CN109560294A - A kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery - Google Patents

A kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery Download PDF

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Publication number
CN109560294A
CN109560294A CN201811453389.XA CN201811453389A CN109560294A CN 109560294 A CN109560294 A CN 109560294A CN 201811453389 A CN201811453389 A CN 201811453389A CN 109560294 A CN109560294 A CN 109560294A
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positive electrode
oxygen battery
lithium oxygen
battery positive
lithium
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CN201811453389.XA
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Chinese (zh)
Inventor
孙灵娜
冯丽霞
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Shenzhen University
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Shenzhen University
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    • HELECTRICITY
    • H01BASIC ELECTRIC 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
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M12/00Hybrid cells; Manufacture thereof
    • H01M12/04Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
    • H01M12/06Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
    • HELECTRICITY
    • H01BASIC ELECTRIC 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
    • 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
    • Y02E60/10Energy storage using batteries

Abstract

The present invention discloses a kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery.The present invention uses simple hydro-thermal method first, using a certain proportion of glycerol and isopropanol as solvent, Co at a certain temperature3+Glycerol alkoxide salt is formed in conjunction with glycerol, by obtaining the Co of hollow structure by high-temperature calcination3O4, finally utilize strong reductant NaBH4Processing obtains the Co containing Lacking oxygen3O4.Compared with existing, the invention has the following advantages that the material of one, hollow structure, which can deposit and decompose discharging product for lithium oxygen battery charge and discharge process, provides adequate space;Two, the Co of layer structure3O4The electric conductivity of material can be increased, reduce battery impedance;Three, the catalytic performance of material can be increased by increasing Lacking oxygen, promote ORR and OER reaction rate;Four, preparation process is simple, safe and efficient.

Description

A kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery
Technical field
The present invention relates to Lacking oxygen catalyst technical field more particularly to a kind of lithium oxygen battery positive electrode and its preparations Method and lithium oxygen battery.
Background technique
With the sustainable development of society and the progress of science and technology, electronic product and electrical equipment have obtained extensively in daily life It applies generally, and these applications are inseparable with the fast development of portable battery technology.How to prepare more stable, more High capacity, direction that is more cheap and to more environment-friendly alternative new energy being always scientific worker's research.
Data statistics, in current energy resource structure, traditional fossil energy accounts for 34 % of global energy, thus The CO given off2Account for about 40 % of global total release, this seriously breaks ring ecological environment and beautiful home, in order to alleviate This energy and environmental crisis even are solved, accelerate ev industry develops into inevitable trend.
Lithium oxygen battery is received more and more attention due to its high theoretical property, uses oxygen as the energy of reactant Density.However, due to high charge-discharge overpotential, low range performance and poor cyclicity stability, these systematic differences by To serious limitation.It is reported that non-aqueous lithium oxygen battery mainly includes oxygen reduction reaction (ORR) and oxygen evolution reaction (OER).Co3O4Tool There is stronger ORR and OER catalytic activity, and as transition metal oxide, it is cheap and easy to get.Porous catalytic cathode material is simultaneously The key of cycle performance is improved, it can provide macropore volume and specific surface area, to deposit discharging product.Therefore, the present invention will Co3O4Being prepared into hollow structure and manufacturing Lacking oxygen improves the chemical property and catalytic performance of material.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of lithium oxygen battery positive electrode and its Preparation method and lithium oxygen battery, it is intended to solve existing lithium oxygen battery positive electrode seriously affect battery efficiency for charge-discharge and The problem of cycle life.
Technical scheme is as follows:
A kind of preparation method of lithium oxygen battery positive electrode, wherein comprising steps of
(1) it takes glycerol and isopropanol to mix, and stirs;
(2) Co (NO is taken3)2·6H2O is transferred in reaction kettle, in 160- in step (1) resulting mixed solution after stirring 6-12h is reacted at 180 DEG C;
(3) it to be cooled to room temperature after reaction, then successively carries out suction filtration separation, washing, alcohol are washed and dried, obtains glyceryl alcohol Presoma;
(4) glyceryl alcohol presoma is ground into a powder the 350-650 DEG C of calcining 2-4h in Muffle furnace, hollow structure Co is made3O4
(5) hollow structure Co is taken3O4It is added in sodium borohydride solution, is filtered after stirring, clean, obtain the hollow knot of oxygen-containing vacancy Structure Co3O4
The preparation method of the lithium oxygen battery positive electrode, wherein in step (1), the glycerol and isopropanol Volume ratio is 1:4.
The preparation method of the lithium oxygen battery positive electrode, wherein in step (2), react 12h at 180 DEG C.
The preparation method of the lithium oxygen battery positive electrode, wherein step (3) includes: to natural after reaction It is cooled to room temperature, then carries out suction filtration separation with Buchner funnel, and wash postposition three times with deionized water and dehydrated alcohol respectively 8 h of freeze-day with constant temperature in 70 DEG C of air dry oven.
The preparation method of the lithium oxygen battery positive electrode, wherein in step (4), 550 DEG C of calcinings in Muffle furnace 2h。
The preparation method of the lithium oxygen battery positive electrode, wherein in step (5), the NaBH4The concentration of solution For 0.5-1M.
The preparation method of the lithium oxygen battery positive electrode, wherein in step (5), the time of the stirring is 0.5-1h。
A kind of lithium oxygen battery positive electrode, wherein the lithium oxygen battery positive electrode is the hollow knot of oxygen-containing vacancy Structure Co3O4, the lithium oxygen battery positive electrode using lithium oxygen battery positive electrode of the present invention preparation method prepare It obtains.
A kind of lithium oxygen battery, including anode, wherein the positive electrode is lithium oxygen battery anode of the present invention Material.
The utility model has the advantages that positive electrode produced by the present invention has the advantage that the material of one, hollow structure can be lithia Gas battery charge and discharge process deposition and decomposition discharging product provide adequate space;Two, the Co of layer structure3O4Material can be increased Electric conductivity, reduce battery impedance;Three, the catalytic performance of material can be increased by increasing Lacking oxygen, promote ORR and OER reaction speed Rate;Four, preparation process is simple, safe and efficient.
Detailed description of the invention
A, b are respectively the SEM figure and XRD diagram of CoA presoma in embodiment in Fig. 1.
A, b are respectively the hollow structure Co of oxygen-containing vacancy in embodiment in Fig. 23O4Scanning electron microscope (SEM) photograph and transmission electron microscope picture.
Fig. 3 is the hollow structure Co of oxygen-containing vacancy in embodiment3O4As anode in 300 mAg-1Current density under 500 mAhg of limited capacity-1Cycle performance figure.
Specific embodiment
The present invention provides a kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery, of the invention to make Purpose, technical solution and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that this place is retouched The specific embodiment stated is only used to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides a kind of preparation method of lithium oxygen battery positive electrode, wherein comprising steps of
(1) it takes glycerol and isopropanol to mix, and stirs;
(2) Co (NO is taken3)2·6H2O is transferred in reaction kettle, in 160- in step (1) resulting mixed solution after stirring 6-12h is reacted at 180 DEG C;In the temperature range, time range, Co3+Can sufficiently be reacted with the hydroxyl of glycerol chelating formed it is sweet Oleyl alcohol presoma.
(3) it to be cooled to room temperature after reaction, then successively carries out suction filtration separation, washing, alcohol are washed and dried, obtains CoA (glyceryl alcohol presoma);
(4) glyceryl alcohol presoma is ground into a powder the 350-650 DEG C of calcining 2-4h in Muffle furnace, hollow structure Co is made3O4;? In the calcination temperature range, glyceryl alcohol presoma slowly can form hollow spherical structure by solid spherical structure by Tyndall effect; Within the scope of the calcination time, glyceryl alcohol forerunner physical efficiency, which is sufficiently reacted, obtains the hollow structure Co3O4, and obtained Co3O4Knot Brilliant degree is high, and electric conductivity is also strong.
(5) hollow structure Co is taken3O4It is added in sodium borohydride solution, is filtered after stirring, clean, obtain in oxygen-containing vacancy Hollow structure Co3O4
Cobalt nitrate is added in glycerol and aqueous isopropanol carries out hydro-thermal reaction generation glyceryl alcohol first by the embodiment of the present invention Presoma is then calcined glyceryl alcohol presoma to obtain the Co of hollow structure in Muffle furnace3O4, finally utilize hydroboration The strong reducing property of sodium is by Co3+It is reduced into Co2+And generate Lacking oxygen;By the above-mentioned means, anode material made from the embodiment of the present invention Material has very high cyclical stability and high rate performance, while the design of hollow structure enhances the rigidity of material and reaction is lived Property site.
Compared with existing, the embodiment of the present invention has the advantage that the material of one, hollow structure can be lithium oxygen battery Charge and discharge process deposition and decomposition discharging product provide adequate space;Two, the Co of layer structure3O4The conduction of material can be increased Property, reduce battery impedance;Three, the catalytic performance of material can be increased by increasing Lacking oxygen, promote ORR and OER reaction rate;Four, Preparation process is simple, safe and efficient.
In step (1), it is preferred that the time of the stirring is 0.5-1h.
In step (1), it is preferred that the volume ratio of the glycerol and isopropanol is 1:4.
In step (2), it is preferred that react 12h at 180 DEG C.
Preferably, step (3) includes: and is then filtered with Buchner funnel to cooled to room temperature after reaction Separation, and 8 h of freeze-day with constant temperature in the air dry oven for be placed on three times 70 DEG C is washed with deionized water and dehydrated alcohol respectively.
In step (4), it is preferred that 550 DEG C of calcining 2h in Muffle furnace.
In step (5), the embodiment of the present invention obtained after being calcined using the lamellar structure of CoA presoma by particle group Co made of conjunction3O4, add it to strong reductant NaBH4In solution, Co3+It is reduced into as Co2+, it is empty that oxygen is formed at the same time Position.Preferably, the NaBH4The concentration of solution is 0.5-1M.
In step (5), it is preferred that the time of the stirring is 0.5-1h.
The embodiment of the present invention provides a kind of lithium oxygen battery positive electrode, wherein the lithium oxygen battery positive electrode is The hollow structure Co of oxygen-containing vacancy3O4, the lithium oxygen battery positive electrode is using lithium oxygen battery anode material of the present invention The preparation method of material is prepared.Positive electrode made from the embodiment of the present invention has very high cyclical stability and forthright again Can, while the design of hollow structure enhances rigidity and the reactivity site of material.
The embodiment of the present invention provides a kind of lithium oxygen battery, including anode, wherein the positive electrode is the lithia Gas cell positive material.
Below by specific embodiment, the present invention is described in detail.
1, the present embodiment provides a kind of preparation methods of lithium oxygen battery positive electrode, wherein comprising steps of
(1) it prepares CoA (glyceryl alcohol) presoma: measuring 15 mL glycerol and 30min is mixed in 60 mL isopropanols;Then weigh 0.5 mM of Co (NO3)2·6H2O is transferred in the reaction kettle of 100 mL after stirring 30 min in above-mentioned mixed solution, 12h is reacted at 180 DEG C.To cooled to room temperature after reaction, product carries out suction filtration separation with Buchner funnel, and respectively 8 h of freeze-day with constant temperature in the air dry oven for be placed on three times 70 DEG C is washed with deionized water and dehydrated alcohol;Form spherical CoA Presoma.
(2) Co of hollow structure is prepared3O4: CoA presoma is ground into a powder 550 DEG C of calcining 2h in Muffle furnace, be made in Hollow structure Co3O4
(3) the hollow structure Co of oxygen-containing vacancy is prepared3O4: first configure 1M (mole every liter) sodium borohydride solution (NaBH4), Weigh 30 milligrams of hollow structure Co3O4It is added in the solution, uses filtered on buchner funnel after stirring 30min, ethyl alcohol cleans 3 times Obtain the hollow structure Co of oxygen-containing vacancy3O4
2, result characterizes:
For the scanning electron microscope (SEM) photograph of CoA material as shown in figure 1 shown in a, Cong Tuzhong can be clearly seen that CoA is in evenly dispersed spherical shape, XRD diagram is as shown in figure 1 shown in b, and have that a diffraction maximum can prove to generate really at 10 ° or so is glyceryl alcohol presoma.Fig. 2 is The hollow structure Co of oxygen-containing vacancy3O4SEM and TEM image, can be proved from figure the material be it is in hollow structure spherical, It is made of lamellar structure;Fig. 3 is the hollow structure Co of oxygen-containing vacancy3O4As lithium oxygen battery anode in 300 mAg-1Electric current 500 mAhg of density limited capacity-1Under cycle performance image, the cyclical stability of material is very outstanding as we can see from the figure.
In conclusion a kind of lithium oxygen battery positive electrode provided by the invention and preparation method thereof and lithium oxygen battery, The present invention uses simple hydro-thermal method first, using a certain proportion of glycerol and isopropanol as solvent, Co at a certain temperature3+ Glycerol alkoxide salt is formed in conjunction with glycerol, obtains the Co of hollow structure by high-temperature calcination3O4, finally utilize strong reductant NaBH4Place Reason obtains the hollow structure Co containing Lacking oxygen3O4.Compared with existing, the invention has the following advantages that the material of one, hollow structure Material can deposit and decompose discharging product for lithium oxygen battery charge and discharge process and provide adequate space;Two, the Co of layer structure3O4 The electric conductivity of material can be increased, reduce battery impedance;Three, the catalytic performance of material can be increased by increasing Lacking oxygen, promote ORR With OER reaction rate;Four, preparation process is simple, safe and efficient.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention Protect range.

Claims (9)

1. a kind of preparation method of lithium oxygen battery positive electrode, which is characterized in that comprising steps of
(1) it takes glycerol and isopropanol to mix, and stirs;
(2) Co (NO is taken3)2·6H2O is transferred in reaction kettle, in 160- in step (1) resulting mixed solution after stirring 6-12h is reacted at 180 DEG C;
(3) it to be cooled to room temperature after reaction, then successively carries out suction filtration separation, washing, alcohol are washed and dried, obtains glyceryl alcohol Presoma;
(4) glyceryl alcohol presoma is ground into a powder the 350-650 DEG C of calcining 2-4h in Muffle furnace, hollow structure Co is made3O4
(5) hollow structure Co is taken3O4It is added in sodium borohydride solution, is filtered after stirring, clean, obtain the hollow knot of oxygen-containing vacancy Structure Co3O4
2. the preparation method of lithium oxygen battery positive electrode according to claim 1, which is characterized in that in step (1), institute The volume ratio for stating glycerol and isopropanol is 1:4.
3. the preparation method of lithium oxygen battery positive electrode according to claim 1, which is characterized in that in step (2), 12h is reacted at 180 DEG C.
4. the preparation method of lithium oxygen battery positive electrode according to claim 1, which is characterized in that step (3) includes: To cooled to room temperature after reaction, suction filtration separation then is carried out with Buchner funnel, and respectively with deionized water and anhydrous Ethanol washing is placed on 8 h of freeze-day with constant temperature in 70 DEG C of air dry oven three times.
5. the preparation method of lithium oxygen battery positive electrode according to claim 1, which is characterized in that in step (4), in 550 DEG C of calcining 2h in Muffle furnace.
6. the preparation method of lithium oxygen battery positive electrode according to claim 1, which is characterized in that in step (5), institute State NaBH4The concentration of solution is 0.5-1M.
7. the preparation method of lithium oxygen battery positive electrode according to claim 1, which is characterized in that in step (5), institute The time for stating stirring is 0.5-1h.
8. a kind of lithium oxygen battery positive electrode, which is characterized in that the lithium oxygen battery positive electrode is in oxygen-containing vacancy Hollow structure Co3O4, the lithium oxygen battery positive electrode is using the described in any item lithium oxygen battery anode materials of claim 1-7 The preparation method of material is prepared.
9. a kind of lithium oxygen battery, including anode, which is characterized in that the positive electrode is lithia gas according to any one of claims 8 Cell positive material.
CN201811453389.XA 2018-11-30 2018-11-30 A kind of lithium oxygen battery positive electrode and preparation method thereof and lithium oxygen battery Pending CN109560294A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110887829A (en) * 2019-12-06 2020-03-17 吉林大学 Nanolase-surface enhanced Raman substrate, fluorine ion detection kit and application thereof
CN111533163A (en) * 2020-05-20 2020-08-14 中国科学技术大学 Black lithium titanate material for lithium ion battery cathode and preparation method and application thereof

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CN107658527A (en) * 2016-07-25 2018-02-02 中国科学院上海硅酸盐研究所 A kind of high-performance transition metal oxide hollow ball air electrode and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN111533163A (en) * 2020-05-20 2020-08-14 中国科学技术大学 Black lithium titanate material for lithium ion battery cathode and preparation method and application thereof

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