CN103208636A - Electro-catalysis material for lithium-air battery and preparation method of electro-catalysis material - Google Patents
Electro-catalysis material for lithium-air battery and preparation method of electro-catalysis material Download PDFInfo
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Abstract
The invention relates to an electro-catalysis material for lithium-air battery and a preparation method of the electro-catalysis material. The technical problem that existing catalysts cannot meet the industrial requirements of high-performance ether lithium-air batteries is solved. The electro-catalysis material provided by the invention is perovskite type composite oxide with a chemical expression as follows: La1-xM1xM2(1-y)M3yO3, wherein 0 <= x <= 1; 0 <= y <= 1; M1 is alkaline-earth metal or rare-earth metal ions; and M2 and M3 are transition metal ions. The electro-catalysis material is of a hollow multi-hole nanotube structure, and is beneficial to exertion of the catalytic activity of the material and mass transfer of the air battery in battery reaction. The invention also provides a preparation method of the electro-catalysis material, which is easy in preparation process, is convenient to operate and low in cost and can easily realize large-scale production. When the prepared electro catalysis is applied to the ether lithium-air batteries, the capacity, multiplying power and cycling stability of the batteries are all greatly improved.
Description
Technical field
The invention belongs to electrochemical energy material technology field, be specifically related to a kind of lithium-air battery electrocatalyst materials and preparation method thereof.
Background technology
Lithium-air battery is subjected to extensive concern owing to having the high theoretical energy density, but wants it realize is used, and also needs to solve a series of problems, and is low such as electrolyte stability, high rate performance is poor, cyclical stability difference etc.The catalyst of lithium-air battery use at present is mainly metal oxide, metal nitride, metal nanoparticle, and the corresponding electrolyte that uses is carbonates with it.These catalyst can be accelerated hydrogen reduction and oxygen evolution reaction to a certain extent, can bring side reaction again in the catalysis electrode reaction, as the decomposition of catalytic electrolysis liquid.Therefore, can there be above-mentioned shortcoming in existing lithium-air battery.
For addressing the above problem, people adopt ethers as the electrolyte of lithium-air battery, and ethers electrolyte can not decomposed by employed catalyst, cause the decomposing phenomenon of electrolyte to take place.The catalyst that has catalytic activity in ethers electrolyte of report mainly contains noble metal, pyrochlore oxide and Co at present
3O
4Deng, still, these catalyst all are to be deposited in the air electrode with granular form, are unfavorable for the mass transfer of air electrode in the performance of its catalytic activity and the cell reaction, cause ethers lithium-air battery performance to reduce.Wherein, also there is the high deficiency of cost in noble metal catalyst.Therefore, above-mentioned existing several catalyst all can not satisfy the requirement of the industrialization of high-performance ether lithium-air battery.
Summary of the invention
The present invention is for solving the technical problem that existing catalyst can not satisfy the requirement of high-performance ether lithium-air battery industrialization, and provide a kind of low cost, high performance ether lithium-air battery to use, lithium-air battery electrocatalyst materials and preparation method thereof.
In order to solve the problems of the technologies described above, technical scheme of the present invention is specific as follows:
A kind of lithium-air battery electrocatalyst materials, this electrocatalyst materials are the perovskite composite oxide of hollow porous nano tubular construction, its chemical expression La
1-xM
1xM
2 (1-y)M
3yO
3, wherein, 0≤x＜1,0≤y≤1; M
1Be alkaline-earth metal or rare earth ion, M
2And M
3Be transition metal ions.
In technique scheme, wherein, when 0.25≤x≤0.5, during y=0, M
1Be Nd
3+, Sr
2+, Sm
3+Or Ba
2+, M
2Be Mn
2+, Co
2+Or Fe
3+Work as x=0, during y=0, M
2Be Mn
2+, Co
2+Or Fe
3+Work as x=0,0＜y≤0.5 o'clock, M
2Be Mn
2+, Co
2+Or Fe
3+, M
3Be Nd
3+Or Sm
3+
In technique scheme, the external diameter of pipe of described electrocatalyst materials is 80～120nm, and wall thickness is 5～20nm.
In technique scheme, the specific area of described electrocatalyst materials is 20～50m
2/ g.
A kind of lithium-air battery preparation method of electrocatalyst materials, this preparation method mainly may further comprise the steps:
(1) is that 0.5%～5% slaine presoma and mass concentration are that 10%～25% PVP is dissolved in the solvent with total mass concentration, obtains spinning presoma stoste;
(2) above-mentioned spinning presoma stoste is obtained fibrous material through electrostatic spinning;
(3) with above-mentioned fibrous material after K cryogenic treatment, in air, in 550～700 ℃ temperature lower calcination, be incubated 3～5 hours, obtain La
1-xM
1xM
2 (1-y)M
3yO
3Electrocatalyst materials;
Described slaine presoma contains a kind of lanthanum salt precursor body at least, and a kind of M
2Or M
3The slaine presoma.
In technique scheme, the molecular weight of described PVP is 500000～2000000.
In technique scheme, described slaine presoma is the nitrate of lanthanum, neodymium, samarium, strontium, barium, cobalt, manganese, iron or in the acetate two or more.
In technique scheme, described solvent is water, ethanol or DMF.
In technique scheme, described in the step (3) fibrous material is carried out K cryogenic treatment, treatment temperature is 70 ℃, the processing time is 10～15 hours.
In technique scheme, the fibrous material calcining heat is to rise to temperature required by the speed that normal temperature begins with 1 ℃/minute in the step (3).
A kind of lithium-air battery of the present invention with the beneficial effect of electrocatalyst materials and preparation method thereof is:
1, lithium-air battery electrocatalyst materials provided by the invention is hollow porous nano tubular construction, and external diameter of pipe is 80～120nm, and wall thickness is 5～20nm, and specific area is 20～50m
2/ g.When hollow porous nano tubular construction electrocatalyst materials is used for the ether lithium-air battery, can enough active places be provided for cell reaction, have good ion transfer ability and conductivity concurrently, that can effectively improve battery discharges and recharges utilization ratio, high rate performance and cyclical stability.Compare with existing ether lithium-air battery, cost is lower, and when being used for the ether lithium-air battery, the capacity of battery, multiplying power and cyclical stability all are increased dramatically, and enough satisfy the requirement of high-performance ether lithium-air battery industrialization.
Fig. 1 is the La of the embodiment of the invention one preparation
0.75Sr
0.25MnO
3Electrocatalyst materials SEM figure.Among the figure as can be seen the embodiment of the invention once the preparation catalyst material be the hollow porous nano tubulose structure of wall thickness 15 nanometers, external diameter of pipe 100 nanometers.Therefore, this Fig. 1 can prove the electrocatalyst materials hollow porous nano tubular construction that the present invention prepares.Fig. 2 is the La of embodiment one preparation
0.75Sr
0.25MnO
3Nitrogen adsorption curve and the graph of pore diameter distribution of electrocatalyst materials.Among the figure as can be seen the electrocatalyst materials of the embodiment of the invention one preparation have wideer distribution, wherein the macropore of 40nm is in the majority, the source in hole may be the hole on the nanotube walls.Fig. 2 proves that electrocatalyst materials of the present invention is loose structure.Fig. 5 is the LaNd of embodiment four preparations
0.5Mn
0.5O
3The SEM figure of electrocatalyst materials.Fig. 5 has proved that equally electrocatalyst materials of the present invention is hollow porous nano tubulose structure.
2, the preparation method of electrocatalyst materials provided by the invention, its preparation technology is simple, easy to operate, cost is low, easily realize industrialization production.This preparation method easily realizes the rapid diffusion of electronics, electrolyte and oxygen in the maximum using of catalyst activity point position and the cell reaction.When the eelctro-catalyst for preparing was used for the ether lithium-air battery, the capacity of battery, multiplying power and cyclical stability all were increased dramatically.Improve 1.2 times with present lithium-air battery phase specific capacity, cycle performance improves 3 times, and cycle life reaches 125 times.
Fig. 3 is the La of embodiment one preparation
0.75Sr
0.25MnO
3Electrocatalyst materials is used for the cycle performance figure of ether lithium-air battery.As can be seen, the ether lithium-air battery cycle performance that includes above-mentioned catalyst has been broken through best 100 circulations in the world of present report, and cycle life has reached 125 times.
Fig. 4 is the La of embodiment one preparation
0.75Sr
0.25MnO
3Electrocatalyst materials is used for the enclosed pasture efficiency chart of ether lithium-air battery.As can be seen, the enclosed pasture efficient that includes the ether lithium-air battery of above-mentioned catalyst almost reaches 100%.
Description of drawings
Fig. 1 is the La of the embodiment of the invention one preparation
0.75Sr
0.25MnO
3Electrocatalyst materials SEM figure.
Fig. 2 is the La of the embodiment of the invention one preparation
0.75Sr
0.25MnO
3Nitrogen adsorption curve and the graph of pore diameter distribution of electrocatalyst materials.
Fig. 3 is the La of the embodiment of the invention one preparation
0.75Sr
0.25MnO
3Electrocatalyst materials is used for the cycle performance figure of ether lithium-air battery.
Fig. 4 is the La of the embodiment of the invention one preparation
0.75Sr
0.25MnO
3Electrocatalyst materials is used for the enclosed pasture efficiency chart of ether lithium-air battery.
Fig. 5 is the LaNd of the embodiment of the invention four preparations
0.5Mn
0.5O
3The SEM figure of electrocatalyst materials.
Embodiment
A kind of lithium-air battery electrocatalyst materials provided by the invention, this electrocatalyst materials is the perovskite composite oxide of hollow porous nano tubular construction, and external diameter of pipe is 80～120nm, and wall thickness is 5～20nm, and specific area is 20～50m
2/ g; Its chemical expression is: La
1-xM
1xM
2 (1-y)M
3yO
3, wherein, 0≤x＜1,0≤y≤1, M
1Be alkaline-earth metal or rare earth ion, M
2And M
3Be transition metal ions.When 0.25≤x≤0.5, during y=0, M
1Be Sr
2+, Sm
3+Or Ba
2+, M
2Be Mn
2+, the chemical expression of this electrocatalyst materials is: La
0.75Sr
0.25MnO
3, La
0.5Sm
0.5MnO
3Or La
0.75Ba
0.25MnO
3Work as x=0, during y=0, M
2Be Mn
2+, Co
2+Or Fe
3+, the chemical expression of this electrocatalyst materials is: LaMnO
3, LaCoO
3Or LaFeO
3Work as x=0, during y=0.5, M
2Be Mn
2+, M
3Be Nd
3+, the chemical expression of this electrocatalyst materials is: LaNd
0.5Mn
0.5O
3
A kind of lithium-air battery electrocatalyst materials provided by the invention is prepared by following method:
(1) is that 0.5%～5% slaine presoma and mass concentration are that 10%～25% PVP is dissolved in the solvent with total mass concentration, obtains spinning presoma stoste;
Described slaine presoma is the nitrate of lanthanum, neodymium, samarium, strontium, barium, cobalt, manganese, iron or in the acetate two or more; Described solvent is water, ethanol or DMF; The molecular weight of described PVP is 500000～2000000;
(2) above-mentioned spinning presoma stoste is obtained fibrous material through electrostatic spinning;
(3) above-mentioned fibrous material K cryogenic treatment in 70 ℃ of vacuum tanks in 550～700 ℃ temperature lower calcination, was incubated 3～5 hours after 10～15 hours in air, the speed that is begun with 1 ℃/minute by normal temperature heats up, and obtains La
1-xM
1xM
2 (1-y)M
3yO
3Electrocatalyst materials.
Embodiment one
With three parts of La (NO
3)
36H
2O, a Sr (NO
3)
2, four parts of Mn (CH
3COO)
24H
2O and PVP are dissolved among the DMF, PVP concentration is 10%, stirred 10 hours, obtain spinning presoma stoste, spinning presoma stoste obtains fibrous material through electrostatic spinning, and fibrous material was handled 10 hours in 70 ℃ of vacuum drying ovens, 650 ℃ of calcinings in air then, be incubated 5 hours, heating rate is 1 ℃/minute, can obtain La
0.75Sr
0.25MnO
3Electrocatalyst materials.
Fig. 1 is the electrocatalyst materials SEM figure of present embodiment one preparation.As can be seen, this catalyst material is the hollow porous nano tubulose structure of wall thickness 15 nanometers, external diameter of pipe 100 nanometers.
Fig. 2 is nitrogen adsorption curve and the graph of pore diameter distribution of the electrocatalyst materials of present embodiment one preparation.As can be seen, electrocatalyst materials has wideer distribution, and wherein the macropore of 40nm is in the majority, and the source in hole may be the hole on the nanotube walls.
Fig. 3 is the cycle performance figure that the electrocatalyst materials of present embodiment one preparation is used for the ether lithium-air battery.As can be seen, the ether lithium-air battery cycle performance that includes above-mentioned eelctro-catalyst has been broken through best 100 circulations in the world of present report, and cycle life has reached 125 times.
Fig. 4 is the enclosed pasture efficiency chart that the electrocatalyst materials of present embodiment one preparation is used for lithium-air battery.As can be seen, the enclosed pasture efficient that includes the ether lithium-air battery of above-mentioned eelctro-catalyst almost reaches 100%.
Embodiment two
With a La (NO
3)
3, a Co (NO
3)
2Be dissolved in the deionized water with PVP, PVP concentration is 25%, stirred 12 hours, obtain spinning presoma stoste, spinning presoma stoste obtains fibrous material through electrostatic spinning, and fibrous material was handled 10 hours in 70 ℃ of vacuum drying ovens, 600 ℃ of calcinings in air then, be incubated 3 hours, heating rate is 1 ℃/minute, can obtain LaCoO
3Electrocatalyst materials.
Embodiment three
With a La (NO
3)
36H
2O, a Fe (NO
3)
39H
2O and PVP are dissolved in the absolute ethyl alcohol, PVP concentration is 15%, stirred 12 hours, obtain spinning presoma stoste, spinning presoma stoste obtains fibrous material through electrostatic spinning, and fibrous material was handled 15 hours in 70 ℃ of vacuum drying ovens, 650 ℃ of calcinings in air then, be incubated 3 hours, heating rate is 1 ℃/minute, can obtain LaFeO
3Electrocatalyst materials.
Embodiment four
With two parts of La (NO
3)
36H
2O, a Nd (NO
3)
36H
2O, a Mn (CH
3COO)
24H
2O and PVP are dissolved among the DMF, PVP concentration is 20%, stirred 12 hours, obtain spinning presoma stoste, spinning presoma stoste obtains fibrous material through electrostatic spinning, and fibrous material was handled 12 hours in 70 ℃ of vacuum drying ovens, 700 ℃ of calcinings in air then, be incubated 3 hours, heating rate is 1 ℃/minute, can obtain LaNd
0.5Mn
0.5O
3Electrocatalyst materials.
Fig. 5 is the SEM figure of the electrocatalyst materials of present embodiment four preparations.As can be seen, this electrocatalyst materials is hollow porous nano tubulose structure.
Embodiment five
With a La (NO
3)
36H
2O, a Sm (NO
3)
3, two parts of Mn (CH
3COO)
24H
2O and PVP are dissolved among the DMF, PVP concentration is 20%, stirred 12 hours, obtain spinning presoma stoste, spinning presoma stoste obtains fibrous material through electrostatic spinning, and fibrous material was handled 12 hours in 70 ℃ of vacuum drying ovens, 700 ℃ of calcinings in air then, be incubated 5 hours, heating rate is 1 ℃/minute, can obtain La
0.5Sm
0.5MnO
3Electrocatalyst materials.
Embodiment six
With three parts of La (NO
3)
36H
2O, a Ba (NO
3)
2, four parts of Mn (CH
3COO)
24H
2O and PVP are dissolved among the DMF, PVP concentration is 10%, stirred 10 hours, obtain spinning presoma stoste, spinning presoma stoste obtains fibrous material through electrostatic spinning, and fibrous material was handled 10 hours in 70 ℃ of vacuum drying ovens, 650 ℃ of calcinings in air then, be incubated 4 hours, heating rate is 1 ℃/minute, can obtain La
0.75Ba
0.25MnO
3Electrocatalyst materials.
Fibrous material carried out " K cryogenic treatment " refer near the processing of temperature 70 ℃ or 70 ℃ described in the present invention.
Obviously, above-described embodiment only is for example clearly is described, and is not the restriction to execution mode.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all execution modes exhaustive.And the apparent variation of being extended out thus or change still are among the protection range of the invention.
Claims (10)
1. a lithium-air battery electrocatalyst materials is characterized in that, this electrocatalyst materials is the perovskite composite oxide of hollow porous nano tubular construction, its chemical expression La
1-xM
1xM
2 (1-y)M
3yO
3, wherein, 0≤x＜1,0≤y≤1; M
1Be alkaline-earth metal or rare earth ion, M
2And M
3Be transition metal ions.
2. electrocatalyst materials as claimed in claim 1 is characterized in that, wherein,
When 0.25≤x≤0.5, during y=0, M
1Be Nd
3+, Sr
2+, Sm
3+Or Ba
2+, M
2Be Mn
2+, Co
2+Or Fe
3+
Work as x=0, during y=0, M
2Be Mn
2+, Co
2+Or Fe
3+
Work as x=0,0＜y≤0.5 o'clock, M
2Be Mn
2+, Co
2+Or Fe
3+, M
3Be Nd
3+Or Sm
3+
3. electrocatalyst materials as claimed in claim 1 is characterized in that, the external diameter of pipe of described electrocatalyst materials is 80～120nm, and wall thickness is 5～20nm.
4. electrocatalyst materials as claimed in claim 1 is characterized in that, the specific area of described electrocatalyst materials is 20～50m
2/ g.
5. a kind of lithium-air battery as claimed in claim 1 is characterized in that this preparation method mainly may further comprise the steps with the preparation method of electrocatalyst materials:
(1) is that 0.5%～5% slaine presoma and mass concentration are that 10%～25% PVP is dissolved in the solvent with total mass concentration, obtains spinning presoma stoste;
(2) above-mentioned spinning presoma stoste is obtained fibrous material through electrostatic spinning;
(3) with above-mentioned fibrous material after K cryogenic treatment, in air, in 550～700 ℃ temperature lower calcination, be incubated 3～5 hours, obtain La
1-xM
1xM
2 (1-y)M
3yO
3Electrocatalyst materials;
Described slaine presoma contains a kind of lanthanum salt precursor body at least, and a kind of M
2Or M
3The slaine presoma.
6. preparation method as claimed in claim 5 is characterized in that, described slaine presoma is the nitrate of lanthanum, neodymium, samarium, strontium, barium, cobalt, manganese, iron or in the acetate two or more.
7. preparation method as claimed in claim 5 is characterized in that, in technique scheme, the molecular weight of described PVP is 500000～2000000.
8. preparation method as claimed in claim 5 is characterized in that, described solvent is water, ethanol or DMF.
9. preparation method as claimed in claim 5 is characterized in that, described in the step (3) fibrous material is carried out K cryogenic treatment, and treatment temperature is 70 ℃, and the processing time is 10～15 hours.
10. preparation method as claimed in claim 5 is characterized in that, the fibrous material calcining heat is to rise to temperature required by the speed that normal temperature begins with 1 ℃/minute in the step (3).
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Cited By (7)
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|---|---|---|---|---|
| CN105489972A (en) * | 2016-01-13 | 2016-04-13 | 深圳先进技术研究院 | Nanotube catalyst for air electrode of lithium-air battery in hierarchical porous structure |
| CN108855110A (en) * | 2018-07-02 | 2018-11-23 | 合肥萃励新材料科技有限公司 | A kind of preparation method of cobalt acid neodymium load oxidation cobalt fiber |
| CN109056114A (en) * | 2018-07-02 | 2018-12-21 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of cobalt acid neodymium fiber |
| CN110152677A (en) * | 2019-05-20 | 2019-08-23 | 宁波大学 | A kind of difunctional compound VPO catalysts of perovskite/cerium oxide with biomimetic features |
| CN110184682A (en) * | 2019-05-31 | 2019-08-30 | 福建师范大学 | It is a kind of to prepare Ca-Ti ore type LaCoO3Low temperature calcination method |
| CN113061934A (en) * | 2021-03-04 | 2021-07-02 | 江南大学 | High-entropy perovskite hollow nanotube efficient oxygen evolution reaction catalytic material and preparation method thereof |
| CN113871638A (en) * | 2021-10-14 | 2021-12-31 | 南京航空航天大学 | Lanthanum ferrite photoelectrode, preparation method thereof and application thereof in lithium-oxygen battery |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105489972A (en) * | 2016-01-13 | 2016-04-13 | 深圳先进技术研究院 | Nanotube catalyst for air electrode of lithium-air battery in hierarchical porous structure |
| CN108855110A (en) * | 2018-07-02 | 2018-11-23 | 合肥萃励新材料科技有限公司 | A kind of preparation method of cobalt acid neodymium load oxidation cobalt fiber |
| CN109056114A (en) * | 2018-07-02 | 2018-12-21 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of cobalt acid neodymium fiber |
| CN110152677A (en) * | 2019-05-20 | 2019-08-23 | 宁波大学 | A kind of difunctional compound VPO catalysts of perovskite/cerium oxide with biomimetic features |
| CN110152677B (en) * | 2019-05-20 | 2022-07-08 | 宁波大学 | Bifunctional perovskite/cerium oxide composite oxygen catalyst with bionic structure |
| CN110184682A (en) * | 2019-05-31 | 2019-08-30 | 福建师范大学 | It is a kind of to prepare Ca-Ti ore type LaCoO3Low temperature calcination method |
| CN113061934A (en) * | 2021-03-04 | 2021-07-02 | 江南大学 | High-entropy perovskite hollow nanotube efficient oxygen evolution reaction catalytic material and preparation method thereof |
| CN113061934B (en) * | 2021-03-04 | 2022-06-07 | 江南大学 | High-entropy perovskite hollow nanotube efficient oxygen evolution reaction catalytic material and preparation method thereof |
| CN113871638A (en) * | 2021-10-14 | 2021-12-31 | 南京航空航天大学 | Lanthanum ferrite photoelectrode, preparation method thereof and application thereof in lithium-oxygen battery |
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Application publication date: 20130717 |