonic processing is 5 ~ 20 min, NaBH
4The mass percentage concentration of solution is 3 ~ 10%.
3. the preparation method who is used for the metal nano eelctro-catalyst of fuel cell oxygen reduction reaction according to claim 1 and 2 is characterized in that described pure water is washed and is: wash twice with pure water, each 1mL; Described absolute ethyl alcohol is washed and is: wash twice with absolute ethyl alcohol, each 1mL.
4. the metal nano eelctro-catalyst of preparation method's preparation of a metal nano eelctro-catalyst that is used for fuel cell oxygen reduction reaction as claimed in claim 1 or 2.
5. the described metal nano eelctro-catalyst of claim 4 is as the application of carbon-supported nano platinum electrode (Pt/C) and carbon-supported nano platinum-cobalt-nickel electrode (PtCoNi/C), concrete grammar is: described carbon-supported nano Pt or carbon are carried platinum-cobalt-nickel ternary metal nanometer electrical catalyst mix with absolute ethyl alcohol, add Nafion(mass percent 5%) solution, then the ultrasonic processing of mixture back is formed pastel, at last this pastel is dripped in titanium plate surface, dry back is as working electrode.
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| CN103007976A (en) * | 2012-12-11 | 2013-04-03 | 湖南科技大学 | Doped polyaniline directly-carbonized composite electrocatalyst, preparation method and application |
| CN106423276A (en) * | 2016-09-13 | 2017-02-22 | 合肥工业大学 | Preparation method of nickel electric Fenton catalyst supported by nitrogen mixed with carbon |
| CN109289835A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of Pt process for synthetic catalyst of hydrogen evolution reaction |
| CN110690463A (en) * | 2019-10-23 | 2020-01-14 | 湖南科技大学 | Preparation method of carbon hollow sphere composite material with low platinum loading capacity, product and application |
| CN110783584A (en) * | 2019-10-31 | 2020-02-11 | 华中科技大学 | Platinum-based intermetallic nanocrystalline oxygen reduction catalyst and preparation method thereof |
| CN112877728A (en) * | 2020-12-10 | 2021-06-01 | 上海航天智慧能源技术有限公司 | Novel platinum-carbon-layer-containing loaded foam nickel electrolytic water electrode and preparation method thereof |
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| RU2783750C1 (en) * | 2022-03-11 | 2022-11-16 | ЮГ Инвестмент Лтд. | Method for manufacturing a catalytic material for a fuel cell |
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| US11196054B2 (en) | 2015-10-06 | 2021-12-07 | International Business Machines Corporation | Proton exchange membrane materials |
| CN106423276A (en) * | 2016-09-13 | 2017-02-22 | 合肥工业大学 | Preparation method of nickel electric Fenton catalyst supported by nitrogen mixed with carbon |
| CN106423276B (en) * | 2016-09-13 | 2018-11-06 | 合肥工业大学 | A kind of preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst |
| CN109289835A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of Pt process for synthetic catalyst of hydrogen evolution reaction |
| CN110690463B (en) * | 2019-10-23 | 2022-04-26 | 湖南科技大学 | Preparation method of carbon hollow sphere composite material with low platinum loading capacity, product and application |
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| CN110783584A (en) * | 2019-10-31 | 2020-02-11 | 华中科技大学 | Platinum-based intermetallic nanocrystalline oxygen reduction catalyst and preparation method thereof |
| CN114588915A (en) * | 2020-12-04 | 2022-06-07 | 中国科学院大连化学物理研究所 | Supported platinum-based catalyst and preparation and application thereof |
| CN112877728A (en) * | 2020-12-10 | 2021-06-01 | 上海航天智慧能源技术有限公司 | Novel platinum-carbon-layer-containing loaded foam nickel electrolytic water electrode and preparation method thereof |
| CN112877728B (en) * | 2020-12-10 | 2022-08-09 | 上海航天智慧能源技术有限公司 | Platinum-carbon-layer-containing loaded foam nickel electrolytic water electrode and preparation method thereof |
| CN114944492A (en) * | 2022-01-28 | 2022-08-26 | 上海应用技术大学 | Preparation method of two-dimensional ultrathin nano composite material |
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