A high-nickel large-particle ternary precursor and preparation method thereof
By using high-nickel large-particle ternary precursors in ternary lithium-ion batteries, using ammonia-free nuclear-making and air oxidation technology, the problem of difficulty in simultaneously improving tap density and specific surface area in the prior art is solved, and a positive electrode material with high electrochemical performance is achieved.
Patent Information
- Application Number
- CN202310148340.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-02-21
- Publication Date
- 2025-03-07
- Estimated Expiration
- 2043-02-21
AI Technical Summary
The prior art is difficult to simultaneously increase the tap density and specific surface area of ternary lithium-ion batteries, resulting in uneven structure of the positive electrode material and affecting electrochemical performance.
A high-nickel large-particle ternary precursor is adopted, with its primary particles slender and secondary particles loose and porous. Through ammonia-free nuclear production process and air oxidation technology, the reaction conditions are controlled to improve the specific surface area and tap density of the particles.
A high-nickel large-particle ternary precursor with high specific surface area and high tap density is realized, which improves the electrochemical performance of the positive electrode material, avoids agglomeration, and improves the spherical degree and morphological characteristics of the molding.
Smart Images

Figure HDA0004089941260000011 
Figure HDA0004089941260000012 
Figure HDA0004089941260000013
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of lithium ion batteries, and in particular to a high-nickel large-particle ternary precursor and a preparation method thereof. Background Art
[0002] Lithium-ion batteries are widely used in electric vehicles, power tools, 3C and other fields due to their advantages such as stable voltage, high capacity, high energy density, low self-discharge, stable cycle, low consumption and environmental friendliness. With the development of science and technology, the energy density and safety requirements of batteries are getting higher and higher. Ternary materials have high reversible specific capacity and can better meet the requirements of increasingly miniaturized and multifunctional electronic products. The physical and chemical indicators of ternary precursors such as morphology, particle size, specific surface area and tap density largely determine the performance of ternary positive electrode materials.
[0003] In actual production, the co-precipitation method is used to prepare a continuous ternary precursor. Due to its wide particle size distribution, it can increase the compaction density of the positive electrode material to a certain extent and improve the physical and chemical indicators and electrical performance indicators of subsequent products.
[0004] In order to improve the energy density and charge-discharge performance of ternary lithium-ion batteries, the ternary precursor materials need to have both high tap density (TD) and high specific surface area (BET). In order to simultaneously improve the tap density and specific surface area, the primary particles need to be refined to a large extent. The current common process for continuous large particles with a D50 of 14-16μm, TD is generally 1.5-2.0g / cm 3 , and BET is unlikely to exceed 20m 2 / g, and is limited by the current continuous preparation solid content, as well as the process characteristics of feeding and discharging at the same time, which will lead to uneven particle structure and easily form "annual rings", affecting the consistency of the precursor structure, thereby reducing the structural stability of the positive electrode material, and ultimately affecting the physical and chemical indicators and electrical performance indicators of the product. Summary of the invention
[0005] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a high-nickel large-particle ternary precursor and a preparation method thereof. The high-nickel large-particle ternary precursor has a large specific surface area, a high tap density, and slender primary particles with small size, loose and porous secondary particles, and high overall consistency. When preparing positive electrode materials, it can effectively improve the electrochemical properties of positive electrode materials.
[0006] To this end, in the first aspect of the present invention, the present invention proposes a high-nickel large-particle ternary precursor, the chemical formula of which is Ni x Co y Mn (1-x-y) (OH)2, where 0.90≤x<0.98, 0 <y<0.05;
[0007] The primary particles of the high-nickel large-particle ternary precursor are slender, and the secondary particles are loose and porous, wherein the length of the primary particles is ≥600nm, and the diameter of the primary particles is ≤31nm.
[0008] In one embodiment, the D50 of the high nickel large particle ternary precursor is 14-16 μm, and the specific surface area is 23-40 m 2 / g, tap density is 1.7~2.1g / cm 3 .
[0009] In a second aspect of the present invention, the present invention provides a method for preparing a high-nickel large-particle ternary precursor, comprising the following steps:
[0010] (1) preparing a metal salt solution, alkali solution and ammonia solution containing nickel, cobalt and manganese;
[0011] (2) adding water to the reaction kettle, adding alkali solution to adjust the pH to 10.5-11.0, and obtaining a reaction bottom solution;
[0012] (3) Adding the metal salt solution and the alkali solution into the reactor to carry out the coprecipitation reaction for 4 to 6 hours, then adding the ammonia solution, controlling the ammonia concentration of the system to be 0.5 to 1.5 g / L, and reacting until the D50 of the material in the reactor is maintained at 14 μm and the particle size is stable, collecting the overflowed material, aging, washing, and drying, and obtaining a high-nickel large-particle ternary precursor;
[0013] Air was introduced during the entire reaction process;
[0014] During the entire reaction process, the reactor is connected to the thickener, and the thickener is used to consolidate the material in the reactor.
[0015] In one embodiment, the metal ion concentration in the metal salt solution is 100-120 g / L, and the molar ratio of the three elements of nickel, cobalt and manganese is nickel: cobalt: manganese = x: y: (100-xy), where 90≤x<98, 0 <y<5。
[0016] In one embodiment, the alkali solution is a 6-12 mol / L sodium hydroxide solution;
[0017] The molar concentration of the ammonia solution is 0.3-1 mol / L.
[0018] In one of the embodiments, the feed rate of the metal salt solution is 500-1000 L / h;
[0019] The feed rate of the alkali solution in step (2) is 150-400 L / h.
[0020] In one of the embodiments, the feed rate of the ammonia water is 10 to 100 L / h;
[0021] The air inlet flow rate is 50 to 500 L / h.
[0022] In one embodiment, the ratio of the metal salt solution feed rate to the air intake is 1:(0.0.5-1);
[0023] The ratio of the metal salt solution feed rate to the concentrator clearing rate is 1:(0.1-0.8).
[0024] The beneficial effects of the present invention are as follows: (1) the high-nickel large-particle ternary precursor described in the present invention has a large specific surface area, a high tap density, and the primary particles are slender and small in size, the secondary particles are loose and porous, and the overall consistency is high. When preparing positive electrode materials, the electrochemical properties of the positive electrode materials can be effectively improved; (2) the present invention can effectively increase the nucleation reaction rate and the number of nuclei through an ammonia-free nucleation process, and can effectively avoid the occurrence of agglomeration through friction between particles and stirring of the reactor, effectively reduce the particle size, improve the sphericity of the later forming, and effectively reduce the size of the primary particles, which is beneficial to the sphericity and morphological characteristics. The invention inherits the characteristics of the reaction and increases the specific surface area; (3) The invention reduces the reaction nucleation point by introducing air oxidation, and further reduces the nucleation point by controlling the lower ammonia concentration, so the pH of the entire reaction process can be stabilized at a lower level, and air oxidation and extremely low pH and extremely low ammonia concentration are beneficial to the refinement and uniformity of the primary particles, thereby facilitating the preparation of a high-nickel large-particle ternary precursor with slender primary particles, small size, and high overall consistency; (4) The invention introduces a thickener into the continuous type to improve the problem of limited solid content in the traditional continuous type, and accurately regulates the solid content of the reaction system by controlling the thickener clearing rate. Since the primary particles of the particle growth will preferentially precipitate and grow at the previous pore position, a relatively high solid content is beneficial to reducing the surface pores, thereby reducing the size of the primary particles, thereby obtaining a continuous ternary precursor with high tap density and large specific surface area. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 This is the SEM image of the precursor prepared in Example 1.
[0026] Figure 2 This is the SEM image of the precursor prepared in Example 2.
[0027] Figure 3 This is the SEM image of the precursor prepared in Comparative Example 1.
[0028] Figure 4 This is the SEM image of the precursor prepared in Comparative Example 2.
[0029] Figure 5 This is the SEM image of the precursor prepared in Comparative Example 3. DETAILED DESCRIPTION
[0030] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0031] In the present invention, there is no particular limitation on the specific dispersion and stirring treatment methods.
[0032] The reagents or instruments used in the present invention without indicating the manufacturer are all conventional products that can be obtained through commercial purchase.
[0033] The present invention provides a high-nickel large-particle ternary precursor, the chemical formula of which is Ni x Co y Mn (1-x-y) (OH)2, where 0.90≤x<0.98, 0 <y<0.05;
[0034] The primary particles of the high-nickel large-particle ternary precursor are slender, and the secondary particles are loose and porous, wherein the length of the primary particles is ≥600nm, and the diameter of the primary particles is ≤31nm.
[0035] In some specific examples, the D50 of the high-nickel large-particle ternary precursor is 14-16 μm, and the specific surface area is 23-40 m 2 / g, tap density is 1.7~2.1g / cm 3 .
[0036] In some specific examples, the primary particles of the high-nickel large-particle ternary precursor are slender, and the secondary particles are loose and porous.
[0037] The high-nickel large-particle ternary precursor described in the present invention has a large specific surface area, a high tap density, and slender primary particles with small size, loose and porous secondary particles, and high overall consistency. When preparing positive electrode materials, it can effectively improve the electrochemical performance of positive electrode materials.
[0038] In a second aspect of the present invention, the present invention provides a method for preparing a high-nickel large-particle ternary precursor, comprising the following steps:
[0039] (1) preparing a metal salt solution, alkali solution and ammonia solution containing nickel, cobalt and manganese;
[0040] (2) adding water to the reaction kettle, adding alkali solution to adjust the pH to 10.5-11.0, and obtaining a reaction bottom solution;
[0041] (3) Adding the metal salt solution and the alkali solution into the reactor to carry out the coprecipitation reaction for 4 to 6 hours, then adding the ammonia solution, controlling the ammonia concentration of the system to be 0.5 to 1.5 g / L, and reacting until the D50 of the material in the reactor is maintained at 14 μm and the particle size is stable, collecting the overflowed material, aging, washing, and drying, and obtaining a high-nickel large-particle ternary precursor;
[0042] Air was introduced during the entire reaction process;
[0043] During the entire reaction process, the reactor is connected to the thickener, and the thickener is used to consolidate the material in the reactor.
[0044] The inventors of the present invention have found through extensive research that the present invention can effectively increase the nucleation reaction rate and the number of nuclei through an ammonia-free nucleation process, and can effectively avoid the occurrence of agglomeration through friction between particles and stirring of the reactor, effectively reduce the particle size, improve the sphericity of later molding, and effectively reduce the size of primary particles, which is beneficial to the inheritance of sphericity and morphological characteristics and increases the specific surface area.
[0045] It should be noted that in the present invention, the reactor and thickener used are conventional equipment in the art.
[0046] The present invention reduces the reaction nucleation point by introducing air for oxidation, and further reduces the nucleation point by controlling a relatively low ammonia concentration, so that the pH value of the entire reaction process can be stabilized at a relatively low level. Air oxidation, extremely low pH value, and extremely low ammonia concentration are all beneficial to the refinement of primary particles and the improvement of uniformity, thereby facilitating the preparation of a high-nickel large-particle ternary precursor with slender primary particles, small size, and high overall consistency.
[0047] The volume flowing out of the reactor is equal to the volume flowing in, that is, the clearing volume + the overflow volume = the feed volume. By controlling the clearing rate of the concentrator, the solid content in the reactor can be accurately increased on the basis of the traditional continuous type, making the sphericity better and the primary particles smaller.
[0048] In one embodiment, the metal ion concentration in the metal salt solution is 100-120 g / L, and the molar ratio of the three elements of nickel, cobalt and manganese is nickel: cobalt: manganese = x: y: (100-xy), where 90≤x<98, 0 <y<5。
[0049] In one embodiment, the alkali solution is a 6-12 mol / L sodium hydroxide solution;
[0050] The molar concentration of the ammonia solution is 0.3-1 mol / L.
[0051] In one of the embodiments, the feed rate of the metal salt solution is 500-1000 L / h;
[0052] The feed rate of the alkali solution in step (2) is 150-400 L / h.
[0053] In one of the embodiments, the feed rate of the ammonia water is 10 to 100 L / h;
[0054] The air inlet flow rate is 50 to 500 L / h.
[0055] By controlling the feed rates of ammonia water and oxidant and the flow rate of air within the above range, a high-nickel large-particle ternary precursor with slender primary particles, small size and high overall consistency can be effectively prepared.
[0056] In one embodiment, the ratio of the metal salt solution feed rate to the air intake is 1:(0.05-1);
[0057] The ratio of the metal salt solution feed rate to the concentrator clearing rate is 1:(0.1-0.8).
[0058] Example 1
[0059] A method for preparing a high-nickel large-particle ternary precursor comprises the following steps:
[0060] (1) nickel sulfate, cobalt sulfate and manganese sulfate are prepared into a sulfate solution with a total metal ion concentration of 115 g / L according to the ratio of nickel ion: cobalt ion: manganese ion = 93:3:4, a 10 mol / L sodium hydroxide solution is used as an alkali solution, and the molar concentration of an ammonia solution is 0.5 mol / L;
[0061] (2) adding water to the reactor, adding alkali solution to adjust the pH to 10.8, obtaining a reaction bottom solution, heating to 60°C, adding the metal salt solution at a feeding rate of 800 L / h and the alkali solution at a feeding rate of 300 L / h to the reactor, stirring at a speed of 300 rpm, and performing a coprecipitation reaction for 5 hours. After reacting for 5 hours, adding an ammonia solution, controlling the ammonia concentration of the system to be 1.0±0.5 g / L, continuing the reaction, adjusting the pH to maintain the D50 of the material in the reactor at 14 μm, and after the particle size is stable, collecting and post-processing the overflowed material, and obtaining a high-nickel large-particle ternary precursor after aging, washing, and drying;
[0062] (3) During the entire reaction process, air was continuously introduced at a flow rate of 50 L / h to oxidize the material;
[0063] During the entire reaction process, the reactor was connected to the thickener, through which the material in the reactor was consolidated, and the thickener clearing rate was controlled to be 480L / h.
[0064] The ratio of the metal salt solution feed rate to the thickener clearing rate is 1:0.6.
[0065] Example 2
[0066] A method for preparing a high-nickel large-particle ternary precursor comprises the following steps:
[0067] (1) nickel sulfate, cobalt sulfate and manganese sulfate are prepared into a sulfate solution with a total metal ion concentration of 115 g / L according to the ratio of nickel ion: cobalt ion: manganese ion = 93:3:4, a 10 mol / L sodium hydroxide solution is used as an alkali solution, and the molar concentration of an ammonia solution is 0.5 mol / L;
[0068] (2) adding water to the reactor, adding alkali solution to adjust the pH to 10.8, obtaining a reaction bottom solution, heating to 60°C, adding the metal salt solution at a feeding rate of 800 L / h and the alkali solution at a feeding rate of 300 L / h to the reactor, stirring at a speed of 300 rpm, and performing a coprecipitation reaction for 5 hours. After reacting for 5 hours, adding an ammonia solution, controlling the ammonia concentration of the system to be 1.0±0.5 g / L, continuing the reaction, adjusting the pH to maintain the D50 of the material in the reactor at 14 μm, and after the particle size is stable, collecting and post-processing the overflowed material, and obtaining a high-nickel large-particle ternary precursor after aging, washing, and drying;
[0069] (3) During the entire reaction process, air was continuously introduced at a flow rate of 500 L / h to oxidize the material;
[0070] During the entire reaction process, the reactor was connected to the thickener, through which the material in the reactor was consolidated, and the thickener clearing rate was controlled to be 480L / h.
[0071] The ratio of the metal salt solution feed rate to the thickener clearing rate is 1:0.6.
[0072] Comparative Example 1
[0073] A method for preparing a high-nickel large-particle ternary precursor comprises the following steps:
[0074] (1) nickel sulfate, cobalt sulfate and manganese sulfate are prepared into a sulfate solution with a total metal ion concentration of 115 g / L according to the ratio of nickel ion: cobalt ion: manganese ion = 93:3:4, a 10 mol / L sodium hydroxide solution is used as an alkali solution, and the molar concentration of an ammonia solution is 0.5 mol / L;
[0075] (2) adding water to the reactor, adding alkali solution to adjust the pH to 10.8, obtaining a reaction bottom solution, heating to 60° C., adding a metal salt solution at 800 L / h and an alkali solution at 300 L / h to the reactor, and adding ammonia water at the same time, controlling the ammonia concentration of the reaction system to 1.0±0.5 g / L, stirring at 300 rpm, adjusting the pH to maintain the D50 of the material in the reactor at 14 μm, collecting and post-processing the overflowed material after the particle size is stable, collecting the overflowed material, aging, washing, and drying, and obtaining a high-nickel large-particle ternary precursor;
[0076] (3) During the entire reaction process, air was continuously introduced at a flow rate of 400 L / h to oxidize the material;
[0077] During the entire reaction process, the reactor was connected to the thickener, through which the material in the reactor was consolidated, and the thickener clearing rate was controlled to be 480L / h.
[0078] The ratio of the metal salt solution feed rate to the thickener clearing rate is 1:0.6.
[0079] Comparative Example 2
[0080] A method for preparing a high-nickel large-particle ternary precursor comprises the following steps:
[0081] (1) nickel sulfate, cobalt sulfate and manganese sulfate are prepared into a sulfate solution with a total metal ion concentration of 115 g / L according to the ratio of nickel ion: cobalt ion: manganese ion = 93:3:4, a 10 mol / L sodium hydroxide solution is used as an alkali solution, and the molar concentration of an ammonia solution is 0.5 mol / L;
[0082] (2) adding water to the reactor, adding alkali solution to adjust the pH to 10.8, obtaining a reaction bottom solution, heating to 60°C, adding the metal salt solution at a feeding rate of 800 L / h and the alkali solution at a feeding rate of 300 L / h to the reactor, stirring at a speed of 300 rpm, and performing a coprecipitation reaction for 5 hours. After reacting for 5 hours, adding an ammonia solution, controlling the ammonia concentration of the system to be 1.0±0.5 g / L, continuing the reaction, adjusting the pH to maintain the D50 of the material in the reactor at 14 μm, and after the particle size is stable, collecting and post-processing the overflowed material, collecting the overflowed material, aging, washing, and drying, and obtaining a high-nickel large-particle ternary precursor;
[0083] During the entire reaction process, the reactor was connected to the thickener, through which the material in the reactor was consolidated, and the thickener clearing rate was controlled to be 480L / h.
[0084] The ratio of the metal salt solution feed rate to the thickener clearing rate is 1:0.6.
[0085] Comparative Example 3
[0086] A method for preparing a high-nickel large-particle ternary precursor comprises the following steps:
[0087] (1) nickel sulfate, cobalt sulfate and manganese sulfate are prepared into a sulfate solution with a total metal ion concentration of 115 g / L according to the ratio of nickel ion: cobalt ion: manganese ion = 93:3:4, a 10 mol / L sodium hydroxide solution is used as an alkali solution, and the molar concentration of an ammonia solution is 0.5 mol / L;
[0088] (2) adding water to the reactor, adding alkali solution to adjust the pH to 10.8, obtaining a reaction bottom solution, heating to 60°C, adding the metal salt solution at a feeding rate of 800 L / h and the alkali solution at a feeding rate of 300 L / h to the reactor, stirring at a speed of 300 rpm, and performing a coprecipitation reaction for 5 hours. After reacting for 5 hours, adding an ammonia solution, controlling the ammonia concentration of the system to be 1.0±0.5 g / L, continuing the reaction, adjusting the pH to maintain the D50 of the material in the reactor at 14 μm, and after the particle size is stable, collecting and post-processing the overflow material, aging, washing, and drying the collected overflow material to obtain a high-nickel large-particle ternary precursor;
[0089] During the entire reaction process, air was continuously introduced at a flow rate of 400 L / h to oxidize the material.
[0090] Test Example 1
[0091] The scanning electron microscope (SEM) images of Examples 1 to 2 and Comparative Examples 1 to 3 are shown as follows: Figures 1 to 5 As shown, the masses of the precursors described in Examples 1 to 2 and Comparative Examples 1 to 3 are shown in Table 1, wherein the specific surface area is tested using a BET tester of type 3H-2000PS2; the tap density is tested using a Rico FT-100A tap density meter; and the D50 and Dmax data are tested using a Malvern laser particle size analyzer 3000.
[0092] Table 1
[0093] Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Primary particle length nm 600 850 1200 1700 1800 Primary particle diameter nm 23 31 80 230 70 <![CDATA[Specific surface area m 2 / g]]> 35.4 27.6 14.7 8.7 9.5 <![CDATA[Tap density g / cm 3 > 1.81 1.76 1.78 1.88 1.45 D50μm 14.27 14.31 14.05 14.06 14.11
[0094] From Table 1 and Figures 1 to 5 It can be seen that the primary particle size of the nickel-cobalt-manganese ternary precursor prepared by the present invention is small; the primary particle size of the nickel-cobalt-manganese ternary precursor prepared in the comparative example is large and thick in diameter.
[0095] Examples 1 and 2 are prepared by the test method of the present invention. The obtained primary particles are short, thin, and densely distributed, but there are fine pores between the particles, so BET is significantly improved, and TD does not decrease. Through the cross-sectional electron microscope, it can be found that the internal pores are small and uniform. Compared with Example 1, Example 2 has a stronger degree of oxidation, so Example 2 has a lower nucleation point, resulting in its primary particles being longer, and the gaps between the primary particles are increased, and BET is slightly lower than Example 1.
[0096] In Comparative Example 1, since ammonia water was introduced throughout the entire reaction process and an ammonia environment was used for nucleation, its sphericity was slightly poor, and due to morphological inheritance, the primary particle size inherited the elongated and coarse morphological characteristics produced by the ammonia conditions, resulting in a decrease in BET. However, since the later process was similar to the embodiment, small and uniform pores could be observed in the overall structure. Therefore, although BET decreased, it was still at a relatively high level. In Comparative Example 2, since oxidation was not used in the process, it can be seen that the primary particles became significantly coarser, and the cross-sectional electron microscope also showed that its internal structure was denser and had very few pores. In Comparative Example 3, since the thickener was not used for consolidation, the density of the particles was reduced, and it can be seen that the surface pores were extremely large, and the number of primary particles on the surface was reduced, resulting in a decrease in its BET. At the same time, observation of its cross-sectional electron microscope showed that its internal structure was consistent with the surface, both of which were extremely loose and had large pores, so its TD was relatively low.
[0097] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.
Claims
1. A high-nickel large-particle ternary precursor, characterized in that: The chemical formula is Ni x Co y Mn (1-x-y) (OH)2, where 0.90≤x<0.98, 0 <y<0.05; The primary particles of the high-nickel large-particle ternary precursor are slender, and the secondary particles are loose and porous, wherein the length of the primary particles is ≥600nm, and the diameter of the primary particles is ≤31nm; The D50 of the high-nickel large-particle ternary precursor is 14-16 μm, and the specific surface area is 23-40 m 2 / g.
2. The high-nickel large-particle ternary precursor according to claim 1, characterized in that: The tap density of the high-nickel large-particle ternary precursor is 1.7 to 2.1 g / cm 3 .
3. A method for preparing a high-nickel large-particle ternary precursor, characterized in that: The following steps are involved: (1) preparing a metal salt solution, alkali solution and ammonia solution containing nickel, cobalt and manganese; (2) adding water to the reaction kettle, adding alkali solution to adjust the pH to 10.5-11.0, and obtaining a reaction bottom solution; (3) Adding the metal salt solution and the alkali solution into the reactor to carry out the coprecipitation reaction for 4 to 6 hours, then adding the ammonia solution, controlling the ammonia concentration of the system to be 0.5 to 1.5 g / L, and reacting until the D50 of the material in the reactor is maintained at 14 μm and the particle size is stable, collecting the overflowed material, aging, washing, and drying, and obtaining a high-nickel large-particle ternary precursor; Air was introduced during the entire reaction process; During the entire reaction process, the reactor is connected to the thickener, and the thickener is used to consolidate the material in the reactor.
4. The method for preparing a high-nickel large-particle ternary precursor according to claim 3, characterized in that: The metal ion concentration in the metal salt solution is 100-120 g / L, and the molar ratio of the three elements of nickel, cobalt and manganese is nickel:cobalt:manganese=x:y:(100-xy), wherein 90≤x<98, 0 <y<5。 5. The method for preparing a high-nickel large-particle ternary precursor according to claim 3, characterized in that: The alkali solution is a 6-12 mol / L sodium hydroxide solution; The molar concentration of the ammonia solution is 0.3-1 mol / L.
6. The method for preparing a high-nickel large-particle ternary precursor according to claim 3, characterized in that: The feed rate of the metal salt solution is 500-1000 L / h; The feed rate of the alkali solution in step (2) is 150-400 L / h.
7. The method for preparing a high-nickel large-particle ternary precursor according to claim 3, characterized in that: The feed rate of the ammonia water is 10 to 100 L / h.
8. The method for preparing a high-nickel large-particle ternary precursor according to claim 3, characterized in that: The air inlet flow rate is 50 to 500 L / h.
9. The method for preparing a high-nickel large-particle ternary precursor according to claim 3, characterized in that: The ratio of the metal salt solution feeding speed to the air introduction amount is 1:(0.05-1).
10. The method for preparing a high-nickel large-particle ternary precursor according to claim 3, characterized in that: The ratio of the metal salt solution feed rate to the concentrator clearing rate is 1:(0.1-0.8).
Citation Information
Patent Citations
Nickel-cobalt-manganese ternary precursor with narrow particle size distribution and small particle size, preparation method of nickel-cobalt-manganese ternary precursor and lithium ion battery
CN115353157A