CN111180724B - Preparation method of ternary monocrystal anode material - Google Patents
Preparation method of ternary monocrystal anode material Download PDFInfo
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- CN111180724B CN111180724B CN202010118544.3A CN202010118544A CN111180724B CN 111180724 B CN111180724 B CN 111180724B CN 202010118544 A CN202010118544 A CN 202010118544A CN 111180724 B CN111180724 B CN 111180724B
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- 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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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The invention provides a preparation method of a ternary monocrystalline cathode material, and belongs to the technical field of lithium ion batteries. The preparation method comprises the following steps: dissolving nickel salt and cobalt salt in a mixed solution of ethanol and water to obtain a mixed salt solution; adding oxalic acid and urea into the mixed salt solution, stirring, and heating to a reaction temperature in a high-pressure reaction kettle to obtain a nickel-cobalt oxalate precursor; uniformly mixing a precursor, a manganese source and a lithium source exceeding the stoichiometric ratio, heating to the presintering temperature in an oxygen atmosphere, preserving heat, heating to the sintering temperature, and preserving heat; and cooling to room temperature to obtain the ternary monocrystalline anode material. The preparation method adopts binary precursors, does not need to accurately regulate and control the pH value and stirring rotation speed of a system, and does not need to be protected by introducing nitrogen; the introduction of a superstoichiometric lithium source reduces the sintering temperature during lithiation. The two points can greatly reduce the production cost of the ternary positive electrode material. The lithium ion battery prepared from the ternary positive electrode material synthesized by the method has high charge and discharge coulomb efficiency and good cycle performance.
Description
Technical Field
The invention relates to a preparation method of a positive electrode material, in particular to a preparation method of a ternary monocrystal positive electrode material, and belongs to the technical field of lithium ion batteries.
Background
With the continuous development of new energy industry, people put higher and higher demands on the energy density and safety of lithium ion power batteries. In order to improve the energy density and reduce the cost, the power battery industry tends to use ternary positive electrode materials with high nickel and low cobalt, namely LiNi 1-x-y Co x Mn y O 2 (x+y is less than 0.2). In the ternary material, the specific capacity and the energy density of the material can be obviously improved by improving the nickel content, but the phase structure of the material can be simultaneously unstable, and the obvious manifestation is that the initial charge-discharge coulomb efficiency of the material is low, the cycle performance is poor, and the industrial use of the high-nickel ternary material is challenged.
The traditional high nickel ternary material synthesis method mainly comprises a solid phase synthesis method and a chemical coprecipitation method. The solid phase synthesis method is to prepare nickel, cobalt and manganese sources (generally oxide or acetate and carbonate) and lithium sources (lithium hydroxide or lithium carbonate) according to a certain stoichiometric ratio, mechanically mix them, and sinter them at 800-1000 deg.C to obtain the high nickel ternary material. The solid phase synthesis method has high sintering temperature and long reaction time, and the synthesized materials have great differences in the aspects of structure, particle size distribution and the like. The chemical coprecipitation method is to synthesize nickel-cobalt-manganese ternary hydroxide as a precursor, and then mix the obtained precursor with a lithium source and bake at high temperature. The co-precipitation method can be adopted to mix the materials at the atomic or molecular level, the obtained precursor has uniform appearance and controllable particle size, and the prepared electrode material has uniform components and good reproducibility, and is a method commonly adopted in the industry at present.
At present, a high nickel ternary material synthesized by a chemical coprecipitation method in industry is micron-sized spherical secondary particles formed by agglomeration of nanometer-sized primary particles. In the synthesis process, firstly, a ternary hydroxide containing nickel, cobalt and manganese is synthesized as a precursor Ni 1-x-y Co x Mn y (OH) 2 The precursor is then mixed with a lithium source and calcined at high temperature in an oxygen atmosphere. Lithium sources are commonly used as lithium hydroxide or lithium carbonate. The ratio of the ternary hydroxide precursor to the lithium source is as follows: the amount of transition metal n (Ni+Co+Mn) the amount of lithium n (Li) =1.00 (1.03-1.06). The excessive proportion of lithium can cause residual alkali (LiOH or Li) on the surface of the ternary material 2 CO 3 ) Is generated. The calcination temperature is 850-950 ℃, the development and growth of crystal grains cannot be fully driven by the too low temperature, and the excessive firing is caused by the too high temperature, so that the lithium nickel mixed discharge in the crystal is aggravated. The secondary spherical particles are easy to break under the condition of high compaction, so that the electrolyte permeates into the material to be fully contacted with the primary particles, side reaction between the electrolyte and the surface of the electrode material is aggravated, and the inherently poor cycle performance of the high-nickel ternary material is further deteriorated. Therefore, in addition to the safety improvement of the high nickel ternary material, how to improve the recycling performance of the material is one of the difficulties to be overcome in the industry.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problem to be solved by the invention is to provide a preparation method of a ternary positive electrode material with excellent cycle performance. The ternary positive electrode material is prepared from a nickel-cobalt oxalate precursor, a manganese source and an excessive lithium source, the surface of the ternary positive electrode material is smooth and clean, the texture is uniform, and the discharge capacity of a battery prepared from the ternary positive electrode material is high and the cycle performance is good.
In order to achieve the technical aim, the invention provides a preparation method of a ternary monocrystalline anode material, which comprises the following steps:
1) Dissolving nickel salt and cobalt salt in a mixed solution of ethanol and water to prepare a mixed salt solution;
2) Adding oxalic acid and urea into the mixed salt solution, stirring for 10-20 min, heating to the reaction temperature of 140-220 ℃ in a high-pressure reaction kettle, and preserving heat for 6-12 h;
3) Cooling to room temperature, filtering, washing the precipitate until the pH value is 6.0-7.0, and vacuum drying the precipitate to obtain a nickel-cobalt oxalate precursor;
4) Dispersing a nickel cobalt oxalate precursor, a manganese source and a lithium source in ethanol, stirring until three substances are uniformly dispersed, and heating to remove ethanol to obtain dry powder; the ratio of the amounts of the substances of nickel salt, cobalt salt and manganese salt is x, y is 1-x-y, x is more than or equal to 0.50 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.20; the molar ratio of lithium (Li) in the lithium source to the sum of transition metal nickel cobalt manganese (Ni+Co+Mn) is 1.2-1.5:1;
5) Placing the uniformly mixed dry powder in a tube furnace, introducing pure oxygen, heating to the presintering temperature of 450-600 ℃, preserving heat for 4-6 h, heating to the sintering temperature of 650-750 ℃, and preserving heat for 12-24 h; and cooling to room temperature to obtain the ternary monocrystal anode material.
The nickel salt and cobalt salt adopted in the method are soluble salts of nickel and cobalt; the manganese source is one or two of manganese nitrate and manganese oxalate, and the lithium source is one or two or more of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate or lithium citrate.
In step 1), the concentration of the mixed salt solution is 0.1mol/L to 1mol/L. Preferably, the volume ratio of the ethanol to the water is 0.2-4.
In step 2), urea and oxalic acid are used as complexing agent and precipitant to make nickel and cobalt produce complex precipitation reaction to produce a nickel-cobalt oxalate (Ni x Co 1-x C 2 O 4 ·2H 2 O)。
The concentration of urea is 0.1mol/L to 4mol/L. The addition amount of urea is 1-4 times of the total substance amount of the nickel-cobalt mixed salt. The adding amount of oxalic acid is 1-2 times of the total substance amount of the nickel-cobalt mixed salt.
In the step 2), when the temperature is raised to the reaction temperature, the temperature raising rate is 0.5 ℃/min-2 ℃/min.
In step 3), the main purpose of washing the precipitate to a filtrate pH of 6.0-7.0 is to wash away alkaline material and excess urea remaining on the precursor surface.
In the step 3), the temperature of vacuum drying is 60-120 ℃, and the time of vacuum drying is 6-12 h.
The preparation method of the invention comprises the step of preparing the ternary positive electrode material by using nickel cobalt oxalate as a precursor. The preparation process of the nickel-cobalt oxalate precursor is simple, and the obtained nickel-cobalt oxalate is a precursor with micron-sized and rod-shaped morphology. The micron rod-shaped nickel cobalt oxalate is used as a precursor, and is mixed with a manganese source and a lithium source with super-stoichiometric ratio, and the ternary monocrystal anode with excellent cycle performance can be prepared by low-temperature calcination.
In a specific embodiment of the present invention, the manganese source used may be one or a combination of two of manganese nitrate and manganese oxalate; the lithium source can be one or a combination of two or more of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate or lithium citrate.
In the preparation method, the lithium source with super-stoichiometric ratio plays a role of molten salt, and is favorable for the growth of ternary material particles during sintering at high temperature, so that the temperature for preparing the ternary single crystal material can be greatly reduced. The sintering temperature is 850-950 ℃ when preparing the high-nickel ternary monocrystal material in the current industry, and 650-750 ℃ when preparing the high-nickel ternary monocrystal material. For industrial mass production, a reduction in temperature at high temperature sintering means a substantial reduction in production costs. The surface of the prepared ternary material is free of LiOH or Li 2 CO 3 This can be verified by XRD patterns and high-magnification TEM patterns of the material. Therefore, no cleaning of the cathode material is required. The two points can greatly reduce the production cost of the ternary positive electrode material.
The ternary positive electrode material prepared by the preparation method provided by the invention has the advantages of smooth and clean surface, uniform texture, high discharge capacity and good cycle performance. The invention also provides a lithium ion battery, and the positive plate of the lithium ion battery is prepared from the ternary positive electrode material.
The method has the beneficial effects that:
1. compared with the common three-element material precursor coprecipitation method, the preparation method has the advantages that the synthesis of the precursor is simpler and easier, and the parameters such as the pH value and the rotating speed of the mixed solution are not required to be accurately controlled in the precipitation process; meanwhile, the preparation method is used for synthesizing the binary precursor, and the precursor does not contain manganese element, so that nitrogen is not required to be introduced into the solution for synthesizing the precursor. The introduction of a superstoichiometric lithium source reduces the sintering temperature during lithiation. The two points of simplifying the synthesis condition of the precursor and reducing the sintering temperature during the lithiation of the precursor can greatly reduce the production cost of industrial production.
2. The manganese-rich layer is formed on the surface of the ternary material obtained by the preparation method, so that the coulomb efficiency of the first-circle charge and discharge of the material and the circulation stability during long-term charge and discharge are greatly improved. The ternary monocrystal anode material prepared by the preparation method has high discharge specific capacity and good cycle performance. The 811 ternary material prepared by the preparation method has a specific capacity of 227.0mAh/g in the first charge-discharge cycle and a coulombic efficiency of 91.3% when being charged and discharged at a rate of 0.1C. When charging and discharging at 1C rate, the capacity retention rate was 95.2% after 100 charge and discharge cycles.
Drawings
Fig. 1 is an SEM image of the nickel cobalt oxalate precursor of example 1.
Fig. 2 is an SEM picture of the ternary cathode material in example 1.
Fig. 3 is a charge-discharge curve of the ternary positive electrode material of example 1 in the first cycle at 0.1C rate of charge-discharge.
Fig. 4 is a cycle curve of the ternary cathode material 1c,100 weeks in example 1.
Detailed Description
The technical solution of the present invention will be described in detail below for a clearer understanding of technical features, objects and advantageous effects of the present invention, but should not be construed as limiting the scope of the present invention.
The preparation method of the ternary single crystal positive electrode material can comprise the following steps in a specific embodiment:
s1: the nickel salt and the cobalt salt are weighed, and are dissolved in a mixed solution of ethanol and water according to the mass ratio of x to 1-x to prepare a solution with the mass concentration of 0.1-1mol/L of total substances. Then adding the solution into a high-pressure reaction kettle with polytetrafluoroethylene as a lining, adding oxalic acid and urea into the mixed solution, stirring for 10-20 min, and then sealing the reaction kettle. The mass concentration of oxalic acid is 0.1-2 mol/L, and the mass concentration of urea is 0.1-4 mol/L. Raising the temperature to 140-220 ℃ from room temperature, and preserving the temperature for 6-12 h.
S2: cooling to room temperature, washing the precipitate with deionized water until the pH of the filtrate is reduced to 6.0-7.0. And then placing the filter cake in a vacuum drying oven at 60-120 ℃ for drying for 6-12h to obtain the nickel-cobalt oxalate precursor.
S3: mixing the nickel-cobalt oxalate precursor obtained in the step S2 with a manganese source and a lithium source with super-stoichiometric ratio, adding ethanol, stirring until three substances are uniformly dispersed in the ethanol, and heating to remove the ethanol to obtain dry powder. The manganese source is one or two of manganese nitrate and manganese oxalate, and the lithium source is one or two or more of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate or lithium citrate.
S4: placing the uniformly mixed powder in a tube furnace, introducing pure oxygen, heating to 450-600 ℃ for presintering, preserving heat for 4-6 h, heating to 650-750 ℃, preserving heat for 12-24 h, and naturally cooling to room temperature to obtain the ternary anode material.
Example 1
The embodiment provides a 811 ternary single crystal positive electrode material, which is prepared by the following steps:
50ml of ethanol and 50ml of deionized water were mixed to form a mixed solution, and 2.2147gNi (CH) 3 COO) 2 ·4H 2 O and 0.2740g Co (CH) 3 COO) 2 ·4H 2 O, stirAfter stirring to complete dissolution, the solution was transferred to a teflon lined autoclave. Adding 1.2607g H into the reaction kettle 2 C 2 O 4 ·2H 2 O and 1.2012g CO (NH) 2 ) 2 Stirring until completely dissolved. The autoclave was sealed, and the temperature was raised from room temperature to 180℃at a heating rate of 2℃per minute, and the autoclave was kept at the temperature for 12 hours. Heating was stopped, cooled to room temperature and the precipitate was washed to a filtrate pH of 6.0. Drying the precipitate in a vacuum drying oven at 80deg.C for 12 hr to obtain precursor Ni 0.89 Co 0.11 C 2 O 4 ·2H 2 O. The precursor is nickel cobalt oxalate with micron level and rod-like morphology, and the SEM image is shown in figure 1.
0.4929g Ni 0.89 Co 0.11 C 2 O 4 ·2H 2 O、0.1889g LiOH·H 2 O and 0.1074g 50wt% Mn (NO 3 ) 2 The solution was added to 15ml of ethanol and stirred until the three substances were uniformly dispersed in the ethanol, at which time the ratio of the amounts of lithium (Li) in lithium hydroxide and the total amount of transition metal (Ni+Co+Mn) was 1.5:1. The temperature was raised to 60℃to remove ethanol. Transferring the obtained dry powder to a tube furnace, heating to 500 ℃ under oxygen atmosphere, preserving heat for 6h, heating to 700 ℃ and preserving heat for 12h. And naturally cooling to room temperature to obtain the 811 ternary positive electrode material. The ternary positive electrode material is small particles with the size of about 1mm, clean surface and uniform texture, and an SEM image of the ternary positive electrode material is shown in figure 2.
And (3) preparing a pole piece by using NMP as a solvent according to the mass ratio of 85:10:5 of the ternary positive electrode material, acetylene black and PVDF, coating the pole piece on aluminum foil, drying the pole piece in a vacuum drying oven at 100 ℃ for 12 hours, and taking out the slice. Lithium metal sheet is used as negative electrode, liPF of 1M is used 6 The solution is electrolyte, cellgard 2300 is taken as a diaphragm, and the cell is assembled with the positive electrode to form a button cell, and charging and discharging are carried out by taking 2.8-4.3V as the cut-off voltage. When the battery is charged and discharged at the rate of 0.1C, the battery circulates for the first time, the specific charge capacity is 248.7mAh/g, the specific discharge capacity is 227.0mAh/g, and the initial coulomb efficiency is 91.3%. When charging and discharging with 1C multiplying power, the first cycle discharge specific capacity is 187.2mAh/g, the first coulomb efficiency is 78.7%, after 100 times of charging and discharging cycle, the discharge specific capacity is 178.1mAh/g,the capacity retention was 95.2%. The first charge-discharge curve when charging and discharging at 0.1C rate is shown in figure 3. The cycle curve of charge and discharge cycles at 1C rate for 100 times is shown in FIG. 4.
Example 2
The embodiment provides a preparation method of 622 ternary single crystal positive electrode material, wherein the lithium hydroxide is in excess of 50%, and the preparation method comprises the following steps:
when preparing the nickel cobalt oxalate precursor, the mass of nickel acetate and cobalt acetate in the example 1 is adjusted to 1.8663g and 0.6227g respectively, and the nickel acetate and cobalt acetate are dissolved in the mixed solution of ethanol and deionized water to prepare the mixed solution with the total mass concentration of 0.1mol/L, and the prepared precursor is Ni 0.75 Co 0.25 C 2 O 4 ·2H 2 O. When lithiating the precursor, the precursor and Mn (NO 3 ) 2 The mass of the solution was 0.4387g and 0.2147g, respectively. At this time, the ratio of the amount of lithium (Li) in lithium hydroxide to the total amount of transition metal (Ni+Co+Mn) was 1.5:1. Other steps are equivalent to those of example 1, namely 622 ternary cathode material is obtained.
Example 3
The embodiment provides a preparation method of 811 ternary positive electrode material, wherein the excess of lithium hydroxide is 30%, and the preparation method comprises the following steps: the mass of lithium hydroxide in example 1 was adjusted to 0.1636g, the reaction temperature was 220 ℃, the pre-firing temperature was 600 ℃, and the other steps were identical to those of example 1. Obtaining 811 type ternary anode material.
Example 4
The embodiment provides a preparation method of 811 ternary positive electrode material, wherein the excess of lithium hydroxide is 20%, and the preparation method comprises the following steps: the mass of lithium hydroxide in example 1 was adjusted to 0.1510g, the reaction temperature in example 1 was adjusted to 140 ℃, the pre-firing temperature 450 ℃, the sintering temperature 650 ℃, and the other steps were identical to those in example 1. Obtaining 811 type ternary anode material.
Claims (5)
1. The preparation method of the ternary monocrystal anode material is characterized by comprising the following steps of:
1) Dissolving nickel salt and cobalt salt in a mixed solution of ethanol and water to prepare a mixed salt solution;
2) Adding oxalic acid and urea into the mixed salt solution, stirring for 10-20 min, heating to the reaction temperature of 140-220 ℃ in a high-pressure reaction kettle, and preserving heat for 6-12 h; the addition amount of urea is 2-4 times of the total substance amount of the nickel-cobalt mixed salt; the adding amount of oxalic acid is 1-2 times of the total substance amount of the nickel-cobalt mixed salt;
3) Cooling to room temperature, filtering, washing the precipitate until the pH value is 6.0-7.0, and vacuum drying the precipitate to obtain a nickel-cobalt oxalate precursor;
4) Dispersing a nickel cobalt oxalate precursor, a manganese source and a lithium source in ethanol, stirring until three substances are uniformly dispersed, and heating to remove ethanol to obtain dry powder; the ratio of the amounts of the substances of nickel salt, cobalt salt and manganese salt is x, y is 1-x-y, x is more than or equal to 0.50 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.20; the molar ratio of lithium in the lithium source to the sum of the transition metal nickel cobalt manganese is 1.2-1.5:1;
5) Placing the dry powder in a tube furnace, introducing pure oxygen, heating to the presintering temperature of 450-600 ℃, preserving heat for 4-6 h, heating to the sintering temperature of 700-750 ℃ and preserving heat for 12-24 h; cooling to room temperature to obtain a ternary monocrystal cathode material, and forming a manganese-rich layer on the surface of the ternary monocrystal cathode material;
the nickel salt and the cobalt salt are soluble salts of nickel and cobalt; the manganese source is one or a combination of two of manganese nitrate and manganese oxalate, and the lithium source is one or a combination of more than two of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate or lithium citrate.
2. The method according to claim 1, wherein in step 1), the concentration of the mixed salt solution is 0.1mol/L to 1mol/L.
3. The method according to claim 1, wherein in step 1), the volume ratio of ethanol to water is 0.2 to 4.
4. The method according to claim 1, wherein in step 2), the temperature is raised to the reaction temperature at a rate of 0.5 ℃/min to 2 ℃/min.
5. The method according to claim 1, wherein in the step 3), the temperature of vacuum drying is 60 to 120 ℃ and the time of vacuum drying is 6 to 12 hours.
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| CN112875767B (en) * | 2021-01-28 | 2023-01-17 | 山东宏匀纳米科技有限公司 | Method for preparing ternary cathode material by using lignin as fuel through solution combustion method |
| CN113707874A (en) * | 2021-08-26 | 2021-11-26 | 天津理工大学 | Preparation method of single-crystal high-nickel layered cathode material |
| CN114000195B (en) * | 2021-11-01 | 2023-09-08 | 佛山科学技术学院 | Preparation method of monodisperse high-nickel ternary monocrystal positive electrode material |
| CN114242997A (en) * | 2021-11-12 | 2022-03-25 | 乳源东阳光新能源材料有限公司 | Ternary single crystal positive electrode material and preparation method and application thereof |
| CN115286055B (en) * | 2022-10-08 | 2023-02-03 | 宜宾锂宝新材料有限公司 | Ternary cathode material, preparation method thereof, cathode and lithium ion battery |
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