CN108172825B - High-voltage high-compaction low-cost lithium cobalt oxide positive electrode material and preparation method thereof - Google Patents
High-voltage high-compaction low-cost lithium cobalt oxide positive electrode material and preparation method thereof Download PDFInfo
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention is suitable for the field of lithium battery anode materials, and provides a high-voltage high-compaction low-cost lithium cobalt oxide anode materialThe method comprises the steps of firstly preparing a large-particle-size lithium cobalt oxide anode material doped with an additive A, then preparing a small-particle-size nickel cobalt manganese ternary anode material doped with an additive B, then mixing the large-particle-size lithium cobalt oxide and the small-particle-size nickel cobalt manganese ternary anode material according to different mass ratios, fully improving the compaction density of the materials, reducing the cost of the anode material, and finally sintering and crushing the anode material and a coating agent C containing indium sulfide to obtain the final finished product lithium cobalt oxide anode material. By doping In3+The structural stability of the lithium cobaltate in a high-voltage state can be ensured, and the cycle life and the safety performance of the material are improved.
Description
Technical Field
The invention belongs to the technical field of lithium battery anode materials, and particularly relates to a high-voltage high-compaction low-cost lithium cobalt oxide anode material and a preparation method thereof.
Background
Among lithium ion positive electrode materials, lithium cobaltate is widely used because it has a high operating voltage and energy density, is easily synthesized, and can be rapidly charged and discharged. In recent years, with further miniaturization and multifunctionalization of electronic products, higher demands have been made on the energy density of battery output, and conventional lithium cobaltate has not been able to meet the demands. On the premise of ensuring safety and proper cyclicity, the energy (mainly volume energy density) of the lithium battery is still the basic development direction of the small lithium battery in the coming years, the energy density is improved, two main ways are not provided, and the capacity of an electrode material is improved or the working voltage of the battery is improved. It would be even better if both high voltage and high capacity could be combined, which is in fact the mainstream of current 3C lithium battery positive electrode material development. The working voltage range of the existing lithium ion battery is basically between 3.0V and 4.3V, and the lithium ion battery taking lithium cobaltate as a positive electrode material can increase about 20 percent of capacity when being charged to 4.5V, but the lithium cobaltate is deeply subjected to Li extraction+Accompanying the phase change process with poor reversibility, the material structure is extremely unstable, and the battery is safeThe completeness can not be ensured, and the cycle performance is also sharply reduced. In addition, the lithium cobaltate material is high in price due to the shortage of cobalt resources, and the material cost of the lithium ion battery is increased.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a high-voltage high-compaction low-cost lithium cobalt oxide positive electrode material and a preparation method thereof, and aims to solve the technical problems of poor cycle performance and high cost of the existing lithium cobalt oxide battery.
On one hand, the preparation method of the high-voltage high-compaction low-cost lithium cobaltate cathode material comprises the following steps of:
s1, adding a lithium source, large-particle-size cobaltosic oxide and an additive A into a high-speed mixer together according to the molar ratio of Li to Co to A (1.02-1.07) to 1 (0.005-0.01), fully mixing uniformly, and then sintering at high temperature, wherein the additive A at least comprises nanoscale In2O3The material also comprises at least one of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide;
s2, crushing the material sintered in the step S1, controlling the median particle size D50 of the sintered material to be 15-25 mu m during crushing, and sieving to obtain a large-particle-size lithium cobalt oxide positive electrode material;
s3, adding a lithium source, a small-particle-size nickel-cobalt-manganese composite precursor and an additive B into a high-speed mixer together according to the molar ratio of Li to Me: B (1.002-1.007) to 1 (0.0002-0.0005), fully and uniformly mixing, wherein Me is the sum of the molar amounts of Ni, Co and Mn, and then sintering at high temperature, wherein the additive B is one or more of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide;
s4, crushing the material sintered in the step S3, controlling the median particle size D50 of the sintered material to be 4-8 mu m during crushing, and sieving to obtain a small-particle-size nickel-cobalt-manganese ternary cathode material;
s5, mixing the large-particle-size lithium cobalt oxide positive electrode material and the small-particle-size nickel cobalt manganese ternary positive electrode material according to the mass ratio (2-9): 1, then adding the mixture and a coating agent C into a high-speed mixer together for fully and uniformly mixing to obtain coated mixed powder, and feeding the coated mixed powder into a mixerHigh-temperature sintering, wherein the coating agent C at least comprises indium sulfide In2S3Also comprises one or more of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide;
and S6, crushing the material sintered in the step S5, controlling the median particle size D50 of the sintered material to be 14-23 mu m during crushing, and sieving to obtain the final finished product of the lithium cobaltate cathode material.
Further, the lithium source used in steps S1 and S3 is lithium carbonate.
Further, in the step S1, the sintering temperature is 1000-1200 ℃, the sintering heat preservation time is 8-15 h, air is blown in the sintering process, and the air flow is 0.2-1.2 m3H; in the step S3, the sintering temperature is 700-1100 ℃, the sintering heat preservation time is 8-15 h, air is blown in during the sintering process, and the air flow is 0.2-1.2 m3And (S5), the sintering temperature is 600-1000 ℃, the sintering heat preservation time is 4-10 hours, air is blown in the sintering process, and the air flow is 0.2-1.2 m3/h。
Further, in the steps S1, S3 and S5, the mixing time of the high-speed mixer is 10-30 min; in steps S2, S4, and S6, an air jet milling method or a high-speed rotational flow milling method is used for milling the material.
Further, the median particle diameter D50 of the additive A, the additive B and the coating agent C is less than 7 μm.
Further, in the steps S1, S3 and S5, the temperature rise rate in the sintering process is 2.0-8.0 ℃/min.
Further, in step S5, the amount of the coating agent C is 0.5% to 2% of the total mass of the large-particle-size lithium cobalt oxide positive electrode material and the small-particle-size nickel cobalt manganese ternary positive electrode material.
On the other hand, the high-voltage high-compaction low-cost lithium cobaltate cathode material is prepared by the method, and the specific surface area of the material is 0.15m2/g～0.25m2Per g, compacted density>＝4.1g/m2。
The invention has the beneficial effects that: firstly, the invention is improved by doping In ions with a proper amount, because In3+And Co3+Have the same valence state, incorporateIn (2) of3+Occupy Co3+Bit, Co ion generates Co during charging3+To Co4+And with the volume shrinkage, if the charging voltage is too high and the charging depth is too large, the volume shrinkage of the material will be irreversible and eventually lose electrochemical activity, while In3+The material has the advantages that the material does not change valence in the charging and discharging process, is electrochemically inert, does not change valence state during charging and discharging, does not change volume, can play a role of a framework, stabilizes a crystal structure, and improves the cycle life and safety performance of the material; secondly, a mode of mixing large-particle lithium cobalt oxide and small-particle nickel-cobalt-manganese ternary positive electrode materials is adopted, so that the compaction density of the materials is improved, and the cost of finished lithium cobalt oxide is reduced.
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 with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preparation method of the high-voltage high-compaction low-cost lithium cobaltate cathode material provided by the invention comprises the following steps of:
s1, adding a lithium source, large-particle-size cobaltosic oxide and an additive A into a high-speed mixer together according to the molar ratio of Li to Co to A (1.02-1.07) to 1 (0.005-0.01), fully mixing uniformly, and then sintering at high temperature, wherein the additive A at least comprises nanoscale In2O3And at least one of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide. The lithium source is lithium carbonate, the sintering temperature is 1000-1200 ℃ in the sintering process, the sintering heat preservation time is 8-15 hours, air is blown in the sintering process, and the air flow is 0.2-1.2 m3The heating rate in the sintering process is 2.0-8.0 ℃/min, and the mixing time of the high-speed mixer is 10-30 min. Median particle diameter D50 of additive A<＝7μm。
And S2, crushing the material sintered in the step S1, controlling the median particle size D50 of the sintered material to be 15-25 mu m during crushing, and sieving the crushed material with a 325-mesh sieve to obtain the large-particle-size lithium cobalt oxide cathode material.
And S3, adding a lithium source, a small-particle-size nickel-cobalt-manganese composite precursor and an additive B into a high-speed mixer together according to the molar ratio of Li to Me: B (1.002-1.007): 1 (0.0002-0.0005), fully and uniformly mixing, wherein Me is the sum of the molar amounts of Ni, Co and Mn, and then sintering at high temperature, wherein the additive B is one or more of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide. The lithium source is lithium carbonate, the sintering temperature is 700-1100 ℃ in the sintering process, the sintering heat preservation time is 8-15 hours, air is blown in the sintering process, and the air flow is 0.2-1.2 m3H, the mixing time of the high-speed mixer is 10-30 min, and the heating rate in the sintering process is 2.0-8.0 ℃/min. Median particle diameter D50 of additive B<＝7μm。
And S4, crushing the material sintered in the step S3, controlling the median particle size D50 of the sintered material to be 4-8 mu m during crushing, and sieving the crushed material with a 325-mesh sieve to obtain the nickel-cobalt-manganese ternary cathode material with small particle size.
S5, mixing the large-particle-size lithium cobalt oxide positive electrode material and the small-particle-size nickel cobalt manganese ternary positive electrode material according to the mass ratio (2-9): 1, then adding the mixture and a coating agent C into a high-speed mixer together, fully and uniformly mixing to obtain coated mixed powder, and sintering the coated mixed powder at high temperature, wherein the coating agent C at least comprises indium sulfide In2S3And also comprises one or more of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide. The heating rate in the sintering process is 2.0-8.0 ℃/min, the sintering temperature is 600-1000 ℃, the sintering heat preservation time is 4-10 h, air is blown in the sintering process, and the air flow is 0.2-1.2 m3And h, mixing time of the high-speed mixer is 10-30 min. Median particle diameter D50 of coating agent C<The amount of the coating agent C is 0.5-2% of the total mass of the large-particle-size lithium cobalt oxide positive electrode material and the small-particle-size nickel-cobalt-manganese ternary positive electrode material, wherein the particle size of the coating agent C is 7 mu m.
And S6, crushing the material sintered in the step S5, controlling the median particle size D50 of the sintered material to be 14-23 mu m during crushing, and sieving to obtain the final finished product of the lithium cobaltate cathode material.
In the above process, gas is used for pulverizing the materialsA flow milling method or a high-speed cyclone milling method. The specific surface area of the finally obtained material is 0.15m2/g～0.25m2Per g, compacted density>＝4.1g/m2。
The present invention is illustrated by the following specific examples.
Example 1
(1) Lithium carbonate, cobaltosic oxide with large particle size and additive A (nanometer In)2O3And nano strontium phosphate) in a molar ratio of Li to Co to a of 1.025: 0.993: 0.007 part of the raw materials are weighed and then added into a high-speed mixer together to be fully and uniformly mixed for 15 min. Placing the mixture in a box furnace for sintering, and introducing 0.5m3And air with flow rate/h, the heating rate is 2 ℃/min, the sintering temperature is 1100 ℃, the sintering temperature is kept for 12h, the sintering material is obtained by cooling along with the furnace, the sintering material is crushed, and the crushed sintering material passes through a 325-mesh screen, so that the lithium cobaltate anode material with large particle size is obtained.
(2) Lithium carbonate, a small-particle-size nickel-cobalt-manganese composite precursor and nanoscale iridium oxide are mixed according to a molar ratio of Li to Me, B is 1.006: 0.994: 0.009 weighing the corresponding raw materials, then adding the raw materials into a high-speed mixer together, and mixing the raw materials uniformly for 15 min. Placing the mixture in a box furnace for sintering, and introducing 0.4m3Air with flow rate per hour, the heating rate is 4 ℃/min, the sintering temperature is 900 ℃, the sintering temperature is kept for 5 hours, the mixture is cooled along with the furnace to obtain a sintered material, the sintered material is crushed, and the crushed material passes through a 325-mesh screen to obtain the small-particle-size nickel-cobalt-manganese ternary cathode material.
(3) And mixing the large-particle-size lithium cobalt oxide positive electrode material and the small-particle-size nickel-cobalt-manganese ternary positive electrode material according to the mass ratio of 7: 3, then mixing with indium sulfide (In)2S3) Adding the powder and coating agents (molybdenum oxide, cerium oxide and bismuth oxide) into a high-speed mixer together, and fully and uniformly mixing to obtain coated mixed powder, wherein the amount of the coating agents is 0.8 percent of the total amount, carrying out secondary high-temperature sintering on the coated mixed powder, the sintering temperature is 950 ℃, the sintering heat preservation time is 6h, air is blown in during the sintering process, and the air flow is 0.5m3And h, obtaining a material after secondary sintering.
(4) And (4) crushing the material after secondary sintering, and screening the crushed material by a 325-mesh screen to obtain the final high-voltage high-compaction low-cost finished lithium cobalt oxide cathode material.
The specific surface area of the finally obtained finished product lithium cobaltate cathode material is 0.15m2/g～0.25m2Per g, compacted density>＝4.1g/m2And carrying out full battery test, wherein the electrochemical performance is as follows: when the lithium battery is charged and discharged at 3-4.4V, the first discharge capacity reaches 180mAh/g, and the cycle capacity retention rate of 50 weeks reaches more than 95%.
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 (8)
1. A preparation method of a high-voltage high-compaction low-cost lithium cobaltate positive electrode material is characterized by comprising the following steps of:
s1, adding a lithium source, large-particle-size cobaltosic oxide and an additive A into a high-speed mixer together according to the molar ratio of Li to Co to A (1.02-1.07) to 1 (0.005-0.01), fully mixing uniformly, and then sintering at high temperature, wherein the additive A at least comprises nanoscale In2O3The material also comprises at least one of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide;
s2, crushing the material sintered in the step S1, controlling the median particle size D50 of the sintered material to be 15-25 mu m during crushing, and sieving to obtain a large-particle-size lithium cobalt oxide positive electrode material;
s3, adding a lithium source, a small-particle-size nickel-cobalt-manganese composite precursor and an additive B into a high-speed mixer together according to the molar ratio of Li to Me: B (1.002-1.007) to 1 (0.0002-0.0005), fully and uniformly mixing, wherein Me is the sum of the molar amounts of Ni, Co and Mn, and then sintering at high temperature, wherein the additive B is one or more of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide;
s4, crushing the material sintered in the step S3, controlling the median particle size D50 of the sintered material to be 4-8 mu m during crushing, and sieving to obtain a small-particle-size nickel-cobalt-manganese ternary cathode material;
s5, mixing the large-particle-size lithium cobalt oxide positive electrode material and the small-particle-size nickel cobalt manganese ternary positive electrode material according to the mass ratio (2-9): 1, then adding the mixture and a coating agent C into a high-speed mixer together, fully and uniformly mixing to obtain coated mixed powder, and sintering the coated mixed powder at high temperature, wherein the coating agent C at least comprises indium sulfide In2S3Also comprises one or more of strontium phosphate, molybdenum oxide, cerium oxide, iridium oxide and bismuth oxide;
s6, crushing the material sintered in the step S5, controlling the median particle size D50 of the sintered material to be 14-23 mu m during crushing, and sieving to obtain a final finished product of the lithium cobaltate cathode material;
in the step S1, the sintering temperature is 1000-1200 ℃, the sintering heat preservation time is 8-15 h, air is blown in during the sintering process, and the air flow is 0.2-1.2 m3H; in the step S3, the sintering temperature is 700-1100 ℃, the sintering heat preservation time is 8-15 h, air is blown in during the sintering process, and the air flow is 0.2-1.2 m3And (S5), the sintering temperature is 600-1000 ℃, the sintering heat preservation time is 4-10 hours, air is blown in the sintering process, and the air flow is 0.2-1.2 m3/h。
2. The method of claim 1, wherein the lithium source used in steps S1 and S3 is lithium carbonate.
3. The method for preparing a high-voltage high-compaction low-cost lithium cobaltate cathode material as claimed in claim 2, wherein in the steps S1, S3 and S5, the mixing time of the high-speed mixer is 10-30 min; in steps S2, S4, and S6, an air jet milling method or a high-speed rotational flow milling method is used for milling the material.
4. The method for preparing a high-voltage, highly compacted, low-cost lithium cobaltate positive electrode material according to claim 3, wherein the median particle diameter D50 of the additive A, the additive B and the coating agent C is not more than 7 μm.
5. The method for preparing a high-voltage high-compaction low-cost lithium cobaltate cathode material according to claim 4, wherein in the steps S1, S3 and S5, the temperature rise rate in the sintering process is 2.0-8.0 ℃/min.
6. The method of claim 5, wherein in step S5, the amount of the coating agent C is 0.5-2% of the total mass of the large-particle-size lithium cobalt oxide positive electrode material and the small-particle-size nickel cobalt manganese ternary positive electrode material.
7. A high-voltage high-compaction low-cost lithium cobalt oxide cathode material, which is prepared by the preparation method of any one of claims 1 to 6.
8. The high-voltage high-compaction low-cost lithium cobalt oxide positive electrode material according to claim 7, wherein the specific surface area of the high-voltage high-compaction low-cost lithium cobalt oxide positive electrode material is 0.15m2/g～0.25m2G, the compacted density is more than or equal to 4.1g/m2。
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| CN110620215B (en) * | 2018-06-20 | 2022-05-13 | 深圳市贝特瑞纳米科技有限公司 | Cathode material, preparation method thereof and lithium ion battery containing cathode material |
| CN109273684A (en) * | 2018-09-07 | 2019-01-25 | 北京泰丰先行新能源科技有限公司 | A kind of lithium ion battery composite cathode material and preparation method thereof |
| CN109638291B (en) * | 2018-12-27 | 2020-12-04 | 清远佳致新材料研究院有限公司 | Positive electrode slurry, preparation method, positive plate and lithium ion battery |
| CN109888250A (en) * | 2019-03-29 | 2019-06-14 | 荆门市格林美新材料有限公司 | A kind of room temperature carbon coating monocrystalline nickel-cobalt-manganternary ternary anode material and preparation method |
| CN110048111A (en) * | 2019-04-25 | 2019-07-23 | 柔电（武汉）科技有限公司 | Cell positive material, battery anode slice and lithium battery |
| CN111916688B (en) * | 2019-05-09 | 2022-04-05 | 天津国安盟固利新材料科技股份有限公司 | Lithium cobaltate composite positive electrode material and preparation method thereof |
| CN114204011B (en) * | 2021-12-07 | 2024-02-27 | 万华化学(四川)有限公司 | Preparation method of nickel cobalt lithium manganate ternary positive electrode material |
| CN114561686B (en) * | 2022-02-28 | 2023-06-27 | 蜂巢能源科技股份有限公司 | Method for improving compaction density of cobalt-free positive electrode material, cobalt-free positive electrode material and lithium ion battery |
| CN115000369A (en) * | 2022-05-31 | 2022-09-02 | 上海瑞浦青创新能源有限公司 | Positive electrode material, positive electrode plate and lithium ion battery |
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