CN114695878A - Single crystal ternary cathode material and preparation method and application thereof - Google Patents
Single crystal ternary cathode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a single crystal ternary cathode material and a preparation method and application thereof, and the preparation method comprises the following steps: A. mixing a precursor of the positive electrode material, lithium salt, single-crystal ternary positive electrode material micro powder and a doping component; B. sampling the mixture, performing lithium proportion test, sintering the mixture for the first time after the mixture is qualified, and crushing the mixture after sintering to obtain powder; C. mixing the powder with a certain amount of coating material, carrying out dry coating, and then carrying out secondary sintering at the temperature of 200-600 ℃, thus obtaining the powder after sintering. According to the invention, when the single crystal ternary cathode material finished product is prepared, a certain amount of single crystal ternary material micro powder is added into the raw materials, so that the electrochemical activity of the cathode material is not reduced, the compaction density, the capacity and the first effect of the cathode material are obviously improved, unexpected positive effects are obtained, and the recycling of the single crystal micro powder is successfully realized.
Description
Technical Field
The invention relates to the technical field of lithium ion battery preparation, in particular to a single crystal ternary cathode material and a preparation method and application thereof.
Background
In recent years, the development of new energy automobile technology is more and more advanced, and the energy density of the lithium ion power battery is required to be higher and higher. The layered nickel cobalt lithium manganate ternary positive electrode material (according to the approximate proportion of nickel salt, cobalt salt and manganese (aluminum) salt, it can be classified into models of NCM333, NCM523, NCM622, NCM811, NCA, etc.), especially high nickel type material, has relatively high specific energy and working voltage, and is the most commercially promising positive electrode material at present. The single crystal is used as a modification process of the secondary spherical particles, makes up the defects of the secondary particles, and has the following advantages: 1) an intercrystalline interface does not exist in the single crystal particles, and intercrystalline breakage does not occur after multiple charge-discharge cycles; 2) the specific surface area of the single crystal particles is small, the contact area with the electrolyte is small, and the side reaction is small; 3) the single crystal material has high mechanical strength, is not easy to break in the compaction process and has high compaction density. The single crystal ternary material gradually becomes the mainstream of the market, but the single crystal ternary material generates a large amount of micro powder (about 100 and 300kg of single crystal ternary material micro powder is generated based on 1 ton of finished product) in the crushing process, the yield of the finished product is reduced, the production cost of the product is greatly improved, and a large amount of data waste is caused.
For the recycling of the single crystal ternary material micro powder, it is proposed to directly use the single crystal ternary material micro powder as a single crystal ternary material raw material, and obtain the anode material particles meeting the requirements in a sintering mode, but the anode material obtained by sintering the single crystal ternary material micro powder has high process requirements during preparation, obviously increases the preparation cost, and the obtained anode material particles belong to the similar single crystal type particles with poor performances, and have poor electrochemical properties (particularly charge-discharge cycle performance) and are difficult to realize effective utilization. The defects of recycling the single-crystal ternary material micro powder as the anode material are obvious, so that the single-crystal ternary material micro powder is difficult to truly realize recycling.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the invention provides a single crystal ternary cathode material and a preparation method and application thereof, based on the purpose of effectively utilizing single crystal ternary cathode material micro powder (hereinafter referred to as single crystal micro powder), a method for effectively utilizing the single crystal micro powder is successfully found through a large number of test summaries and verifications, and a certain amount of single crystal micro powder is added into raw materials when a single crystal ternary cathode material finished product is prepared, so that the electrochemical activity of the cathode material is not reduced, the compaction density, the capacity and the first effect of the cathode material are obviously improved, unexpected positive effects are obtained, the recycling of the single crystal micro powder is realized, and the defects in the prior art are overcome.
The technical scheme adopted by the invention is as follows: a preparation method of a single crystal ternary cathode material comprises the following steps:
A. mixing a precursor of the positive electrode material and lithium salt in a lithium proportion, adding a certain amount of single crystal ternary positive electrode material micro powder and doping components during mixing, and uniformly mixing to obtain a mixture;
B. sampling the mixture, performing lithium proportioning test, sintering the mixture for the first time after the mixture is qualified, wherein the temperature of the first sintering is 800-1000 ℃, the sintering atmosphere is air or oxygen, and performing airflow crushing or mechanical crushing after the sintering is finished to obtain powder;
C. mixing the powder with a certain amount of coating, carrying out dry coating, and then carrying out secondary sintering at the temperature of 200-600 ℃, thus obtaining the coating after sintering.
In the preparation method of the invention, the main innovation points are as follows: a certain amount of single crystal ternary cathode material micro powder is used as one of raw materials for preparing the single crystal ternary cathode material, although the electrochemical performance of the cathode material can be obviously reduced by the single crystal ternary cathode material micro powder, the electrochemical performance of the prepared cathode material is not reduced, the compaction density, the capacity and the first effect of the prepared cathode material are obviously improved by controlling the adding amount of the single crystal ternary cathode material micro powder and regulating and controlling the preparation process, unexpected technical effects are obtained while the single crystal ternary cathode material micro powder is successfully recycled, and the defects existing in the recycling of the single crystal ternary cathode material micro powder are overcome.
Further, the single crystal ternary cathode material micro powder is micro powder generated in the single crystal ternary material crushing process.
In the invention, the doping amount of the single crystal ternary cathode material micro powder is a very critical parameter, which not only concerns whether the single crystal ternary cathode material micro powder can be effectively utilized, but also concerns the recycling effect. The inventor obtains the single crystal ternary cathode material through a large number of experimental summaries and verifications, when the doping amount of the single crystal ternary cathode material micro powder is not more than 10% of the mass of the cathode material precursor, the effective recycling can be realized, the effects of improving the compaction density, the capacity and the first effect of the single crystal ternary cathode material can be achieved, if the doping amount of the single crystal ternary cathode material micro powder exceeds 10%, the defects of the single crystal ternary cathode material micro powder are obviously exposed, the electrochemical performance of the obtained single crystal ternary cathode material can be obviously reduced, and the recycling of the single crystal micro powder cannot be realized.
Further, the granularity of the single crystal ternary cathode material micro powder is not more than 3 μm.
In the present invention, the doping component is preferably nano zirconia, and the addition amount of the doping component is 1% to 5% of the mass of the positive electrode material precursor, and may be, for example, 1%, 1.5%, 2%, 2.1%, 2.2%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.8%, 4%, 4.2%, 4.5%, 5%, or the like, and may be specifically selected according to actual needs.
The coating is selected from one of nano alumina, nano boron oxide and nano titanium oxide, preferably nano titanium oxide, and the addition amount of the coating is 1% to 5% of the mass of the positive electrode material precursor, and may be, for example, 1%, 1.5%, 2%, 2.2%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.8%, 4%, 4.5%, 5%, or the like, and may be specifically selected according to actual needs.
In the invention, during one-time sintering, the heating rate is 3-6 ℃/min, the sintering time is 15-22 h, and the air input amount is 1-10m for carrying out the high-speed upward cultivation. The invention introduces the single crystal micro powder, so that the crystallization temperature of the material is reduced, and the primary sintering temperature is reduced. Meanwhile, after the single crystal fine powder is doped, the amount of air taken in the primary sintering needs to be increased in order to reduce the residual alkali on the surface of the material.
Furthermore, the heating rate can be 3 ℃/min, 4 ℃/min, 5 ℃/min, 5.5 ℃/min, 6 ℃/min and the like, preferably 5 ℃/min, after the preset temperature is reached, the heat is preserved and sintered for a certain time, for example, the heat can be preserved for 15h, the sintering time is controlled according to the actual situation, and the total time is controlled to be 15h-22 h. Taking the air atmosphere as an example, the air atmosphere typically comprises a top-up speed of 1m, a bottom-up speed of 1.2 m, a top-down speed of 1.5 m, a top-down speed of 1.7 m, a top-down speed of 2m, a top-down speed of 2.5m, a top-down speed of 3m, a top-down speed of 3.5 m, a top-down speed of 4m, a top-down speed of 5m, and the like, preferably a top-down speed of 2 m.
Further, in the step B, the qualified range of the lithium proportioning test is 1.01-1.05.
Further, the invention also comprises a single crystal ternary cathode material which is prepared by the preparation method.
The invention further comprises a lithium ion battery which comprises a positive electrode, a negative electrode and a diaphragm positioned between the positive electrode and the negative electrode, wherein the positive electrode material used by the positive electrode is the single-crystal ternary positive electrode material.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the invention, when the single crystal ternary cathode material finished product is prepared, a certain amount of single crystal ternary material micro powder is added into the raw material, so that the electrochemical activity of the cathode material is not reduced, the compacted density, the capacity and the first effect of the cathode material are obviously improved, unexpected positive effects are obtained, and the recycling of the single crystal micro powder is successfully realized;
2. the invention carries out single crystal micro powder mixing and sintering in the original production process, not only does not influence the production efficiency, but also can continuously recover the micro powder generated in the ternary material production process, greatly reduces the production cost, improves the product competitiveness and solves the problem that the single crystal micro powder can not be effectively utilized in the prior art.
Drawings
Fig. 1 is a graph comparing charge and discharge curves at 0.1C rate of a battery assembled from example 1 and comparative example 1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
A523 type single crystal ternary positive electrode material (NCM 523) is prepared by the following steps:
s1, weighing 2kg of 523 type (NCM 523) single crystal precursor, 0.85kg of lithium carbonate, 7g of nano-zirconia and 0.8g of single crystal 523 micropowder with corresponding weight according to the lithium proportion of 1.05, uniformly mixing the obtained mixture with Taixian powder VCH-5, loading the mixture into a sagger by using the sagger, wherein the height of the sagger is 70mm, hollowing the mixture, sintering the mixture in a box furnace, and carrying out sintering at the sintering temperature of 945 ℃ (945 ℃ and the heat preservation time of 15 h), wherein the temperature rise and reduction rate is 5 ℃/min, the air atmosphere is sintered, and the flow rate is 2.2m of the rack/h;
and S2, after sintering, carrying out gas flow crushing, dry coating of nano titanium oxide (the doping amount of the nano titanium oxide is 2% of the mass of the 523-type single crystal precursor), and then carrying out secondary sintering (the sintering temperature is 550 ℃, and after sintering, obtaining the micro powder-doped single crystal 523 positive electrode material.
Example 2
A811 type single crystal ternary positive electrode material (NCM 811) is prepared by the following steps:
s1, weighing 2kg of 811 type (NCM 811) single crystal precursor, 0.95kg of lithium hydroxide, 7g of nano zirconia and 0.6g of single crystal 811 micropowder with corresponding weight according to the lithium proportion of 1.045, uniformly mixing the precursor and the micropowder by using Taixian powder VCH-5, loading the mixture into a sagger with the height of 50mm, hollowing the mixture, sintering the mixture in a box furnace at the sintering temperature of 830 ℃ (830 ℃ for 13 h), heating and cooling at the rate of 3 ℃/min, and sintering atmosphere oxygen with the flow of 1.8m for each hour;
and S2, after sintering, carrying out gas flow crushing, washing, filter pressing and drying, carrying out dry coating on the nano boron oxide (the doping amount of the nano boron oxide is 1.5 percent of the mass of the 811 type single crystal precursor), then carrying out secondary sintering (the sintering temperature is 280 ℃, and obtaining the micro powder-doped single crystal 811 cathode material after sintering.
Example 3
A622 type single crystal ternary positive electrode material (NCM 622) is prepared by the following steps:
s1, weighing 2kg of 622 type (NCM 622) single crystal precursor, 0.85kg of lithium carbonate, 7g of nano zirconia and 0.8g of single crystal 622 micropowder with corresponding weight according to the lithium proportion of 1.05, uniformly mixing the precursor and the micropowder by using saggar powder VCH-5, loading the mixture into a saggar with the height of 60mm, hollowing the mixture, sintering the mixture in a box furnace at the sintering temperature of 960 ℃ (960 ℃ for 14 h), heating and cooling at the rate of 5 ℃/min, and sintering the atmosphere air with the flow of 2.4m for 2.4 m;
and S2, after sintering, carrying out gas flow crushing, dry coating of nano titanium oxide (the doping amount of the nano titanium oxide is 2.5 percent of the mass of the 622 type single crystal precursor), then carrying out secondary sintering (the sintering temperature is 600 ℃, and after sintering, obtaining the micro powder doped single crystal 622 positive electrode material.
Comparative example 1
Comparative example 1 is the same as example 1 except that the fine powder of the single crystal 523 was not doped, and the other conditions were the same, to obtain a positive electrode material of the single crystal 523 which was not doped with the fine powder of the single crystal 523.
Comparative example 2
Comparative example 2 is the same as example 1 except that the amount of fine powder of the single crystal 523 was 300g (> 10%), and the other conditions were the same, to obtain a fine powder-doped single crystal 523 positive electrode material.
Comparative example 3
Comparative example 3 is the same as example 1 except that the primary sintering temperature was 1100 ℃ and the other conditions were the same, to obtain a single crystal 523 positive electrode material doped with a fine powder.
Comparative example 4
Comparative example 4 is the same as example 1 except that the air inflow was 0.5 m/h and the conditions were the same, and a single crystal 523 positive electrode material blended with the fine powder was obtained.
The positive electrode materials prepared in example 1 and comparative examples 1 to 4 were assembled into button half cells: taking N-methylpyrrolidone (NMP) as a solvent, mixing a positive electrode active material: conductive carbon black: uniformly mixing polyvinylidene fluoride (PVDF) =8:1:1, coating the mixture on aluminum foil, drying the mixture at 80 ℃ to obtain a positive electrode piece, and assembling the positive electrode piece into a CR2025 type button half-cell in an argon glove box, wherein the positive electrode is the positive electrode piece, the counter electrode is a lithium piece, the diaphragm is Celgard 2500, the electrolyte is dimethyl carbonate, diethyl carbonate and ethyl carbonate which are in a volume ratio of 1:1:1, and 1mol/L LiPF is used as a solvent6The solution is prepared from solute, and then a battery performance test is carried out, wherein the test voltage is 2.8V-4.35V. The test results are shown below:
example 1: the compacted density is 3.82g/cm3The discharge specific capacity is 184.2mAh/g, and the first effect is 90.25%;
comparative example 1: the compacted density is 3.35g/cm3The discharge specific capacity is 179.0mAh/g, and the first effect is 88.45%;
comparative example 2: the compacted density is 3.30g/cm3The discharge specific capacity is 180.5mAh/g, and the first effect is 89.03%;
comparative example 3: the compacted density is 3.28g/cm3The discharge specific capacity is 175.8mAh/g, and the first effect is 86.42%;
comparative example 4: the compacted density is 3.76g/cm3The discharge specific capacity is 182.5mAh/g, and the first effect is 89.86%;
from the above, it can be obtained by comparing example 1 with comparative example 1 that the single crystal material produced by the present invention is improved in the single crystal compacted density by 0.5g/cm as compared with the single crystal of the undoped fine powder3To reach 3.8 g/cm3Above, the discharge specific capacity is improved by 5mAh/g, and the first effect is improved by 1.8%, thereby showing that the addition of the single crystal micro powder is successfulRealizes recycling, improves the compaction density, the discharge specific capacity and the first efficiency performance of the single crystal ternary material, and achieves positive technical effects. Further, from the test results of comparative example 2, it is seen that when the content of the fine single crystal powder exceeds 10%, the electrochemical performance of the ternary single crystal material tends to be lowered, and therefore, the content of the fine single crystal powder needs to be controlled within 10%. Accordingly, from the test results of comparative example 3, when the primary sintering temperature is too high, the chemical properties of the single crystal ternary material are significantly reduced, thereby illustrating that appropriately lowering the primary sintering temperature is helpful to obtain a single crystal ternary material with better electrochemical properties. Accordingly, from the test results of comparative example 4, when the amount of intake air is insufficient in one sintering process, the electrochemical performance of the single crystal ternary material is in a downward trend, thereby illustrating that the amount of intake air affects the electrochemical performance of the single crystal ternary material, and properly increasing the amount of intake air helps to improve the electrochemical performance of the single crystal ternary material.
Meanwhile, as can be seen from fig. 1, the charge and discharge properties of the single crystal 523 positive electrode material prepared by the method are almost consistent compared with those of the single crystal 523 positive electrode material not doped with the single crystal micro powder, which shows that the single crystal micro powder is introduced, so that the electrochemical properties of the positive electrode material are not negatively affected, the compaction density, the capacity and the first effect of the positive electrode material are improved, unexpected positive effects are obtained, and the recycling of the single crystal micro powder is successfully realized.
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 (10)
1. The preparation method of the single crystal ternary cathode material is characterized by comprising the following steps of:
A. mixing a precursor of the positive electrode material and lithium salt in a lithium proportion, adding a certain amount of single crystal ternary positive electrode material micro powder and doping components during mixing, and uniformly mixing to obtain a mixture;
B. sampling the mixture, performing lithium proportioning test, sintering the mixture for the first time after the mixture is qualified, wherein the temperature of the first sintering is 800-1000 ℃, the sintering atmosphere is air or oxygen, and performing airflow crushing or mechanical crushing after the sintering is finished to obtain powder;
C. mixing the powder with a certain amount of coating material, carrying out dry coating, and then carrying out secondary sintering at the temperature of 200-600 ℃, thus obtaining the powder after sintering.
2. The method for preparing a single crystal ternary cathode material according to claim 1, wherein the micro powder of the single crystal ternary cathode material is micro powder generated in the process of crushing the single crystal ternary cathode material.
3. The method for preparing a single crystal ternary cathode material according to claim 2, wherein the doping amount of the single crystal ternary cathode material micro powder is not more than 10% of the mass of the cathode material precursor.
4. A method for producing a single-crystal ternary positive electrode material according to claim 3, wherein the particle size of the single-crystal ternary positive electrode material fine powder is not more than 3 μm.
5. The method for preparing a single crystal ternary cathode material as in any one of claims 1 to 4, wherein the doping component is nano zirconia, and the addition amount of the doping component is 1 to 5 percent of the mass of the precursor of the cathode material.
6. The preparation method of the single crystal ternary cathode material as claimed in claim 5, wherein the coating is selected from one of nano alumina, nano boron oxide and nano titanium oxide, and the addition amount of the coating is 1% -5% of the mass of the precursor of the cathode material.
7. The method for preparing the single crystal ternary cathode material according to claim 1, wherein during one-time sintering, the temperature rise rate is 3 ℃/min to 6 ℃/min, the sintering time is 15h to 22h, and the air inflow is 1m to 10m during cultivation/h.
8. The method for producing a single-crystal ternary positive electrode material according to claim 1, wherein in step B, a pass range of a lithium proportion test is 1.01 to 1.05.
9. A single crystal ternary cathode material, characterized in that the single crystal ternary cathode material is prepared by the preparation method of any one of the preceding claims 1 to 8.
10. A lithium ion battery, comprising a positive electrode, a negative electrode and a diaphragm positioned between the positive electrode and the negative electrode, wherein the positive electrode material used by the positive electrode is the single crystal ternary positive electrode material in claim 9.
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CN116199278A (en) * | 2023-05-05 | 2023-06-02 | 四川新能源汽车创新中心有限公司 | Preparation method of ternary positive electrode material of lithium battery |
CN116332250A (en) * | 2023-05-29 | 2023-06-27 | 四川新能源汽车创新中心有限公司 | Positive electrode material, preparation method thereof and solid-state battery |
WO2024146003A1 (en) * | 2023-01-06 | 2024-07-11 | 广东邦普循环科技有限公司 | Ternary positive electrode material having core-shell structure and preparation method therefor, and lithium ion battery |
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