CN113044893A - Method for carrying out carbon coating modification on high-nickel ternary material - Google Patents
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- CN113044893A CN113044893A CN202110269909.7A CN202110269909A CN113044893A CN 113044893 A CN113044893 A CN 113044893A CN 202110269909 A CN202110269909 A CN 202110269909A CN 113044893 A CN113044893 A CN 113044893A
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- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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Abstract
The invention relates to a method for carrying out carbon coating modification on a high-nickel ternary material, and belongs to the technical field of lithium ion batteries. The carbon-coated high-nickel ternary material is prepared by coating carbon on the surface of the high-nickel ternary material by using radio frequency plasma. The carbon coating layer formed on the surface of the high-nickel ternary material can be carried out at a lower temperature in a shorter time without damaging the structure of the high-nickel ternary material. The carbon coating on the surface effectively improves the interface stability of the high-nickel ternary material, reduces residual lithium on the surface to generate residual alkali, and inhibits the surface of the high-nickel ternary material from generating side reaction with electrolyte. The carbon coating layer effectively reduces parasitic reaction on the surface of the high-nickel ternary material, and is beneficial to improving the first discharge capacity and improving the circulation stability.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for carrying out carbon coating modification on a high-nickel ternary material.
Background
With the development of new energy automobiles and wearable electronic products, development of lithium ion batteries is receiving wide attention, and ternary electrode materials, particularly high-nickel ternary materials, become one of research hotspots of researchers. The lithium-nickel composite material has the advantages of high specific capacity, high energy density, high standard vertebral voltage, high compaction density, low cost and the like, but the defects of the lithium-nickel composite material cause that lithium-nickel mixed discharge is easy to occur, the surface of the material absorbs water easily to generate residual alkali, and the surface of the material and electrolyte undergo side reaction, so that the circulation stability and the safety performance are poor, and the large-scale commercial application of the lithium-nickel composite material is influenced.
Researchers can inhibit the lithium-nickel mixed-discharge proportion of the material by doping elements such as magnesium, aluminum, titanium, zirconium, fluorine and the like in a bulk phase, stabilize the structure of the material and improve the cycling stability. The surface is coated with aluminum oxide, lithium metaaluminate, polypyrrole and the like to inhibit the side reaction between the surface of the material and the electrolyte, so that concentration gradient is formed to reduce the side reaction between the internal material and the surface of the electrolyte, the cycle life and the thermal stability are prolonged, the high-nickel ternary material is modified, and the cycle stability of the material is improved. However, the cycle stability, the first discharge capacity and the first discharge efficiency of the conventional high-nickel ternary material still need to be further improved, so that further modification is needed. In view of the above, it is necessary to select an effective surface coating method to further improve the electrochemical performance of the nickel ternary material.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides a method for carrying out carbon coating modification on a high-nickel ternary material so as to reduce the generation of residual alkali on the surface of the high-nickel ternary material, reduce the side reaction between the surface of an electrode material and electrolyte and improve the cycle stability, the first discharge capacity and the first efficiency of the electrode material.
In order to solve the technical problem, an embodiment of the invention provides a method for carrying out carbon coating modification on a high-nickel ternary material, which specifically comprises the steps of placing the high-nickel ternary material in a reaction chamber, reacting for 20-120 min in diluted reactive gas under radio frequency plasma, wherein the reaction temperature is 100-300 ℃, the total gas pressure of the reaction chamber is maintained at 10-1000 Pa, the power output power of the radio frequency plasma is 100-300W, and the diluted reactive gas is formed by mixing diluent gas and the reactive gas according to the volume ratio of 1: 1-10, so that the carbon-coated high-nickel ternary material is prepared.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the reactive gas is one or a mixture of several of methane, ethane, acetylene and carbon tetrafluoride.
Further, the diluent gas is any one of argon, nitrogen, helium and neon.
Further, the preparation method of the high-nickel ternary material comprises the following steps:
(1) preparing a solution A: dissolving a nickel source, a cobalt source and a manganese source in deionized water according to a stoichiometric ratio of 8:1:1 to prepare a solution A of 0.5-4 mol/L;
(2) preparing a solution B: preparing a precipitator into 0.5-4 mol/L solution B;
(3) preparing a solution C: preparing 1-4 mol/L ammonia water into a solution C;
(4) pumping the solution A, B, C into a reaction kettle, controlling the pH value to be 10-12 at the rotating speed of 300-1000 r/min, wherein the reaction time is 12-36 h, the reaction temperature is 50-60 ℃, and the reaction atmosphere is a nitrogen protective atmosphere, so as to obtain a first reactant;
(5) sequentially filtering, washing and drying the first reactant to obtain a precursor material;
(6) and mixing and grinding the precursor material and a lithium source according to a ratio of 1:1.05, heating to 450-500 ℃ at a speed of 2-5 ℃/min in an oxygen atmosphere for pre-sintering, and heating to 750-800 ℃ at a speed of 2-5 ℃/min for calcining to obtain the high-nickel ternary material.
Further, the nickel source is selected from one or more of nickel sulfate, nickel nitrate and nickel chloride, the cobalt source is selected from one or more of cobalt sulfate, cobalt nitrate and cobalt chloride, and the manganese source is selected from one or more of manganese sulfate, manganese nitrate and manganese chloride.
Further, the precipitating agent is selected from one or more of sodium hydroxide, sodium carbonate, sodium oxalate and urea.
Further, the lithium source is selected from one or more of lithium carbonate, lithium nitrate and lithium hydroxide.
Further, the solution A, B, C is pumped into the reaction kettle by a peristaltic pump at a feeding speed of 0.5-2 ml/min.
Further, deionized water is adopted for filtration treatment, ethanol is adopted for washing treatment, and the drying treatment time is 24 hours.
In order to solve the technical problem, an embodiment of the present invention provides a carbon-coated high-nickel ternary material, which is prepared by the method for performing carbon-coating modification on the high-nickel ternary material.
Further, the carbon-coated high-nickel ternary material comprises a coating layer and a central layer; the central layer is a high-nickel ternary material with a laminated structure; the coating layer is made of carbon material, and the thickness of the coating layer is 1 nm-200 nm.
Furthermore, the chemical formula of the high-nickel ternary material is LiNixCoyMn1-x-yO2Wherein x is more than or equal to 0.6 and less than 1, and y is more than or equal to 0 and less than or equal to 0.4.
In order to solve the technical problem, an embodiment of the present invention provides an application of the carbon-coated high-nickel ternary material in a lithium ion battery.
The invention has the beneficial effects that: according to the method for carrying out carbon coating modification on the high-nickel ternary material, the carbon coating layer is formed on the surface of the high-nickel ternary material, the structure of the high-nickel ternary material is not damaged, the carbon coating layer on the surface avoids direct contact between the high-nickel ternary electrode material and electrolyte, so that side reaction between the surface of the electrode material and the electrolyte is effectively inhibited, namely LiOH and Li2CO3 on the surface of the electrode material are reduced to react with LiPF6 in the electrolyte to generate HF, damage to an SEI film is reduced, the electrode material is protected from being corroded, the interface stability of the high-nickel ternary material is effectively improved, residual lithium on the surface is reduced to generate residual alkali, the first discharge capacity is improved, and the circulation stability is improved.
Drawings
FIG. 1 is a scanning electron microscope image of a high nickel ternary material prepared in comparative example 1;
FIG. 2 is a scanning electron microscope image of a carbon-coated high-nickel ternary material prepared in example 1 of the present invention;
fig. 3 is a cycle comparison plot at 1C rate for the high nickel ternary material prepared in comparative example 1 and the carbon-coated high nickel ternary material prepared in example 1 of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Comparative example 1
Preparation of LiNi according to preferred conditions0.8Co0.1Mn0.1O2The nickel source, the cobalt source and the manganese source are respectively selected from nickel sulfate, cobalt sulfate and manganese sulfate, and are prepared according to the ratio of 8:1: 1; the precipitator is selected from sodium hydroxide, the solution A is prepared into 2mol/L solution, the solution B is prepared into 4mol/L solution, and the solution C is prepared into 1mol/L solution; pumping the solution A, B, C into a reaction kettle at a feeding speed of 1.2mL/min, controlling the stirring speed in the reaction kettle to be 800r/min, controlling the pH to be about 11 in the reaction process, the reaction time to be 24h, the reaction temperature to be 55 ℃, keeping the whole reaction process in a nitrogen protective atmosphere, respectively washing and filtering the solution with deionized water and ethanol for three times, and drying the solution for 24h to obtain the LiNi0.8Co0.1Mn0.1O2Precursor Ni of (2)0.8Co0.1Mn0.1O2(OH)2. The precursor Ni0.8Co0.1Mn0.1O2(OH)2Mixing and grinding the mixture and lithium source lithium hydroxide according to the ratio of 1:1.05, then heating the mixture to 500 ℃ at the pre-sintering heating rate selected from 5 ℃/min, heating the mixture to 800 ℃ at the calcining heating rate selected from 2 ℃/min to obtain the high-nickel ternary material LiNi0.8Co0.1Mn0.1O2The surface topography is shown in figure 1.
Example 1
LiNi of comparative example 1 was selected0.8Co0.1Mn0.1O2As a preferred high nickel ternary material. High nickel ternary material LiNi0.8Co0.1Mn0.1O2Is arranged in a crucibleWherein, the reaction gas is methane, the diluent gas is argon (methane: argon is 1:1), the gas flow is controlled at 10sscm, the reaction time is 20min under the radio frequency plasma, the output power of the reaction radio frequency plasma is 250W, and the reaction temperature is 100 ℃.
The surface appearance of the obtained carbon-coated high-nickel ternary material is shown in figure 2 through observation of a scanning electron microscope, and compared with the comparative example 1, the surface appearance is not obviously changed, and the particle size is not obviously changed, which shows that the surface modification technology can well maintain the original appearance and structure of the anode material.
Example 2
LiNi of comparative example 1 was selected0.8Co0.1Mn0.1O2As a preferred high nickel ternary material. High nickel ternary material LiNi0.8Co0.1Mn0.1O2Placing the mixture into a crucible, wherein the reaction gas is methane, the diluent gas is nitrogen (methane: nitrogen is 1:1), the gas flow is controlled at 10sscm, the reaction time is 20min under radio frequency plasma, the output power of the radio frequency plasma is 250W, and the reaction temperature is 100 ℃.
The surface appearance of the obtained carbon-coated high-nickel ternary material observed by a scanning electron microscope has similar results with example 2.
Example 3
LiNi of comparative example 1 was selected0.8Co0.1Mn0.1O2As a preferred high nickel ternary material. High nickel ternary material LiNi0.8Co0.1Mn0.1O2Placing the mixture into a crucible, wherein the reaction gas is methane, the diluent gas is argon (methane: argon is 3:8), the gas flow is controlled to be 10sscm, the reaction time is 20min under radio frequency plasma, the output power of the radio frequency plasma is 250W, and the reaction temperature is 300 ℃.
The surface appearance of the obtained carbon-coated high-nickel ternary material observed by a scanning electron microscope has similar results with example 2.
Example 4
LiNi of comparative example 1 was selected0.8Co0.1Mn0.1O2As a preferred high nickel ternary material. High nickel ternary material LiNi0.8Co0.1Mn0.1O2Placing the mixture into a crucible, wherein the reaction gas is acetylene, the diluent gas is argon (acetylene: argon is 1:1), the gas flow is controlled to be 10sscm, the reaction time is 20min under radio frequency plasma, the output power of the radio frequency plasma is 250W, and the reaction temperature is 300 ℃.
The surface appearance of the obtained carbon-coated high-nickel ternary material observed by a scanning electron microscope has similar results with example 2.
Example 5
LiNi of comparative example 1 was selected0.8Co0.1Mn0.1O2As a preferred high nickel ternary material. High nickel ternary material LiNi0.8Co0.1Mn0.1O2Placing the mixture into a crucible, wherein the reaction gas is methane, the diluent gas is argon (methane: argon is 1:1), the gas flow is controlled to be 10sscm, the reaction time is 40min under radio frequency plasma, the output power of the radio frequency plasma is 300W, and the reaction temperature is 100 ℃.
The surface appearance of the obtained carbon-coated high-nickel ternary material observed by a scanning electron microscope has similar results with example 2.
Example 6
LiNi of comparative example 1 was selected0.8Co0.1Mn0.1O2As a preferred high nickel ternary material. High nickel ternary material LiNi0.8Co0.1Mn0.1O2Placing the mixture in a crucible, wherein the reaction gas is ethane, the diluent gas is nitrogen (ethane: nitrogen is 1:1), the gas flow is controlled at 10sscm, the reaction time is 40min under radio frequency plasma, the output power of the radio frequency plasma is 250W, and the reaction temperature is 100 ℃.
The surface appearance of the obtained carbon-coated high-nickel ternary material observed by a scanning electron microscope has similar results with example 2.
Example 7
LiNi of comparative example 1 was selected0.8Co0.1Mn0.1O2As a preferred high nickel ternary material. High nickel ternary material LiNi0.8Co0.1Mn0.1O2Placing the mixture into a crucible, wherein the reaction gas is methane, the diluent gas is nitrogen (methane: nitrogen is 1:1), the gas flow is controlled at 10sscm, the reaction time is 120min under radio frequency plasma, the output power of the radio frequency plasma is 100W, and the reaction temperature is 100 ℃.
The surface appearance of the obtained carbon-coated high-nickel ternary material observed by a scanning electron microscope has similar results with example 2.
The surface of the high-nickel ternary material is easy to generate LiOH and Li2CO3 with H2O and CO2 in the air, and the surface of the high-nickel ternary material is coated with carbon, so that the generation of LiOH and Li2CO3 with the surface of the high-nickel ternary electrode material and H2O and CO2 can be effectively reduced. And LiOH on the surface of the high-nickel ternary material reacts with LiPF6 in the electrolyte to generate HF, so that an SEI film is damaged, and parts of the battery are corroded. At a high potential, the surface-generated Li2CO3 is easy to decompose CO2, which causes swelling of the battery and leakage of the electrolyte, and the dense Li2CO3 hinders diffusion of Li ions. The surface carbon coating is carried out on the high-nickel ternary electrode material, so that the generation of side reactions between the surface of the electrode material and electrolyte can be reduced, the stability of the surface of the electrode material is improved, and the circulation stability of the electrode material can be obviously improved.
As shown in FIG. 3, the capacity of example 1 after 100 cycles is 188.5mAh/g, which is 83.9% higher than 102.5mAh/g of comparative example 1, the first discharge capacity is increased from 181.1mAh/g of comparative example 1 to 198.3mAh/g of example 1, which is 9.5% higher, the first efficiency is increased from 76.15% of comparative example 1 to 84.69% of example 1, and the first efficiency is increased by 11.2%. Therefore, compared with the material which is not coated with carbon, the carbon coating by the radio frequency plasma can obviously improve the cycle stability, the first discharge capacity and the first efficiency.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
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, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for carrying out carbon coating modification on a high-nickel ternary material is characterized by placing the high-nickel ternary material in a reaction chamber, reacting for 20-120 min in diluted reactive gas under radio frequency plasma, wherein the reaction temperature is 100-300 ℃, the total gas pressure of the reaction chamber is maintained at 10-1000 Pa, the power output of a power supply of the radio frequency plasma is 100-300W, and the diluted reactive gas is formed by mixing diluent gas and the reactive gas according to the volume ratio of 1: 1-10, so that the carbon-coated high-nickel ternary material is prepared.
2. The method for carbon-coating modification of the high-nickel ternary material, according to claim 1, characterized in that the reactive gas is one or more of methane, ethane, acetylene and carbon tetrafluoride.
3. The method of claim 1, wherein the diluent gas is any one of argon, nitrogen, helium and neon.
4. The method for carbon-coating modification of the high-nickel ternary material according to claim 1, wherein the preparation method of the high-nickel ternary material comprises the following steps:
(1) preparing a solution A: dissolving a nickel source, a cobalt source and a manganese source in deionized water according to a stoichiometric ratio of 8:1:1 to prepare a solution A of 0.5-4 mol/L;
(2) preparing a solution B: preparing a precipitator into 0.5-4 mol/L solution B;
(3) preparing a solution C: preparing 1-4 mol/L ammonia water into a solution C;
(4) pumping the solution A, B, C into a reaction kettle, controlling the pH value to be 10-12 at the rotating speed of 300-1000 r/min, wherein the reaction time is 12-36 h, the reaction temperature is 50-60 ℃, and the reaction atmosphere is a nitrogen protective atmosphere, so as to obtain a first reactant;
(5) sequentially filtering, washing and drying the first reactant to obtain a precursor material;
(6) and mixing and grinding the precursor material and a lithium source according to a ratio of 1:1.05, heating to 450-500 ℃ at a speed of 2-5 ℃/min in an oxygen atmosphere for pre-sintering, and heating to 750-800 ℃ at a speed of 2-5 ℃/min for calcining to obtain the high-nickel ternary material.
5. The method for carbon-coating modification of the high-nickel ternary material, according to claim 1, characterized in that the nickel source is selected from one or more of nickel sulfate, nickel nitrate and nickel chloride, the cobalt source is selected from one or more of cobalt sulfate, cobalt nitrate and cobalt chloride, and the manganese source is selected from one or more of manganese sulfate, manganese nitrate and manganese chloride.
6. The method for carbon-coating modification of the high-nickel ternary material according to claim 1, wherein the precipitating agent is one or more selected from sodium hydroxide, sodium carbonate, sodium oxalate and urea.
7. The method for carbon-coating modification of the high-nickel ternary material, according to claim 1, is characterized in that the lithium source is one or more selected from lithium carbonate, lithium nitrate and lithium hydroxide.
8. A carbon-coated high-nickel ternary material, which is prepared by the method for carrying out carbon-coating modification on the high-nickel ternary material according to any one of claims 1 to 7.
9. The carbon-coated high-nickel ternary material according to claim 8, wherein the chemical formula of the high-nickel ternary material is LiNixCoyMn1-x-yO2Wherein x is more than or equal to 0.6 and less than 1, and y is more than or equal to 0 and less than or equal to 0.4.
10. Use of the carbon-coated high nickel ternary material according to any of claims 8 to 9 in a lithium ion battery.
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| CN114988492A (en) * | 2022-05-31 | 2022-09-02 | 西安合升汇力新材料有限公司 | Nickel-rich ternary cathode material and preparation method and application thereof |
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