CN105449226A - Novel three-dimensional electrode material for lithium air battery and preparation method for novel three-dimensional electrode material - Google Patents
Novel three-dimensional electrode material for lithium air battery and preparation method for novel three-dimensional electrode material Download PDFInfo
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- CN105449226A CN105449226A CN201510793179.5A CN201510793179A CN105449226A CN 105449226 A CN105449226 A CN 105449226A CN 201510793179 A CN201510793179 A CN 201510793179A CN 105449226 A CN105449226 A CN 105449226A
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/8803—Supports for the 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
- H01M4/88—Processes of manufacture
- H01M4/8817—Treatment of supports before application 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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8853—Electrodeposition
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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 invention discloses a novel three-dimensional electrode material for a lithium air battery and a preparation method for the novel three-dimensional electrode material, and belongs to the field of a chemical power source. The novel three-dimensional electrode material comprises carbon paper, 1-20% of carbon nanotube and 1-20% of catalyst based on the mass percent of the overall electrode material; the carbon nanotube is deposited on the carbon paper by chemical vapor deposition; and the catalyst is loaded on the carbon nanotube by electrochemical deposition. The preparation of a binder-less electrode material is realized; a complex powder electrode preparation process is avoided; and an oxygen electrode is simple in structure and easy to assemble.
Description
Technical field
The invention belongs to field of chemical power source, be specifically related to a kind of Novel lithium air cell three-diemsnional electrode material and preparation method thereof.
Background technology
Chemical energy storage, as a kind of important energy storage method, can carry out energy storage and release fast.But traditional lead acid accumulator, nickel-hydrogen accumulator energy density and power density can not meet the requirement of following energy-storage system, the lithium ion battery generally used in the market, specific capacity close to its theoretical value, the space significantly do not promoted.The extensive use of the various portable electric appts such as digital camera, notebook computer and smart mobile phone, in addition the greatly developing of electric automobile, have higher requirement to the high-energy-density of battery, reversible memory capacity and cyclical stability etc.Lithium-air battery is high with its energy density, have invertibity, advantages of environment protection demonstrates good application prospect.
Lithium-air battery is owing to having specific energy high (11400Wh/kg), and positive active material oxygen is directed to air, is the advantages such as the inexhaustible energy, has now become the focus of whole world research.Lithium-air battery has substantially increased its specific capacity and cyclicity stability through years of researches development.But be insoluble in organic solvent at the discharging product lithia of nonaqueous lithium air cell, can only deposit at cathode surface, easily cause oxygen channel to block, electric discharge is forced to the problems such as termination, at present, the preparation of lithium air electrode material adopts traditional making beating rubbing method mostly, and the use of binding agent makes surface reactive material large area reunite, and porosity reduces greatly, oxygen channel reduces, and binding agent itself is non-conductive, makes electric charge effectively can not arrive reaction interface, energy is suffered a loss.Therefore exploration have developed a kind of high performance electrode material and preparation method thereof becomes one of the important topic in current field.
Summary of the invention
The object of the present invention is to provide a kind of Novel lithium O for cathode of air battery material and preparation method thereof, this method substantially increases the surface area of material, for catalyst provides more avtive spot, and eliminate the use of binding agent, improve the utilance of electrode material.
The object of the invention is to be achieved through the following technical solutions:
A kind of Novel lithium air cell three-diemsnional electrode material, it is characterized in that, three-diemsnional electrode material is made up of carbon paper, carbon nano-tube and catalyst, and wherein carbon nanotube mass is the 1%-20% of whole electrode material quality, and catalyst quality accounts for the 1%-20% of whole electrode material quality.
Described catalyst is Pt nanoparticle, gold nano grain, palladium nano-particles, MnO
2nano particle, Co
3o
4nano particle, Fe
2o
3one or more in nano particle and NiO nano particle.
A preparation method for Novel lithium air cell three-diemsnional electrode material, comprises the following steps:
(1) preparation of carbon nano-tube/carbon paper three-dimensional composite material
The carbon paper of a, to be 2*5cm quality by a slice size be 44-46mg, at dilute sulfuric acid anodic oxidation 3min, wherein carbon paper is as anode, and titanium plate is as negative electrode, and deionized water is washed, dry;
B, the carbon paper after step a process is immersed in 50-250mL contains NiCl
2ethanolic solution in, take out after 5min, 80 DEG C of dryings obtain NiCl
2/ CFP;
C, by NiCl
2/ CFP puts into quartz reactor, prepares multi-walled carbon nano-tubes and is deposited on the surface of carbon paper, namely obtain multi-walled carbon nano-tubes/carbon paper three-dimensional composite material by vapour deposition process;
(2) load of catalyst and the formation of three-diemsnional electrode material
A, the salpeter solution carbon nano-tube prepared/carbon paper three-dimensional composite material being put into 50-250mL30% soak 2h, then with deionized water washing, and 80 DEG C of dryings;
B, the product of dried above (a) step is put into the 500-1000mL electric depositing solution configured, using the product of (a) step as work electrode, Pb, Ti or Ni, as to electrode, are 0-100mA/cm in current density
2electric current under electro-deposition 0-10min, wash 2-3 time with deionized water, after vacuumize, namely obtain novel three-diemsnional electrode material.
The gas that in described step (1), vapour deposition process uses is argon gas, hydrogen and ethene.
Described step (1) prepares the process of the vapour deposition process of carbon nano-tube for pass into argon gas as protective gas at temperature-rise period; ethene is as carbon source; constant temperature 1h after temperature reaches 1023k; logical hydrogen replaces argon gas; change the mist of logical hydrogen and argon gas after 20min, after 40min, naturally cool to room temperature under an argon atmosphere., the heating rate of described temperature-rise period is 10K/min.
Described carbon nano-tube is multi-walled carbon nano-tubes, the unordered staggered growth of multi-walled carbon nano-tubes, and the diameter of multi-walled carbon nano-tubes is 10-100nm.
The preparation method of described catalyst is electrodeposition process.
Beneficial effect of the present invention is: the preparation that present invention achieves binder free electrode material, eliminates complicated powder electrode preparation process, and oxygen electrode structure is simply easy to assembling.
Accompanying drawing explanation
In order to be illustrated more clearly in patent Example of the present invention and technical scheme of the prior art, below the accompanying drawing used required in embodiment or description of the prior art is briefly described.
Fig. 1 is the SEM figure that multi-walled carbon nano-tubes is deposited on carbon paper;
The SEM figure of Fig. 2 manganese dioxide that has been electro-deposition on multi-walled carbon nanotubes;
Fig. 3 nickel rear oxidation that has been electro-deposition on multi-walled carbon nanotubes generates the SEM figure of nickel oxide;
The SEM figure of the cobalt/cobalt oxide that Fig. 4 cobalt rear oxidation that has been electro-deposition on multi-walled carbon nanotubes becomes.
Embodiment
Embodiment 1
The carbon paper of to be 2*5cm quality by a slice size be 44.6mg, at dilute sulfuric acid Anodic Oxidation 3min, wherein carbon paper is as anode, and titanium plate is as negative electrode, and deionized water is washed, and puts into NiCl after drying
26H
2soak 5min in the ethanolic solution of O, take out 80 DEG C of dryings, obtain NiCl
2/ CFP.
By NiCl obtained above
2/ CFP puts into quartz reactor, heat up with the heating rate of 10K/min, temperature-rise period passes into argon gas as protective gas using the speed of 100mL/min, ethene is as carbon source, constant temperature 1h after temperature reaches 1023k, logical hydrogen replaces argon gas, the speed passed into is 200mL/min, the mist of logical hydrogen and argon gas is changed after 20min, wherein hydrogen: argon gas=8:5, be 130mL/min by the speed of mist, room temperature is naturally cooled under an argon atmosphere after 40min, namely multi-walled carbon nano-tubes/carbon paper three-dimensional composite material is obtained, the diameter of multi-walled carbon nano-tubes is 10-100nm.
With deionized water washing after the three-dimensional composite material prepared is soaked 2h in the solution of the nitric acid of 50mL30%, after drying with the three-dimensional composite material after process for work electrode, with containing 0.1mol/LMn (CH
3cOO)
2with 0.1mol/LNa
2sO
4solution 500mL be electric depositing solution, be to electrode with stereotype, at 8mA/cm
2under current density, deposition 30s, then with deionized water washing, 80 DEG C of dryings, namely obtain with MnO
2nano particle is the novel three-dimensional electrode material of catalyst.
Embodiment 2
The carbon paper of to be 2*5cm quality by a slice size be 45.5mg, at dilute sulfuric acid Anodic Oxidation 3min, wherein carbon paper is as anode, and titanium plate is as negative electrode, and deionized water is washed, and puts into NiCl after drying
26H
2soak 5min in the ethanolic solution of O, take out 80 DEG C of dryings, obtain NiCl
2/ CFP.
By NiCl obtained above
2/ CFP puts into quartz reactor, heat up with the heating rate of 10K/min, temperature-rise period passes into argon gas as protective gas using the speed of 100mL/min, ethene is as carbon source, constant temperature 1h after temperature reaches 1023k, logical hydrogen replaces argon gas, the speed passed into is 200mL/min, the mist of logical hydrogen and argon gas is changed after 20min, wherein hydrogen: argon gas=8:5, be 130mL/min by the speed of mist, room temperature is naturally cooled under an argon atmosphere after 40min, both multi-walled carbon nano-tubes/carbon paper three-dimensional composite material had been obtained, the diameter of multi-walled carbon nano-tubes is 10-100nm.
With deionized water washing after the three-dimensional composite material prepared is soaked 2h in the solution of the nitric acid of 150mL30%, with the three-dimensional composite material after processing for work electrode, with containing 1.5mol/LMnSO
4being electrodeposit liquid with the solution 800mL of 0.2g/L dodecyl sodium sulfate, is to electrode with stereotype, at 5mA/cm
2under current density, deposition 2min, then with deionized water washing, 80 DEG C of dryings, namely obtain with MnO
2nano particle is the novel three-dimensional electrode material of catalyst.
Embodiment 3
The carbon paper of to be 2*5cm quality by a slice size be 45.3mg, at dilute sulfuric acid Anodic Oxidation 3min, wherein carbon paper is as anode, and titanium plate is as negative electrode, and deionized water is washed, and puts into NiCl after drying
26H
2soak 5min in the ethanolic solution of O, take out 80 DEG C of dryings, obtain NiCl
2/ CFP.
By NiCl obtained above
2/ CFP puts into quartz reactor, heat up with the heating rate of 10K/min, temperature-rise period passes into argon gas as protective gas using the speed of 100mL/min, ethene is as carbon source, constant temperature 1h after temperature reaches 1023k, logical hydrogen replaces argon gas, the speed passed into is 200mL/min, the mist of logical hydrogen and argon gas is changed after 20min, wherein hydrogen: argon gas=8:5, be 130mL/min by the speed of mist, room temperature is naturally cooled under an argon atmosphere after 40min, namely multi-walled carbon nano-tubes/carbon paper three-dimensional composite material is obtained, the diameter of multi-walled carbon nano-tubes is 10-100nm.
Wash with deionized water after the three-dimensional composite material prepared is soaked 2h in the solution of the nitric acid of 200mL30%, with the three-dimensional composite material after process for work electrode, with the 800mL solution containing six hydration nickel sulfate 100g/L, Nickel dichloride hexahydrate 60g/L, boric acid 40g/L, dodecyl sodium sulfate 0.1g/L and thiocarbamide 0.1g/L for electrodeposit liquid, be to electrode with nickel plate, at 5mA/cm
2under current density, deposition 2min, then with deionized water washing, dry, 600 DEG C of roasting 3h, the novel three-dimensional electrode material that namely to obtain with NiO nano particle be catalyst.
Embodiment 4
The carbon paper of to be 2*5cm quality by a slice size be 45.8mg, at dilute sulfuric acid Anodic Oxidation 3min, wherein carbon paper is as anode, and titanium plate is as negative electrode, and deionized water is washed, and puts into NiCl after drying
26H
2soak 5min in the ethanolic solution of O, take out 80 DEG C of dryings, obtain NiCl
2/ CFP.
By NiCl obtained above
2/ CFP puts into quartz reactor, heat up with the heating rate of 10K/min, temperature-rise period passes into argon gas as protective gas using the speed of 100mL/min, ethene is as carbon source, constant temperature 1h after temperature reaches 1023k, logical hydrogen replaces argon gas, the speed passed into is 200mL/min, the mist of logical hydrogen and argon gas is changed after 20min, wherein hydrogen: argon gas=8:5, be 130mL/min by the speed of mist, room temperature is naturally cooled under an argon atmosphere after 40min, namely multi-walled carbon nano-tubes/carbon paper three-dimensional composite material is obtained, the diameter of multi-walled carbon nano-tubes is 10-100nm.
Wash with deionized water after the three-dimensional composite material prepared is soaked 2h in the solution of the nitric acid of 250mL30%, with the three-dimensional composite material after process for work electrode, with the 1000mL solution containing cobaltous sulfate 20g/L and natrium citricum 50g/L for electrodeposit liquid, be to electrode with titanium plate, at 10mA/cm
2under current density, deposition 2min, then with deionized water washing, dry, 350 DEG C of roasting 3h, namely obtain with Co
3o
4nano particle is the novel three-dimensional electrode material of catalyst.
Claims (9)
1. a Novel lithium air cell three-diemsnional electrode material, it is characterized in that, described three-diemsnional electrode material is made up of carbon paper, carbon nano-tube and catalyst, and wherein carbon nanotube mass is the 1%-20% of whole electrode material quality, and catalyst quality accounts for the 1%-20% of whole electrode material quality.
2. three-diemsnional electrode material according to claim 1, is characterized in that, described catalyst is Pt nanoparticle, gold nano grain, palladium nano-particles, MnO
2nano particle, Co
3o
4nano particle, Fe
2o
3one or more in nano particle and NiO nano particle.
3. a preparation method for Novel lithium air cell three-diemsnional electrode material as claimed in claim 1, is characterized in that, comprise the following steps:
(1) preparation of carbon nano-tube/carbon paper three-dimensional composite material
The carbon paper of to be a. 2*5cm quality by a slice size be 44-46mg, at dilute sulfuric acid anodic oxidation 3min, wherein carbon paper is as anode, and titanium plate is as negative electrode, and deionized water is washed, dry;
B. the carbon paper after step a process is immersed in 50-250mL and contains NiCl
2ethanolic solution in, take out after 5min, 80 DEG C of dryings obtain NiCl
2/ CFP;
C. by NiCl
2/ CFP puts into quartz reactor, prepares carbon nano-tube and is deposited on the surface of carbon paper, namely obtain carbon nano-tube/carbon paper three-dimensional composite material by vapour deposition process;
(2) load of catalyst and the formation of three-diemsnional electrode material
A. the salpeter solution carbon nano-tube prepared/carbon paper three-dimensional composite material being put into 50-250mL30% soaks 2h, then with deionized water washing, and 80 DEG C of dryings;
B. the product of dried above (a) step is put into the 500-1000mL electric depositing solution configured, using the product of (a) step as work electrode, Pb, Ti or Ni, as to electrode, are 0-100mA/cm in current density
2electric current under electro-deposition 0-10min, wash 2-3 time with deionized water, after drying, namely obtain novel three-diemsnional electrode material.
4. the preparation method of three-diemsnional electrode material according to claim 3, is characterized in that, the gas that in described step (1), vapour deposition process uses is argon gas, hydrogen and ethene.
5. the preparation method of three-diemsnional electrode material according to claim 3; it is characterized in that: described step (1) prepares the process of the vapour deposition process of carbon nano-tube for pass into argon gas as protective gas at temperature-rise period; ethene is as carbon source; constant temperature 1h after temperature reaches 1023k; logical hydrogen replaces argon gas; change the mist of logical hydrogen and argon gas after 20min, after 40min, naturally cool to room temperature under an argon atmosphere.
6. the preparation method of three-diemsnional electrode material according to claim 5, is characterized in that, the heating rate of described temperature-rise period is 10K/min.
7. the preparation method of three-diemsnional electrode material according to claim 3, is characterized in that, described carbon nano-tube is multi-walled carbon nano-tubes, the unordered staggered growth of multi-walled carbon nano-tubes.
8. the preparation method of three-diemsnional electrode material according to claim 3, is characterized in that, the diameter of described multi-walled carbon nano-tubes is 10-100nm.
9. the preparation method of three-diemsnional electrode material according to claim 3, is characterized in that: the preparation method of described catalyst is electrodeposition process.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107359341A (en) * | 2017-07-26 | 2017-11-17 | 青岛大学 | A kind of one-step method synthesizes the method and its application of black phosphorus on carbon paper |
| CN107863494A (en) * | 2017-10-25 | 2018-03-30 | 北京理工大学 | A kind of Its Preparation Method And Use of flexible gas electrode for lithium-air battery |
| CN110416529A (en) * | 2019-07-08 | 2019-11-05 | 中山大学 | Flexible zinc negative electrode material and preparation method and application thereof |
| CN112160075A (en) * | 2020-10-22 | 2021-01-01 | 广西师范大学 | Preparation method and application of ethylene-vinyl acetate/carbon composite nanofiber |
| CN113725444A (en) * | 2020-05-25 | 2021-11-30 | 中国科学院大连化学物理研究所 | Ruthenium/carbon nanotube flexible positive electrode material and preparation method and application thereof |
| CN115538147A (en) * | 2022-09-26 | 2022-12-30 | 贵州梅岭电源有限公司 | Preparation method of three-dimensional fluorinated carbon fiber flexible electrode |
| US11876207B2 (en) | 2016-07-01 | 2024-01-16 | Nippon Telegraph And Telephone Corporation | Battery and method of manufacturing cathode of the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US11876207B2 (en) | 2016-07-01 | 2024-01-16 | Nippon Telegraph And Telephone Corporation | Battery and method of manufacturing cathode of the same |
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| CN110416529A (en) * | 2019-07-08 | 2019-11-05 | 中山大学 | Flexible zinc negative electrode material and preparation method and application thereof |
| CN110416529B (en) * | 2019-07-08 | 2021-06-25 | 中山大学 | Flexible zinc negative electrode material and preparation method and application thereof |
| CN113725444A (en) * | 2020-05-25 | 2021-11-30 | 中国科学院大连化学物理研究所 | Ruthenium/carbon nanotube flexible positive electrode material and preparation method and application thereof |
| CN113725444B (en) * | 2020-05-25 | 2023-05-02 | 中国科学院大连化学物理研究所 | Ruthenium/carbon nano tube flexible positive electrode material and preparation method and application thereof |
| CN112160075A (en) * | 2020-10-22 | 2021-01-01 | 广西师范大学 | Preparation method and application of ethylene-vinyl acetate/carbon composite nanofiber |
| CN112160075B (en) * | 2020-10-22 | 2021-07-27 | 广西师范大学 | Preparation method and application of ethylene-vinyl acetate/carbon composite nanofiber |
| CN115538147A (en) * | 2022-09-26 | 2022-12-30 | 贵州梅岭电源有限公司 | Preparation method of three-dimensional fluorinated carbon fiber flexible electrode |
| CN115538147B (en) * | 2022-09-26 | 2023-10-17 | 贵州梅岭电源有限公司 | Preparation method of three-dimensional carbon fluoride fiber flexible electrode |
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