CN108598502A - A kind of Ni-Co metal oxides air cell electrode catalyst and its preparation method and application - Google Patents
A kind of Ni-Co metal oxides air cell electrode catalyst and its preparation method and application Download PDFInfo
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- CN108598502A CN108598502A CN201810247306.5A CN201810247306A CN108598502A CN 108598502 A CN108598502 A CN 108598502A CN 201810247306 A CN201810247306 A CN 201810247306A CN 108598502 A CN108598502 A CN 108598502A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
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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
- H01M4/9091—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
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- 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
- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to novel energy resource material technology field, a kind of Ni Co metal oxide air cell electrode catalysts and its preparation method and application are disclosed.The electrode catalyst is that cobalt nitrate, nickel nitrate and hexamethylenetetramine precipitating reagent are dissolved in solution A and are uniformly mixed, it adds carbon material and carries out hydro-thermal reaction, products therefrom is washed, is made after being roasted at 350 DEG C after dry, and the molecular formula of the oxygen electrode catalyst is NixCo3‑xO4, wherein 0.1<X ＜ 3.The preparation method of the Ni Co metal oxide air cell electrode catalyst materials of the present invention is simple, of low cost.The Ni of preparationxCo3‑xO4It can be used for the electrocatalytic oxidation reduction reaction of metal-air battery, and show good hydrogen reduction performance.
Description
Technical field
The invention belongs to novel energy resource material technology fields, more particularly, to a kind of Ni-Co metal oxides air cell
Electrode catalyst and its preparation method and application.
Background technology
Metal-air battery is due to high theoretical energy density, being far above lithium battery, as power electric of new generation
Cell system is concerned.The reduction reaction of the mainly oxygen occurred on metal air battery cathodes, since this is sluggish
Kinetic characteristics so that the process that must accelerate reaction by the effect of elctro-catalyst improves efficiency.Currently, hydrogen reduction
The best catalyst of energy is precious metals pt catalyst series, but since Pt is expensive, scarcity of resources, makes its commercialization by very
Big limitation.Wherein, carbon material and metal oxide are the expense noble metal catalysts to attract attention.Having for carbon material is preferably led
Electrically, but in charge and discharge process, swelling easily occurs and shrinks, to make its stability and corrosion resistance be deteriorated；And metal oxygen
Compound material it is cheap, stability is good, but electric conductivity is slightly poor.Therefore, seek the oxygen reduction reaction catalyst of high performance-price ratio
As one of the hot spot of metal-air battery research.
Invention content
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, primary mesh of the invention is to provide a kind of Ni-Co
Metal oxide air cell electrode catalyst.The electrode catalyst is the oxide Ni for having spinel structurexCo3-xO4(0.1
<X ＜ 3).With abundant pore structure, and the electric conductivity of the catalyst is also increased, improves hydrogen reduction performance.
It is a further object of the present invention to provide the preparation sides of above-mentioned Ni-Co metal oxides air cell electrode catalyst
Method.The raw material for preparing of this method is conveniently easy to get, cheap.
Another object of the present invention is to provide the application of above-mentioned Ni-Co metal oxides air cell electrode catalyst.
The purpose of the present invention is realized by following technical proposals：
A kind of Ni-Co metal oxides air cell electrode catalyst, the oxygen electrode catalyst are by cobalt nitrate, nitric acid
Nickel and hexamethylenetetramine precipitating reagent are dissolved in solution A and are uniformly mixed, and add carbon material and carry out hydro-thermal reaction, gained
Product is washed, it is dry after roasted at 350 DEG C after be made, the molecular formula of the oxygen electrode catalyst is NixCo3-xO4, wherein
0.1<X ＜ 3.
Preferably, the sum of molar concentration of the cobalt nitrate and nickel nitrate is 0.06mol/L, the hexamethylenetetramine
Molar concentration is 0.12~0.24mol/L.
It is further preferable that the molar ratio of the cobalt nitrate and nickel nitrate is (1~5)：(5~1).
Preferably, the solution A is one or more of water, methanol or ethyl alcohol.
Preferably, the carbon material is graphene oxide, carbon nanotube or g-C3N4One or more of, the carbon materials
The mass concentration of material is 0.1~0.5%.
Preferably, the temperature of the hydro-thermal reaction is 160~220 DEG C, and the time of the hydro-thermal reaction is 10~14h.
Preferably, the time of the roasting is 1~4h.
The preparation method of above-mentioned Ni-Co metal oxide air cell electrode catalysts, comprises the following specific steps that：
S1. cobalt nitrate, nickel nitrate and hexamethylenetetramine precipitating reagent are dissolved in the mixture stirred evenly in solution A；
S2. carbon material is added in mixture obtained by step S1 and carries out hydro-thermal reaction, products therefrom washs through deionized water,
Metal-air battery electrode catalyst is made after being roasted at 350 DEG C after drying.
Preferably, temperature dry described in step S2 is 60~80 DEG C.
Above-mentioned Ni-Co metal oxides air cell electrode catalyst answering in metal-air battery electrode catalyst
With.
Compared with prior art, the invention has the advantages that：
1. the Ni-Co metal oxide air cell electrode catalysts of the present invention are made by adding micro carbon material
NixCo3-xO4Catalyst not only has abundant pore structure, but also also increases the electric conductivity of the catalyst, improves oxygen also
Originality energy.The electrode catalyst shows good electrocatalysis characteristic in hydrogen reduction performance test.
2. the preparation method of the present invention has many advantages, such as that method is simple, of low cost.
Description of the drawings
Fig. 1 is Ni prepared by embodiment 10.5Co2.5O4XRD diagram.
Fig. 2 is Ni prepared by embodiment 10.5Co2.5O4TEM photos.
Fig. 3 is Ni prepared by embodiment 10.5Co2.5O4Hydrogen reduction performance polarization curve.
Fig. 4 is Ni prepared by comparative example 10.5Co2.5O4Hydrogen reduction performance polarization curve.
Specific implementation mode
The content further illustrated the present invention with reference to specific embodiment, but should not be construed as limiting the invention.
Embodiment 1
1. preparing：By six first of precipitating reagent of the nickel nitrate and 0.12mol/L of 0.01mol/L cobalt nitrates and 0.05mol/L
Urotropine, which is dissolved in the water, to be uniformly mixed, and the graphene oxide that mass concentration is 0.2% is added, at a temperature of 180 DEG C
Hydro-thermal reaction 12h, products therefrom is washed through deionized water, 60 DEG C of dryings then roast 2h at 350 DEG C and obtain metal-air
Cell electrode catalyst material Ni0.5Co2.5O4。
2. performance test：Fig. 1 is Ni manufactured in the present embodiment0.5Co2.5O4XRD diagram.As can be known from Fig. 1, the material with
NiCo2O4It is corresponding with standard card PDF#20-0781 with similar lattice structure.Fig. 2 is manufactured in the present embodiment
Ni0.5Co2.5O4TEM photos.As it is clear from fig. 2 that catalyst present porous state, due to porous surface be conducive to electrolyte and from
Son transmission, to improve the electro catalytic activity of electrode catalyst.
Prepared metal-air battery electrode catalyst is made electrode under the conditions of alkaline solution, different rotating speeds to test
Oxygen reducing ability (prepared by electrode and experimentation is existing public technology, repeats no more).Fig. 3 is manufactured in the present embodiment
Ni0.5Co2.5O4Hydrogen reduction performance polarization curve.As can be known from Fig. 3, initial reduction current potential is 0.9v at 1600 rpm,
Limiting current density is 5.25mAcm-2, it is shown that more excellent hydrogen reduction performance.
Comparative example 1
Ni is prepared using condition same as Example 10.5Co2.5O4, difference lies in oxidation stone is not added in preparation process
Black alkene, test gained Ni0.5Co2.5O4The oxygen reducing ability of material, as shown in figure 4, the limit of material under the conditions of 1600rpm
Current density is 4.25mAcm-2, performance is less than the catalyst for being added to graphene oxide in embodiment 1.
Embodiment 2
The precipitating reagent hexamethylenetetramine of the nickel nitrate and 0.12mol/L of 0.02mol/L cobalt nitrates and 0.04mol/L is molten
Solution is uniformly mixed in methanol, adds the graphene oxide that mass concentration is 0.1%, hydro-thermal is anti-at a temperature of 180 DEG C
12h is answered, products therefrom is washed through deionized water, 60 DEG C of dryings then roast 2h at 350 DEG C and obtain metal-air battery electricity
Electrode catalyst material Ni Co2O4。
Embodiment 3
The precipitating reagent hexamethylenetetramine of the nickel nitrate and 0.24mol/L of 0.03mol/L cobalt nitrates and 0.03mol/L is molten
It is uniformly mixed in Xie Yushui, adds the carbon nanotube that mass concentration is 0.5%, hydro-thermal reaction at a temperature of 220 DEG C
12h, products therefrom is washed through deionized water, 60 DEG C of dryings then roast 2h at 350 DEG C and obtain metal-air battery electrode
Catalyst material Ni1.5Co1.5O4。
Embodiment 4
The precipitating reagent hexamethylenetetramine of the nickel nitrate and 0.18mol/L of 0.04mol/L cobalt nitrates and 0.02mol/L is molten
Solution is uniformly mixed in ethyl alcohol, adds the g-C that mass concentration is 0.3%3N4, hydro-thermal reaction 12h at a temperature of 200 DEG C,
Products therefrom is washed through deionized water, 60 DEG C of dryings then roast 2h at 350 DEG C and obtain metal-air battery electrode catalyst
Agent material Ni2CoO4。
Embodiment 5
The precipitating reagent hexamethylenetetramine of the nickel nitrate and 0.12mol/L of 0.05mol/L cobalt nitrates and 0.01mol/L is molten
It is uniformly mixed in Xie Yushui, adds the graphene oxide that mass concentration is 0.25%, hydro-thermal reaction at a temperature of 160 DEG C
12h, products therefrom is washed through deionized water, 60 DEG C of dryings then roast 2h at 350 DEG C and obtain metal-air battery electrode
Catalyst material Ni2.5Co0.5O4。
Embodiment 6
The precipitating reagent hexamethylenetetramine of the nickel nitrate and 0.18mol/L of 0.04mol/L cobalt nitrates and 0.02mol/L is molten
Solution is uniformly mixed in ethyl alcohol, adds the g-C that mass concentration is 0.3%3N4, hydro-thermal reaction 10h at a temperature of 200 DEG C,
Products therefrom is washed through deionized water, 60 DEG C of dryings then roast 1h at 350 DEG C and obtain metal-air battery electrode catalyst
Agent material Ni2CoO4。
Embodiment 7
The precipitating reagent hexamethylenetetramine of the nickel nitrate and 0.18mol/L of 0.04mol/L cobalt nitrates and 0.02mol/L is molten
Solution is uniformly mixed in ethyl alcohol, adds the g-C that mass concentration is 0.3%3N4, hydro-thermal reaction 14h at a temperature of 200 DEG C,
Products therefrom is washed through deionized water, 80 DEG C of dryings then roast 4h at 350 DEG C and obtain metal-air battery electrode catalyst
Agent material Ni2CoO4。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitute, combination and simplify,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of Ni-Co metal oxides air cell electrode catalyst, which is characterized in that the oxygen electrode catalyst is by nitre
Sour cobalt, nickel nitrate and hexamethylenetetramine precipitating reagent are dissolved in solution A and are uniformly mixed, and add carbon material and carry out hydro-thermal
Reaction, products therefrom is washed, it is dry after roasted at 350 DEG C after be made, the molecular formula of the oxygen electrode catalyst is
NixCo3-xO4, wherein 0.1<X ＜ 3.
2. Ni-Co metal oxides air cell electrode catalyst according to claim 1, which is characterized in that the nitre
The sum of molar concentration of sour cobalt and nickel nitrate is 0.06mol/L, the molar concentration of the hexamethylenetetramine is 0.12~
0.24mol/L。
3. Ni-Co metal oxides air cell electrode catalyst according to claim 2, which is characterized in that the nitre
The molar ratio of sour cobalt and nickel nitrate is (1~5)：(5~1).
4. Ni-Co metal oxides air cell electrode catalyst according to claim 1, which is characterized in that described
Solution A is one or more of water, methanol or ethyl alcohol.
5. Ni-Co metal oxides air cell electrode catalyst according to claim 1, which is characterized in that described
Carbon material is graphene oxide, carbon nanotube or g-C3N4One or more of, the mass concentration of the carbon material is 0.1~
0.5%.
6. Ni-Co metal oxides air cell electrode catalyst according to claim 1, which is characterized in that the water
The temperature of thermal response is 160~220 DEG C, and the time of the hydro-thermal reaction is 10~14h.
7. Ni-Co metal oxides air cell electrode catalyst according to claim 1, which is characterized in that the roasting
The time of burning is 1~4h.
8. according to the preparation method of claim 1-7 any one of them Ni-Co metal oxide air cell electrode catalysts,
It is characterised in that it includes following specific steps：
S1. cobalt nitrate, nickel nitrate and hexamethylenetetramine precipitating reagent are dissolved in the mixture stirred evenly in solution A；
S2. carbon material is added in mixture obtained by step S1 and carries out hydro-thermal reaction, products therefrom washs through deionized water, is dry
Metal-air battery electrode catalyst is made after being roasted at 350 DEG C afterwards.
9. the preparation method of Ni-Co metal oxides air cell oxygen electrode catalyst according to claim 8, feature
It is, dry temperature described in step S2 is 60~80 DEG C.
10. claim 1-7 any one of them Ni-Co metal oxide air cell electrode catalysts are in metal-air battery
In application.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109755600A (en) * | 2019-01-29 | 2019-05-14 | 天津大学 | The application of carbon cloth nickel-loaded cobalt oxide nano-sheet composite material and preparation method and electrode |
| CN111530474A (en) * | 2020-06-23 | 2020-08-14 | 中国科学院长春应用化学研究所 | Noble metal monoatomic regulation spinel array catalyst and preparation method and application thereof |
| CN114497588A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Flow battery anode catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111530474A (en) * | 2020-06-23 | 2020-08-14 | 中国科学院长春应用化学研究所 | Noble metal monoatomic regulation spinel array catalyst and preparation method and application thereof |
| CN114497588A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Flow battery anode catalyst and preparation method and application thereof |
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Application publication date: 20180928 |