CN104505522B - 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 PDF

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CN104505522B
CN104505522B CN201410847961.6A CN201410847961A CN104505522B CN 104505522 B CN104505522 B CN 104505522B CN 201410847961 A CN201410847961 A CN 201410847961A CN 104505522 B CN104505522 B CN 104505522B
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lithium
air battery
catalyst
mixed oxides
lanthanum
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CN104505522A (en
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魏中山
屈德扬
董鸣
董一鸣
张新河
李中延
郑新宇
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Mcnair Technology Co Ltd
Dongguan Mcnair New Power Co Ltd
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Mcnair Technology Co Ltd
Dongguan Mcnair New Power Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90Selection of catalytic material
    • H01M4/9016Oxides, hydroxides or oxygenated metallic salts
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8825Methods for deposition of the catalytic active composition
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M2004/8678Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
    • H01M2004/8689Positive electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Inert Electrodes (AREA)
  • Hybrid Cells (AREA)

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

A kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst
Technical field
The present invention relates to lithium-air battery catalyst technical field, and in particular to a kind of lithium-air battery is compound with lanthanum nickel The hydrothermal preparing process of oxide catalyst.
Background technology
Lithium-air battery with higher theoretical energy density due to receiving significant attention.Battery advantage is positive pole Active material oxygen is to be directed to air, it is not necessary to be stored in inside battery, had so not only reduced cost but also had alleviated electricity The weight in pond.But want to be realized application, in addition it is also necessary to solve series of problems, such as electrolyte stability is low, forthright again Poor, cyclical stability difference of energy etc., and the catalyst that lithium-air battery is used directly affects these performances.
At present the catalyst with catalysis activity in ethers electrolyte of report mainly has noble metal, pyrochlore oxide With Co3O4 etc., but, these catalyst are deposited in air electrode with granular form, are unfavorable for its catalysis activity Performance and cell reaction in air electrode mass transfer, cause ethers lithium-air battery performance reduce.Wherein, precious metal catalyst Also there is the deficiency of high cost in agent.Therefore, above-mentioned existing several catalyst can not meet high-performance ether lithium-air The requirement of the industrialization of battery.
The content of the invention
It is an object of the invention to provide a kind of requirement that disclosure satisfy that high-performance ether lithium-air battery industrialization is low Cost, the hydrothermal preparing process of high performance lithium-air battery La-Ni mixed oxides catalyst.
The purpose of the present invention is achieved through the following technical solutions:A kind of lithium-air battery La-Ni mixed oxides catalyst Hydrothermal preparing process, comprise the following steps:
A kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, according to stoichiometric proportion 2:1 weighs respectively lanthanum salt and nickel salt, in being dissolved in 60-80mL deionized waters, stirs shape Into mixed solution, it is 0.0005-0.0015mol/L to control nickel salt concentration in mixed solution;
B, to the mixed solution and dripping 0.002-0.004mol glycine of step A, glycine make gel and pH buffering Agent;
C, will be added dropwise to be added in the mixed solution of glycine in step B and pH value regulator and stirred, adjusting pH value has been 7.6-7.8;
D, by the mixed solution of step C under the conditions of 175-185 DEG C airtight heating 10-14h, obtain product;
E, by the product washing and drying of step D;
F, the product after the process of step E is sintered to form nanostructured in oxygen-enriched atmosphere high temperature, first with 2-4 DEG C The heating rate of/min is warming up to 600-700 DEG C, is then incubated 2-4 hours, obtains lithium-air battery La-Ni mixed oxides Catalyst.
Preferably, in step A, lanthanum salt is lanthanum nitrate hexahydrate, and the nickel salt is nickel nitrate.Nitrate anion can be at high temperature Decompose, it is to avoid introduce non-catalytic residue.
Preferably, in step A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
Preferably, in step C, the rotating speed of stirring is 150 revs/min.
Preferably, in the step C pH value regulator be ammoniacal liquor, ammoniacal liquor can pH value adjust after loss, it is to avoid introduce it is non- Catalyst residue.
Preferably, airtight heating is carried out in hydrothermal reaction kettle in step D.
Preferably, the drying in step E is carried out under 80 DEG C of temperature conditionss.
Preferably, the step F high temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole of the preparation of utilization lithium-air battery La-Ni mixed oxides catalyst.
Lithium ion battery prepared by a kind of utilization lithium-air battery positive pole.
The beneficial effects of the present invention is:The lithium-air battery prepared by preparation method that the present invention is provided is compound with lanthanum nickel Oxide catalyst is the La with cube crystal structure2NiO4Material, its size uniform, cube crystal structure relative support is stronger, Not easily run off, so as to improve units activity area and the life-span of catalyst;Electro-chemical test is also indicated that and prepared using the method Lithium-air battery it is superior with La-Ni mixed oxides catalyst cycle life, have higher practical value, disclosure satisfy that height The requirement of performance ether lithium-air cell industrialization;The cost of raw material that the present invention is taken is relatively low, and preparation work is easily simple, easily In industrialized production.
Description of the drawings
Fig. 1 is that the life-span of the lithium ion battery that the lithium-air battery of the present invention is prepared with La-Ni mixed oxides catalyst is bent Line.
Fig. 2 is filling first for lithium ion battery prepared by the lithium-air battery La-Ni mixed oxides catalyst of the present invention Discharge curve.
Fig. 3 is that the lithium-air battery of the present invention is schemed with SEM prepared by La-Ni mixed oxides catalyst.
Fig. 4 is the XRD that the lithium-air battery of the present invention is prepared with La-Ni mixed oxides catalyst.
Specific embodiment
For the ease of the understanding of those skilled in the art, further is made to the present invention with reference to embodiment and accompanying drawing 1-4 Explanation, the content that embodiment is referred to not limitation of the invention.
Embodiment 1
A kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, according to stoichiometric proportion 2:1 weighs respectively lanthanum salt and nickel salt, and in being dissolved in 60mL deionized waters, stirring forms mixed Solution is closed, it is 0.0005mol/L to control nickel salt concentration in mixed solution;
B, to the mixed solution and dripping 0.002mol glycine of step A;
C, will be added dropwise to be added in the mixed solution of glycine in step B and pH value regulator and stirred, adjusting pH value has been 7.6;
D, by the mixed solution of step C under the conditions of 175 DEG C airtight heating 14h, obtain product;
E, by the product washing and drying of step D;
F, the product after the process of step E is sintered in oxygen-enriched atmosphere high temperature, first with the heating rate of 2 DEG C/min 600 DEG C are warming up to, then 4 hours is incubated, lithium-air battery La-Ni mixed oxides catalyst is obtained.
In step A, lanthanum salt is lanthanum nitrate hexahydrate, and the nickel salt is nickel nitrate.
In step A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In step C, the rotating speed of stirring is 150 revs/min.
PH value regulator is ammoniacal liquor in step C.
Airtight heating is carried out in hydrothermal reaction kettle in step D.
Drying in step E is carried out under 80 DEG C of temperature conditionss.
The step F high temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole of the preparation using above-mentioned lithium-air battery La-Ni mixed oxides catalyst. A kind of lithium ion battery prepared using above-mentioned lithium-air battery positive pole.
Specifically, by the La-Ni mixed oxides catalyst La of lithium-air battery obtained in the present embodiment2NiO4, conductive agent Ketjen black, binding agent PTFE are according to mass ratio 3.5:4.5:1 is well mixed, and is adjusted in this mixture with 1-METHYLPYRROLIDONE NMP Slurry is made, is evenly applied on Copper Foil, be put into 90 DEG C of drying 2h in baking oven, taking-up is washed into pole piece, and 120 DEG C are vacuum dried 12h, Carry out roll-in, 85 DEG C of vacuum drying 12h, prepared laboratory cells pole piece.Using lithium piece as to electrode, electrolyte is 1mol/L LiTFSI (Double trifluoromethanesulfonimide lithiums)TEGDME(TRIGLYME)Solution, barrier film is glass fibre, is being filled The glove box of full argon gas atmosphere is assembled into the special button cell of CR2025 types carries out in atmosphere discharge and recharge, charge cutoff voltage For 4.4V, discharge cut-off voltage is 2.1V, and charging and discharging currents density is set to 51mA/g, and the quality in current density unit is positive pole Catalyst and conductive carbon quality and.Battery first discharge specific capacity is measured for 3750mAh/g.
Embodiment 2
A kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, according to stoichiometric proportion 2:1 weighs respectively lanthanum salt and nickel salt, and in being dissolved in 70mL deionized waters, stirring forms mixed Solution is closed, it is 0.001mol/L to control nickel salt concentration in mixed solution;
B, to the mixed solution and dripping 0.003mol glycine of step A;
C, will be added dropwise to be added in the mixed solution of glycine in step B and pH value regulator and stirred, it has been 7. to adjust pH value 7;
D, by the mixed solution of step C under the conditions of 180 DEG C airtight heating 12h, obtain product;
E, by the product washing and drying of step D;
F, the product after the process of step E is sintered in oxygen-enriched atmosphere high temperature, first with the heating rate of 3 DEG C/min 650 DEG C are warming up to, then 3 hours is incubated, lithium-air battery La-Ni mixed oxides catalyst is obtained.
In step A, lanthanum salt is lanthanum nitrate hexahydrate, and the nickel salt is nickel nitrate.
In step A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In step C, the rotating speed of stirring is 150 revs/min.
PH value regulator is ammoniacal liquor in step C.
Airtight heating is carried out in hydrothermal reaction kettle in step D.
Drying in step E is carried out under 80 DEG C of temperature conditionss.
The step F high temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole of the preparation using above-mentioned lithium-air battery La-Ni mixed oxides catalyst. A kind of lithium ion battery prepared using above-mentioned lithium-air battery positive pole.
Specifically, by the La-Ni mixed oxides catalyst La of lithium-air battery obtained in the present embodiment2NiO4, conductive agent Ketjen black, binding agent PTFE are according to mass ratio 3.5:4.5:1 is well mixed, and is adjusted in this mixture with 1-METHYLPYRROLIDONE NMP Slurry is made, is evenly applied on Copper Foil, be put into 90 DEG C of drying 2h in baking oven, taking-up is washed into pole piece, and 120 DEG C are vacuum dried 12h, Carry out roll-in, 85 DEG C of vacuum drying 12h, prepared laboratory cells pole piece.Using lithium piece as to electrode, electrolyte is 1mol/L LiTFSI (Double trifluoromethanesulfonimide lithiums)TEGDME(TRIGLYME)Solution, barrier film is glass fibre, is being filled The glove box of full argon gas atmosphere is assembled into the special button cell of CR2025 types, and discharge and recharge, charge cutoff voltage are carried out in atmosphere For 4.5V, discharge cut-off voltage is 2.0V, and charging and discharging currents density is set to 50mA/g, and the quality in current density unit is positive pole Catalyst and conductive carbon quality and.Battery first discharge specific capacity is measured for 3751mAh/g.
Embodiment 3
A kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, according to stoichiometric proportion 2:1 weighs respectively lanthanum salt and nickel salt, and in being dissolved in 70mL deionized waters, stirring forms mixed Solution is closed, it is 0.0011mol/L to control nickel salt concentration in mixed solution;
B, to the mixed solution and dripping 0.003mol glycine of step A;
C, will be added dropwise to be added in the mixed solution of glycine in step B and pH value regulator and stirred, adjusting pH value has been 7.8;
D, by the mixed solution of step C under the conditions of 179 DEG C airtight heating 13h, obtain product;
E, by the product washing and drying of step D;
F, the product after the process of step E is sintered in oxygen-enriched atmosphere high temperature, first with the heating rate of 3 DEG C/min 680 DEG C are warming up to, then 3 hours is incubated, lithium-air battery La-Ni mixed oxides catalyst is obtained.
In step A, lanthanum salt is lanthanum nitrate hexahydrate, and the nickel salt is nickel nitrate.
In step A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In step C, the rotating speed of stirring is 150 revs/min.
PH value regulator is ammoniacal liquor in step C.
Airtight heating is carried out in hydrothermal reaction kettle in step D.
Drying in step E is carried out under 80 DEG C of temperature conditionss.
The step F high temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole of the preparation using above-mentioned lithium-air battery La-Ni mixed oxides catalyst. A kind of lithium ion battery prepared using above-mentioned lithium-air battery positive pole.
Specifically, by the La-Ni mixed oxides catalyst La of lithium-air battery obtained in the present embodiment2NiO4, conductive agent Ketjen black, binding agent PTFE are according to mass ratio 3.5:4.5:1 is well mixed, and is adjusted in this mixture with 1-METHYLPYRROLIDONE NMP Slurry is made, is evenly applied on Copper Foil, be put into 90 DEG C of drying 2h in baking oven, taking-up is washed into pole piece, and 120 DEG C are vacuum dried 12h, Carry out roll-in, 85 DEG C of vacuum drying 12h, prepared laboratory cells pole piece.Using lithium piece as to electrode, electrolyte is 1mol/L LiTFSI (Double trifluoromethanesulfonimide lithiums)TEGDME(TRIGLYME)Solution, barrier film is glass fibre, is being filled The glove box of full argon gas atmosphere is assembled into the special button cell of CR2025 types, and discharge and recharge, charge cutoff voltage are carried out in atmosphere For 4.4V, discharge cut-off voltage is 2.0V, and charging and discharging currents density is set to 50mA/g, and the quality in current density unit is positive pole Catalyst and conductive carbon quality and.Battery first discharge specific capacity is measured for 3750mAh/g.
Embodiment 4
A kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst, comprises the following steps:
A, according to stoichiometric proportion 2:1 weighs respectively lanthanum salt and nickel salt, and in being dissolved in 80mL deionized waters, stirring forms mixed Solution is closed, it is 0.0015mol/L to control nickel salt concentration in mixed solution;
B, to the mixed solution and dripping 0.004mol glycine of step A;
C, will be added dropwise to be added in the mixed solution of glycine in step B and pH value regulator and stirred, adjusting pH value has been 7.8;
D, by the mixed solution of step C under the conditions of 185 DEG C airtight heating 10h, obtain product;
E, by the product washing and drying of step D;
F, the product after the process of step E is sintered in oxygen-enriched atmosphere high temperature, first with the heating rate of 4 DEG C/min 700 DEG C are warming up to, then 2 hours is incubated, lithium-air battery La-Ni mixed oxides catalyst is obtained.
In step A, lanthanum salt is lanthanum nitrate hexahydrate, and the nickel salt is nickel nitrate.
In step A, the rotating speed of stirring is 150 revs/min, and the time of stirring is 0.5 hour.
In step C, the rotating speed of stirring is 150 revs/min.
PH value regulator is ammoniacal liquor in step C.
Airtight heating is carried out in hydrothermal reaction kettle in step D.
Drying in step E is carried out under 80 DEG C of temperature conditionss.
The step F high temperature oxygen-enriched atmosphere is carried out in tube furnace.
A kind of lithium-air battery positive pole of the preparation using above-mentioned lithium-air battery La-Ni mixed oxides catalyst. A kind of lithium ion battery prepared using above-mentioned lithium-air battery positive pole.
Specifically, by the La-Ni mixed oxides catalyst La of lithium-air battery obtained in the present embodiment2NiO4, conductive agent Ketjen black, binding agent PTFE are according to mass ratio 3.5:4.5:1 is well mixed, and is adjusted in this mixture with 1-METHYLPYRROLIDONE NMP Slurry is made, is evenly applied on Copper Foil, be put into 90 DEG C of drying 2h in baking oven, taking-up is washed into pole piece, and 120 DEG C are vacuum dried 12h, Carry out roll-in, 85 DEG C of vacuum drying 12h, prepared laboratory cells pole piece.Using lithium piece as to electrode, electrolyte is 1mol/L LiTFSI (Double trifluoromethanesulfonimide lithiums)TEGDME(TRIGLYME)Solution, barrier film is glass fibre, is being filled The glove box of full argon gas atmosphere is assembled into the special button cell of CR2025 types, and discharge and recharge, charge cutoff voltage are carried out in atmosphere For 4.5V, discharge cut-off voltage is 2.0V, and charging and discharging currents density is set to 50mA/g, and the quality in current density unit is positive pole Catalyst and conductive carbon quality and.Battery first discharge specific capacity is measured for 3751mAh/g.
As seen in Figure 1 application battery cycle life of the invention illustrates the lithium air electricity of the present invention up to 50 times The life-span in pond is higher than the average life span of current lithium-air battery.
As seen in Figure 2 application battery capacity of the invention has illustrated the battery capacity of the present invention up to 3751mAh Reach 1.3 times of current lithium-air battery average level.
As seen in Figure 3 the particle size of catalyst of the invention illustrates the catalyst of the present invention in 100nm or so Size has reached Nano grade and even particle size distribution.
As seen in Figure 4 marker peak represents the characteristic peak of nickel acid lanthanum, illustrates that the catalyst prepared is nickel acid lanthanum.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with alternate manner, Any obvious replacement is within protection scope of the present invention on the premise of without departing from present inventive concept.

Claims (10)

1. a kind of hydrothermal preparing process of lithium-air battery La-Ni mixed oxides catalyst, it is characterised in that:Including following Step:
A, according to stoichiometric proportion 2:1 weighs respectively lanthanum salt and nickel salt, and in being dissolved in 60-80mL deionized waters, stirring forms mixed Solution is closed, it is 0.0005-0.0015mol/L to control nickel salt concentration in mixed solution;
B, to the mixed solution and dripping 0.002-0.004mol glycine of step A;
C, will be added dropwise to be added in the mixed solution of glycine in step B and pH value regulator and stirred, regulations pH value has been 7.6- 7.8;
D, by the mixed solution of step C under the conditions of 175-185 DEG C airtight heating 10-14h, obtain product;
E, by the product washing and drying of step D;
F, the product after the process of step E is sintered in oxygen-enriched atmosphere high temperature, first with the heating rate liter of 2-4 DEG C/min Temperature is incubated 2-4 hours to 600-700 DEG C, then, obtains 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, It is characterized in that:In step A, lanthanum salt is lanthanum nitrate hexahydrate, and the 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, It is characterized in that:In step A, 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, It is characterized in that:In step C, 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, It is characterized in that:PH value regulator is ammoniacal liquor in step C.
6. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, It is characterized in that:Airtight heating is carried out in hydrothermal reaction kettle in step D.
7. the hydrothermal preparing process of a kind of lithium-air battery La-Ni mixed oxides catalyst according to claim 1, It is characterized in that:Drying in 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, It is characterized in that:The step F high temperature oxygen-enriched atmosphere is carried out in tube furnace.
9. a kind of a kind of lithium of the preparation of the lithium-air battery La-Ni mixed oxides catalyst described in utilization claim 1- O for cathode of air battery.
10. the lithium ion battery that prepared by the lithium-air battery positive pole described in a kind of utilization claim 9.
CN201410847961.6A 2014-12-31 2014-12-31 Hydrothermal preparation method of lanthanum-nickel composite oxide catalyst for lithium air battery Expired - Fee Related CN104505522B (en)

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