CN114261996B - Preparation method and application of single crystal high nickel ternary material with completely modified surface - Google Patents
Preparation method and application of single crystal high nickel ternary material with completely modified surface Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a single crystal high nickel ternary material with completely modified surface, wherein the method is to synthesize the single crystal high nickel ternary material by adopting a high temperature solid phase method, and then realize M on the surface of a single crystal high nickel ternary positive electrode material by adopting oxidation-reduction reaction and complexation reaction x B y And (3) complete modification. The method has simple and reliable process and low cost, can improve the material circulation performance and the internal resistance of the material, and the prepared monocrystal high-nickel ternary material has good electrochemical performance, is suitable for industrial production, and has good development prospect in the field of power batteries, particularly in the application of battery anode materials.
Description
Technical Field
The invention relates to a new energy material technology, in particular to a preparation method and application of a single crystal high nickel ternary material with a completely modified surface.
Background
With the development of new energy technologies, advanced cathode materials having excellent discharge capacity and good stability are urgently needed to meet the increasing demand for high energy density Lithium Ion Batteries (LIBs). Among them, the high nickel ternary cathode material is considered to be an ideal cathode material because of its high specific capacity, better electrochemical properties and environmental friendliness.
The most widely studied high nickel ternary positive electrode material is formed by agglomeration of small-grain crystals. However, the presence of grain boundaries in the primary particles limits Li + This makes it difficult for the high nickel ternary cathode material to fully exploit its high volumetric energy density advantages. In addition, a series of phase changes may occur during charge and discharge, resulting in severe lattice distortion and formation of microcracks. Microcracks act as a major factor in capacity fade and can cause significant changes in interface chemistry, for example, the formation of microcracks can lead to destruction of the initially formed solid electrolyte interface film, resulting in more active material exposure, further accelerating interface side reactions, and in addition, lithium ion diffusion resistance will increase due to impaired diffusion pathways. The submicron particle size single crystal high nickel ternary cathode material can well avoid the problem of polycrystalline particles, and single crystal particles can effectively reduce the formation of microcracks and maintain structural integrity due to uniform stress distribution and good structural stability, and unfortunately, the high specific surface area of the single crystal material makes side reactions at the electrode/electrolyte interface severe, resulting in low coulombic efficiency and dissolution of transition metals into the organic electrolyte.
Surface modification is a widely used method to improve the stability of high nickel ternary cathode materials, and although surface modification layers with high stability and catalytic inertness are helpful, it is often difficult to achieve 100% coverage in the synthesis due to solid-to-solid wetting problems and the need to maintain shape during electrochemical cycling. The Atomic Layer Deposition (ALD) is a method for uniformly and 100% modification of the surface of the currently known high-nickel ternary cathode material, but the atomic layer deposition requires high-end technical equipment, special raw materials, has high cost, and cannot realize industrial production. How to realize the complete surface modification of the monocrystal high-nickel ternary material by using a simple method is a challenge to be solved.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and provides a preparation method and application of a single crystal high nickel ternary material with completely modified surface. The method has simple and reliable process and low cost, can improve the material circulation performance and the internal resistance of the material, and the prepared monocrystal high-nickel ternary material has good electrochemical performance, is suitable for industrial production, and has good development prospect in the field of power batteries, particularly in the application of battery anode materials.
The technical scheme for realizing the aim of the invention is as follows:
a preparation method of a single crystal high nickel ternary material with a completely modified surface comprises the following steps:
1) Uniformly mixing the high-nickel ternary precursor and a lithium source according to the molar ratio of the lithium source to the high-nickel ternary precursor of 1.0-1.06 to obtain a mixture, wherein the mixing speed is 200r/min-300r/min, and the mixing time is 30min-120min;
2) Calcining the mixture obtained in the step 1) in an oxygen atmosphere to obtain a monocrystal high-nickel ternary material matrix, wherein the oxygen concentration in the oxygen atmosphere is higher than 99.9%, the calcining temperature and the calcining time are kept at 450-480 ℃ for 5h, and the calcining temperature is kept at 750-900 ℃ for 15-h;
3) Crushing and sieving the base material obtained in the step 2) to obtain monocrystal particles of the monocrystal high-nickel ternary material with uniformly dispersed particle sizes, wherein a sieving screen is 300-500 meshes, and the particle size of the crushed monocrystal particles of the monocrystal high-nickel ternary material is 2um-3.5um;
4) Dispersing single crystal high nickel ternary material single crystal particles obtained in the step 3) in a material containing M x (NO 3 ) y Or M x Cl y Slowly stirring at room temperature under inert gas condition for 1. 1h, and then adding MBH with concentration of 0.078-M-0.1M 4 Slowly dripping ethanol solution with the acceleration of 2ml/min-30ml/min into the mixed solution, slowly stirring for 2h after dripping, and mixing the mixed solutionFiltering the solution, and drying the obtained filter residue, wherein the monocrystal high-nickel ternary material and M x (NO 3 ) y Or M x Cl y The mass ratio of the ethanol solution is 1:10-50, M x (NO 3 ) y Or M x Cl y The concentration of the ethanol solution is 0.009M-0.02M, M x B y The addition amount of the surface modification layer is 0.5-5% of the mass of the monocrystal high-nickel ternary material matrix, the stirring speed is 20r/min-100r/min, the stirring time is 1h-3h, the drying temperature is 80-120 ℃, and the drying time is 12h;
5) Calcining the filter residue obtained in the step 4) under the protection of inert gas to obtain the single crystal high nickel ternary material with the surface completely modified, wherein the calcining temperature and the calcining time are kept at 500 ℃ for 120min, and the atmosphere is one or more of argon or nitrogen.
The monocrystal high-nickel ternary precursor in the step 1) is nickel cobalt manganese or nickel cobalt aluminum hydroxide, and the molecular formula is Ni x Co y M 1-x-y (OH) 2 Wherein x=0.65-0.95 and y=0.01-0.2.
The lithium source in the step 1) is one or more of lithium hydroxide or lithium carbonate.
M as described in step 4) x (NO 3 ) y Is Mg (NO) 3 ) 2 、Co(NO 3 ) 3 、Mn(NO 3 ) 4 、Fe(NO 3 ) 2 、Al(NO 3 ) 3 、Ca(NO 3 ) 2 One or more of the following.
M as described in step 4) x Cl y Is TiCl 4 、MgCl 2 One or more of the following.
MBH as described in step 4) 4 Is one or more of sodium borohydride or potassium borohydride or lithium borohydride.
M as described in step 4) x B y Is MgB 2 Or ZrB 2 Or CaB 6 Or TiB 2 Or CrB 2 Or AlB 2 Or Co 2 B.
The surface-completely-modified single-crystal high-nickel ternary material prepared by the preparation method of the surface-completely-modified single-crystal high-nickel ternary material.
The monocrystalline high-nickel ternary material with the completely modified surface is applied to the anode material of the lithium ion battery.
The technical scheme firstly prepares the monocrystal high-nickel ternary material with uniform particle size distribution, then uses a simple liquid-solution method to construct a monocrystal high-nickel ternary positive electrode material coating with uniform surface and 100% modification by adopting reactive wetting with a reductive active material, and the monocrystal high-nickel ternary positive electrode material with completely modified surface can remarkably improve the cycle performance and the multiplying power performance, and the positive electrode material has the advantages of low manufacturing cost, simple process flow and easy realization of industrial production, and adopts M in the technical scheme x B y The surface modification layer can inhibit the generation of microcracks and reduce side reactions, so that the material cycle performance is improved, and the material has good development prospect in the field of power batteries.
The method has simple and reliable process and low cost, can improve the material circulation performance and the internal resistance of the material, and the prepared monocrystal high-nickel ternary material has good electrochemical performance, is suitable for industrial production, and has good development prospect in the field of power batteries, particularly in the application of battery anode materials.
Drawings
FIG. 1 is an SEM image of a ternary nickel cobalt manganese single crystal material of example 1 and comparative example 1;
FIG. 2 is a graph showing the rate performance of the nickel cobalt manganese single crystal ternary materials of example 1 and comparative example 1;
FIG. 3 is a graph showing the cycle performance of the nickel cobalt manganese single crystal ternary materials of example 1 and comparative example 1.
Detailed Description
The present invention will now be further illustrated with reference to the drawings and examples, but is not limited thereto.
Example 1:
MgB (MgB) 2 The preparation method of the single crystal high nickel ternary material with the completely modified surface comprises the following steps:
1) Weigh 200 g Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Then according to the lithium source: the molar ratio of the ternary precursor is 1.05, lithium hydroxide is weighed, then the lithium hydroxide is put into a mixer for uniform mixing, the uniformly mixed mixture is put into an atmosphere furnace which is pre-ventilated with oxygen, a calcination procedure is set, firstly, the temperature is kept at 480 ℃ for 5h, then the temperature is kept at 750 ℃ for 15h, and the heating rate is 5 ℃/min;
2) Crushing the high-nickel ternary material obtained in the step 1), and then sieving the crushed high-nickel ternary material with a 400-mesh screen to obtain a monocrystal high-nickel ternary material with uniformly dispersed particle size;
3) Weighing 100 g of the monocrystal high-nickel ternary material obtained in the step 2), adding the monocrystal high-nickel ternary material into a vacuum stirring reaction kettle of 5L, and adding 2L and 0.009M of Mg (NO) 3 ) 2 Slowly stirring 1. 1h, introducing inert gas into the solution to remove air, and adding 50 ml of 0.078M NaBH 4 Injecting the solution into the reaction kettle, wherein the dripping speed is 2ml/min, slowly stirring for 3h after dripping is finished, fully reacting, and filtering, washing and drying the solution;
4) Weighing 50 and g of the material obtained in the step 3), placing the material in an atmosphere furnace which is pre-filled with argon, setting a calcining procedure, preserving heat at 400 ℃ for 2h, heating at a rate of 5 ℃/min, naturally cooling, and sieving with a 400-mesh sieve to obtain MgB 2 A single crystal high nickel ternary material with completely modified surface.
Example 2:
co (cobalt) 2 The preparation method of the single crystal high nickel ternary material with the completely modified surface comprises the following steps:
1) Weigh 200 g Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Then according to the lithium source: the molar ratio of the ternary precursor is 1.05, lithium hydroxide is weighed, then the lithium hydroxide is put into a mixer for uniform mixing, the uniformly mixed mixture is put into an atmosphere furnace which is pre-ventilated with oxygen, a calcination procedure is set, firstly, the temperature is kept at 480 ℃ for 5h, then the temperature is kept at 750 ℃ for 15h, and the heating rate is 5 ℃/min;
2) Crushing the high-nickel ternary material obtained in the step 1), and then sieving the crushed high-nickel ternary material with a 400-mesh screen to obtain a monocrystal high-nickel ternary material with uniformly dispersed particle size;
3) Weighing 100 g of the monocrystal high-nickel ternary material obtained in the step 2), adding the monocrystal high-nickel ternary material into a vacuum stirring reaction kettle of 5L, and adding 2L and 0.009M of Mg (NO) 3 ) 2 Slowly stirring 1. 1h, introducing inert gas into the solution to remove air, and adding 40 ml of 0.078M KBH 4 The solution was injected into the reaction vessel at a dropping rate of 2ml/min, and after the completion of the dropping, the solution was slowly stirred for 3h to allow the reaction to proceed sufficiently. Filtering, washing and drying the solution;
4) Weighing 50 and g the material obtained in the step 3), placing the material in an atmosphere furnace which is pre-filled with argon, setting a calcining procedure, preserving heat at 400 ℃ for 2h, heating at a rate of 5 ℃/min, naturally cooling, and sieving with a 400-mesh sieve to obtain Co 2 B surface is completely modified.
Example 3:
a preparation method of a FeB surface-completely-modified single-crystal high-nickel ternary material comprises the following steps of
1) Weigh 200 g Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Then according to the lithium source: the molar ratio of the ternary precursor is 1.05, lithium hydroxide is weighed, then the lithium hydroxide is put into a mixer for uniform mixing, the uniformly mixed mixture is put into an atmosphere furnace which is pre-ventilated with oxygen, a calcination procedure is set, firstly, the temperature is kept at 480 ℃ for 5h, then the temperature is kept at 750 ℃ for 15h, and the heating rate is 5 ℃/min;
2) Crushing the high-nickel ternary material obtained in the step 1), and then sieving the crushed high-nickel ternary material with a 400-mesh screen to obtain a monocrystal high-nickel ternary material with uniformly dispersed particle size;
3) Weighing 100 g of the monocrystal high-nickel ternary material obtained in the step 2), adding the monocrystal high-nickel ternary material into a vacuum stirring reaction kettle of 5L, and adding 2L and 0.009M of Fe (NO) 3 ) 2 Slowly stirring 1. 1h, introducing inert gas into the solution to sufficiently remove air therein, and then adding 23 ml of 0.078M KBH 4 Injecting the solution into the aboveIn the reaction kettle, the dropping speed is 2ml/min, and after the dropping is finished, the mixture is slowly stirred for 3h so as to fully react. Filtering, washing and drying the solution;
4) Weighing the material obtained in the step 3) of 50 g, placing the material in an atmosphere furnace which is pre-filled with argon, setting a calcining procedure, preserving heat at 400 ℃ for 2h, heating at a rate of 5 ℃/min, naturally cooling, and sieving with a 400-mesh sieve to obtain the single crystal high nickel ternary material with the FeB surface completely modified.
Experimental comparative example 1:
1) Weigh 200 g Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 Then according to the lithium source: the molar ratio of the ternary precursor is 1.05, lithium hydroxide is weighed, then the lithium hydroxide is put into a mixer for uniform mixing, the uniformly mixed mixture is put into an atmosphere furnace which is pre-ventilated with oxygen, a calcination procedure is set, firstly, the temperature is kept at 480 ℃ for 5h, then the temperature is kept at 750 ℃ for 15h, and the heating rate is 5 ℃/min;
2) Crushing the nickel-cobalt-manganese ternary material obtained in the step 1), and then sieving the crushed material with a 400-mesh sieve to obtain the monocrystal high-nickel ternary material with uniform particle size dispersion.
Performance test:
the tests carried out in this example were all based on a 2025 button cell, and were carried out by first using a sintered single crystal ternary material and a modified composite material as positive electrode active materials, using a 5130 PVDF as binder, using SP and KS-6 as conductive agents, using NMP as solvent, and following the active materials: and (2) a binder: the mass ratio of the conductive agent is 85:5:10, and stirring and mixing the mixture to a uniform slurry state.
Uniformly coating the prepared positive electrode slurry on an aluminum foil by adopting a preparation device, transferring the aluminum foil to a vacuum drying oven at 120 ℃ for vacuum drying 12h, calculating the thickness of a pole piece to be rolled according to the compaction density, carrying out rolling treatment, cutting the pole piece with a cutting machine into pole pieces with the diameter of 12 mm and uniform thickness, and assembling the pole pieces into a button cell in a vacuum glove box, wherein a lithium piece is used as a counter electrode, a Celgard 2300 type diaphragm is adopted, and LiFP is adopted 6 Electric of baseAnd (5) dissolving the solution.
The single-crystal high-nickel ternary materials in example 1 and experimental comparative example 1 were subjected to electrochemical performance test (the test method is power buckling) and electrochemical specific capacity curves were obtained, the results are shown in fig. 2 and 3, and the test results are shown in table 1:
as can be seen from Table 1, the single crystal high nickel ternary material prepared by the method of this example, i.e. example 1, has superior cycle performance compared with the capacity retention rate after 450 cycles at 1C multiplying power and compared with the experimental comparative example 1, and by test, the single crystal high nickel ternary material prepared by the method of this example, i.e. example 1, has significantly improved performance and is very suitable for industrial scale-up production, as shown in FIG. 1, it can be seen that MgB prepared by the method of this example, i.e. example 1 2 The surface of the single crystal high nickel ternary material with the completely modified surface is provided with a very compact and uniform surface modification layer, and the surface of the single crystal high nickel ternary material without the modification is very smooth without the surface modification layer.
Claims (4)
1. The preparation method of the single crystal high nickel ternary material with the completely modified surface is characterized by comprising the following steps of:
1) Uniformly mixing the high-nickel ternary precursor and a lithium source according to the molar ratio of the lithium source to the high-nickel ternary precursor of 1.0-1.06 to obtain a mixture, wherein the mixing speed is 200r/min-300r/min, and the mixing time is 30min-120min;
2) Calcining the mixture obtained in the step 1) in an oxygen atmosphere to obtain a monocrystal high-nickel ternary matrix material, wherein the oxygen concentration in the oxygen atmosphere is higher than 99.9%, the calcining temperature and the calcining time are 450-480 ℃ and the temperature is kept for 5h and 750-900 ℃ and 15h;
3) Crushing and sieving the base material obtained in the step 2) to obtain monocrystal particles of the monocrystal high-nickel ternary material with uniformly dispersed particle sizes, wherein a sieving screen is 300-500 meshes, and the particle size of the crushed monocrystal particles of the monocrystal high-nickel ternary material is 2-3.5 um;
4) Dispersing single crystal high nickel ternary material single crystal particles obtained in the step 3) in a material containing M x (NO 3 ) y Or M x Cl y Is slowly stirred for 1h at room temperature under the condition of inert gas, and then MBH with the concentration of 0.078M-0.1M is added 4 Slowly dripping ethanol solution with the acceleration of 2ml/min-30ml/min into the mixed solution, slowly stirring for 2 hr, filtering the mixed solution, and drying the obtained residue, wherein the monocrystal high nickel ternary material and M x (NO 3 ) y Or M x Cl y The mass ratio of the ethanol solution is 1:10-50, M x (NO 3 ) y Or M x Cl y The concentration of the ethanol solution is 0.009M-0.02. 0.02M, M x B y The addition amount of the surface modification layer is 0.5-5% of the mass of the monocrystal high-nickel ternary material matrix, the stirring speed is 20-100 r/min, the stirring time is 1-3 h, the drying temperature is 80-120 ℃, and the drying time is 12h;
5) Calcining the filter residue obtained in the step 4) under the protection of inert gas to obtain a single crystal high nickel ternary material with completely modified surface, wherein the calcining temperature and the calcining time are kept at 500 ℃ for 120min, and the atmosphere is one or more of argon or nitrogen;
the lithium source in the step 1) is one or more of lithium hydroxide or lithium carbonate;
m as described in step 4) x (NO 3 ) y Is Mg (NO) 3 ) 2 、Co(NO 3 ) 3 、Mn(NO 3 ) 4 、Fe(NO 3 ) 2 、Al(NO 3 ) 3 、Ca(NO 3 ) 2 One or more of the following;
m as described in step 4) x Cl y Is TiCl 4 、MgCl 2 One or more of the following;
MBH as described in step 4) 4 Is one or more of sodium borohydride or potassium borohydride or lithium borohydride;
m as described in step 4) x B y Is MgB 2 Or ZrB 2 Or CaB 6 Or TiB 2 Or CrB 2 Or AlB 2 Or Co 2 B.
2. The method for preparing a single crystal high nickel ternary material with completely modified surface according to claim 1, wherein the single crystal high nickel ternary precursor in step 1) is nickel cobalt manganese or nickel cobalt aluminum hydroxide, and the molecular formula is Ni x Co y M 1-x-y (OH) 2 Wherein x=0.65-0.95 and y=0.01-0.2.
3. The surface-modified single crystal high nickel ternary material prepared by the method for preparing the surface-modified single crystal high nickel ternary material according to any one of claims 1 to 2.
4. The use of the surface-modified single-crystal high-nickel ternary material of claim 3 in a positive electrode material of a lithium ion battery.
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| CN115990497A (en) * | 2023-02-14 | 2023-04-21 | 广西师范大学 | CoPOx-Co 2 Preparation method of sodium borohydride hydrolysis catalyst |
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