CN111600014B - Modified high-specific-capacity high-nickel ternary cathode material and preparation method thereof - Google Patents
Modified high-specific-capacity high-nickel ternary cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a modified high-specific-capacity high-nickel ternary cathode material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Weighing lithium salt and aluminum salt according to the molar ratio of various elements in the solid electrolyte LATP, and dissolving the lithium salt and the aluminum salt in water to obtain a clear and transparent solution; (2) Adding titanium salt into the solution in the step (1), stirring, and adding citric acid until a clear and transparent solution is obtained; (3) adding a high-nickel ternary cathode material; (4) Adding an aqueous solution containing phosphate into the solution in the step (3), and stirring; (5) Carrying out suction filtration on the solution obtained in the step (4) to obtain a filter cake, and drying the filter cake; (6) And (3) carrying out heat treatment on the dried sample to obtain the high-nickel ternary cathode material coated with the solid electrolyte. According to the invention, the surface of the high-nickel ternary cathode material is coated with a layer of fast ion conductor LATP, so that the specific capacity of the high-nickel ternary cathode material is effectively improved on the premise of considering other electrochemical properties and not increasing the nickel content.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a modified high-specific-capacity high-nickel ternary cathode material and a preparation method thereof.
Background
Due to the structural safety of energy and the pressure of environmental protection, the concept of green energy has gradually become a global consensus and attracted attention from governments and research institutions of various countries. Governments around the world actively develop energy-saving and environment-friendly new energy automobiles, and the rapid development of the industry drives the great increase of the demand of power lithium ion batteries. Whether policy-oriented, market demand or technical development direction, increasingly higher requirements are put forward on the energy density of the lithium ion battery. The high-nickel ternary material becomes an important technical route for improving the energy density, and the current high-nickel productThe permeability is low, the industry demand will maintain high-speed growth in the future, and the nickel enrichment of the ternary material has become a necessary trend for the development of power battery materials. Wherein, the nickel cobalt lithium manganate ternary material (NCM) has high reversible specific capacity (after the nickel content is higher than 80 percent, the specific capacity can reach 200mAh g -1 The method has the advantages of low material cost, high safety and the like, is one of the preferred anode materials of the power lithium battery, and has high later-stage potential demand. However, continuing to increase the nickel content to increase the specific capacity results in rapid capacity fade and poor cycling performance. In addition, an increase in the nickel content may result in deterioration of structural stability and thermal stability of the material. Therefore, on the premise of fixing the nickel content, further improving the specific capacity of the material becomes a current research hotspot.
Surface coating is considered to be a simple and effective method for improving the electrochemical properties of materials, and commonly used coating agents are oxides, fluorides and the like. Among them, mgO and Al are common oxides 2 O 3 、TiO 2 、SiO 2 The metal oxide coating layer with stable property can improve the stability of an electrode/electrolyte interface, thereby improving the cycle performance of the electrode material. AlF 3 The coating layer can inhibit the decomposition of electrolyte and the dissolution of metal ions, reduce the side reaction between active substances and the electrolyte, stabilize the crystal structure of the ternary material and further improve the safety performance and the cycle performance of the electrode material.
However, oxides and fluorides are not electrochemically active and have low lithium ion conductivity, and the presence of such a coating layer affects the deintercalation process of lithium ions, which eventually leads to capacity fade. The use of a lithium ion conductor as the cladding layer improves this situation. Particularly, the solid electrolyte has high lithium ion conductivity, is beneficial to the de-intercalation process of lithium ions, can reduce the surface charge transfer impedance, and finally realizes the obvious improvement of the electrochemical performance.
Journal of Power Sources (doi.org/10.1016/j.jp owsource.2018.09.082) published a solution method for coating Li with solid electrolyte LATP 1.2 Ni 0.2 Mn 0.6 O 2 The article of (1). Lithium ion conductivity based on LATP (Latin oxide) is highAnd the structure stability, successfully improves the electrochemical properties of the electrode material, including specific capacity, cycle performance and rate performance. The Journal of the American Chemical Society (doi: 10.1021/jacs.8b03319) coated LATP on the surface of NCM622 by using a sol-gel method, thereby realizing excellent cycle performance and rate performance. However, the specific capacity of the coated NCM622 decreased.
Disclosure of Invention
The invention aims to overcome the technical defects of the background technology and provides a modified high-specific-capacity high-nickel ternary cathode material and a preparation method thereof. The invention coats a layer of fast ion conductor Li on the surface of a high-nickel ternary cathode material 1+x1 Al x1 Ti 2-x1 (PO 4 ) 3 (LATP), under the premise of giving consideration to other electrochemical properties and not increasing the content of nickel, the specific capacity of the high-nickel ternary cathode material is effectively improved.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a modified high-specific-capacity high-nickel ternary cathode material and a preparation method thereof comprise the following steps:
(1) According to the solid electrolyte Li 1+x1 Al x1 Ti 2-x1 (PO 4 ) 3 Weighing appropriate amount of lithium salt and aluminum salt according to the molar ratio of various elements, and dissolving the lithium salt and the aluminum salt in water with a certain volume to obtain a clear and transparent solution;
(2) Slowly adding a certain amount of titanium salt into the solution in the step (1), stirring for a period of time, and adding a proper amount of citric acid to stabilize titanium ions until a clear and transparent solution is obtained;
(3) Under a certain coating proportion, a proper amount of high-nickel ternary positive electrode material LiNi is added x Co y Mn 1-x-y O 2 Wherein x is more than 0.8 and less than 1, and x + y is more than 0 and less than 1;
(4) Slowly adding an aqueous solution containing a proper amount of phosphate into the solution in the step (3), and stirring for a period of time;
(5) Carrying out suction filtration on the solution obtained in the step (4) to obtain a filter cake, and then drying the filter cake at a certain temperature;
(6) And (3) taking a proper amount of dried sample, and carrying out heat treatment at a certain temperature for a period of time to obtain the high-nickel ternary cathode material (marked as coated NCM) coated with the solid electrolyte.
Preferably, in the step (1), x1 is 0.1 to 0.9, more preferably 0.2 to 0.5, and most preferably 0.3.
Preferably, in the step (1), the lithium salt is LiNO 3 、CH 3 COOLi·2H 2 O、Li 2 CO 3 And LiOH, more preferably CH 3 COOLi·2H 2 O。
Preferably, in the step (1), the aluminum salt is Al (NO) 3 ) 3 ·9H 2 O、C 9 H 21 AlO 3 、Al(OH) 3 More preferably Al (NO) 3 ) 3 ·9H 2 O。
Preferably, in the step (2), the titanium salt is TiCl 4 、C 16 H 36 O 4 Ti、C 12 H 28 O 4 Any one of Ti, more preferably C 12 H 28 O 4 Ti。
Preferably, in the step (3), the solid electrolyte coating ratio is 0.1% to 10%, more preferably 0.5% to 5%, still more preferably 0.5% to 2%, and most preferably 1% by mass, and the coating ratio = the solid electrolyte Li in the step (1) 1+x1 Al x1 Ti 2-x1 (PO 4 ) 3 (LATP) mass/mass of the high-nickel ternary positive electrode material of step (3).
Preferably, in the step (3), the nickel content of the high-nickel ternary cathode material is x,0.80 < x ≦ 0.98, more preferably 0.85 ≦ x ≦ 0.9, and most preferably x =0.88.
Preferably, in the step (3), the high-nickel ternary cathode material is LiNi 0.88 Co 0.09 Mn 0.03 O 2 。
Preferably, in the step (4), the phosphate is H 3 PO 4 、(NH 4 ) 2 HPO 4 、NH 4 H 2 PO 4 、C 6 H 15 PO 4 More preferably NH 4 H 2 PO 4 。
Preferably, in the step (5), the drying temperature is 50 to 500 ℃, more preferably 100 to 200 ℃, and most preferably 120 ℃.
Preferably, in the step (6), the heat treatment temperature is 200 to 1000 ℃, more preferably 400 to 800 ℃, and most preferably 750 ℃.
In the step (6), the temperature increase rate during the heat treatment is preferably 1 to 20 ℃/min, more preferably 1 to 10 ℃/min, even more preferably 1 to 5 ℃/min, and most preferably 2 ℃/min.
Preferably, in the step (6), the heat treatment time is 1 to 24 hours, more preferably 2 to 10 hours, and most preferably 2 hours.
The modified high-specific-capacity high-nickel ternary cathode material is prepared by the preparation method of the modified high-specific-capacity high-nickel ternary cathode material.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention provides a preparation method of a modified high-specific-capacity high-nickel ternary cathode material, which is simple to operate, can finish coating operation in the washing process of the cathode material, and is beneficial to large-scale preparation of the high-specific-capacity high-nickel ternary cathode material;
(2) The invention provides a modified high-specific-capacity high-nickel ternary cathode material, which effectively improves the specific capacity of the high-nickel ternary cathode material by optimizing the coating proportion and the firing procedure on the premise of not changing the nickel content, and the improvement range of the specific capacity can reach 9.3 percent for the high-nickel ternary cathode material with specific nickel content (the nickel content is 88 percent).
Drawings
FIG. 1 is a scanning electron micrograph of a modified high specific capacity high nickel ternary positive electrode material of example 1;
FIG. 2 is a graph of the energy spectrum analysis of a modified high specific capacity high nickel ternary positive electrode material of example 1;
FIG. 3 is first round charge and discharge curves at 0.1C for the modified high-nickel ternary positive electrode material of example 1 and the modified high-nickel ternary positive electrode material of comparative example 1;
fig. 4 is a 100-cycle discharge cycle curve of the modified high-nickel ternary positive electrode material of example 1 and the modified high-nickel ternary positive electrode material of comparative example 1 under 0.5C charge and 1C discharge.
Detailed Description
For a better understanding of the present invention, reference is made to the following detailed description and accompanying drawings. It is to be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. In addition, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
Example 1
The coating of the high-nickel ternary cathode material is completed in a water washing process. According to the solid electrolyte Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 The ratio of the elements in (A) was measured and 0.38g of CH was weighed 3 COOLi·2H 2 O、0.3g Al(NO 3 ) 3 ·9H 2 O was dissolved in 35mL of water to give a clear and transparent solution. Then 1.33g of C 12 H 28 O 4 Ti was slowly added to the above solution, and after stirring for a period of time, 3g of citric acid was added to stabilize the titanium ions until a clear and transparent solution was obtained. Under the coating proportion of 1 percent, 100g of high nickel ternary cathode material LiNi with the nickel content of 88 percent is added 0.88 Co 0.09 Mn 0.03 O 2 . Then 65mL of the solution contained 0.9g of NH 4 H 2 PO 4 The aqueous solution of (2) was slowly added to the above solution, and stirred for 20min. And carrying out suction filtration on the mixed solution to obtain a filter cake, and then drying the filter cake at 120 ℃. And taking a proper amount of dried sample, raising the temperature to 750 ℃ at the heating rate of 2 ℃/min, and preserving the heat at 750 ℃ for 2h to obtain the high-nickel ternary cathode material (marked as coated NCM) coated with the solid electrolyte.
Comparative example 1
The preparation of the high-nickel ternary cathode material needs to be subjected to a water washing process to reduce surface residual lithium so as to improve specific capacity. 100g of nickel is added88% high nickel ternary positive electrode material LiNi 0.88 Co 0.09 Mn 0.03 O 2 And adding 100mL of water, stirring for the same time as in example 1, and filtering to obtain a high-nickel ternary cathode material filter cake. And drying the filter cake at 120 ℃ to obtain the water-washed high-nickel ternary cathode material (recorded as washed NCM). The material is used as a reference group to compare the performance with the modified high-nickel ternary cathode material in the example 1.
Effects of the embodiment
(1) Morphology characterization and energy spectrum analysis of modified high-nickel ternary cathode material
An electron microscope photograph (fig. 1, scale is 25 μm) of the high-nickel ternary cathode material after heat treatment in example 1 shows that the prepared modified high-nickel ternary cathode material has good sphericity, the particle size is 5-30 μm, and the surface is smooth. Energy spectrum analysis (figure 2, the scales are all 5 μm) shows that Al, ti and P elements are uniformly distributed on the surface of the secondary sphere, which suggests that LATP successfully coats the surface of the anode material, which is beneficial to reducing the contact area of the high-nickel ternary anode material and the electrolyte, and inhibiting the side reaction between the anode material and the electrolyte, thereby improving the electrochemical performance of the material.
(2) Electrochemical performance characterization of high-nickel ternary positive electrode material before and after modification
The high-nickel ternary positive electrode materials before and after modification are made into button cells, wherein the active substance, the conductive agent and the binder are = 90: 5 (mass ratio), the conductive agent is Super P, the binder is PVDF, and the electrolyte is 1M LiPF dissolved in a mixed solvent (volume ratio is 1: 1) of EC, DEC and DMC 6 The test voltage range is 2.8-4.3V. And testing a first round charge-discharge curve at 0.1C, wherein the cycle curve is obtained by charging at 0.5C and discharging at 1C.
The first round charging and discharging curve is shown in fig. 3. As can be seen from the dotted line in FIG. 3, the first round discharge specific capacity of the washed NCM material is 208.1mAh/g. The solid line in FIG. 3 shows that the specific capacity of the coated NCM material reaches 227.5mAh/g after a layer of solid electrolyte LATP is coated. Compared with the washed NCM, the specific capacity of the coated NCM is improved by 9.3 percent.
Fig. 4 is a 100-cycle performance curve of the positive electrode material before and after coating modification. As can be seen from the dotted line in the figure, the specific capacity of the washed NCM material after 100 circles is 151.2mAh/g, and the capacity retention rate is 78.3%. In contrast, the coated NCM material (solid line) had a specific capacity of 172.2mAh/g at 100 cycles and a capacity retention of 81.8%. After the solid electrolyte LATP is coated, the capacity retention rate of the high-nickel ternary material is obviously improved, which shows that the cycle performance of the material is effectively improved.
The increase in specific capacity and improvement in cycling performance can be attributed to the coating of the solid electrolyte LATP. This is probably because the coating of the LATP layer reduces the contact between the electrode material and the electrolyte, suppresses a side reaction between the two, and suppresses elution of transition metal ions. More importantly, the LATP has higher lithium ion conductivity, and is beneficial to the de-intercalation process of lithium ions. Finally, the electrochemical performance of the high-nickel cathode material is effectively improved.
The above description is not intended to limit the invention, nor is the invention limited to the examples set forth above. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.
Claims (8)
1. A preparation method of a modified high-specific-capacity high-nickel ternary cathode material is characterized by comprising the following steps of:
(1) According to the solid electrolyte Li 1+x1 Al x1 Ti 2-xl (PO 4 ) 3 Weighing appropriate amount of lithium salt and aluminum salt according to the molar ratio of various elements, and dissolving the lithium salt and the aluminum salt in water with a certain volume to obtain a clear and transparent solution;
(2) Slowly adding a certain amount of titanium salt into the solution in the step (1), stirring for a period of time, and adding a proper amount of citric acid to stabilize titanium ions until a clear and transparent solution is obtained;
(3) Under a certain coating proportion, a proper amount of high-nickel ternary positive electrode material LiNi is added x Co y Mn 1-x-y O 2 Wherein x is more than 0.8 and less than 1, and x + y is more than 0 and less than 1;
(4) Slowly adding an aqueous solution containing a proper amount of phosphate into the solution in the step (3), and stirring for a period of time;
(5) Carrying out suction filtration on the solution obtained in the step (4) to obtain a filter cake, and then drying the filter cake at a certain temperature;
(6) Taking a proper amount of dried sample, and carrying out heat treatment at a certain temperature for a period of time to obtain a high-nickel ternary positive electrode material coated with a solid electrolyte;
in the step (3), the coating proportion of the solid electrolyte is 0.5-5% by mass;
in the step (3), the nickel content of the high-nickel ternary cathode material is x, and x is more than or equal to 0.85 and less than or equal to 0.9.
2. The method for preparing the modified ternary positive electrode material with high specific capacity and high nickel content according to claim 1, wherein in the step (1), x1 is 0.1-0.9.
3. The method for preparing the modified ternary positive electrode material with high specific capacity and high nickel content according to claim 1, wherein in the step (1), the lithium salt is LiNO 3 、CH 3 COOLi·2H 2 O、Li 2 CO 3 And LiOH.
4. The method of claim 1, wherein in step (1), the aluminum salt is Al (NO) 3 ) 3 ·9H 2 O、C 9 H 21 AlO 3 、Al(OH) 3 Any one of them.
5. The method for preparing the modified ternary cathode material with high specific capacity and high nickel content according to claim 1, wherein in the step (2), the titanium salt is TiCl 4 、C 16 H 36 O 4 Ti、C 12 H 28 O 4 Any one of Ti.
6. The method of claim 1, wherein the modified ternary positive electrode material with high specific capacity and high nickel content, it is characterized in that the preparation method is characterized in that,in the step (4), the phosphate is H 3 PO 4 、(NH 4 ) 2 HPO 4 、NH 4 H 2 PO 4 、C 6 H 15 PO 4 Any one of them.
7. The method for preparing the modified ternary positive electrode material with high specific capacity and high nickel content according to claim 1, wherein in the step (6), the heat treatment temperature is 200-1000 ℃.
8. The modified high-specific-capacity high-nickel ternary cathode material is characterized by being prepared by the preparation method of the modified high-specific-capacity high-nickel ternary cathode material according to any one of claims 1 to 7.
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| CN113113588B (en) * | 2021-04-09 | 2022-11-08 | 合肥工业大学 | Method for preparing lithium fast ion conductor material coated high-nickel ternary layered oxide by using covalent interface engineering strategy |
| CN114551819B (en) * | 2021-07-16 | 2023-06-09 | 万向一二三股份公司 | LATP/high nickel composite positive electrode material, positive electrode plate and battery |
| CN116031386A (en) * | 2023-01-31 | 2023-04-28 | 重庆长安新能源汽车科技有限公司 | Lithium ion battery anode material, lithium ion battery and preparation method |
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