CN108878862A - A kind of lithium ion battery lithium-rich manganese base and its spray drying preparation - Google Patents
A kind of lithium ion battery lithium-rich manganese base and its spray drying preparation Download PDFInfo
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- CN108878862A CN108878862A CN201810507776.0A CN201810507776A CN108878862A CN 108878862 A CN108878862 A CN 108878862A CN 201810507776 A CN201810507776 A CN 201810507776A CN 108878862 A CN108878862 A CN 108878862A
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- lithium
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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
- 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
- H01M4/52—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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- 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 belongs to lithium ion battery material technical field, in particular to a kind of lithium ion battery lithium-rich manganese base and its spray drying preparation.The battery material is Li1.2Ni0.13Co0.13Mn0.54O2, preparation method is to be dissolved in nickel compound, cobalt compound, manganese compound and lithium compound after water is mixed being spray-dried to obtain presoma, then roast using two-stage method lithium-rich manganese-based anode material is made in air.The present invention obtains the presoma of uniform compact, obtains the lithium battery lithium-rich manganese-based anode material of stable electrochemical property by baking inphases using rapid evaporation water is spray-dried.The technological operation is simple, short preparation period and pollution-free.
Description
Technical field
The present invention relates to the present invention relates to anode material for lithium-ion batteries technical fields, more particularly to a kind of lithium-ion electric
Pond lithium-rich manganese-based anode material and its spray drying preparation.
Background technique
Lithium-ion-power cell is because its operating voltage is high, specific energy is big, good cycle, operating temperature range are wide, safety
The advantages that memory-less effect, is used widely on electric car, and with the rapid development of electric car, market is for high ratio
The needs of the positive electrode of capacity and high-energy-density are constantly increasing.
Traditional lithium nickelate (LiNiO2) it is used as power battery anode material, although specific capacity with higher, it
Poor circulation, limit it in the development in market.Its performance, fusion can be improved by doping Co and Mn
LiCoO2、LiNiO2And LiMnO2The advantages of, doping Co can improve LiNiO2Cycle performance, incorporation Mn can improve its heat
Stability.The advantages of inheriting cobalt acid lithium, lithium nickelate, LiMn2O4 because of ternary nickel-cobalt lithium manganate material has specific capacity height, platform
The features such as voltage is high, and tap density is big, and crystal structure is stablized, and preparation process is simple, and operating cost is low, it has also become lithium ion battery
One of indispensable selection of positive electrode.
The main method of synthesis of ternary nickle cobalt lithium manganate has solid phase method, sol-gel method, coprecipitation etc., solid phase method work
Skill is simple, at low cost, but nickel cobalt manganese cannot reach the uniform mixing of atomic level, cause product chemical property poor；Colloidal sol-
Gel method synthesis technology is complicated, at high cost, is not suitable for large-scale industrial production；Long preparation period needed for coprecipitation, work
Sequence is various, and product chemical property homogeneity is poor.Therefore, the preparation method of positive electrode is further developed with extremely important
Meaning.
The Chinese patent application of Publication No. CN107180950A discloses a kind of ternary cathode material of lithium ion battery
The spray drying process preparation method of NCM, NCA, using coprecipitation, solid material is by being sanded the method being spray-dried again preparation
Presoma, then high-temperature roasting obtain tertiary cathode material, need still aging during the preparation process and can generate waste water.
Summary of the invention
Problem in view of the prior art, it is good that the purpose of the present invention is to provide a kind of chemical properties, simple process, preparation
The method that period is short and free of contamination spray drying prepares lithium-rich manganese-based anode material.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of spray drying preparation of lithium battery lithium-rich manganese-based anode material, the chemistry of the lithium-rich manganese-based anode material
Formula is Li1.2Ni0.13Co0.13Mn0.54O2, preparation method includes the following steps：
(1) by nickel salt, cobalt salt and manganese salt according to molar ratio Ni:Co:Mn=1:1:4 are dissolved in 200ml pure water preparation into metal
Ion solubility is the homogeneous solution of 0.2mol/L, according still further to molar ratio Li:(Ni+Co+Mn)=1.3~1.6:1, which is added lithium source, mixes
It closes, obtains mixed solution；
(2) citric acid is dissolved in the homogeneous solution B that 1.5mol/L is stirred to get in 150ml pure water；
(3) citric acid solution of dissolution is added dropwise in the mixed solution in step (1), mixed solution during being somebody's turn to do
In the state stirred always；
(4) after adding citric acid, 25% ammonium hydroxide is added into the mixed solution stirred always and adjusts pH value to 7~11.
(5) presoma is made on spray dryer；
(6) by presoma under air environment in Muffle kiln roasting, lithium-rich manganese-based anode material is made.
Further, the nickel salt be nickel nitrate, it is nickel sulfate, nickel acetate, a kind of in nickel oxalate.
Further, the cobalt salt be cobalt nitrate, it is cobaltous sulfate, cobalt acetate, a kind of in cobalt oxalate.
Further, the manganese salt be manganese nitrate, it is manganese sulfate, manganese acetate, a kind of in manganese oxalate.
Further, the lithium source be lithium carbonate, it is lithium acetate, lithium hydroxide, lithium oxalate, a kind of in lithium fluoride.
Further, the charging rate of spray drying is 300-1500ml/h, blower frequency setting value in 40-60Hz, into
At 120-200 DEG C, leaving air temp is controlled at 20-120 DEG C for air temperature control.
Further, the charging rate of spray drying is 300-1500ml/h, blower frequency setting value in 40-60Hz, into
At 120-200 DEG C, leaving air temp is controlled at 20-120 DEG C for air temperature control.
Further, the roasting is roasted using two-stage method, and first segment maturing temperature is 400-500 DEG C, when roasting
Between be 4-12h, will roasting gains grinding after carry out second segment roasting, maturing temperature be 650-850 DEG C of sintering 8-24h, linearly
1-5 DEG C of heating rate/min.
The lithium ion battery lithium-rich manganese base of the spray drying preparation preparation, it is characterised in that：It should
The chemical general formula of lithium-rich manganese-based anode material is Li1.2Ni0.13Co0.13Mn0.54O2, the microstructure of the positive electrode is at dendritic
Particle, the dendritic particles are gathered closely together by oval nano particle.
Popular " the first Co deposited synthesis nickel cobalt manganese hydroxide precursor, then mix with Li compound with the prior art
Sintering obtain nickel-cobalt lithium manganate cathode material " two-step synthesis method compare, the present invention using spray drying synthetic method, improve body
Now：
(1) simple process, short preparation period.
(2) this product is synthesized in the citric acid systems of colorless and odorless, is process for cleanly preparing.
(3) ammonia nitrogen waste water can be generated when coprecipitation prepares presoma, not only pollute environment but also wastewater treatment also increases
Production cost, the present invention use liquid phase method, and the drying of mixed solution Direct spraying prepares presoma, prepares using two-stage roasting
Positive electrode has preparation time short without waiting for standing and will not generate waste water waste material, easy to operate, clean and environmental protection
Advantage.
(4) present invention evaporates moisture rapidly using the technique of spray drying, and material is sufficiently dried, and is obtained uniform
Fine and close presoma, the lithium battery lithium-rich manganese-based anode material being prepared have outstanding charge-discharge performance and cycle performance.
Detailed description of the invention
Fig. 1 is the flow chart of the spray drying preparation of lithium battery lithium-rich manganese-based anode material of the present invention.
Fig. 2 be 1 drying process with atomizing of embodiment preparation positive electrode under 1C multiplying power discharge cycle performance and first three weeks
Charging and discharging curve.
The SEM figure of (a), (b), the lithium-rich manganese-based anode material that (c) is the preparation of 1 drying process with atomizing of example in Fig. 3.
Fig. 4 be 2 drying process with atomizing of embodiment preparation positive electrode under 1C multiplying power discharge cycle performance and first three weeks
Charging and discharging curve.
Fig. 5 be 3 drying process with atomizing of embodiment preparation positive electrode under 1C multiplying power discharge cycle performance and first three weeks
Charging and discharging curve.
Fig. 6 be 4 drying process with atomizing of embodiment preparation positive electrode under 1C multiplying power discharge cycle performance and first three weeks
Charging and discharging curve.
Specific embodiment
Present invention will be further explained with reference to the attached drawings and specific examples, but protection scope of the present invention is simultaneously
It is without being limited thereto.
As shown in Figure 1, the spray drying preparation of lithium battery lithium-rich manganese-based anode material of the present invention, the richness lithium
The chemical formula of manganese-based anode material is Li1.2Ni0.13Co0.13Mn0.54O2, preparation method includes the following steps：
(1) by nickel salt, cobalt salt and manganese salt according to molar ratio Ni:Co:Mn=1:1:4 are dissolved in 200ml pure water preparation into metal
Ion solubility is the homogeneous solution of 0.2mol/L, according still further to molar ratio Li:(Ni+Co+Mn)=1.3~1.6:1, which is added lithium source, mixes
It closes, obtains mixed solution；
(2) citric acid is dissolved in the homogeneous solution B that 1.5mol/L is stirred to get in 150ml pure water；
(3) citric acid solution of dissolution is added dropwise in the mixed solution in step (1), mixed solution during being somebody's turn to do
In the state stirred always；
(4) after adding citric acid, 25% ammonium hydroxide is added into the mixed solution stirred always and adjusts pH value to 7~11.
(5) presoma is made on spray dryer；
(6) by presoma under air environment in Muffle kiln roasting, lithium-rich manganese-based anode material is made.
Embodiment 1
(1) by nickel acetate tetrahydrate, four acetate hydrate cobalts and four acetate hydrate manganese according to molar ratio Ni:Co:Mn=1:1:4
It is dissolved in 200ml pure water being mixed and is configured to metal ion solubility for 0.2mol/L homogeneous solution, according still further to molar ratio Li:
(Ni+Co+Mn)=1.5:1 addition lithium acetate is mixed to get mixed solution；Citric acid stirring in 150ml pure water is dissolved in simultaneously to match
1.5mol/L homogeneous solution is made；
(2) citric acid of dissolution is added dropwise in the mixed solution in step (1).During being somebody's turn to do in step (1)
Mixed solution is in the state stirred always；After adding citric acid, 25% ammonium hydroxide tune is added into the mixed solution stirred always
PH value is saved to 9.
(3) obtained mixed solution is spray-dried, by adjusting charging rate 400ml/h, inlet air temperature 180
DEG C, blower frequency 55Hz, be made presoma；
(4) above-mentioned presoma is roasted in Muffle furnace using two-stage method under air environment, lithium-rich manganese-based anode is made
Material.First segment maturing temperature is 480 DEG C, calcining time 5h, will carry out second segment roasting, roasting after roasting gains grinding
Temperature is 850 DEG C, sintering time 10h, 5 DEG C/min of linear temperature increase speed.
Fig. 2 be spray drying preparation lithium-rich manganese-based anode material discharge under 1C multiplying power cyclic specific capacity curve and first three
All charging and discharging curves, after 120 weeks circulations, specific discharge capacity is maintained at 260mAh/g or so, and efficiency for charge-discharge is maintained at 100
Left and right illustrates that the material has preferable cyclical stability and charge-discharge performance.Fig. 3 is the SEM figure for the positive electrode prepared,
It can be seen that it is 1 μm of dendritic particles that the material, which is grain diameter size, the dendritic particles are by 100nm size and equally distributed
Oval nano particle is gathered closely together.
Embodiment 2
(1) by nickel nitrate, cobalt nitrate and manganese nitrate according to molar ratio Ni:Co:Mn=1:1:4 be dissolved in 200ml pure water mix
Closing stirring and being configured to metal ion solubility is 0.2mol/L homogeneous solution, according still further to molar ratio Li:(Ni+Co+Mn)=1.3:1 adds
Enter lithium carbonate mixing；Citric acid is dissolved in stirring in 150ml pure water simultaneously and is configured to 1.5mol/L homogeneous solution；
(2) citric acid of dissolution is added dropwise in the mixed solution in step (1).During being somebody's turn to do in step (1)
Mixed solution is in the state stirred always；After adding citric acid, 25% ammonium hydroxide tune is added into the mixed solution stirred always
PH value is saved to 8.
(3) obtained mixed solution is spray-dried, by adjusting charging rate 450ml/h, inlet air temperature 150
DEG C, blower frequency 45Hz, be made presoma；
(4) above-mentioned presoma is roasted in Muffle furnace using two-stage method under air environment, lithium-rich manganese-based anode is made
Material.First segment maturing temperature is 400 DEG C, calcining time 6h, will carry out second segment roasting, roasting after roasting gains grinding
Temperature is 700, sintering time 12h, 2 DEG C/min of linear temperature increase speed.
Fig. 4 be spray drying preparation lithium-rich manganese-based anode material discharge under 1C multiplying power cyclic specific capacity curve and first three
All charging and discharging curves, after 80 weeks circulations, specific discharge capacity is maintained at 150mAh/g or so, and it is preferable to illustrate that the material has
Cyclical stability, but volumetric properties are bad compared with Example 1.
Embodiment 3
(1) by nickel sulfate, cobaltous sulfate and manganese sulfate according to molar ratio Ni:Co:Mn=1:1:4 be dissolved in 200ml pure water mix
Closing stirring and being configured to metal ion solubility is 0.2mol/L homogeneous solution, according still further to molar ratio Li:(Ni+Co+Mn)=1.4:1 adds
Enter lithium hydroxide mixing；Citric acid is dissolved in stirring in 150ml pure water simultaneously and is configured to 1.5mol/L homogeneous solution；
(2) citric acid of dissolution is added dropwise in the mixed solution in step (1).During being somebody's turn to do in step (1)
Mixed solution is in the state stirred always；After adding citric acid, 25% ammonium hydroxide tune is added into the mixed solution stirred always
PH value is saved to 9.5.
(3) obtained mixed solution is spray-dried, by adjusting charging rate 500ml/h, inlet air temperature 170
DEG C, blower frequency 50Hz, be made presoma；
(4) above-mentioned presoma is roasted in Muffle furnace using two-stage method under air environment, lithium-rich manganese-based anode is made
Material.First segment maturing temperature is 450 DEG C, calcining time 8h, will carry out second segment roasting, roasting after roasting gains grinding
Temperature is 750 DEG C, sintering time 14h, 3 DEG C/min of linear temperature increase speed.
Fig. 5 be spray drying preparation lithium-rich manganese-based anode material discharge under 1C multiplying power cyclic specific capacity curve and first three
All charging and discharging curves, after 120 weeks circulations, specific discharge capacity is maintained at 180mAh/g or more, and it is preferable to illustrate that the material has
Charging and discharging capacity, but curve is on a declining curve, and cyclical stability is bad compared with Example 1.
Embodiment 4
(1) by nickel oxalate, cobalt oxalate and manganese oxalate according to molar ratio Ni:Co:Mn=1:1:4 be dissolved in 200ml pure water mix
Closing stirring and being configured to metal ion solubility is 0.2mol/L homogeneous solution, according still further to molar ratio Li:(Ni+Co+Mn)=1.6:1 adds
Enter lithium oxalate mixing；Citric acid is dissolved in stirring in 150ml pure water simultaneously and is configured to 1.5mol/L homogeneous solution；
(2) citric acid of dissolution is added dropwise in the mixed solution in step (1).During being somebody's turn to do in step (1)
Mixed solution is in the state stirred always；After adding citric acid, 25% ammonium hydroxide tune is added into the mixed solution stirred always
PH value is saved to 10.
(3) obtained mixed solution is spray-dried, by adjusting charging rate 350ml/h, inlet air temperature 160
DEG C, blower frequency 60Hz, be made presoma；
(4) above-mentioned presoma is roasted in Muffle furnace using two-stage method under air environment, lithium-rich manganese-based anode is made
Material.First segment maturing temperature is 500 DEG C, calcining time 7h, will carry out second segment roasting, roasting after roasting gains grinding
Temperature is 800 DEG C, sintering time 16h, 4 DEG C/min of linear temperature increase speed.
Fig. 6 be spray drying preparation lithium-rich manganese-based anode material discharge under 1C multiplying power cyclic specific capacity curve and first three
All charging and discharging curves, after 90 weeks circulations, specific discharge capacity is maintained at 160mAh/g or more, compared with Example 1, the material
Cycle performance is poor, and charging and discharging capacity is lower.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (8)
1. a kind of spray drying preparation of lithium battery lithium-rich manganese-based anode material, which is characterized in that comprise the following steps：
(1) by nickel salt, cobalt salt and manganese salt according to molar ratio Ni:Co:Mn=1:1:4 are dissolved in 200ml pure water preparation into metal ion
Solubility is the homogeneous solution of 0.2mol/L, according still further to molar ratio Li:(Ni+Co+Mn)=1.3~1.6:1 is added lithium source mixing, obtains
To mixed solution；
(2) citric acid is dissolved in the homogeneous solution that 1.5mol/L is stirred to get in 150ml pure water；
(3) citric acid solution of dissolution is added dropwise in the mixed solution in step (1), mixed solution is in during being somebody's turn to do
The state stirred always；
(4) after adding citric acid, 25% ammonium hydroxide is added into the mixed solution stirred always and adjusts pH value to 7~11；
(5) presoma is made on spray dryer；
(6) by presoma under air environment in Muffle kiln roasting, lithium battery lithium-rich manganese-based anode material is made.
2. spray drying preparation according to claim 1, it is characterised in that：The nickel salt be nickel nitrate, nickel sulfate,
It is a kind of in nickel acetate, nickel oxalate.
3. spray drying preparation according to claim 1, it is characterised in that：The cobalt salt is cobalt nitrate, cobaltous sulfate, vinegar
It is a kind of in sour cobalt, cobalt oxalate.
4. spray drying preparation according to claim 1, it is characterised in that：The manganese salt be manganese nitrate, manganese sulfate,
It is a kind of in manganese acetate, manganese oxalate.
5. spray drying preparation according to claim 1, it is characterised in that：The lithium source be lithium carbonate, lithium acetate,
It is lithium hydroxide, lithium oxalate, a kind of in lithium fluoride.
6. spray drying preparation according to claim 1, which is characterized in that the charging rate of spray drying is 300-
1500ml/h, blower frequency setting value is in 40-60Hz, and at 120-200 DEG C, leaving air temp is controlled in 20-120 for inlet air temperature control
℃。
7. spray drying preparation according to claim 1, which is characterized in that the roasting is roasted using two-stage method
It burns, first segment maturing temperature is 400-500 DEG C, calcining time 4-12h, will carry out second segment roasting after roasting gains grinding
It burns, maturing temperature is 650-850 DEG C of sintering 8-24h, 1-5 DEG C of linear temperature increase speed/min.
8. the lithium ion battery lithium-rich manganese-based anode material of spray drying preparation preparation of any of claims 1-7
Material, it is characterised in that：The chemical general formula of the lithium-rich manganese-based anode material is Li1.2Ni0.13Co0.13Mn0.54O2, the positive electrode
Microstructure at dendritic particles, the dendritic particles are gathered closely together by oval nano particle.
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| WO2023010970A1 (en) * | 2021-08-03 | 2023-02-09 | 广东邦普循环科技有限公司 | Lithium nickel manganese cobalt oxide positive electrode material of high-performance power battery and preparation method therefor |
| US11919071B2 (en) | 2020-10-30 | 2024-03-05 | 6K Inc. | Systems and methods for synthesis of spheroidized metal powders |
| US11963287B2 (en) | 2020-09-24 | 2024-04-16 | 6K Inc. | Systems, devices, and methods for starting plasma |
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Application publication date: 20181123 |