CN111180724A - Preparation method of ternary single crystal cathode material - Google Patents
Preparation method of ternary single crystal cathode material Download PDFInfo
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- CN111180724A CN111180724A CN202010118544.3A CN202010118544A CN111180724A CN 111180724 A CN111180724 A CN 111180724A CN 202010118544 A CN202010118544 A CN 202010118544A CN 111180724 A CN111180724 A CN 111180724A
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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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- 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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Abstract
The invention provides a preparation method of a ternary single crystal 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 into 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 the reaction temperature in a high-pressure reaction kettle to obtain a nickel-cobalt oxalate precursor; uniformly mixing the precursor, a manganese source and a lithium source with the stoichiometric ratio exceeding, heating to a pre-sintering temperature in an oxygen atmosphere, preserving heat, heating to a sintering temperature, and preserving heat; and cooling to room temperature to obtain the ternary single crystal cathode material. The preparation method adopts a binary precursor, does not need to accurately regulate and control the pH value and the stirring speed of the system, and does not need to be protected by introducing nitrogen; the introduction of a superstoichiometric ratio of lithium source reduces the sintering temperature during lithiation. The production cost of the ternary cathode material can be greatly reduced by the two points. The lithium ion battery prepared by the ternary cathode material synthesized by the method has high charging and discharging coulombic efficiency and good cycle performance.
Description
Technical Field
The invention relates to a preparation method of a cathode material, in particular to a preparation method of a ternary single crystal cathode material, and belongs to the technical field of lithium ion batteries.
Background
With the continuous development of new energy industry, people have energy density on lithium ion power batteriesThe degree and safety put increasing demands on the system. In order to increase energy density and reduce cost, the power battery industry is mostly inclined to use a ternary cathode material with high nickel and low cobalt, namely LiNi1-x-yCoxMnyO2(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 increasing the content of nickel, but the phase structure of the material can simultaneously become unstable, and the obvious performance is that the first charge and discharge coulombic efficiency of the material is low, the cycle performance is poor, and the challenge is brought to the industrial use of the high-nickel ternary material.
The traditional method for synthesizing the high-nickel ternary material mainly comprises a solid-phase synthesis method and a chemical coprecipitation method. The solid phase synthesis method is to mix nickel, cobalt and manganese sources (generally oxides or acetates and carbonates) and lithium sources (lithium hydroxide or lithium carbonate) according to a certain stoichiometric ratio, mechanically mix, and sinter at 800-1000 ℃ 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 larger difference in structure, particle size distribution and the like. The chemical coprecipitation method is to synthesize the nickel-cobalt-manganese ternary hydroxide as a precursor, and then mix and roast the obtained precursor and a lithium source at high temperature. The coprecipitation method can be adopted to mix the materials at an 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, the high nickel ternary material synthesized by using a chemical coprecipitation method in industry is micron-sized spherical secondary particles formed by agglomeration of nanoscale primary particles. In the synthesis process, firstly, ternary hydroxide containing nickel, cobalt and manganese is synthesized and used as precursor Ni1-x-yCoxMny(OH)2And then mixing the precursor with a lithium source and calcining at high temperature in an oxygen atmosphere. Lithium hydroxide or lithium carbonate is commonly used as the lithium source. The proportion of the ternary hydroxide precursor to the lithium source is as follows: the amount of transition metal n (Ni + Co + Mn) and the amount of lithium n (Li) are 1.00 (1.03-1.06). The excessive high proportion of lithium can cause residual alkali (LiOH or Li) on the surface of the ternary material2CO3) And (4) generating. The calcining temperature is 850-950%And C, the temperature is too low to drive the growth and development of crystal grains, and the temperature is too high to cause over-burning, so that the mixed arrangement of lithium and nickel in the crystal is intensified. The secondary spherical particles are easy to break under the high compaction condition, so that the electrolyte permeates into the material and is fully contacted with the primary particles, the side reaction of the electrolyte and the surface of the electrode material is aggravated, and the originally poor cycle performance of the high-nickel ternary material is further deteriorated. Therefore, in addition to the need to improve the safety of the high nickel ternary material, how to improve the cycle performance of the material is one of the problems to be overcome by the industry.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a ternary cathode material with excellent cycle performance. The method is prepared from a nickel-cobalt oxalate precursor, a manganese source and an excessive lithium source, the prepared ternary cathode material has a smooth and clean surface and uniform texture, and a battery prepared from the ternary cathode material has high discharge capacity and good cycle performance.
In order to achieve the technical purpose, the invention provides a preparation method of a ternary single crystal cathode 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 carrying out vacuum drying on 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 the three substances are uniformly dispersed, and heating to remove the ethanol to obtain dry powder; the mass ratio of the nickel salt, the cobalt salt and the manganese salt is x: y:1-x-y, x is more than or equal to 0.50 and less than or equal to 1, and y is more than 0 and less than or equal to 0.20; the molar weight 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) putting the uniformly mixed dry powder into a tubular furnace, introducing pure oxygen, heating to the pre-sintering 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 single crystal cathode material.
The nickel salt and the cobalt salt adopted in the method are soluble salts of nickel and cobalt; the manganese source is one or the combination of two of manganese nitrate and manganese oxalate, and the lithium source is one or the combination of two or more of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate or lithium citrate.
In the step 1), the concentration of the mixed salt solution is 0.1mol/L-1 mol/L. Preferably, the volume ratio of the ethanol to the water is 0.2-4.
In the step 2), urea and oxalic acid are used as a complexing agent and a precipitator together to carry out complexing precipitation reaction on nickel and cobalt to generate nickel-cobalt oxalate (Ni)xCo1-xC2O4·2H2O)。
The concentration of the urea is 0.1mol/L-4 mol/L. The adding amount of the urea is 1-4 times of the total amount of the nickel-cobalt mixed salt. The adding amount of the oxalic acid is 1-2 times of the total 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 the step 3), the main purpose of washing the precipitate until the pH value of the filtrate is 6.0-7.0 is to wash off alkaline substances and redundant urea remained on the surface of the precursor.
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 comprises the step of preparing the ternary cathode 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-grade and rod-shaped appearance. The micron rod-shaped nickel-cobalt oxalate is used as a precursor, is mixed with a manganese source and a lithium source with a super-stoichiometric ratio, and is calcined at a low high temperature to prepare the ternary single crystal anode with excellent cycle performance.
In the embodiment of the invention, the manganese source can be one or the combination of two of manganese nitrate and manganese oxalate; the lithium source may be one or a combination of two or more of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate, and lithium citrate.
In the preparation method, the lithium source with the over-stoichiometric ratio plays a role of molten salt, and is beneficial to the growth of ternary material particles when being sintered at high temperature, so that the temperature for preparing the ternary single crystal material can be greatly reduced. At present, the sintering temperature for preparing the high-nickel ternary single crystal material in the industry is 850-950 ℃, and the sintering temperature for preparing the high-nickel ternary single crystal material by the method is 650-750 ℃. For industrial mass production, the temperature reduction during high-temperature sintering means a great reduction in production cost. The surface of the prepared ternary material has no LiOH or Li2CO3This can be verified by the XRD spectrum and high-power TEM images of the material. Therefore, the positive electrode material does not need to be cleaned. The production cost of the ternary cathode material can be greatly reduced by the two points.
The ternary cathode material prepared by the preparation method provided by the invention has the advantages that the surface is smooth and clean, the texture is uniform, and the discharge capacity and the cycle performance of a battery prepared from the ternary cathode material are high. 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 coprecipitation method of the common ternary material precursor, the synthesis of the precursor in the preparation method is simpler and easier, and the parameters such as the pH value, the rotating speed and the like of the mixed solution do not need to be accurately controlled in the precipitation process; meanwhile, the preparation method is a binary precursor synthesis method, and the precursor is free of manganese elements, so that the solution for synthesizing the precursor is not required to be protected by introducing nitrogen. The introduction of a superstoichiometric ratio of lithium source reduces the sintering temperature during lithiation. The simplification of the synthesis condition of the precursor and the reduction of 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 charge and discharge of the material and the cycle stability of the material during long-term charge and discharge are greatly improved. The ternary single crystal anode material prepared by the preparation method has high discharge specific capacity and good cycle performance. When the 811 ternary material prepared by the preparation method is charged and discharged at a multiplying power of 0.1C, the first cycle specific discharge capacity of charge and discharge cycle is 227.0mAh/g, and the coulombic efficiency is 91.3%. When the battery is charged and discharged at a multiplying power of 1C, the capacity retention rate is 95.2 percent after 100 times of charge and discharge cycles.
Drawings
Fig. 1 is an SEM picture of a nickel cobalt oxalate precursor in 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 first cycle at 0.1C-rate charge-discharge of the ternary cathode material in example 1.
Fig. 4 is a 100-cycle plot of the ternary positive electrode material 1C of example 1.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
In a specific embodiment, the preparation method of the ternary single crystal cathode material of the invention may include the following steps:
s1: weighing nickel salt and cobalt salt, dissolving in mixed solution of ethanol and water according to the mass ratio of x:1-x, and preparing into solution with the total mass concentration of 0.1-1 mol/L. Then adding the solution into a high-pressure reaction kettle with a polytetrafluoroethylene 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 from room temperature to 140-220 ℃, and preserving the heat for 6-12 h.
S2: cooling to room temperature, washing the precipitate with deionized water until the pH value of the filtrate is reduced to 6.0-7.0. And then the filter cake is placed in a vacuum drying oven at the temperature of 60-120 ℃ for drying for 6-12h, and the nickel cobalt oxalate precursor is obtained.
S3: mixing the nickel-cobalt oxalate precursor obtained in S2 with a manganese source and a lithium source with a super-stoichiometric ratio, adding ethanol, stirring until the three substances are uniformly dispersed in the ethanol, and heating to remove the ethanol to obtain dry powder. The manganese source is one or the combination of two of manganese nitrate and manganese oxalate, and the lithium source is one or the combination of two or more of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate or lithium citrate.
S4: and (3) 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 cathode material.
Example 1
The embodiment provides a 811 ternary single crystal cathode material, which is prepared by the following steps:
50ml of ethanol and 50ml of deionized water were taken to prepare a mixed solution, and 2.2147gNi (CH) was added to the mixed solution3COO)2·4H2O and 0.2740g Co (CH)3COO)2·4H2And O, stirring until the solution is completely dissolved, and then transferring the solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining. 1.2607g H is added into the reaction kettle2C2O4·2H2O and 1.2012g CO (NH)2)2And stirring until the mixture is completely dissolved. Sealing the autoclave, heating from room temperature to 180 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 12 h. Stopping heating, cooling to room temperature, and washing the precipitate until the pH value of the filtrate is 6.0. Putting the precipitate into a vacuum drying oven at 80 ℃ for drying for 12h to obtain a precursor Ni0.89Co0.11C2O4·2H2And O. The precursor is nickel cobalt oxalate with micron grade and rod-shaped appearance, and the SEM picture is shown in figure 1.
0.4929g of Ni are taken0.89Co0.11C2O4·2H2O、0.1889g LiOH·H2O and 0.1074g 50wt% Mn (NO)3)2The 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 amount of lithium (Li) in the lithium hydroxide to the amount of substances of the total amount of transition metals (Ni + Co + Mn) was 1.5: 1. Heating to 60 deg.C to remove BAn alcohol. Transferring the obtained dry powder to a tube furnace, heating to 500 ℃ in an oxygen atmosphere, preserving heat for 6h, heating to 700 ℃ again, and preserving heat for 12 h. And naturally cooling to room temperature to obtain the 811 type ternary cathode material. The ternary cathode material is small particles with the size of about 1mm, a clean surface and uniform texture, and an SEM image of the ternary cathode material is shown in an attached figure 2.
And (2) preparing a pole piece by using the ternary cathode material, the acetylene black and the PVDF according to the mass ratio of 85:10:5 and NMP as a solvent, coating the pole piece on an aluminum foil, drying the pole piece for 12 hours in a vacuum drying oven at 100 ℃, and taking out the pole piece for slicing. Using a metal lithium sheet as a negative electrode and 1M LiPF6The solution is used as electrolyte, Cellgard 2300 is used as a diaphragm, the button cell is assembled with the anode, and 2.8-4.3V is taken as cut-off voltage for charging and discharging. When the lithium ion battery is charged and discharged at a multiplying power of 0.1C, the lithium ion battery is circulated for the first time, the charging specific capacity is 248.7mAh/g, the discharging specific capacity is 227.0mAh/g, and the first coulombic efficiency is 91.3%. When the lithium ion battery is charged and discharged at the rate of 1C, the first cyclic specific discharge capacity is 187.2mAh/g, the first coulombic efficiency is 78.7%, after 100 cycles of charging and discharging, the specific discharge capacity is 178.1mAh/g, and the capacity retention rate is 95.2%. The first charge-discharge curve of the charge-discharge circuit at 0.1C rate is shown in figure 3. The cycle curve of 100 times of charge-discharge cycle at 1C rate is shown in figure 4.
Example 2
This example provides a method for preparing a 622 ternary single crystal cathode material, in which lithium hydroxide is in excess of 50%, which is prepared by the following steps:
when preparing a nickel cobalt oxalate precursor, the mass of nickel acetate and cobalt acetate in example 1 was adjusted to 1.8663g and 0.6227g, respectively, and the mixture was dissolved in a mixed solution of ethanol and deionized water to prepare a mixed solution with a total concentration of 0.1mol/L, and the precursor prepared was Ni0.75Co0.25C2O4·2H2And O. When the precursor was lithiated, the precursor and Mn (NO) in example 1 were adjusted3)2The mass of the solution was 0.4387g and 0.2147g, respectively. At this time, the ratio of the amount of lithium (Li) to the total amount of transition metals (Ni + Co + Mn) in the lithium hydroxide was 1.5: 1. The other steps are equal to the example 1, namely the 622 type ternary cathode material is obtained.
Example 3
This example provides a method for preparing a 811 ternary cathode material with a 30% excess of lithium hydroxide, which is prepared by 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 example 1. A811-type ternary positive electrode material was obtained.
Example 4
This example provides a method for preparing a 811 ternary cathode material with a 20% excess of lithium hydroxide, which was prepared by 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 was 450 ℃, the sintering temperature was 650 ℃, and the other steps were identical to example 1. A811-type ternary positive electrode material was obtained.
Claims (7)
1. The preparation method of the ternary single crystal cathode 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;
3) cooling to room temperature, filtering, washing the precipitate until the pH value is 6.0-7.0, and carrying out vacuum drying on 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 the three substances are uniformly dispersed, and heating to remove the ethanol to obtain dry powder; the mass ratio of the nickel salt, the cobalt salt and the manganese salt is x: y:1-x-y, x is more than or equal to 0.50 and less than or equal to 1, and y is more than 0 and less than or equal to 0.20; the molar weight ratio of lithium in the lithium source to the sum of the transition metal nickel cobalt manganese is 1.2-1.5: 1;
5) putting the dry powder in a tube furnace, introducing pure oxygen, heating to the pre-sintering 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 single crystal cathode material.
2. The method according to claim 1, wherein the concentration of the mixed salt solution in the step 1) is 0.1mol/L to 1 mol/L.
3. The preparation method according to claim 1, wherein the volume ratio of the ethanol to the water in the step 1) is 0.2 to 4.
4. The preparation method according to claim 1, wherein the amount of urea added is 2 to 4 times of the total amount of the nickel-cobalt mixed salt; the adding amount of the oxalic acid is 1-2 times of the total amount of the nickel-cobalt mixed salt.
5. The method according to claim 1, wherein the temperature is raised to the reaction temperature in step 2) at a rate of 0.5 ℃/min to 2 ℃/min.
6. The preparation 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 6h to 12 h.
7. The preparation method according to claim 1, wherein the nickel salt and the cobalt salt are soluble salts of nickel and cobalt; the manganese source is one or the combination of two of manganese nitrate and manganese oxalate, and the lithium source is one or the combination of two or more of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate or lithium citrate.
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| CN112875767A (en) * | 2021-01-28 | 2021-06-01 | 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 |
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| CN112831838A (en) * | 2020-12-31 | 2021-05-25 | 南通瑞翔新材料有限公司 | Preparation method of single crystal type nickel cobalt lithium aluminate anode material |
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| CN114000195A (en) * | 2021-11-01 | 2022-02-01 | 佛山科学技术学院 | Preparation method of monodisperse high-nickel ternary single crystal positive electrode 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 |
| CN115286055A (en) * | 2022-10-08 | 2022-11-04 | 宜宾锂宝新材料有限公司 | Ternary cathode material, preparation method thereof, cathode and lithium ion battery |
| 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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