CN110350209A - A kind of preparation method and applications of the NiO/C bifunctional electrocatalyst with core-shell structure - Google Patents
A kind of preparation method and applications of the NiO/C bifunctional electrocatalyst with core-shell structure Download PDFInfo
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- CN110350209A CN110350209A CN201910678842.5A CN201910678842A CN110350209A CN 110350209 A CN110350209 A CN 110350209A CN 201910678842 A CN201910678842 A CN 201910678842A CN 110350209 A CN110350209 A CN 110350209A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The preparation method and applications of the invention discloses a kind of NiO/C bifunctional electrocatalyst with core-shell structure, cobalt chloride, urea and carbon source are dissolved in distilled water, it is uniformly mixed to be placed in reaction kettle and obtains green precipitate in 140 DEG C of reaction 10h, then vacuum drying obtains NiO/C presoma after secondary water and dehydrated alcohol washing for several times；It step S1 is obtained NiO/C presoma is placed in tube furnace to obtain the NiO/C bifunctional electrocatalyst with core-shell structure in 200-500 DEG C of calcining 2h.Bifunctional electrocatalyst in the present invention with core-shell structure has biggish specific surface area, and active site exposure is more, and can preferably contact with electrolyte, can effectively improve the electro catalytic activity of bifunctional electrocatalyst.
Description
Technical field
The invention belongs to zinc and air cell catalyst technical fields, and in particular to a kind of bis- function of NiO/C with core-shell structure
The preparation method and applications of energy elctro-catalyst.
Background technique
Zinc and air cell has the advantages such as high-energy-density, low cost, pollution-free, in many fields as a kind of clean energy resource
There is substantial application, becomes the hot spot of Recent study.In zinc and air cell, catalyst is core component, and certainly
Determine the critical material of battery cost and performance.In recent years, the research about zinc and air cell single function catalyst emerges one after another, so
And it is still challenging to synthesize ORR and OER bifunctional electrocatalyst.Therefore, developing a kind of bifunctional electrocatalyst becomes zinc
Empty cell catalyst synthesis technical field has one of major issue to be solved.
Recently, the synthesis of many transition metal base elctro-catalysts, such as transition metal oxide, due to its height are had been realized in
Latent active, perfect stability and brilliance electric conductivity be applied to OER/ORR reaction, caused the extensive pass of people
Note.Wherein transition metal oxide specific surface area is larger, and active site exposure is more, therefore has good OER performance, however
Its structure in catalytic process is more easily damaged, unstable, these deficiencies restrict the application of amorphous transition metal oxide.
Carbon-based non-precious metal catalyst is because it is with certain ORR catalytic activity, excellent anti-toxicity energy and good
Stability causes extensive research.Meanwhile high-temperature calcination carbon material can form graphited carbon, further improve carbon-based
The electric conductivity of material, to improve its catalytic performance however carbon-based material is due to slow dynamic characteristic, most of table
Reveal weaker OER performance, these problems need further to be solved.
Summary of the invention
That the technical problem to be solved by the present invention is to provide a kind of synthetic operations is simple, reaction condition is mild and reaction efficiency compared with
The preparation method of the high NiO/C bifunctional electrocatalyst with core-shell structure, the difunctional electro-catalysis of NiO/C made from this method
Agent effectively increases the electrocatalysis characteristic of zinc and air cell catalyst.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of bis- function of NiO/C with core-shell structure
The preparation method of energy elctro-catalyst, it is characterised in that specific steps are as follows:
Step S1: cobalt chloride, urea and carbon source are dissolved in distilled water, are uniformly mixed and are placed in reaction kettle in 140 DEG C
Reaction 10h obtains green precipitate, then vacuum drying obtains NiO/C presoma, institute after secondary water and dehydrated alcohol washing for several times
Stating carbon source is one of glucose, citric acid or ascorbic acid or a variety of；
Step S2: it step S1 is obtained NiO/C presoma is placed in tube furnace to obtain in 200-500 DEG C of calcining 2h with nucleocapsid knot
The NiO/C bifunctional electrocatalyst of structure, the NiO/C bifunctional electrocatalyst are core-shell nano spherical structure, and the diameter of internal layer ball exists
Between 1-2 μm, the average thickness of outer shell is 270nm.
Preferably, the mass ratio that feeds intake of cobalt chloride described in step S1, urea and carbon source is 1.2:0.3:0.12-0.24.
NiO/C bifunctional electrocatalyst of the present invention with core-shell structure is applied in preparing zinc and air cell,
It is characterized in that detailed process are as follows: it disperses the NiO/C bifunctional electrocatalyst with core-shell structure in alcohol dispersant, then plus
Enter carbon black, by mixed liquor ultrasound uniformly after be coated in glassy carbon electrode surface, using three-electrode system, measured by electrochemical workstation
The performance of the catalyst, the bifunctional electrocatalyst show the difunctional electro catalytic activity of higher OER, ORR, have nucleocapsid
The NiO/C bifunctional electrocatalyst of structure can provide ideal solid-liquid-gas threephase region for electrode reaction, be the biography of electrolyte
Defeated offer more multichannel, and then the specific surface area of bifunctional electrocatalyst is improved, increase the catalytic activity of bifunctional electrocatalyst,
Good synergistic effect has been played between two component of NiO and graphitic carbon simultaneously, not only shows double-function catalyzing activity, and due to
The protective effect of outer layer carbon effectively reduces the destruction of nickel oxide structure in catalytic process, has contained the tendency of electrical property decaying.
Compared with the prior art, the invention has the following beneficial effects:
1, the NiO/C bifunctional electrocatalyst with core-shell structure that the present invention synthesizes, synthetic method is easy to operate, reacts item
Part is mild, reaction efficiency is high；
2, the bifunctional electrocatalyst with core-shell structure has a biggish specific surface area in the present invention, active site it is exposed compared with
It is more, and can preferably be contacted with electrolyte, it can effectively improve the electro catalytic activity of bifunctional electrocatalyst；
3, the NiO/C zinc and air cell catalyst with core-shell structure that the present invention synthesizes, the presence of outer layer carbon can be improved NiO's
Electric conductivity accelerates the transmission and conduction of electronics in catalytic process, realizes the bis- function of OER, ORR with higher under alkaline condition
Energy electro catalytic activity, has broad application prospects on zinc and air cell.
Detailed description of the invention
Fig. 1 is the SEM figure of the NiO/C zinc and air cell catalyst obtained with core-shell structure of the embodiment of the present invention 1；
Fig. 2 is the TEM figure of the NiO/C zinc and air cell catalyst obtained with core-shell structure of the embodiment of the present invention 1；
Fig. 3 is product electrochemical property test figure made from the embodiment of the present invention 1 and comparative example 1, comparative example 2.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
1.2g nickel chloride, 0.3g urea and 0.24g citric acid are dissolved in 60mL distilled water, are placed into after being uniformly mixed
In 100mL reaction kettle, by 140 DEG C, obtain green precipitate after 10h reaction, after secondary water and dehydrated alcohol washing for several times
NiO/C presoma is dried to obtain in vacuum oven；NiO/C presoma obtained above is calcined in tube furnace in 300 DEG C
2h finally obtains the NiO/C zinc and air cell catalyst with core-shell structure.
It takes NiO/C bifunctional electrocatalyst made from 2mg the present embodiment to be dispersed in alcohol dispersant, adds carbon black,
By mixed liquor ultrasound uniformly after be coated in glassy carbon electrode surface, using three-electrode system, which is measured by electrochemical workstation
The performance of agent, electric performance test result are as shown in Figure 3.
Embodiment 2
1.2g nickel chloride, 0.3g urea and 0.12g citric acid are dissolved in 60mL distilled water, are placed into after being uniformly mixed
In 100mL reaction kettle, by 140 DEG C, obtain green precipitate after 10h reaction, after secondary water and dehydrated alcohol washing for several times
NiO/C presoma is dried to obtain in vacuum oven；NiO/C presoma obtained above is calcined in tube furnace in 300 DEG C
2h finally obtains the NiO/C zinc and air cell catalyst with core-shell structure.
Embodiment 3
1.2g nickel chloride, 0.3g urea and 0.24g citric acid are dissolved in 60mL distilled water, are placed into after being uniformly mixed
In 100mL reaction kettle, by 140 DEG C, obtain green precipitate after 10h reaction, after secondary water and dehydrated alcohol washing for several times
NiO/C presoma is dried to obtain in vacuum oven；NiO/C presoma obtained above is calcined in tube furnace in 500 DEG C
2h finally obtains the NiO/C zinc and air cell catalyst with core-shell structure.
Comparative example 1
1.2g nickel chloride and 0.3g urea are dissolved in 60mL distilled water, are placed into after being uniformly mixed in 100mL reaction kettle,
By 140 DEG C, green precipitate is obtained after 10h reaction, is done in a vacuum drying oven after secondary water and dehydrated alcohol washing for several times
It is dry to obtain Ni2CO3(OH)2Sphere；By Ni obtained above2CO3(OH)2Sphere in tube furnace in 300 DEG C of calcining 2h, it is final
To NiO zinc and air cell catalyst.
It takes NiO catalyst made from this comparative example of 2mg to be dispersed in alcohol dispersant, adds carbon black, mixed liquor is surpassed
It is coated in glassy carbon electrode surface after sound is uniform, using three-electrode system, the performance of the catalyst is measured by electrochemical workstation, electricity
The performance test results are as shown in Figure 3.
Comparative example 2
1.2g nickel chloride, 0.3g urea and 0.24g citric acid are dissolved in 60mL distilled water, are placed into after being uniformly mixed
In 100mL reaction kettle, by 140 DEG C, obtain green precipitate after 10h reaction, after secondary water and dehydrated alcohol washing for several times
NiO/C presoma is dried to obtain in vacuum oven.
It takes NiO/C presoma made from this comparative example of 2mg to be dispersed in alcohol dispersant as catalyst, adds charcoal
It is black, by mixed liquor ultrasound uniformly after be coated in glassy carbon electrode surface, using three-electrode system, this is measured by electrochemical workstation and is urged
The performance of agent, electric performance test result are as shown in Figure 3.
NiO/C zinc and air cell catalyst produced by the present invention with core-shell structure has good OER, ORR difunctional
Electro catalytic activity.In Fig. 3 electric performance test result, (a) is that the ORR polarization of the catalyst of embodiment 1 and comparative example 1-2 preparation is bent
Line is (b) the OER polarization curve of embodiment 1 and comparative example the 1-2 catalyst prepared, and compared with comparative example 1-2, embodiment 1 is made
The bifunctional electrocatalyst obtained shows the difunctional electro catalytic activity of higher OER, ORR；We are according to the analysis, the present invention mentions
The NiO/C bifunctional electrocatalyst with core-shell structure supplied can provide ideal solid-liquid-gas threephase region for electrode reaction,
More multichannel is provided for the transmission of electrolyte, and then improves the specific surface area of bifunctional electrocatalyst, increases difunctional electro-catalysis
The catalytic activity of agent, while good synergistic effect has been played between two component of NiO and graphitic carbon, not only show difunctional urge
Change activity, and since the protective effect of outer layer carbon reduces the destruction of nickel oxide structure in catalytic process, contains electrical property
The tendency of decaying shows the electro catalytic activity performance of the NiO/C bifunctional electrocatalyst produced by the present invention with core-shell structure
It is excellent, it is a kind of zinc and air cell catalyst with broad prospect of application.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (3)
1. a kind of preparation method of the NiO/C bifunctional electrocatalyst with core-shell structure, it is characterised in that specific steps are as follows:
Step S1: cobalt chloride, urea and carbon source are dissolved in distilled water, are uniformly mixed and are placed in reaction kettle in 140 DEG C
Reaction 10h obtains green precipitate, then vacuum drying obtains NiO/C presoma, institute after secondary water and dehydrated alcohol washing for several times
Stating carbon source is one of glucose, citric acid or ascorbic acid or a variety of；
Step S2: it step S1 is obtained NiO/C presoma is placed in tube furnace to obtain in 200-500 DEG C of calcining 2h with nucleocapsid knot
The NiO/C bifunctional electrocatalyst of structure, the NiO/C bifunctional electrocatalyst are core-shell nano spherical structure, and the diameter of internal layer ball exists
Between 1-2 μm, the average thickness of outer shell is 270nm.
2. the preparation method of the NiO/C bifunctional electrocatalyst according to claim 1 with core-shell structure, feature exist
In: the mass ratio that feeds intake of cobalt chloride described in step S1, urea and carbon source is 1.2:0.3:0.12-0.24.
3. the NiO/C bifunctional electrocatalyst obtained with core-shell structure is preparing zinc according to the method for claim 1
It is applied in empty battery, it is characterised in that detailed process are as follows: disperse second for the NiO/C bifunctional electrocatalyst with core-shell structure
In alcohol dispersing agent, add carbon black, by mixed liquor ultrasound uniformly after be coated in glassy carbon electrode surface, using three-electrode system, pass through
Electrochemical workstation measures the performance of the catalyst, which shows the difunctional electricity of higher OER, ORR
Catalytic activity, the NiO/C bifunctional electrocatalyst with core-shell structure can provide ideal solid-liquid-gas three for electrode reaction
Phase region provides more multichannel for the transmission of electrolyte, and then improves the specific surface area of bifunctional electrocatalyst, increases difunctional electricity
The catalytic activity of catalyst, while good synergistic effect has been played between two component of NiO and graphitic carbon, it not only shows difunctional
Catalytic activity, and since the protective effect of outer layer carbon effectively reduces the destruction of nickel oxide structure in catalytic process, containment
The tendency of electrical property decaying.
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| CN112877711A (en) * | 2020-12-10 | 2021-06-01 | 杭州师范大学 | Ni-NiO/C core-shell structure nano material electrocatalyst and preparation method thereof |
| CN113913857A (en) * | 2021-09-23 | 2022-01-11 | 杭州师范大学 | Ni-Ni3C/NC core-shell structure nano material electrocatalyst and preparation method thereof |
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| CN112877711A (en) * | 2020-12-10 | 2021-06-01 | 杭州师范大学 | Ni-NiO/C core-shell structure nano material electrocatalyst and preparation method thereof |
| CN113913857A (en) * | 2021-09-23 | 2022-01-11 | 杭州师范大学 | Ni-Ni3C/NC core-shell structure nano material electrocatalyst and preparation method thereof |
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