CN112436123A - Composite coated nickel-based ternary positive electrode material and preparation method thereof - Google Patents
Composite coated nickel-based ternary positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a composite coated nickel-based ternary cathode material and a preparation method thereofx[(Ni(1‑a‑b)CoaMb)(1‑k)Ak]yO2(ii) a Wherein M is Mn or Al, A is one or more of Al, Mg, Ti, Zr, Si, Ca, Sr, Ba, Sn, La, Y, Cu, Bi, Sb, Nb, Mo, Fe, Zn, V, Cr, Ge, Ga and Be, 1-a-b is more than or equal to 0.5, a is more than 0, b is more than 0, k is more than or equal to 0 and less than or equal to 0.05, x is more than or equal to 0.95 and less than or equal to 1.06, and x + Y is more than or equal to x + Y2. The composite coated nickel-based ternary cathode material can effectively inhibit side reaction between the nickel-based ternary cathode material and electrolyte and ensure good conductivity.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery anode materials, and particularly relates to a composite coated nickel-based ternary anode material and a preparation method thereof.
Background
The lithium ion battery has the advantages of high voltage platform, high discharge specific capacity, long cycle life, no memory effect and the like, and is widely applied to various digital products, electric tools and new energy automobiles. In the lithium ion battery, the anode material is the most critical component, and plays a decisive role in the performance of the lithium ion battery. At present, LiCoO is the three main positive electrode materials used in lithium ion batteries2、LiFePO4And nickel-based ternary positive electrode materials (including LiNi)xCoyMnzO2And LiNixCoyAlzO2) Wherein L isiCoO2Co is scarce, so the price is high; LiFePO4Cheap, but low energy density; the nickel-based ternary cathode material has high energy density, rich Ni and Mn resources and moderate price, and becomes the most favored cathode material for the power lithium ion battery for the new energy automobile. However, the nickel-based ternary cathode material has been developed to a certain extent, but the conductivity is still not very ideal.
On the other hand, in the nickel-based ternary positive electrode material, Ni is an important electrochemical active transition metal element, and Ni in a high oxidation state can generate side reaction with an electrolyte due to strong oxidizability in the charging and discharging processes of the battery, generate gas, release heat and damage the function of the electrolyte, so that the battery fails. Therefore, the surface of the nickel-based ternary cathode material needs to be coated, so that the direct contact surface between the material particles and the electrolyte is reduced, the stability of the surface of the nickel-based ternary cathode material is effectively improved, and the side reaction between the surface of the material and the electrolyte is inhibited. At present, the surface of the nickel-based ternary positive electrode material is coated, and the adopted coating layers mainly comprise metal oxides (aluminum oxide, zirconium oxide, titanium oxide, boron oxide and the like), phosphates (aluminum phosphate, lithium iron phosphate and the like), carbon coating and the like. However, since the electron conductivity of the metal oxide and phosphate materials is poor, after the surface coating method is adopted for the nickel-based ternary cathode material, the overall conductivity of the nickel-based ternary cathode material is not improved, the overall conductivity of the nickel-based ternary cathode material is reduced, and the effective exertion of the electrical property of the nickel-based ternary cathode material is influenced. When carbon is coated, organic matters are generally used as carbon sources, and carbon coating is realized through high-temperature carbonization in an inert gas environment, but because the nickel-based ternary positive electrode material is a layered oxide, the surface of the material can be reduced by carbon under the inert gas and high-temperature state, so that the surface of the nickel-based ternary positive electrode material is damaged, and the exertion of the electrical property of the nickel-based ternary positive electrode material is seriously influenced.
Disclosure of Invention
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a composite coated nickel-based ternary positive electrode material which can effectively suppress a side reaction between the nickel-based ternary positive electrode material and an electrolyte and can ensure good conductivity, and a method for producing the same.
Namely, the present invention provides a composite clad nickel-based ternary positive electrode material, wherein the nickel-based ternary positive electrode material is clad with a clad layer comprising a boron-containing compound, carbon, and a metal oxide, and the chemical formula of the nickel-based ternary positive electrode material is Lix[(Ni(1-a-b)CoaMb)(1-k)Ak]yO2(ii) a Wherein M is Mn or Al, A is one or more of Al, Mg, Ti, Zr, Si, Ca, Sr, Ba, Sn, La, Y, Cu, Bi, Sb, Nb, Mo, Fe, Zn, V, Cr, Ge, Ga and Be, 1-a-b is more than or equal to 0.5, a is more than 0, b is more than 0, k is more than or equal to 0 and less than or equal to 0.05, x is more than or equal to 0.95 and less than or equal to 1.06, and x + Y is 2.
In addition, the coating layer is formed by the following compounds which are subjected to heat preservation for 5-8h at the temperature of 200-:
the boron-containing compound accounts for 0.02-0.15 percent of the whole composite cladding type nickel-based ternary anode material in terms of the mass percentage of the boron element;
the carbon source accounts for 0.02 to 1.50 percent of the whole composite cladding type nickel-based ternary anode material in percentage by mass of the carbon element;
the metal oxide accounts for 0.01-0.20% of the whole composite cladding type nickel-based ternary anode material in percentage by mass of metal elements.
Wherein the boron-containing compound is H3BO3、B2O3、Li2B4O7、Li3BO3One or more than two of the above; the carbon source is one or more than two of carbon nano tube, SP conductive carbon black and graphene; the metal oxide is Al2O3、ZrO2、TiO2、SiO2One or more than two of them.
In addition, the invention also provides a preparation method of the composite cladding type nickel-based ternary cathode material, which comprises the following steps:
(1) according to the mass ratio of Li: ni(1-a-b)CoaMb(OH)2: a ═ x: (1-k) y: weighing lithium source and Ni in ky(1-a-b)CoaMb(OH)2Uniformly mixing the powder and the source A, and calcining the mixture for 5 to 10 hours at 700 to 950 ℃ to obtain Lix[(Ni(1-a-b)CoaMb)(1-k)Ak]yO2。
(2) Weighing a boron-containing compound accounting for 0.02-0.15 percent of the total composite cladding type nickel-based ternary cathode material in percentage by mass of boron, a carbon source accounting for 0.02-1.50 percent of the total composite cladding type nickel-based ternary cathode material in percentage by mass of carbon, a metal oxide accounting for 0.01-0.20 percent of the total composite cladding type nickel-based ternary cathode material in percentage by mass of metal elements, and Lix[(Ni(1-a-b)CoaMb)(1-k)Ak]yO2Uniformly mixing to obtain a mixture to be subjected to heat treatment;
(3) and (3) preserving the heat of the mixture to be subjected to heat treatment at the temperature of 200-400 ℃ for 5-8h to obtain the composite cladding type nickel-based ternary cathode material.
Wherein in the step (1), M is Mn or Al, A is one or more of Al, Mg, Ti, Zr, Si, Ca, Sr, Ba, Sn, La, Y, Cu, Bi, Sb, Nb, Mo, Fe, Zn, V, Cr, Ge, Ga and Be, 1-a-b is more than or equal to 0.5, a is more than 0, b is more than 0, k is more than or equal to 0 and less than or equal to 0.05, x is more than or equal to 0.95 and less than or equal to 1.06, and x + Y is 2.
Further, in the step (2), the boron-containing compound is H3BO3、B2O3、Li2B4O7、Li3BO3One or more than two of the above; the carbon source is one or more than two of carbon nano tube, SP conductive carbon black and graphene; the metal oxide is Al2O3、ZrO2、TiO2、SiO2One or more than two of them.
Effects of the invention
The invention adopts nickel-based ternary anode material Lix[(Ni(1-a-b)CoaMb)(1-k)Ak]yO2The composite coated nickel-based ternary cathode material has the advantages that the surface is coated with a coating layer consisting of a boron-containing compound, carbon and a metal oxide, the carbon has high conductivity, the boron-containing compound has a low melting point, the metal oxide has excellent stability, and a carbon source and the metal oxide are firmly coated on the surface of the nickel-based ternary cathode material through the low-melting-point boron-containing compound, so that the composite coated nickel-based ternary cathode material can effectively inhibit the side reaction of the nickel-based ternary cathode material and electrolyte and can ensure the good conductivity of the nickel-based ternary cathode material.
Drawings
Fig. 1 is a graph comparing the 2C specific discharge capacity of the nickel-based ternary positive electrode materials of example 1 and comparative example.
Fig. 2 is a graph comparing the cycle performance of the nickel-based ternary positive electrode materials of example 1 and comparative example.
Detailed Description
Examples
Example 1
(1) Weighing 2mol of Ni0.6Co0.2Mn0.2(OH)2Uniformly mixing the powder and 2.08mol of LiOH, sintering for 10 hours at 830 ℃, and then crushing and sieving to obtain a material Li1.02(Ni0.6Co0.2Mn0.2)0.98O2。
(2) 100g of the resulting material Li were weighed out1.02(Ni0.6Co0.2Mn0.2)0.98O2Weigh 0.28g H3BO30.1g of SP conductive carbon black, 0.076g of Al2O3(nanoscale), and mixing uniformly.
(3) Preserving the heat of the mixture mixed in the step (2) for 5 hours at the temperature of 300 ℃ to obtain the carbon-boron-aluminum composite coated nickel-based ternary cathode material Li1.02(Ni0.6Co0.2Mn0.2)0.98O2Wherein, the content of B is 0.049 percent, the content of C is 0.099 percent, and the content of Al is 0.040 percent.
The application comprises the following steps: composite coated nickel-based ternary positive electrode material Li compositely coated by prepared carbon, boron and aluminum1.02(Ni0.6Co0.2Mn0.2)0.98O2The button cell is manufactured to test the electrical performance, wherein the weight proportion of the electrode components is that the composite cladding type nickel-based ternary anode material: conductive agent (acetylene black): binder (PVDF) 90:5: 5; the negative electrode adopts a lithium sheet. The specific 2C discharge capacity of the button cell is shown in fig. 1, and the cycling performance is shown in fig. 2.
Example 2
(1) Weighing 2mol of Ni0.88Co0.09Al0.03(OH)2Powder and 2.10mol of LiOH are evenly mixed, sintered for 8 hours at the temperature of 750 ℃, and then crushed and sieved to obtain a material Li1.024(Ni0.88Co0.09Al0.03)0.976O2。
(2) 100g of the resulting material Li were weighed out1.024(Ni0.88Co0.09Al0.03)0.976O2Weighing 0.066g B2O30.03g of SP conductive carbon black, 0.014g of ZrO2(nanoscale), and mixing uniformly.
(3) Preserving the heat of the mixture mixed in the step (2) for 8 hours at the temperature of 250 ℃ to obtain the carbon-boron-zirconium composite coated nickel-based ternary cathode material Li1.024(Ni0.88Co0.09Al0.03)0.976O2Wherein, the content of B is 0.021 percent, the content of C is 0.029 percent, and the content of Zr is 0.012 percent.
Example 3
(1) Weighing 1.96mol of Ni0.5Co0.2Mn0.3(OH)2Powder, 0.04mol ZrO2 powder, 1.05mol Li2CO3Uniformly mixing, sintering for 5h at 950 ℃, and then crushing and sieving to obtain a material Li1.024[(Ni0.5Co0.2Mn0.3)0.98Zr0.02]0.976O2。
(2) 100g of the resulting material Li were weighed out1.024[(Ni0.5Co0.2Mn0.3)0.98Zr0.02]0.976O2Weighing 0.84g H3BO31.50g of carbon nanotubes, 0.378g of Al2O3(nanoscale), and mixing uniformly.
(3) Preserving the heat of the mixture mixed in the step (2) for 5 hours at the temperature of 400 ℃ to obtain the carbon-boron-aluminum composite coated nickel-based ternary cathode material Li1.024[(Ni0.5Co0.2Mn0.3)0.98Zr0.02]0.976O2Wherein, the content of B is 0.142 percent, the content of C is 1.49 percent, and the content of Al is 0.198 percent.
Example 4
(1) Weighing 1.98mol of Ni0.83Co0.12Mn0.05(OH)2Powder, 0.02mol TiO2Uniformly mixing the powder and 2.04mol of LiOH, sintering for 8 hours at the temperature of 770 ℃, and then crushing and sieving to obtain a material Li1.01[(Ni0.83Co0.12Mn0.05)0.99Ti0.01]0.99O2。
(2) 100g of the resulting material Li were weighed out1.01[(Ni0.83Co0.12Mn0.05)0.99Ti0.01]0.99O2Weighing 0.56g H3BO31.00g of graphene, 0.19g of Al2O3(nanoscale), and mixing uniformly.
(3) Preserving the heat of the mixture mixed in the step (2) for 6 hours at the temperature of 200 ℃ to obtain the carbon-boron-aluminum composite coated nickel-based ternary cathode material Li1.01[(Ni0.83Co0.12Mn0.05)0.99Ti0.01]0.99O2Wherein, the content of B is 0.098%, the content of C is 0.99%, and the content of Al is 0.099%.
Comparative example
(1) Weighing 2mol of Ni0.6Co0.2Mn0.2(OH)2Powder and 2.08mol of LiOH are evenly mixed, sintered for 8 hours at the temperature of 830 ℃, and then crushed and sieved to obtain a material Li1.02(Ni0.6Co0.2Mn0.2)0.98O2。
(2) 100g of the resulting material Li were weighed out1.02(Ni0.6Co0.2Mn0.2)0.98O20.075g of Al is weighed out2O3(nanoscale), evenly mixing, and keeping the temperature for 5 hours at 300 ℃ to obtain the aluminum-coated cladding type nickel-based ternary cathode material Li1.02(Ni0.6Co0.2Mn0.2)0.98O2Wherein the Al content is 0.040%.
The application comprises the following steps: cladding type nickel-based ternary cathode material Li coated with prepared aluminum1.02(Ni0.6Co0.2Mn0.2)0.92O2The button cell is manufactured to test the electrical performance, wherein the weight proportion of the electrode components is that the aluminum is coated with the coated nickel-based ternary anode material: conductive agent (acetylene black): binder (PVDF) 90:5: 5; the negative electrode adopts a lithium sheet. The specific 2C discharge capacity of the button cell is shown in fig. 1, and the cycling performance is shown in fig. 2.
As shown in fig. 1 and fig. 2, the button cell prepared in example 1 has a 2.75-4.30V specific discharge capacity of 132.6mAh/g at 25 ℃ and a retention rate of 99.2% at 1C cycle 50 cycles. The button cell prepared by the comparative example has the specific discharge capacity of 128.8mAh/g at 25 ℃ and 2.75-4.30V at 2C, and the retention rate of 50 cycles of 1C circulation is 98.5%. The composite coated nickel-based ternary cathode material prepared by the method can effectively inhibit side reaction between the nickel-based ternary cathode material and electrolyte and can ensure good conductivity.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The composite coated nickel-based ternary cathode material is characterized in that the nickel-based ternary cathode material is coated with a coating layer consisting of boron-containing compounds, carbon and metal oxides, and the chemical formula of the nickel-based ternary cathode material is Lix[(Ni(1-a-b)CoaMb)(1-k)Ak]yO2；
Wherein M is Mn or Al, A is one or more of Al, Mg, Ti, Zr, Si, Ca, Sr, Ba, Sn, La, Y, Cu, Bi, Sb, Nb, Mo, Fe, Zn, V, Cr, Ge, Ga and Be, 1-a-b is more than or equal to 0.5, a is more than 0, b is more than 0, k is more than or equal to 0 and less than or equal to 0.05, x is more than or equal to 0.95 and less than or equal to 1.06, and x + Y is 2.
2. The composite coated nickel-based ternary cathode material as claimed in claim 1, wherein the coating layer is formed by heat preservation of the following compounds at 200-400 ℃ for 5-8 h:
the boron-containing compound accounts for 0.02-0.15 percent of the whole composite cladding type nickel-based ternary anode material in terms of the mass percentage of the boron element;
the carbon source accounts for 0.02 to 1.50 percent of the whole composite cladding type nickel-based ternary anode material in percentage by mass of the carbon element;
the metal oxide accounts for 0.01-0.20% of the whole composite cladding type nickel-based ternary anode material in percentage by mass of metal elements.
3. The composite clad nickel-based ternary positive electrode material as claimed in claim 2, wherein the boron-containing compound is H3BO3、B2O3、Li2B4O7、Li3BO3One or more than two of the above; the carbon source is one or more than two of carbon nano tube, SP conductive carbon black and graphene; the metal oxide is Al2O3、ZrO2、TiO2、SiO2One or more than two of them.
4. The preparation method of the composite coated nickel-based ternary cathode material as claimed in any one of claims 1 to 3, characterized by comprising the following steps:
(1) according to the mass ratio of Li: ni(1-a-b)CoaMb(OH)2: a ═ x: (1-k) y: weighing lithium source and Ni in ky(1-a-b)CoaMb(OH)2Powder and A sourceUniformly mixing, calcining at 700-950 ℃ for 5-10h to obtain Lix[(Ni(1-a-b)CoaMb)(1-k)Ak]yO2。
(2) Weighing a boron-containing compound accounting for 0.02-0.15 percent of the total composite cladding type nickel-based ternary cathode material in percentage by mass of boron, a carbon source accounting for 0.02-1.50 percent of the total composite cladding type nickel-based ternary cathode material in percentage by mass of carbon, a metal oxide accounting for 0.01-0.20 percent of the total composite cladding type nickel-based ternary cathode material in percentage by mass of metal elements, and Lix[(Ni(1-a-b)CoaMb)(1-k)Ak]yO2Uniformly mixing to obtain a mixture to be subjected to heat treatment;
(3) and (3) preserving the heat of the mixture to be subjected to heat treatment at the temperature of 200-400 ℃ for 5-8h to obtain the composite cladding type nickel-based ternary cathode material.
5. The production method according to claim 4, wherein, in the step (1),
m is Mn or Al, A is one or more of Al, Mg, Ti, Zr, Si, Ca, Sr, Ba, Sn, La, Y, Cu, Bi, Sb, Nb, Mo, Fe, Zn, V, Cr, Ge, Ga and Be, 1-a-b is more than or equal to 0.5, a is more than 0, b is more than 0, k is more than or equal to 0 and less than or equal to 0.05, x is more than or equal to 0.95 and less than or equal to 1.06, and x + Y is 2.
6. The production method according to claim 4, wherein in the step (2), the boron-containing compound is H3BO3、B2O3、Li2B4O7、Li3BO3One or more than two of the above; the carbon source is one or more than two of carbon nano tube, SP conductive carbon black and graphene; the metal oxide is Al2O3、ZrO2、TiO2、SiO2One or more than two of them.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113258072A (en) * | 2021-06-16 | 2021-08-13 | 浙江帕瓦新能源股份有限公司 | Nickel-cobalt-manganese positive electrode material and preparation method thereof |
| CN113363476A (en) * | 2021-03-24 | 2021-09-07 | 万向一二三股份公司 | Ternary cathode material of lithium ion battery and preparation method thereof |
| CN117410478A (en) * | 2023-12-11 | 2024-01-16 | 英德市科恒新能源科技有限公司 | Polycrystalline ternary positive electrode material, preparation method thereof and lithium ion battery |
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2020
- 2020-11-29 CN CN202011366166.7A patent/CN112436123A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113363476A (en) * | 2021-03-24 | 2021-09-07 | 万向一二三股份公司 | Ternary cathode material of lithium ion battery and preparation method thereof |
| CN113363476B (en) * | 2021-03-24 | 2022-05-13 | 万向一二三股份公司 | Ternary cathode material of lithium ion battery and preparation method thereof |
| WO2022198843A1 (en) * | 2021-03-24 | 2022-09-29 | 万向一二三股份公司 | Ternary positive electrode material for lithium ion battery, and preparation method therefor |
| CN113258072A (en) * | 2021-06-16 | 2021-08-13 | 浙江帕瓦新能源股份有限公司 | Nickel-cobalt-manganese positive electrode material and preparation method thereof |
| CN113258072B (en) * | 2021-06-16 | 2021-10-15 | 浙江帕瓦新能源股份有限公司 | Nickel-cobalt-manganese positive electrode material and preparation method thereof |
| CN117410478A (en) * | 2023-12-11 | 2024-01-16 | 英德市科恒新能源科技有限公司 | Polycrystalline ternary positive electrode material, preparation method thereof and lithium ion battery |
| CN117410478B (en) * | 2023-12-11 | 2024-03-29 | 英德市科恒新能源科技有限公司 | Polycrystalline ternary positive electrode material, preparation method thereof and lithium ion battery |
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