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 PDFInfo
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- H—ELECTRICITY
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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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for 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
- H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
- H01M2004/8689—Positive electrodes
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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, 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.
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