CN110854370A - Preparation method of high nickel cobalt lithium manganate positive electrode material - Google Patents
Preparation method of high nickel cobalt lithium manganate positive electrode material Download PDFInfo
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Abstract
The invention discloses a preparation method of a high nickel cobalt lithium manganate positive electrode material, which comprises the following steps: with Ni0.83Co0.11Mn0.06(OH)2And LiOH. H2O is used as a raw material, and A (Zr or Mg or Ti or Nb) is doped and mixed uniformly; sintering the mixed material for the first time; adding A to the primary sinter massl2O3、TiO2Or Na2TiO3After secondary sintering, A is obtainedl2O3、TiO2Or Na2TiO3Coated positive electrode material LiNi0.83‑ xCo0.11Mn0.06AxO2And X is 0.001-0.002. According to the invention, the nickel cobalt lithium manganate material is prepared by taking high nickel cobalt manganese hydroxide and lithium hydroxide monohydrate as raw materials and doping metal elements, so that the structural stability and the thermal stability of the material are improved, and then the circulation performance and the rate performance of the material are improved by performing surface coating by using a coating agent.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a high nickel cobalt lithium manganate positive electrode material.
Background
The nickel cobalt lithium manganate ternary composite material (NCM) is a hot positive electrode material in the current market, and has the advantages of low cost, large discharge capacity, good cycle performance, good thermal stability, relatively stable structure and the like0.33Co0.33Mn0.33O2(111 type) LiNi0.5Co0.2Mn0.3O2(523 type), LiNi0.6Co0.2Mn0.2O2(type 622) and Ni0.8Co0.1Mn0.1O2(811 type), the material capacity increases with the increase of the nickel content, but the cation-shuffling phenomenon becomes more and more severe, the cycle stability and the thermal stability become gradually poor, and the surface Li2CO3And an increase in LiOH content. In order to meet the requirements of the current automobile battery industry, the development and research of the high nickel-based nickel cobalt lithium manganate material are imperative.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: according to the figure, the cycle performance and the rate performance of the high-nickel cobalt lithium manganate cathode material are improved, and the preparation method of the high-nickel cobalt lithium manganate cathode material is provided for solving the problems.
The invention is realized by the following technical scheme:
a preparation method of a high nickel cobalt lithium manganate positive electrode material comprises the following steps:
step 1, with Ni0.83Co0.11Mn0.06(OH)2And LiOH. H2O is used as a raw material, is doped with any one element of Zr, Mg, Ti and Nb, and is uniformly mixed to obtain a mixed material;
step 2, sintering the mixed material for the first time to obtain a primary sintered material;
step 3, adding A to the primary sintering materiall2O3、TiO2Or Na2TiO3After secondary sintering, A is obtainedl2O3、TiO2Or Na2TiO3Coated lithium nickel cobalt manganese oxide ternary positive electrode material LiNi0.83-xCo0.11Mn0.06AxO2Wherein A is Zr or Mg or Ti or Nb, and X is 0.001-0.002.
In step 1, the material ratio is Mn: Li: a ═ 1:1.07:0.2, wherein a ═ Zr or Mg or Ti or Nb.
Further, in the step 1, the raw material and the doping element are uniformly mixed by a high-speed mixer in a low-speed and high-speed combination mode.
Further, the primary sintering is carried out in an oxygen atmosphere, the sintering temperature is 780-820 ℃, and the sintering time is 11-16 h.
Further, the secondary sintering is carried out in an oxygen atmosphere, the sintering temperature is 500-600 ℃, and the sintering time is 7-9 h.
Further, the addition of Al2O3、TiO2Or Na2TiO3The addition amount of the substance is 1 wt% -3 wt%.
Further, the oxygen content in the oxygen atmosphere is > 96%.
Further, in the step 3, the primary sintering material is washed with water, and Al is added under stirring in the washing process2O3Sol or TiO2The water solution is stirred evenly, and the filter cake is sintered for the second time after filtration.
Further, in the step 3, one is addedSecondary sinter material and Na2TiO3And uniformly mixing the raw materials by a high-speed mixer, and then performing secondary sintering.
The invention has the following advantages and beneficial effects:
the present invention uses nickel-cobalt-manganese hydroxide (Ni) of high nickel series0.83Co0.11Mn0.06(OH)2) And lithium hydroxide monohydrate is used as a raw material to prepare the lithium nickel cobalt manganese oxide material by doping any one element of Zr, Mg, Ti and Nb, the structural stability and the thermal stability of the material are improved, and then a coating agent Al is utilized2O3、TiO2Or Na2TiO3The material is coated on the surface, so that the cycle performance and the rate capability of the material are improved.
The invention utilizes the combination of low speed (200r/min) and high speed (900r/min) to mix materials, so that the temperature of the materials is reduced when the materials are repeatedly operated at low speed, and the phenomenon of condensation to cause uneven mixing of lumps is avoided; the doping of Zr, Mg, Ti and Nb elements can improve the crystallization stability and thermal stability of the material, and further Al is added2O3、TiO2Or Na2TiO3The material is coated on the surface, so that the cycle performance and the rate capability of the material are improved. The material is prevented from being contacted with water and carbon dioxide in the air by sintering under the oxygen-enriched condition, and the reaction is more complete; in addition, water washing reduces the residual lithium content on the surface of the material to improve the safety and stability of the material.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 shows Zr-doped Al of example 12O3XRD spectrogram of the coating material;
FIG. 2 shows Zr-doped Al of example 12O3SEM image of coating material;
FIG. 3 is Zr-doped Al of example 12O3A charge-discharge curve chart of the coating material;
FIG. 4 shows Zr-doped Al of example 12O3Cycling stability test of clad materialsFigure (a).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
The embodiment provides a preparation method of a high nickel cobalt lithium manganate positive electrode material, which comprises the following steps:
step 1, metal doping: with Ni0.83Co0.11Mn0.06(OH)2And LiOH. H2O is taken as a raw material, a doping element Zr is added, and the adding proportion of Mn to Li to Zr is 1:1.07: 0.2; mixing at low speed (200r/min) for 2min and at high speed (900r/min) for 15min by using a high-speed mixer, uncovering to clean the wall, and repeatedly mixing at low speed (200r/min) for 2min and at high speed (900r/min) for 15min to obtain a mixed material; mixing the materials at 810 deg.C under pure oxygen atmosphere (oxygen content)>96%) for 14h to obtain a primary sintering material;
step 2, coating with oxide: and (2) washing the primary sintering material obtained in the step (1) with 1-1.5 times of deionized water at room temperature, wherein the washing operation method comprises the following steps: firstly, adding the primary sintering material prepared in the step 1 into water while stirring, and then adding 1-3 wt% of Al within 1-3 min2O3The sol is added by slowly spraying with a spray can while stirring, continuously stirring for 10-20 min, performing suction filtration with a cloth-type funnel and a suction filter, wearing latex gloves, and pressing to obtain a filter cake material under pure oxygen condition (oxygen content)>96%) is sintered for 8 hours at 540 ℃ to obtain Al2O3Coated high nickel cobalt lithium manganate ternary positive electrode material LiNi0.829Co0.11Mn0.06Zr0.001O2。
Example 2
The embodiment provides a preparation method of a high nickel cobalt lithium manganate positive electrode material, which comprises the following steps:
step 1, metal doping: with Ni0.83Co0.11Mn0.06(OH)2And LiOH. H2O is taken as a raw material, and a doping element Mg is added, wherein the adding proportion of Mn to Li to Mg is 1:1.07: 0.2; mixing at low speed (200r/min) for 2min and at high speed (900r/min) for 15min by using a high-speed mixer, uncovering to clean the wall, and repeatedly mixing at low speed (200r/min) for 2min and at high speed (900r/min) for 15min to obtain a mixed material; mixing the materials at 780 deg.C under pure oxygen atmosphere (oxygen content)>96%) for 16h to obtain a primary sintering material;
step 2, coating with oxide:
and (2) washing the primary sintering material obtained in the step (1) with 1-1.5 times of deionized water at room temperature, wherein the washing operation method comprises the following steps: firstly, 1 to 3 weight percent of TiO is added into 0.1 time of deionized water2Stirring while adding, and stirring for 5-10 min to obtain TiO2A solution; simultaneously adding the primary sintering material obtained in the step 1 into deionized water of which the volume is 0.9-1.4 times that of the deionized water, and stirring while adding to obtain a suspension; then adding TiO2Adding the solution into the suspension within 1-3 min, wherein the adding method comprises slowly spraying with a spray can while stirring, continuously stirring for 10-20 min, performing suction filtration with a cloth-type funnel and a suction filtration machine, wearing latex gloves, and pressing to obtain filter cake material under pure oxygen condition (oxygen content)>96%) at 580 deg.C for 8h to obtain TiO2Coated high nickel cobalt lithium manganate ternary positive electrode material LiNi0.828Co0.11Mn0.06Mg0.002O2。
Example 3
The embodiment provides a preparation method of a high nickel cobalt lithium manganate positive electrode material, which comprises the following steps:
step 1, metal doping: with Ni0.83Co0.11Mn0.06(OH)2And LiOH. H2O is taken as a raw material, a doping element Nb is added, and the adding proportion is that Mn and Li are added, wherein Nb is 1:1.07: 0.2; mixing at low speed (200r/min) for 2min and at high speed (900r/min) for 15min, cleaning wall, and mixing at low speed (200r/min) and high speed (9)00r/min) for 15min to obtain a mixed material; mixing the materials at 800 deg.C under pure oxygen atmosphere (oxygen content)>96%) for 15h to obtain a primary sintering material;
step 2, coating with oxide: mixing the primary sintering material obtained in the step 1 and 1-3 wt% of Na2TiO3Mixing sequentially in a high-speed mixer at low speed (200r/min) for 2min, at high speed (900r/min) for 5min, at low speed (200r/min) for 1min, and at high speed (900r/min) for 3min, and mixing under pure oxygen condition (oxygen content)>96%) at 600 ℃ for 7h to obtain Na2TiO3Coated high nickel cobalt lithium manganate ternary positive electrode material LiNi0.829Co0.11Mn0.06Nb0.001O2。
Comparative example 1
The preparation method of the high nickel cobalt lithium manganate positive electrode material based on the embodiment 1 is characterized by comprising the following steps: with Ni0.5Co0.2Mn0.3(OH)2And LiOH. H2O is taken as a raw material; final preparation of Al2O3Coated low nickel cobalt lithium manganate ternary positive electrode material LiNi0.499Co0.2Mn0.3Zr0.001O2。
Comparative example 2
The preparation method of the high nickel cobalt lithium manganate positive electrode material based on the embodiment 1 is characterized by comprising the following steps: mixing the primary sintering material with 1-3 wt% of Al2O3Mixing sequentially in a high-speed mixer at low speed (200r/min) for 2min, at high speed (900r/min) for 5min, at low speed (200r/min) for 1min, and at high speed (900r/min) for 3min, and mixing under pure oxygen condition (oxygen content)>96%) is sintered for 7-9 h at 500-600 ℃ to obtain Al2O3Coated high nickel cobalt lithium manganate ternary positive electrode material LiNi0.829Co0.11Mn0.06Zr0.001O2。
Comparative example 3
The preparation method of the high nickel cobalt lithium manganate positive electrode material based on the embodiment 1 is characterized by comprising the following steps: the high-nickel ternary cathode material is prepared only by metal doping, and no coating treatment step is required.
Comparative example 4
The preparation method of the high nickel cobalt lithium manganate positive electrode material based on the embodiment 1 is characterized by comprising the following steps: with Ni0.83Co0.11Mn0.06(OH)2、LiOH·H2Preparing a primary sintering material from O, and mixing the primary sintering material with Al2O3Mixing sequentially in a high-speed mixer at low speed (200r/min) for 2min, at high speed (900r/min) for 5min, at low speed (200r/min) for 1min, and at high speed (900r/min) for 3min, and mixing under pure oxygen condition (oxygen content)>96%) is sintered for 7-9 h at 500-600 ℃ to obtain Al2O3The coated high nickel cobalt lithium manganate ternary positive electrode material does not have a metal doping treatment step.
Comparative example 5
The preparation method of the high nickel cobalt lithium manganate positive electrode material based on the embodiment 1 is characterized by comprising the following steps: the primary sintering and the secondary sintering are both carried out in an air atmosphere.
And (3) performance testing:
1. manufacturing a battery: the doped and coated positive electrode material provided by the embodiment is used as an active material: superp: PVDF 90: and 5:5, weighing, uniformly mixing, adding N-methyl pyrrolidone according to 40 wt% of solid content, uniformly stirring, coating on an Al foil, baking, rolling, cutting into pieces, and assembling to obtain the button cell for testing the electrochemical performance.
2. And (3) rate performance test:
multiplying power performance test conditions: and assembling the half cells in a glove box under the condition of high dehumidification dew point of-40 ℃, wherein a blue cell test system is utilized, the charging and discharging voltage ranges are 3.0V-4.3V, and the constant current charging and discharging currents of 0.1C, 0.2C, 0.5C and 1C are 0.19mA, 0.38mA, 0.96mA and 1.92mA respectively. The test sample was the ternary positive electrode material prepared in example 1.
And (3) testing results: as shown in fig. 3, the discharge capacities of the positive electrode material at 0.1C, 0.2C, 0.5C and 1C were 206.0mAh/g, 202.2mAh/g, 194.7mAh/g and 189.3mAh/g, respectively, and the charge capacities were: 225.0mAh/g, 208.3mAh/g, 202.9mAh/g and 195.0 mAh/g. First charge of 0.1CThe discharge efficiency was 91.56%. Al can be seen from the electron micrograph of FIG. 22O3The coating layer is uniform, the gas production reaction can be effectively inhibited, the material cycle stability and the thermal stability are improved, and the XRD spectrogram in figure 1 shows that the material belongs to α -NaFeO2The layered structure has no other miscellaneous peak, and the diffraction peak is sharp, which shows that the doped and coated sample has better crystallization performance, and the multiplying power performance of the material is improved.
The rate performance of the ternary cathode materials prepared in comparative examples 1-5 is as follows from large to small: comparative example 1 has discharge capacities of 168.8mAh/g, 163.8mAh/g, 156.3mAh/g, 149.5mAh/g > 0.1C, 0.2C, 0.5C, and 1C of 203.1mAh/g, 198.5mAh/g, 189.9mAh/g, 183.2mAh/g > 0.1C, 0.2C, 0.5C, and 1C of 206.3mAh/g, 201.2mAh/g, 189.6mAh/g, 179.6mAh/g > 3 of 0.1C, 0.2C, 0.5C, 1C of 210.4mAh/g, 202.3mAh/g, 188.3mAh/g, 175.2mAh/g > 3 of 0.193 mAh/g, 0.5C of 1C of 161 mAh/g, and 169C of 1mAh/g of 1 of 3 of 1mAh/g of 1mAh of 1 mAh.
3. And (3) testing the cycling stability:
and (3) testing conditions are as follows: assembling half cells in a glove box under the condition of high dehumidification dew point of-40 ℃, and performing cycle performance test under the condition of 1C by using a blue cell test system, wherein the charge-discharge voltage range is 3.0V-4.3V, the constant current charge-discharge current of 1C is 1.92mA respectively
As shown in FIG. 4, the capacity retention rate of the positive electrode material after 50 times of 1C discharge cycle is 96.20%, and the capacity retention rate after 100 times of cycle is 81.56%2The layered structure has no other miscellaneous peak, the diffraction peak is sharp, the crystal structure of the anode material is better, and the multiplying power performance of the material is improved. Al can be seen from the electron micrograph of FIG. 22O3The coating layer is uniform, the surface pulverization and gas production reaction of the anode material can be effectively inhibited, the generation of microcracks in the anode material is reduced, and the material circulation stability is improved.
The capacity retention rates of the ternary cathode materials prepared in comparative examples 1 to 5 after 100 discharge cycles at 1C are as follows from large to small: the retention ratio of comparative example 1 is 87.1% > the retention ratio of comparative example 2 is 80.6% > the retention ratio of comparative example 4 is 79.5% > the retention ratio of comparative example 3 is 58.3% > the retention ratio of comparative example 5 is 32.5%.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. The preparation method of the high nickel cobalt lithium manganate positive electrode material is characterized by comprising the following steps:
step 1, with Ni0.83Co0.11Mn0.06(OH)2And LiOH. H2O is used as a raw material, is doped with any one element of Zr, Mg, Ti and Nb, and is uniformly mixed to obtain a mixed material;
step 2, sintering the mixed material for the first time to obtain a primary sintered material;
step 3, adding A to the primary sintering materiall2O3、TiO2Or Na2TiO3After secondary sintering, Al is obtained2O3、TiO2Or Na2TiO3Coated lithium nickel cobalt manganese oxide ternary positive electrode material LiNi0.83-xCo0.11Mn0.06AxO2Wherein A is Zr or Mg or Ti or Nb, and X is 0.001-0.002.
2. The method for preparing the high nickel cobalt lithium manganate positive electrode material according to claim 1, wherein in the step 1, the material ratio is Mn: Li: a: 1:1.07:0.2, wherein a: Zr or Mg or Ti or Nb.
3. The method for preparing the high nickel cobalt lithium manganate positive electrode material of claim 1, wherein in the step 1, the raw material and the doping element are uniformly mixed by a high mixer in a low-speed and high-speed combination manner.
4. The method for preparing the high nickel cobalt lithium manganate positive electrode material of claim 1, wherein the primary sintering is carried out in an oxygen atmosphere, the sintering temperature is 780-820 ℃, and the sintering time is 11-16 h.
5. The method for preparing the high nickel cobalt lithium manganate positive electrode material of claim 1, wherein the secondary sintering is carried out in an oxygen atmosphere, the sintering temperature is 500-600 ℃, and the sintering time is 7-9 h.
6. The method for preparing the high nickel cobalt lithium manganate positive electrode material of claim 1, wherein said Al is added2O3、TiO2Or Na2TiO3The addition amount of the substance is 1 wt% -3 wt%.
7. The method for preparing the high nickel cobalt lithium manganate positive electrode material of claim 5 or 6, characterized in that, in the oxygen atmosphere, the oxygen content is > 96%.
8. The method for preparing the high nickel cobalt lithium manganate positive electrode material of claim 1 or 6, wherein in the step 3, the primary sintering material is washed with water, and Al is added under stirring during washing with water2O3Sol or TiO2The water solution is stirred evenly, and the filter cake is sintered for the second time after filtration.
9. The method for preparing the high nickel cobalt lithium manganate positive electrode material of claim 1 or 6, characterized in that in step 3, the primary sintering material is mixed with Na2TiO3And uniformly mixing the raw materials by a high-speed mixer, and then performing secondary sintering.
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CN112993242A (en) * | 2021-05-11 | 2021-06-18 | 蜂巢能源科技有限公司 | Nickel-cobalt-manganese positive electrode material and recovery method of waste nickel-cobalt-manganese positive electrode material |
CN113594433A (en) * | 2021-07-19 | 2021-11-02 | 广东佳纳能源科技有限公司 | High-nickel ternary electrode composite material, preparation method thereof and lithium ion battery |
CN113851633A (en) * | 2021-11-29 | 2021-12-28 | 中南大学 | Niobium-doped high-nickel ternary cathode material coated with niobium phosphate and preparation method thereof |
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