CN107399756A - A kind of preparation method of the ternary metal oxide as lithium sky cell catalyst - Google Patents

A kind of preparation method of the ternary metal oxide as lithium sky cell catalyst Download PDF

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CN107399756A
CN107399756A CN201710673136.2A CN201710673136A CN107399756A CN 107399756 A CN107399756 A CN 107399756A CN 201710673136 A CN201710673136 A CN 201710673136A CN 107399756 A CN107399756 A CN 107399756A
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metal oxide
ternary metal
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卢荣红
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    • C01F17/00—Compounds of rare earth metals
    • C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M12/00—Hybrid cells; Manufacture thereof
    • H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
    • 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
    • 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
    • H01M4/9091—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
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    • C01P2004/50—Agglomerated particles
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • 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
    • Y02E60/10—Energy storage using batteries
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention discloses a kind of preparation method of the ternary metal oxide as lithium sky cell catalyst, including step：By La (NO3)3、Sr(NO3)2、Zn(NO3)2According to certain mol proportion dissolving in deionized water, it is made into the mixed solution that total concentration of metal ions is 0.5mol/L；20 milliliters of 50mM cetyl trimethylammonium bromide is added in 70ml mixed solution, stirred 0.5 hour；Ammoniacal liquor is instilled simultaneously adjusts pH value to 13 14；It is then transferred into autoclave, is heated to 180 250 DEG C and is incubated 12 15 hours.Room temperature is cooled to afterwards, sediment is filtered, and is washed repeatedly with deionized water and ethanol.Cleaned sediment is put into boiler tube afterwards to be annealed, 750 800 DEG C of annealing temperature, finally it is made La, Sr and Zn ternary metal oxide, its microscopic appearance is with overlapping out substantial amounts of space between unordered scattered, nanometer rods for nanometer rods and nanometer rods, show porous character.It is used as the catalyst of lithium sky battery, due to substantial amounts of space, being limited without potential barrier, therefore can be rapidly performed by electron transfer；The high rate performance and cyclical stability of battery will be strengthened.

Description

A kind of preparation method of the ternary metal oxide as lithium sky cell catalyst
Technical field
The present invention relates to a kind of lithium sky field of batteries, more particularly to a kind of ternary metal oxygen as lithium sky cell catalyst The preparation method of compound.
Background technology
Although the electrochemical specific capacity of lithium metal up to 3860mAh/g, the electrochemical specific capacity of most of positive electrode Only about 200mAh/g, in addition, diffusion coefficients of the Li+ in metal positive-pole material is generally 10-10-11Cm2/g/s, also limit The energy output of battery.Metal-air battery is by theoretical energy density is high, raw material resources is abundant, operating temperature range is wide And a series of advantages such as environmentally safe, gradually show up prominently in world today's new energy field.It is wherein especially empty with lithium Pneumoelectric pond has the ratio energy (1140Wh/kg) of superelevation, and for lithium-air battery using the oxygen in air as positive pole, energy density is reachable More than 15 times of lithium sky battery.In theory, because oxygen is unrestricted as anode reactant, relative to other metals, air Battery, the ratio energy of lithium-air battery is higher, and pollutes very little, the competitive advantage such as compact-sized, light quality, in recent years by Increasing concern.
But lithium-air battery is also not carried out commercially producing a few days ago, because many problems also be present and need to be solved in its application Certainly.Influence the limiting factor of lithium-air battery performance, such as the catalyst activity that air electrode uses.It is expected to drop using catalyst Low electrode overpotential, the asymmetry observed in charging and discharging curve can also be reduced in addition, increase battery capacity.When non-aqueous For electrolyte lithium air secondary battery in charging, the use of catalyst can also effectively facilitate oxide and peroxide caused by electric discharge The decomposition of compound, improve cycle performance of battery.The catalyst of conventional lithium-air battery mainly have metallic catalyst such as Au, Pt, Pd, Ru, Co etc..Most, higher initial discharge electric capacity can be provided and higher put by making the lithium-air battery of catalyst with metal Potential, but maintain the time of electric capacity to grow without metal oxide corresponding to them.And lithium air secondary battery is in electric car The major obstacle of middle application is exactly cycle life problem, and for lithium air secondary battery, the recycling ability of battery will It is more important than its initial performance.So in this respect, metal oxide catalyst is than metallic catalyst advantageously.
The content of the invention
The problem of present invention exists for the actual demand of lithium sky battery development and prior art, offer one kind is provided and is used as lithium The preparation method of the ternary metal oxide of empty cell catalyst.
The invention provides the method for preparing the ternary metal oxide as lithium sky cell catalyst, preparation process is such as Under：
By La (NO3)3、Sr(NO3)2、Zn(NO3)2According to certain mol proportion (0.5-0.8：0.2-0.5：1) it is dissolved in In ionized water, the mixed solution that total concentration of metal ions is 0.5mol/L is made into；By 20 milliliters of 50mM cetyl front three Base ammonium bromide is added in 70ml mixed solution, stirs 0.5 hour；Ammoniacal liquor is instilled simultaneously adjusts pH value to 13-14；Then turn Move on in autoclave, be heated to 180-250 DEG C of insulation 12-15 hour.Be cooled to room temperature afterwards, sediment filtered, spend from Sub- water and ethanol wash repeatedly.Cleaned sediment is put into boiler tube afterwards to be annealed, 750-800 DEG C of annealing temperature, most La, Sr and Zn ternary metal oxide are made afterwards.
La, Sr and Zn for preparing according to the method described above ternary metal oxide, in unordered scattered, tool on microscopic appearance There are the nanometer rods that average diameter is 15 nanometers and length is 100 nanometers, overlap out substantial amounts of space between nanometer rods, show porous spy Sign；Specific surface area and 0.302-0.521cm with 71.5m2/g-82.7m2/g3/g.Big specific surface area and its porous knot Structure, effective catalytic activity point is conducive to provide, improves catalytic capability, and porous nanometer material does not have due to its substantial amounts of space There is potential barrier limitation, therefore electron transfer can be rapidly performed by；It is applied in lithium sky battery, it will strengthen the multiplying power of battery Performance and cyclical stability.
Brief description of the drawings
Fig. 1 is the ESEM scanning figure that ternary metal oxide composite is made in embodiment 1
Embodiment
The present invention is further illustrated below in conjunction with drawings and the specific embodiments.
Embodiment 1
By La (NO3)3、Sr(NO3)2、Zn(NO3)2Dissolving is 4 according to mol ratio in deionized water：1：5, it is made into total Concentration of metal ions is 0.5mol/L mixed solution；20 milliliters of 50mM cetyl trimethylammonium bromide is added to In 70ml mixed solution, stir 0.5 hour；Ammoniacal liquor is instilled simultaneously adjusts pH value to 13；It is then transferred into autoclave, heats 15 hours are incubated to 180 DEG C.
Room temperature is cooled to afterwards, sediment is filtered, and is washed repeatedly with deionized water and ethanol.Cleaned is sunk afterwards Starch is put into boiler tube and annealed, 750 DEG C of annealing temperature, and La, Sr and Zn ternary metal oxide is finally made, its chemistry Formula is La0.8Sr0.2ZnO.
Embodiment 2
By La (NO3)3、Sr(NO3)2、Zn(NO3)2Dissolving is 3 according to mol ratio in deionized water：2：5, it is made into total Concentration of metal ions is 0.5mol/L mixed solution；20 milliliters of 50mM cetyl trimethylammonium bromide is added to In 70ml mixed solution, stir 0.5 hour；Ammoniacal liquor is instilled simultaneously adjusts pH value to 13；It is then transferred into autoclave, heats 12 hours are incubated to 250 DEG C.
Room temperature is cooled to afterwards, sediment is filtered, and is washed repeatedly with deionized water and ethanol.Cleaned is sunk afterwards Starch is put into boiler tube and annealed, 800 DEG C of annealing temperature, and La, Sr and Zn ternary metal oxide is finally made, its chemistry Formula is La0.6Sr0.4ZnO.
Embodiment 3
By La (NO3)3、Sr(NO3)2、Zn(NO3)2Dissolving is 1 according to mol ratio in deionized water：1：1, it is made into total Concentration of metal ions is 0.5mol/L mixed solution；20 milliliters of 50mM cetyl trimethylammonium bromide is added to In 70ml mixed solution, stir 0.5 hour；Ammoniacal liquor is instilled simultaneously adjusts pH value to 14；It is then transferred into autoclave, heats 15 hours are incubated to 200 DEG C.Room temperature is cooled to afterwards, sediment is filtered, and is washed repeatedly with deionized water and ethanol.
Cleaned sediment is put into boiler tube afterwards to be annealed, 750 DEG C of annealing temperature, finally be made La, Sr and Zn ternary metal oxide, its chemical formula are La0.5Sr0.5ZnO.
Embodiment 4
By La (NO3)3、Sr(NO3)2、Zn(NO3)2Dissolving is 7 according to mol ratio in deionized water：3：10, it is made into total Concentration of metal ions is 0.5mol/L mixed solution；20 milliliters of 50mM cetyl trimethylammonium bromide is added to In 70ml mixed solution, stir 0.5 hour；Ammoniacal liquor is instilled simultaneously adjusts pH value to 13-14；It is then transferred into autoclave, It is heated to 180-250 DEG C of insulation 12-15 hour.Room temperature is cooled to afterwards, sediment is filtered, with deionized water and ethanol repeatedly Washing.
Cleaned sediment is put into boiler tube afterwards to be annealed, 750-800 DEG C of annealing temperature, La, Sr is finally made And Zn ternary metal oxide, its chemical formula are La0.7Sr0.3ZnO.
Pass through the test of the isothermal adsorption of carbon dioxide, La, Sr and Zn of preparation ternary metal oxide nanometer rods Show porous character, by the isothermal adsorption of carbon dioxide conciliate inspiration row specific surface area, the survey in pore volume and aperture Examination；Test result shows that the ternary metal oxide of La, Sr and Zn made from embodiment 1 have 71.5m2/g specific surface area And 0.302cm3/ g pore volume, aperture averaging 1.2nm, so big specific surface area and its loose structure, are advantageous to carry For effective catalytic activity point, catalytic capability is improved.The ternary metal oxide nanometer rods as made from following table one is each embodiment The specific data of performance test.
Table one
Detailed morphology analysis is carried out to obtained La, Sr and Zn ternary metal oxide by ESEM.Such as Fig. 1 Scheme for the SEM of final sample made from embodiment 1, it can be seen that porous ternary metal oxide is to disperse, have in unordered The nanometer rods that average diameter is about 15 nanometers and length is about 100 nanometers.
It is described above, it will only be presently preferred embodiments of the present invention, any formal limitation not is made to the present invention. Any those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the disclosure above Methods and technical content makes many possible changes and modifications to technical solution of the present invention, or is revised as the equivalent of equivalent variations Embodiment.Therefore, every content without departing from technical scheme, the technical spirit according to the present invention is to above example Any simple modifications, equivalents, and modifications done, still fall within technical solution of the present invention protection in the range of.

Claims (6)

  1. A kind of 1. preparation method of the ternary metal oxide as lithium sky cell catalyst, it is characterised in that：The ternary gold Belong to the oxide for the ternary metal that oxide is La, Sr and Zn, its chemical formula is LaxSryZnO, wherein x+y=1.
  2. 2. a kind of preparation method of ternary metal oxide as lithium sky cell catalyst according to claim 1, its It is characterised by：Wherein x is 0.5-0.8, y 0.2-0.5.
  3. 3. a kind of preparation method of ternary metal oxide as lithium sky cell catalyst according to claim 2, its It is characterised by：It is 15 nanometers with average diameter that the microscopic appearance of the ternary metal oxide, which is, and length is 100 nanometers Nanometer rods and nanometer rods overlap out substantial amounts of space between unordered scattered, nanometer rods, show porous character.
  4. 4. a kind of preparation method of ternary metal oxide as lithium sky cell catalyst according to claim 3, its It is characterised by：The ternary metal oxide has 71.5m2/g-82.7m2/g specific surface area and 0.302-0.521cm3/g Pore volume.
  5. A kind of 5. preparation of ternary metal oxide as lithium sky cell catalyst according to claim any one of 1-4 Method, it is characterised in that including step：
    By La (NO3)3、Sr(NO3)2、Zn(NO3)2According to certain mol proportion dissolving in deionized water, it is made into total metal ion Concentration is 0.5mol/L mixed solution；20 milliliters of 50mM cetyl trimethylammonium bromide is added to 70ml mixing In solution, stir 0.5 hour；Ammoniacal liquor is instilled simultaneously adjusts pH value to 13-14；It is then transferred into autoclave, is heated to 180- 250 DEG C of insulation 12-15 hours.Room temperature is cooled to afterwards, sediment is filtered, and is washed repeatedly with deionized water and ethanol；Afterwards Cleaned sediment is put into boiler tube to be annealed, 750-800 DEG C of annealing temperature, La, Sr and Zn ternary is finally made Metal oxide.
  6. 6. a kind of preparation method of ternary metal oxide as lithium sky cell catalyst according to claim 5, its It is characterised by：La(NO3)3、Sr(NO3)2、Zn(NO3)2The mol ratio of mixing is 0.5-0.8：0.2-0.5：1.
CN201710673136.2A 2017-08-08 2017-08-08 A kind of preparation method of the ternary metal oxide as lithium sky cell catalyst Withdrawn CN107399756A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109755526A (en) * 2019-01-04 2019-05-14 中南大学 A kind of preparation method and applications of manganese chromium zinc ternary metal oxide energy storage material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103427094A (en) * 2012-05-23 2013-12-04 中国科学院物理研究所 Oxide with perovskite-type structure, preparation methods and applications
CN104538647A (en) * 2015-01-04 2015-04-22 合肥国轩高科动力能源股份公司 Lithium-air battery catalyst and preparation method thereof
CN104659359A (en) * 2015-02-15 2015-05-27 湘潭大学 Preparation method of nanometer plate overlaid and stacked cube Mn<3-x>CoxO4 negative material of lithium-ion battery

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103427094A (en) * 2012-05-23 2013-12-04 中国科学院物理研究所 Oxide with perovskite-type structure, preparation methods and applications
CN104538647A (en) * 2015-01-04 2015-04-22 合肥国轩高科动力能源股份公司 Lithium-air battery catalyst and preparation method thereof
CN104659359A (en) * 2015-02-15 2015-05-27 湘潭大学 Preparation method of nanometer plate overlaid and stacked cube Mn<3-x>CoxO4 negative material of lithium-ion battery

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109755526A (en) * 2019-01-04 2019-05-14 中南大学 A kind of preparation method and applications of manganese chromium zinc ternary metal oxide energy storage material
CN109755526B (en) * 2019-01-04 2021-05-11 中南大学 Preparation method and application of manganese-chromium-zinc ternary metal oxide energy storage material

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