CN104505522A - Hydrothermal preparation method of lanthanum-nickel composite oxide catalyst for lithium air battery - Google Patents
Hydrothermal preparation method of lanthanum-nickel composite oxide catalyst for lithium air battery Download PDFInfo
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- 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
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- H—ELECTRICITY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
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Abstract
The invention relates to the technical field of catalysts for lithium air batteries, and particularly relates to a hydrothermal preparation method of a lanthanum-nickel composite oxide catalyst for a lithium air battery. The hydrothermal preparation method comprises the following steps: weighing lanthanum salt and nickel salt at the stoichiometric ratio of 2 to 1, and dissolving the lanthanum salt and the nickel salt into deionized water; dropwise adding 0.002-0.004 mol of glycine, adding a pH modifier and stirring; heating in an airtight way for 10-14h at temperature of 175-185 DEG C to obtain a product, washing the product and drying the obtained product; and sintering at high temperature in an oxygen-enriched atmosphere, so as to obtain the lanthanum-nickel composite oxide catalyst for the lithium air battery. The catalyst prepared by adopting the method is a La2NiO4 material with a cubic lattice structure, the size is uniform, the relative supporting property of the cubic lattice structure is high, and is not prone to lose, so that the unit active area of the catalyst is increased, and the service life of the catalyst is prolonged; the electrochemical testing also shows that the cycle life of the catalyst is excellent, the catalyst has the relatively high practical value, and can meet industrial requirements on high-performance ether-base lithium air batteries.
Description
Technical field
The present invention relates to lithium-air battery catalyst technical field, be specifically related to a kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst.
Background technology
Lithium-air battery is subject to extensive concern owing to having higher theoretical energy density.Battery advantage is the active material oxygen of positive pole is be directed to air, does not need to be stored in inside battery, has so not only reduced cost but also has alleviated the weight of battery.But want to be realized application, also need to solve series of problems, such as electrolyte stability is low, high rate performance is poor, cyclical stability is poor, and the catalyst that lithium-air battery uses directly affects these performances.
The catalyst in ethers electrolyte with catalytic activity of current report mainly contains noble metal, pyrochlore oxide and Co3O4 etc., but, these catalyst are all be deposited in air electrode with granular form, be unfavorable for the mass transfer of air electrode in the performance of its catalytic activity and 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 meet the requirement of the industrialization of high-performance ether lithium-air cell.
Summary of the invention
The object of the present invention is to provide a kind of low cost that can meet the requirement of high-performance ether lithium-air battery industrialization, the hydrothermal preparing process of high performance lithium-air battery La-Ni mixed oxides catalyst.
Object of the present invention is achieved through the following technical solutions: a kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A hydrothermal preparing process for lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, take lanthanum salt and nickel salt respectively according to stoichiometric proportion 2:1, be dissolved in 60-80mL deionized water, stir and form mixed solution, controlling nickel salt concentration in mixed solution is 0.0005-0.0015mol/L;
B, mixed solution and dripping 0.002-0.004mol glycine to steps A, glycine makes gel and pH buffer;
C, will add pH value regulator in the mixed solution dripping glycine in step B and stir, adjust ph be 7.6-7.8;
D, by the mixed solution of step C airtight heating 10-14h under 175-185 DEG C of condition, obtain product;
E, by the product washing and drying of step D;
F, the high temperature sintering in oxygen-enriched atmosphere of the product after step e process, to form nanostructure, is first warming up to 600-700 DEG C with the heating rate of 2-4 DEG C/min, is then incubated 2-4 hour, obtains lithium-air battery La-Ni mixed oxides catalyst.
Preferably, in described steps A, lanthanum salt is lanthanum nitrate hexahydrate, and described nickel salt is nickel nitrate.Nitrate anion can at high temperature decompose, and avoids introducing non-catalytic residue.
Preferably, in described steps A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
Preferably, in described step C, the rotating speed of stirring is 150 revs/min.
Preferably, in described step C, pH value regulator is ammoniacal liquor, and ammoniacal liquor can regulate rear loss in pH value, avoids introducing non-catalytic residue.
Preferably, in described step D, airtight heating carries out in hydrothermal reaction kettle.
Preferably, the oven dry in described step e carries out under 80 DEG C of temperature conditions.
Preferably, in described step F, high-temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole utilizing the preparation of lithium-air battery La-Ni mixed oxides catalyst.
A kind of lithium ion battery utilizing lithium-air battery positive pole to prepare.
Beneficial effect of the present invention is: the lithium-air battery La-Ni mixed oxides catalyst prepared by preparation method provided by the invention is the La with cubic crystal structure
2niO
4material, its size uniform, cubic crystal structure relative support is comparatively strong, not easily runs off, thus improves units activity area and the life-span of catalyst; Electro-chemical test also shows that the lithium-air battery La-Ni mixed oxides catalyst cycle life adopting the method to prepare is superior, has higher practical value, can meet the requirement of high-performance ether lithium-air cell industrialization; The cost of raw material that the present invention takes is lower, and preparation work is easily simple, is easy to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the life curve of lithium ion battery prepared by lithium-air battery La-Ni mixed oxides catalyst of the present invention.
Fig. 2 is the first charge-discharge curve of lithium ion battery prepared by lithium-air battery La-Ni mixed oxides catalyst of the present invention.
Fig. 3 is SEM figure prepared by lithium-air battery La-Ni mixed oxides catalyst of the present invention.
Fig. 4 is XRD figure prepared by lithium-air battery La-Ni mixed oxides catalyst of the present invention.
Embodiment
For the ease of the understanding of those skilled in the art, below in conjunction with embodiment and accompanying drawing 1-4, the present invention is further illustrated, and the content that execution mode is mentioned not is limitation of the invention.
embodiment 1
A hydrothermal preparing process for lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, take lanthanum salt and nickel salt respectively according to stoichiometric proportion 2:1, be dissolved in 60mL deionized water, stir and form mixed solution, controlling nickel salt concentration in mixed solution is 0.0005mol/L;
B, mixed solution and dripping 0.002mol glycine to steps A;
C, will add pH value regulator in the mixed solution dripping glycine in step B and stir, adjust ph be 7.6;
D, by the mixed solution of step C airtight heating 14h under 175 DEG C of conditions, obtain product;
E, by the product washing and drying of step D;
F, by the high temperature sintering in oxygen-enriched atmosphere of the product after step e process, be first warming up to 600 DEG C with the heating rate of 2 DEG C/min, be then incubated 4 hours, obtain lithium-air battery La-Ni mixed oxides catalyst.
In described steps A, lanthanum salt is lanthanum nitrate hexahydrate, and described nickel salt is nickel nitrate.
In described steps A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In described step C, the rotating speed of stirring is 150 revs/min.
In described step C, pH value regulator is ammoniacal liquor.
In described step D, airtight heating carries out in hydrothermal reaction kettle.
Oven dry in described step e carries out under 80 DEG C of temperature conditions.
In described step F, high-temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole utilizing the preparation of above-mentioned lithium-air battery La-Ni mixed oxides catalyst.A kind of lithium ion battery utilizing above-mentioned lithium-air battery positive pole to prepare.
Concrete, the lithium-air battery La-Ni mixed oxides catalyst La obtained by the present embodiment
2niO
4, conductive agent Ketjen black, binding agent PTFE mix according to mass ratio 3.5:4.5:1, with 1-METHYLPYRROLIDONE NMP, this mixture is modulated into slurry, evenly be coated on Copper Foil, put into 90 DEG C, baking oven and dry 2h, taking-up is washed into pole piece, and 120 DEG C of vacuumize 12h, carry out roll-in, 85 DEG C of vacuumize 12h, obtained laboratory cells pole piece.Using lithium sheet as to electrode, electrolyte is the TEGDME(TRIGLYME of 1mol/L LiTFSI (two trifluoromethanesulfonimide lithium)) solution, barrier film is glass fibre, be assembled into the special button cell of CR2025 type at the glove box being full of argon gas atmosphere and carry out discharge and recharge in atmosphere, charge cutoff voltage is 4.4V, discharge cut-off voltage is 2.1V, and charging and discharging currents density is set to 51mA/g, the quality in current density unit be anode catalyst and conductive carbon quality and.Recording battery first discharge specific capacity is 3750mAh/g.
embodiment 2
A hydrothermal preparing process for lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, take lanthanum salt and nickel salt respectively according to stoichiometric proportion 2:1, be dissolved in 70mL deionized water, stir and form mixed solution, controlling nickel salt concentration in mixed solution is 0.001mol/L;
B, mixed solution and dripping 0.003mol glycine to steps A;
C, will add pH value regulator in the mixed solution dripping glycine in step B and stir, adjust ph be 7. 7;
D, by the mixed solution of step C airtight heating 12h under 180 DEG C of conditions, obtain product;
E, by the product washing and drying of step D;
F, by the high temperature sintering in oxygen-enriched atmosphere of the product after step e process, be first warming up to 650 DEG C with the heating rate of 3 DEG C/min, be then incubated 3 hours, obtain lithium-air battery La-Ni mixed oxides catalyst.
In described steps A, lanthanum salt is lanthanum nitrate hexahydrate, and described nickel salt is nickel nitrate.
In described steps A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In described step C, the rotating speed of stirring is 150 revs/min.
In described step C, pH value regulator is ammoniacal liquor.
In described step D, airtight heating carries out in hydrothermal reaction kettle.
Oven dry in described step e carries out under 80 DEG C of temperature conditions.
In described step F, high-temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole utilizing the preparation of above-mentioned lithium-air battery La-Ni mixed oxides catalyst.A kind of lithium ion battery utilizing above-mentioned lithium-air battery positive pole to prepare.
Concrete, the lithium-air battery La-Ni mixed oxides catalyst La obtained by the present embodiment
2niO
4, conductive agent Ketjen black, binding agent PTFE mix according to mass ratio 3.5:4.5:1, with 1-METHYLPYRROLIDONE NMP, this mixture is modulated into slurry, evenly be coated on Copper Foil, put into 90 DEG C, baking oven and dry 2h, taking-up is washed into pole piece, and 120 DEG C of vacuumize 12h, carry out roll-in, 85 DEG C of vacuumize 12h, obtained laboratory cells pole piece.Using lithium sheet as to electrode, electrolyte is the TEGDME(TRIGLYME of 1mol/L LiTFSI (two trifluoromethanesulfonimide lithium)) solution, barrier film is glass fibre, the special button cell of CR2025 type is assembled at the glove box being full of argon gas atmosphere, carry out discharge and recharge in atmosphere, charge cutoff voltage is 4.5V, and discharge cut-off voltage is 2.0V, charging and discharging currents density is set to 50mA/g, the quality in current density unit be anode catalyst and conductive carbon quality and.Recording battery first discharge specific capacity is 3751mAh/g.
Embodiment 3
A hydrothermal preparing process for lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, take lanthanum salt and nickel salt respectively according to stoichiometric proportion 2:1, be dissolved in 70mL deionized water, stir and form mixed solution, controlling nickel salt concentration in mixed solution is 0.0011mol/L;
B, mixed solution and dripping 0.003mol glycine to steps A;
C, will add pH value regulator in the mixed solution dripping glycine in step B and stir, adjust ph be 7.8;
D, by the mixed solution of step C airtight heating 13h under 179 DEG C of conditions, obtain product;
E, by the product washing and drying of step D;
F, by the high temperature sintering in oxygen-enriched atmosphere of the product after step e process, be first warming up to 680 DEG C with the heating rate of 3 DEG C/min, be then incubated 3 hours, obtain lithium-air battery La-Ni mixed oxides catalyst.
In described steps A, lanthanum salt is lanthanum nitrate hexahydrate, and described nickel salt is nickel nitrate.
In described steps A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In described step C, the rotating speed of stirring is 150 revs/min.
In described step C, pH value regulator is ammoniacal liquor.
In described step D, airtight heating carries out in hydrothermal reaction kettle.
Oven dry in described step e carries out under 80 DEG C of temperature conditions.
In described step F, high-temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole utilizing the preparation of above-mentioned lithium-air battery La-Ni mixed oxides catalyst.A kind of lithium ion battery utilizing above-mentioned lithium-air battery positive pole to prepare.
Concrete, the lithium-air battery La-Ni mixed oxides catalyst La obtained by the present embodiment
2niO
4, conductive agent Ketjen black, binding agent PTFE mix according to mass ratio 3.5:4.5:1, with 1-METHYLPYRROLIDONE NMP, this mixture is modulated into slurry, evenly be coated on Copper Foil, put into 90 DEG C, baking oven and dry 2h, taking-up is washed into pole piece, and 120 DEG C of vacuumize 12h, carry out roll-in, 85 DEG C of vacuumize 12h, obtained laboratory cells pole piece.Using lithium sheet as to electrode, electrolyte is the TEGDME(TRIGLYME of 1mol/L LiTFSI (two trifluoromethanesulfonimide lithium)) solution, barrier film is glass fibre, the special button cell of CR2025 type is assembled at the glove box being full of argon gas atmosphere, carry out discharge and recharge in atmosphere, charge cutoff voltage is 4.4V, and discharge cut-off voltage is 2.0V, charging and discharging currents density is set to 50mA/g, the quality in current density unit be anode catalyst and conductive carbon quality and.Recording battery first discharge specific capacity is 3750mAh/g.
embodiment 4
A hydrothermal preparing process for lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, take lanthanum salt and nickel salt respectively according to stoichiometric proportion 2:1, be dissolved in 80mL deionized water, stir and form mixed solution, controlling nickel salt concentration in mixed solution is 0.0015mol/L;
B, mixed solution and dripping 0.004mol glycine to steps A;
C, will add pH value regulator in the mixed solution dripping glycine in step B and stir, adjust ph be 7.8;
D, by the mixed solution of step C airtight heating 10h under 185 DEG C of conditions, obtain product;
E, by the product washing and drying of step D;
F, by the high temperature sintering in oxygen-enriched atmosphere of the product after step e process, be first warming up to 700 DEG C with the heating rate of 4 DEG C/min, be then incubated 2 hours, obtain lithium-air battery La-Ni mixed oxides catalyst.
In described steps A, lanthanum salt is lanthanum nitrate hexahydrate, and described nickel salt is nickel nitrate.
In described steps A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In described step C, the rotating speed of stirring is 150 revs/min.
In described step C, pH value regulator is ammoniacal liquor.
In described step D, airtight heating carries out in hydrothermal reaction kettle.
Oven dry in described step e carries out under 80 DEG C of temperature conditions.
In described step F, high-temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole utilizing the preparation of above-mentioned lithium-air battery La-Ni mixed oxides catalyst.A kind of lithium ion battery utilizing above-mentioned lithium-air battery positive pole to prepare.
Concrete, the lithium-air battery La-Ni mixed oxides catalyst La obtained by the present embodiment
2niO
4, conductive agent Ketjen black, binding agent PTFE mix according to mass ratio 3.5:4.5:1, with 1-METHYLPYRROLIDONE NMP, this mixture is modulated into slurry, evenly be coated on Copper Foil, put into 90 DEG C, baking oven and dry 2h, taking-up is washed into pole piece, and 120 DEG C of vacuumize 12h, carry out roll-in, 85 DEG C of vacuumize 12h, obtained laboratory cells pole piece.Using lithium sheet as to electrode, electrolyte is the TEGDME(TRIGLYME of 1mol/L LiTFSI (two trifluoromethanesulfonimide lithium)) solution, barrier film is glass fibre, the special button cell of CR2025 type is assembled at the glove box being full of argon gas atmosphere, carry out discharge and recharge in atmosphere, charge cutoff voltage is 4.5V, and discharge cut-off voltage is 2.0V, charging and discharging currents density is set to 50mA/g, the quality in current density unit be anode catalyst and conductive carbon quality and.Recording battery first discharge specific capacity is 3751mAh/g.
Application battery cycle life of the present invention can reach 50 times as seen in Figure 1, illustrates that the life-span of lithium-air battery of the present invention is higher than the average life span of current lithium-air battery.
Application battery capacity of the present invention can reach 3751mAh as seen in Figure 2, illustrates that battery capacity of the present invention has reached 1.3 times of current lithium-air battery average level.
The particle size of catalyst of the present invention is at about 100nm as seen in Figure 3, illustrates that catalyst size of the present invention has reached Nano grade and even particle size distribution.
Marker peak represents the characteristic peak of nickel acid lanthanum as seen in Figure 4, illustrates that the catalyst prepared is nickel acid lanthanum.
Above-described embodiment is the present invention's preferably implementation, and in addition, the present invention can also realize by alternate manner, and any apparent replacement is all within protection scope of the present invention without departing from the inventive concept of the premise.
Claims (10)
1. a hydrothermal preparing process for lithium-air battery La-Ni mixed oxides catalyst, is characterized in that: comprise the following steps:
A, take lanthanum salt and nickel salt respectively according to stoichiometric proportion 2:1, be dissolved in 60-80mL deionized water, stir and form mixed solution, controlling nickel salt concentration in mixed solution is 0.0005-0.0015mol/L;
B, mixed solution and dripping 0.002-0.004mol glycine to steps A;
C, will add pH value regulator in the mixed solution dripping glycine in step B and stir, adjust ph be 7.6-7.8;
D, by the mixed solution of step C airtight heating 10-14h under 175-185 DEG C of condition, obtain product;
E, by the product washing and drying of step D;
F, by the high temperature sintering in oxygen-enriched atmosphere of the product after step e process, be first warming up to 600-700 DEG C with the heating rate of 2-4 DEG C/min, be then incubated 2-4 hour, obtain lithium-air battery La-Ni mixed oxides catalyst.
2. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, is characterized in that: in described steps A, and lanthanum salt is lanthanum nitrate hexahydrate, and described nickel salt is nickel nitrate.
3. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, is characterized in that: in described steps A, and the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
4. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, is characterized in that: in described step C, and the rotating speed of stirring is 150 revs/min.
5. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, is characterized in that: in described step C, pH value regulator is ammoniacal liquor.
6. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, is characterized in that: in described step D, airtight heating carries out in hydrothermal reaction kettle.
7. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, is characterized in that: the oven dry in described step e is carried out at 80 DEG C.
8. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, is characterized in that: in described step F, high-temperature oxygen-enriched atmosphere is carried out in tube furnace.
9. one kind utilizes the lithium-air battery positive pole of the preparation of a kind of lithium-air battery La-Ni mixed oxides catalyst described in claim 1.
10. the lithium ion battery utilizing the lithium-air battery positive pole described in claim 9 to prepare.
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Cited By (2)
| 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 |
| CN107570162A (en) * | 2017-08-09 | 2018-01-12 | 浙江海洋大学 | A kind of nickel-base catalyst for reverse water-gas-shift reaction and preparation method thereof |
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| CN101186328A (en) * | 2007-12-07 | 2008-05-28 | 北京工业大学 | Method for preparing single-crystal perovskite type oxide La2CuO4 nano and micron rod |
| CN101564690A (en) * | 2009-06-04 | 2009-10-28 | 天津渤海职业技术学院 | Preparation method of perovskite-like La*NiO* and applications |
| US20120003548A1 (en) * | 2009-03-18 | 2012-01-05 | Showa Denko K.K. | Air battery catalyst and air battery using the same |
| KR20130123621A (en) * | 2012-05-03 | 2013-11-13 | 한국에너지기술연구원 | Cathode catalyst for lithium-air battery, method of manufacturing the same, and lithium-air battery comprising the same |
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Patent Citations (4)
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| CN101186328A (en) * | 2007-12-07 | 2008-05-28 | 北京工业大学 | Method for preparing single-crystal perovskite type oxide La2CuO4 nano and micron rod |
| US20120003548A1 (en) * | 2009-03-18 | 2012-01-05 | Showa Denko K.K. | Air battery catalyst and air battery using the same |
| CN101564690A (en) * | 2009-06-04 | 2009-10-28 | 天津渤海职业技术学院 | Preparation method of perovskite-like La*NiO* and applications |
| KR20130123621A (en) * | 2012-05-03 | 2013-11-13 | 한국에너지기술연구원 | Cathode catalyst for lithium-air battery, method of manufacturing the same, and lithium-air battery comprising the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN107570162A (en) * | 2017-08-09 | 2018-01-12 | 浙江海洋大学 | A kind of nickel-base catalyst for reverse water-gas-shift reaction and preparation method thereof |
| CN107570162B (en) * | 2017-08-09 | 2020-06-16 | 浙江海洋大学 | Nickel-based catalyst for reverse water gas shift reaction and preparation method thereof |
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| CN104505522B (en) | 2017-05-03 |
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