CN108264098A - The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen - Google Patents
The preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen Download PDFInfo
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- CN108264098A CN108264098A CN201810159662.1A CN201810159662A CN108264098A CN 108264098 A CN108264098 A CN 108264098A CN 201810159662 A CN201810159662 A CN 201810159662A CN 108264098 A CN108264098 A CN 108264098A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- 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
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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
- 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
Abstract
The invention discloses a kind of preparation methods of two-dimensional sheet lithium nickel cobalt manganese oxygen, which is characterized in that is prepared as follows：Sodium carbonate, nickel source, cobalt source, manganese source are dissolved in the mixed solution of ammonium hydroxide and ethylene glycol; hydro-thermal reaction is carried out after being uniformly mixed; product is filtered, washed after the completion of reaction, is dried to obtain predecessor; gained predecessor and lithium source are mixed again; two-dimensional sheet lithium nickel cobalt manganese oxygen is made by high-temperature calcination under inert gas shielding, molecular formula is：LiNixCoyMnzO2, wherein x+y+z=1.The chemical property of electrode material can be improved, enhances its cyclical stability, energy density is high.The present invention is had many advantages, such as that low energy consumption, applicability is wide, step is simple, is easy to control, being easy to repeat and be amplified using simple hydro-thermal method and the calcination method synthesis nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of two-dimensional sheet.
Description
Technical field
The present invention relates to a kind of ternary anode material for lithium-ion batteries, specifically, being related to a kind of two-dimensional sheet lithium nickel cobalt
The preparation method of manganese oxygen.
Background technology
Electrochemical energy storage can switch to the various renewable and clean energy resources moved on room and time on room and time
Controllable energy form is conducive to the efficient application of clean reproducible energy, meets the growth requirement of human society energy-saving and emission-reduction.
Simultaneous electrochemical energy storage can adjust the peak change of grid power supply and demand, and the exploitation use for making the energy is more rationally and steady.
Battery accounts for one seat as a kind of time-honored electric energy storing device in storing and discharging power process.It is storing
In the process, battery energy storage effect can be utilized good, it small the advantages that being easily installed, will be multiple by comprehensive connection mode
Battery fits together, it is possible to realize the storage of a large amount of electric energy.Currently, the differentiation of energy-storage battery mainly from battery material with
And electrolyte is distinguish.Wherein, lithium ion battery is a kind of energy accumulating device efficiently, environmentally friendly, safe, extensively
Applied to portable electronic product, large-sized power power supply, electric vehicle, aerospace, military affairs etc..High-capacity lithium-ion electricity
Pond is tried out in electric vehicle, by one of major impetus power supply as 21 century electric vehicle, in artificial satellite, boat
It is applied in terms of empty space flight and energy storage.For lithium ion battery because it has high-energy density, high power density and length use the longevity
The characteristics of life, shows one's talent in chemical energy storage device, and in portable electronic product field, technology maturation extensively should now
With.Nowadays under the policy support of country, the demand in electric automobiles and extensive energy storage field is also in explosion type
Increase.Other than lithium ion battery voltage height, since the protection board of lithium-ion-power cell group can be to each monomer electricity
Pond carries out high precision monitor, and low power-consumption intelligent management has perfect overcharge, overdischarge, temperature, overcurrent, short-circuit protection, lock
Determine self-recovering function and reliable equalizaing charge function, greatly extend the service life of battery.
Lithium ion battery material is divided into positive electrode, negative material, diaphragm, electrolyte etc..Positive electrode be manufacture lithium from
One of critical material of sub- battery occupies more than the 40% of battery cost, and the properties that performance directly affects battery refer to
Mark, occupies core status in lithium ion battery.Ternary anode material for lithium-ion batteries by nickel, cobalt, manganese synergistic effect, knot
Cobalt acid lithium good cycle is closed, lithium nickelate height ratio capacity and LiMn2O4 the advantages of having a safety feature at low cost.Ternary lithium from
Nickel determines electricity in each component of sub- cell positive material, and cobalt determines charge/discharge rates, and manganese determines stability, with nickel content
Increase, the specific discharge capacity of battery is consequently increased, and thermal stability and capacity retention ratio decrease.But with ternary lithium from
Sub- cell positive material safety is improved to be contained with technique evolution, the nickel element improved in ternary anode material for lithium-ion batteries
Amount is trend of the times.
In addition conventional ternary anode material for lithium-ion batteries is secondary spherical particle (such as Shen that primary particle reunion forms
Please be number for a kind of high-density spherical lithium nickel cobalt manganese oxygen and preparation method thereof disclosed in the patent document of 200810026600.X), by
It can be crushed under higher pressure reality in second particle, so as to limit the compacting of ternary material electrode, this also limits battery core energy
The further promotion of metric density.
Invention content
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of preparations of two-dimensional sheet lithium nickel cobalt manganese oxygen
Method.Energy density can effectively be increased and improve cyclical stability.
To achieve these goals, technical scheme is as follows：A kind of preparation side of two-dimensional sheet lithium nickel cobalt manganese oxygen
Method, which is characterized in that be prepared as follows：Sodium carbonate, nickel source, cobalt source, manganese source are dissolved in the mixed of ammonium hydroxide and ethylene glycol
It closes in solution, carries out hydro-thermal reaction after being uniformly mixed, product is filtered, washed after the completion of reaction, is dried to obtain predecessor,
Gained predecessor and lithium source are mixed again, two-dimensional sheet lithium nickel cobalt manganese oxygen is made by high-temperature calcination under inert gas shielding,
Molecular formula is：LiNixCoyMnzO2, wherein x+y+z=1.
The present invention uses the reaction system of sodium carbonate, ammonium hydroxide and ethylene glycol, and obtain predecessor after hydro-thermal reaction passes through again
Calcination processing is crossed, obtains the lithium nickel cobalt manganese oxygen of two-dimensional sheet, unique two-dimensional sheet structure is avoided that under higher pressure reality
Fragmentation Phenomena is conducive to promote battery core energy density, can effectively increase energy density, can extend to electric vehicle course continuation mileage
500km。
The lithium nickel cobalt manganese oxygen pattern rule that the present invention obtains, it is uniform in size, it is unique as anode material for lithium-ion batteries
Two-dimensional sheet structure can shorten the transmission range of lithium ion in charge and discharge process and can prevent material from reuniting, so as to carry
The chemical property of high electrode material enhances its cyclical stability.
In said program：Wherein X is 0.7.The microscopic appearance of two-dimensional sheet lithium nickel cobalt manganese oxygen is 10~100nm of thickness, long
Spend 500~4000nm, the flaky nanometer structure of 200~1000nm of width.
Ternary anode material for lithium-ion batteries is compared with other power battery materials, its its maximum advantage is energy
Density is high, can alleviate mileage worry, increases the course continuation mileage of automobile.The discharge voltage that second point advantage is is high, output power
It is bigger.Its cryogenic property of third is very good, is adapted to round-the-clock temperature.And the ternary lithium ion battery of the present invention is just
As one of main active substances in cell positive material Ni mainly occurs in charge and discharge process for nickel in the material of pole2+And Ni3 +Mutual conversion, nickel element exist make cell parameter c and a increase and reduce c/a, help to improve and ensure the height of material
Capacity.The ternary material energy density of the present invention is high, along with nickel content height, electric vehicle course continuation mileage can be made to extend to 500km.
Co is one of main active substances of material, can stabilizing material well layer structure, inhibit material surface oxidation, contribute to
The deintercalation speed and quality of lithium ion improve the high-rate discharge ability of material.Mn4+Be not involved in cyclic process oxidation-
Reduction reaction has good electrochemicaUy inert, can reduce cost and improve structural stability and the safety of material.
In said program：The nickel source is Ni (NO3)2；The cobalt source is Co (NO3)2；The manganese source is Mn (NO3)2；Institute
Lithium source is stated as LiCO3, Li2C2O4Or at least one of LiOH.
In said program：The molar ratio of ethylene glycol and ammonium hydroxide is 1~2 in the mixed solution of ethylene glycol and ammonium hydroxide：1.
Concentration of sodium carbonate is 0.1~0.3mol/L in mixed solution.
In said program：The temperature of hydro-thermal reaction is 150~200 DEG C, the reaction time 12~for 24 hours.
In said program：The temperature of calcination processing is 620~750 DEG C, and the time is 1~4h.
Advantageous effect：Lithium nickel cobalt manganese oxygen prepared by the present invention is as anode material for lithium-ion batteries, unique two-dimensional slice
Shape structure can shorten the transmission range of lithium ion in charge and discharge process and can prevent material from reuniting, so as to improve electrode material
The chemical property of material enhances its cyclical stability, moreover it is possible to effectively increase energy density.The present invention uses simple hydro-thermal method
The nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of two-dimensional sheet synthesized with calcination method, with low energy consumption, is applicable in
Property it is wide, step is simple, be easy to control, be easy to repeat and amplify the advantages that.
Figure of description
Fig. 1 is the FE-SEM photos of the present invention.
Specific embodiment
The present invention is further elaborated with reference to the accompanying drawings and detailed description：
Embodiment 1
Sodium carbonate, nickel nitrate, cobalt nitrate, manganese nitrate are dissolved in 30ml ethylene glycol and ammonium hydroxide mixed solution, mixing is molten
The molar ratio of ethylene glycol and ammonium hydroxide is 1 in liquid：1, it is uniformly mixed, sodium carbonate is a concentration of in the mixed solution of final gained
0.25mol/L, a concentration of 0.28mol/L of nickel nitrate, a concentration of 0.08mol/L of cobalt nitrate, manganese nitrate it is a concentration of
0.04mol/L.Mixed solution is transferred in reaction kettle, reaction kettle is sealed, hydro-thermal reaction is carried out in 170 DEG C of air dry ovens,
Reaction time 20h by sediment centrifuge washing obtained by the reaction, is then dried to obtain predecessor.
Obtained predecessor is calcined under argon atmosphere in tube furnace after mixing with lithium carbonate, calcination temperature is
700 DEG C, calcination time 2h, product is the nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of two-dimensional sheet, point
Minor is：LiNi0.7Co0.2Mn0.1O2。
Embodiment 2
Sodium carbonate, nickel nitrate, cobalt nitrate, manganese nitrate are dissolved in 30ml ethylene glycol and ammonium hydroxide mixed solution, mixing is molten
The molar ratio of ethylene glycol and ammonium hydroxide is 2 in liquid：1, it is uniformly mixed, sodium carbonate is a concentration of in the mixed solution of final gained
0.1mol/L, a concentration of 0.28mol/L of nickel nitrate, a concentration of 0.08mol/L of cobalt nitrate, manganese nitrate it is a concentration of
0.04mol/L.Mixed solution is transferred in reaction kettle, reaction kettle is sealed, hydro-thermal reaction is carried out in 200 DEG C of air dry ovens,
Reaction time 12h by sediment centrifuge washing obtained by the reaction, is then dried to obtain predecessor.
Obtained predecessor is calcined under argon atmosphere in tube furnace after mixing with lithium carbonate, calcination temperature is
750 DEG C, calcination time 1h, product is the nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of two-dimensional sheet, point
Minor is：LiNi0.7Co0.2Mn0.1O2。
Embodiment 3
Sodium carbonate, nickel nitrate, cobalt nitrate, manganese nitrate are dissolved in 30ml ethylene glycol and ammonium hydroxide mixed solution, mixing is molten
The molar ratio of ethylene glycol and ammonium hydroxide is 1.5 in liquid：1, it is uniformly mixed, the concentration of sodium carbonate in the mixed solution of final gained
For 0.3mol/L, a concentration of 0.28mol/L of nickel nitrate, a concentration of 0.08mol/L of cobalt nitrate, manganese nitrate it is a concentration of
0.04mol/L.Mixed solution is transferred in reaction kettle, reaction kettle is sealed, hydro-thermal reaction is carried out in 150 DEG C of air dry ovens,
Reaction time for 24 hours, by sediment centrifuge washing obtained by the reaction, is then dried to obtain predecessor.
Obtained predecessor is calcined under argon atmosphere in tube furnace after mixing with lithium oxalate, calcination temperature is
620 DEG C, calcination time 4h, product is the nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of two-dimensional sheet, point
Minor is：LiNi0.7Co0.2Mn0.1O2。
Embodiment 4
Sodium carbonate, nickel nitrate, cobalt nitrate, manganese nitrate are dissolved in the mixed solution of 30ml ethylene glycol and ammonium hydroxide, mixed
The molar ratio of ethylene glycol and ammonium hydroxide is 1.2 in solution：1, it is uniformly mixed, sodium carbonate is dense in the mixed solution of final gained
Spend for 0.28mol/L, a concentration of 0.28mol/L of nickel nitrate, a concentration of 0.08mol/L of cobalt nitrate, manganese nitrate it is a concentration of
0.04mol/L.Mixed solution is transferred in reaction kettle, reaction kettle is sealed, hydro-thermal reaction is carried out in 180 DEG C of air dry ovens,
Reaction time 20h by sediment centrifuge washing obtained by the reaction, is then dried to obtain predecessor.
Obtained predecessor is calcined under argon atmosphere in tube furnace after mixing with lithium hydroxide, calcination temperature
It is 720 DEG C, calcination time 3h, product is the nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of two-dimensional sheet,
Molecular formula is：LiNi0.7Co0.2Mn0.1O2。
The embodiment 1-4 lithium nickel cobalt manganese oxygens prepared are detected to obtain FE-SEM photos, it can be seen that two from photo
Tie up the nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of sheet.It can prepare on a large scale.
Table one is the nickelic ternary anode material for lithium-ion batteries (lithium nickel cobalt manganese oxygen) of two-dimensional sheet made from case study on implementation 1-4
Discharge capacity and cycle performance.
Table one
As can be seen from Table I, nickelic ternary anode material for lithium-ion batteries (the lithium nickel cobalt of two-dimensional sheet that prepared by the present invention
Manganese oxygen) there is excellent charge-discharge performance, energy density is high, good cycling stability.
The present invention is not limited to above-mentioned specific embodiment, it should be understood that those of ordinary skill in the art are without creative
Labour, which according to the present invention can conceive, makes many modifications and variations.In short, all technician in the art are according to this
The design of invention passes through the available technical side of logical analysis, reasoning, or a limited experiment on the basis of existing technology
Case, all should be in the protection domain being defined in the patent claims.
Claims (8)
1. a kind of preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen, which is characterized in that be prepared as follows：By sodium carbonate,
Nickel source, cobalt source, manganese source are dissolved in the mixed solution of ammonium hydroxide and ethylene glycol, and hydro-thermal reaction is carried out after being uniformly mixed, reaction
Product is filtered, washed after the completion, is dried to obtain predecessor；Gained predecessor and lithium source are mixed again, in inert gas shielding
Lower that two-dimensional sheet lithium nickel cobalt manganese oxygen is made by high-temperature calcination, molecular formula is：LiNixCoyMnzO2, wherein x+y+z=1.
2. the preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen according to claim 1, it is characterised in that：Wherein X is 0.7.
3. the preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen according to claim 2, it is characterised in that：Two-dimensional sheet lithium nickel cobalt
The microscopic appearance of manganese oxygen be 10~100nm of thickness, 500~4000nm of length, the flaky nanometer structure of 200~1000nm of width.
4. according to the preparation method of any one of the claim 1-3 two-dimensional sheet lithium nickel cobalt manganese oxygens, it is characterised in that：The nickel
Source is Ni (NO3)2；The cobalt source is Co (NO3)2；The manganese source is Mn (NO3)2；The lithium source is LiCO3、Li2C2O4Or LiOH
At least one of.
5. the preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen according to claim 4, it is characterised in that：Ethylene glycol and ammonium hydroxide
The molar ratio of ethylene glycol and ammonium hydroxide is 1~2 in mixed solution：1.
6. the preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen according to claim 5, it is characterised in that：Carbonic acid in mixed solution
Na concn is 0.1~0.3mol/L.
7. the preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen according to claim 6, it is characterised in that：The temperature of hydro-thermal reaction
It is 150~200 DEG C, the reaction time 12~for 24 hours.
8. the preparation method of two-dimensional sheet lithium nickel cobalt manganese oxygen according to claim 7, it is characterised in that：The temperature of calcination processing
It it is 620~750 DEG C, the time is 1~4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115490277A (en) * | 2022-09-30 | 2022-12-20 | 山东精工电子科技股份有限公司 | Magnetic field modified ternary material for lithium ion battery and preparation method thereof |
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| CN115490277B (en) * | 2022-09-30 | 2024-02-13 | 山东精工电子科技股份有限公司 | Magnetic field modified ternary material for lithium ion battery and preparation method thereof |
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| CN108264098B (en) | 2019-10-25 |
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