CN114267841A - Preparation method and application of surface-fully-coated high-nickel single crystal ternary material - Google Patents
Preparation method and application of surface-fully-coated high-nickel single crystal ternary material Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a surface-fully-coated high-nickel single crystal ternary material, wherein the method comprises the following steps: uniformly mixing a high-nickel ternary precursor and a lithium source in proportion to obtain a mixture, calcining the mixture in an oxygen atmosphere to obtain high-nickel single crystal ternary material matrix particles, crushing and sieving the high-nickel single crystal ternary material matrix particles to obtain high-nickel single crystal ternary material single crystal particles; and adsorbing the single crystal particles by using a solution containing a reducing boron hydride, filtering, drying and calcining to obtain the high-nickel single crystal ternary material with the fully-coated surface. The method has simple and reliable process and low cost, can improve the cycle performance of the material and the internal resistance of the material, and the prepared high-nickel single crystal ternary material has good electrochemical performance 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 battery anode material technology, in particular to a preparation method and application of a surface-fully-coated high-nickel single crystal ternary material.
Background
With the increasing expansion of electric vehicle scale, Lithium Ion Batteries (LIBs) have become a promising candidate that can meet the requirements of high energy and power density, especially layered Li [ Ni ]xCoy(Al or Mn)1-x-y]O2(Al = NCA or Mn = NCM) positive electrodes are attracting attention because of their advantages of high energy density and low cost. With the successful commercialization of medium nickel content (x ≦ 0.5) single crystal metal oxide positive electrodes (NCM/NCA), the most effective way to further increase energy density and reduce cost to improve the competitiveness of next generation lithium ion batteries is to increase the nickel content.
The traditional high nickel ternary material is secondary particles stacked by nano particles, and has high compaction density and energy density. However, the practical application of the high nickel ternary cathode material is limited by severe cycle degradation and thermal instability, and particularly in the high delithiation state, the high nickel ternary cathode material has large anisotropic volume change, damages the mechanical stability and generates intergranular cracks between primary particles, and the intergranular cracks propagate along the grain boundaries of the particles, so that the secondary microspheres are exfoliated and then pulverized, and finally, the mechanical integrity and the cycle stability are reduced. In addition, the interfacial region between the electrolyte and the positive electrode is significantly damaged, thereby exacerbating the penetration of the electrolyte along intergranular cracks, resulting in decomposition of the electrolyte and transformation of the crystal structure. In addition, when the Ni content exceeds 0.6, intergranular cracks are aggravated, which is the reason of the continuous attenuation of the capacity of the high-nickel ternary positive electrode, the adverse effect can be relieved by adopting a mode of making the high-nickel ternary positive electrode material into single crystal particles, the integrated primary particles can effectively relieve the internal strain generated by anisotropic volume change due to the absence of grain boundaries, and finally, the surface electrolyte corrosion is reduced and the formation of intergranular cracks is slowed down. Although the introduction of quasi-single crystalline structures can enhance cycling stability by hindering micro/nano-crack formation, side reactions at the positive electrode/electrolyte interface at high charge cut-off (> 4.3V) remain a challenge.
Surface modification is generally considered to be an effective method for suppressing structural deterioration and enhancing electrochemical performance, because it can improve the problem of interface reaction between positive electrode/electrolyte and enhance Li+The transfer efficiency is improved, the increase of impedance is inhibited, and particularly, a coating with excellent mechanical property is selected for coating, so that the cracking of a grain boundary caused by internal stress can be inhibited. However, the existing coating technology is difficult to realize surface full coating, non-uniform and incomplete coating of the high-nickel ternary cathode material, so that the effect of blocking the de-intercalation of lithium ions is achieved, and the transmission of the lithium ions is not facilitated.
Disclosure of Invention
The invention aims to provide a preparation method and application of a high-nickel single crystal ternary material with a fully-coated surface, aiming at the defects of the prior art. The method has simple and reliable process and low cost, can improve the cycle performance of the material and the internal resistance of the material, and the prepared high-nickel single crystal ternary material has good electrochemical performance 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 purpose of the invention is as follows:
a preparation method of a high-nickel single crystal ternary material with a fully-coated surface comprises the following steps:
1) uniformly mixing the high-nickel ternary precursor and a lithium source according to a molar ratio of 1.0-1.06 to obtain a mixture, wherein the mixing speed is 200 r/min-300 r/min, and the mixing time is 30 min-120 min;
2) calcining the mixture obtained in the step 1) in an oxygen atmosphere to obtain a high-nickel single crystal ternary material matrix, 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 5 hours, and 750-900 ℃ is kept for 15 hours;
3) crushing and sieving the base material obtained in the step 2) to obtain high-nickel single crystal ternary material single crystal particles with uniformly dispersed particle sizes, wherein a sieving screen is 300-500 meshes, and the particle size of the crushed high-nickel single crystal ternary material particles is 2-3.5 um;
4) dispersing the high-nickel single crystal ternary material particles obtained in the step 3) in absolute ethyl alcohol, adding a solution containing reducing boron hydride into the ethanol by using a peristaltic pump, and performing adsorption, filtration, drying and calcination on the solution containing reducing boron hydride to obtain a high-nickel single crystal ternary material with a fully-coated surface, wherein the mass ratio of the high-nickel single crystal ternary material particles to the absolute ethyl alcohol is 1: 10 to 20 percent, the mass ratio of the solution containing the reducing boron compound to the high-nickel monocrystal ternary material matrix monocrystal particles is 0.5 to 3 percent, the concentration is 0.078M to 0.1M, the liquid injection amount of a peristaltic pump is 10 ml/min to 120ml/min, the stirring speed is 20 r/min to 100 r/min, the stirring time is 1 h to 3 h, the drying temperature is 80 to 120 ℃, the drying time is 12 h, the calcining temperature and the calcining time are kept at 500 ℃ for 120 min, and the atmosphere is argon.
The high nickel ternary precursor in the step 1) is nickel-cobalt-manganese or nickel-cobalt-aluminum hydroxide with a molecular formula of NixCoyM1-x-y(OH)2Wherein x is 0.65-0.95, and y is 0.01-0.2.
The lithium source in the step 1) is one or more of lithium hydroxide or lithium carbonate.
The reducing boron-containing compound in the step 4) is one or more of sodium borohydride, potassium borohydride or lithium borohydride.
The surface-fully-coated high-nickel single crystal ternary material prepared by the preparation method of the surface-fully-coated high-nickel single crystal ternary material.
The surface-fully-coated high-nickel single crystal ternary material is applied to a lithium ion battery anode material.
According to the technical scheme, the high-nickel single crystal ternary material with uniform particle size distribution is prepared, then the base material is treated by the reductive borohydride, and as the high-nickel ternary material has oxidizability, the reductive borohydride solution can generate an oxidation-reduction reaction on the surface of the base body, so that a metal boride precursor is generated, and is uniformly distributed on the surface of the base material, and the metal boride is generated through calcination treatment, is a semiconductor material and has certain toughness, so that the generation of microcracks can be inhibited, the conductivity of the base material is enhanced, the generation of interface side reactions is inhibited, the discharge capacity, the rate capability and the cycle performance of the material are improved, and the electrochemical performance of the material is improved.
The technical scheme realizes uniform surface full coating by means of redox reaction, does not need a special high-end technical means, has simple and reliable process method and low cost, obviously improves the discharge capacity, the cycle performance and the internal resistance of the obtained high-nickel single crystal ternary material, and is suitable for industrial production.
The method has simple and reliable process and low cost, can improve the cycle performance of the material and the internal resistance of the material, and the prepared high-nickel single crystal ternary material has good electrochemical performance 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 nickel-cobalt-manganese single crystal ternary material in example 1 and comparative example 1;
FIG. 2 is a graph of rate capability of nickel cobalt manganese single crystal ternary materials in example 1 and comparative example 1;
fig. 3 is a graph of cycle performance of the nickel-cobalt-manganese single crystal ternary materials in example 1 and comparative example 1.
Detailed Description
The invention will be further illustrated by the following figures and examples, but is not limited thereto.
Example 1:
a preparation method of a nickel-cobalt-manganese single crystal ternary material fully coated with a metal boride comprises the following steps:
1) 200 g of Ni are weighed0.8Co0.1Mn0.1(OH)2Then, as a lithium source: weighing lithium hydroxide according to the molar ratio of the ternary precursor of 1.05, then putting the lithium hydroxide into a mixer to be uniformly mixed, putting the uniformly mixed mixture into an atmosphere furnace which is pre-aerated with oxygen, setting a calcination program, firstly preserving heat at 480 ℃ for 5h, then preserving heat at 750 ℃ for 15 h, and increasing the temperature at the rate of 5 ℃/min;
2) crushing the nickel-cobalt-manganese ternary material obtained in the step 1), and then screening the crushed material through a 400-mesh screen to obtain the nickel-cobalt-manganese ternary material with uniformly dispersed particle sizes;
3) weighing 100 g of the nickel-cobalt-manganese single crystal ternary material obtained in the step 2), adding the nickel-cobalt-manganese single crystal ternary material into a 5L vacuum stirring reaction kettle, adding 2L of absolute ethyl alcohol, slowly stirring for 30 min, then injecting 100 ml of 0.078M sodium borohydride solution into the reaction kettle by using a peristaltic pump, wherein the injection rate is 10 ml/min, after the injection is finished, slowly stirring for 3 h, fully reacting, and then filtering, washing and drying the solution;
4) weighing 50 g of the material obtained in the step 3), placing the material in an atmosphere furnace which is pre-filled with argon, setting a calcination procedure, keeping the temperature at 450 ℃ for 2 h, raising the temperature at a rate of 5 ℃/min, naturally cooling, and then sieving with a 400-mesh sieve to obtain the nickel-cobalt-manganese single crystal ternary material fully coated with the metal boride.
Example 2:
a preparation method of a nickel-cobalt-manganese single crystal ternary material fully coated with a metal boride comprises the following steps:
1) 500 g of Ni are weighed0.65Co0.1Mn0.25(OH)2Then, as a lithium source: weighing lithium hydroxide according to the molar ratio of the ternary precursor of 1.05, then putting the lithium hydroxide into a mixer to be uniformly mixed, putting the uniformly mixed mixture into an atmosphere furnace with oxygen in advance, setting a calcination program, firstly preserving heat at 480 ℃ for 5h, then preserving heat at 780 ℃ for 15 h, and increasing the temperature rate at 5 ℃/min;
2) crushing the nickel-cobalt-manganese ternary material obtained in the step 1), and then screening the crushed material through a 400-mesh screen to obtain the nickel-cobalt-manganese ternary material with uniformly dispersed particle sizes;
3) weighing 100 g of the single crystal nickel-cobalt-manganese ternary material obtained in the step 2), adding the single crystal nickel-cobalt-manganese ternary material into a 5L vacuum stirring reaction kettle, adding 2L of absolute ethyl alcohol, slowly stirring for 30 min, then injecting 100 ml of 0.09M sodium borohydride solution into the reaction kettle by using a peristaltic pump, wherein the injection rate is 10 ml/min, after the injection is finished, slowly stirring for 3 h, fully reacting, filtering, washing and drying the solution;
4) weighing 50 g of the material obtained in the step 3), placing the material in an atmosphere furnace which is pre-filled with argon, setting a calcination procedure, keeping the temperature at 400 ℃ for 2 h, raising the temperature at a rate of 5 ℃/min, naturally cooling, and then sieving with a 400-mesh sieve to obtain the nickel-cobalt-manganese single crystal ternary material fully coated with the metal boride.
Example 3:
a preparation method of a nickel-cobalt-aluminum single crystal ternary material fully coated with a metal boride comprises the following steps:
1) 500 g of Ni are weighed0.8Co0.1Al0.1(OH)2Then, as a lithium source: weighing lithium carbonate with the molar ratio of the ternary precursor of 1.06, then putting the lithium carbonate into a mixer to be uniformly mixed, putting the uniformly mixed mixture into an atmosphere furnace with oxygen in advance, setting a calcination program, firstly preserving heat at 500 ℃ for 5h, then preserving heat at 880 ℃ for 15 h, and increasing the temperature rate at 5 ℃/min;
2) crushing the nickel-cobalt-aluminum ternary material obtained in the step 1), and then screening the crushed material through a 400-mesh screen to obtain the nickel-cobalt-aluminum ternary material with uniformly dispersed particle sizes;
3) weighing 100 g of the single crystal nickel-cobalt-aluminum ternary material obtained in the step 2), adding the single crystal nickel-cobalt-aluminum ternary material into a 5L vacuum stirring reaction kettle, adding 2L of absolute ethyl alcohol, slowly stirring for 30 min, then injecting 100 ml of 0.09M sodium borohydride solution into the reaction kettle by using a peristaltic pump, wherein the injection rate is 10 ml/min, slowly stirring for 3 h after the injection is finished, fully reacting, filtering, washing and drying the solution;
4) weighing 50 g of the material obtained in the step (3), placing the material in an atmosphere furnace which is pre-filled with argon, setting a calcination program, keeping the temperature at 400 ℃ for 2 h, wherein the heating rate is 5 ℃/min, naturally cooling, and then sieving with a 400-mesh sieve to obtain the nickel-cobalt-aluminum single crystal ternary material fully coated with the metal boride.
Experimental comparative example 1:
1) 200 g of Ni are weighed0.8Co0.1Mn0.1(OH)2Then, as a lithium source: weighing lithium hydroxide according to the molar ratio of the ternary precursor of 1.05, then putting the lithium hydroxide into a mixer to be uniformly mixed, putting the uniformly mixed mixture into an atmosphere furnace which is pre-aerated with oxygen, setting a calcination program, firstly preserving heat at 480 ℃ for 5h, then preserving heat at 750 ℃ for 15 h, and increasing the temperature rate at 5 ℃/min;
2) crushing the nickel-cobalt-manganese ternary material obtained in the step 1), and then screening the crushed material through a 400-mesh screen to obtain the nickel-cobalt-manganese ternary material with uniformly dispersed particle sizes.
Experimental comparative example 2:
1) 500 g of Ni are weighed0.65Co0.1Mn0.25(OH)2Then, as a lithium source: weighing lithium hydroxide according to the molar ratio of the ternary precursor of 1.05, then putting the lithium hydroxide into a mixer to be uniformly mixed, putting the uniformly mixed mixture into an atmosphere furnace with oxygen in advance, setting a calcination program, firstly preserving heat at 480 ℃ for 5h, then preserving heat at 780 ℃ for 15 h, and increasing the temperature rate at 5 ℃/min;
2) crushing the nickel-cobalt-manganese ternary material obtained in the step 1), and then screening the crushed material through a 400-mesh screen to obtain the nickel-cobalt-manganese ternary material with uniformly dispersed particle sizes.
Experimental comparative example 3:
1) 500 g of Ni are weighed0.8Co0.1Al0.1(OH)2Then, as a lithium source: weighing lithium carbonate with the molar ratio of the ternary precursor of 1.06, then putting the lithium carbonate into a mixer to be uniformly mixed, putting the uniformly mixed mixture into an atmosphere furnace with oxygen in advance, setting a calcination program, firstly preserving heat at 500 ℃ for 5h, then preserving heat at 880 ℃ for 15 h, and increasing the temperature rate at 5 ℃/min;
2) crushing the nickel-cobalt-aluminum ternary material obtained in the step 1), and then screening the crushed material through a 400-mesh screen to obtain the nickel-cobalt-aluminum ternary material with uniformly dispersed particle sizes.
And (3) performance testing: the tests carried out in the experiment of this example were carried out on a 2025 button cell basis, starting with sintered single-crystal ternary material and modified composite material as positive electrode active material, PVDF of type 5130 as binder, SP and KS-6 as conductive agents, NMP as solvent, in terms of active material: adhesive: the mass ratio of the conductive agent is 85: 5: 10 to a uniform slurry state, uniformly coating the prepared anode slurry on an aluminum foil by adopting a preparation device, and then transferring the anode slurry into a vacuum drying oven at 120 ℃ for vacuum drying for 12 hours. Calculating the thickness to be achieved by rolling the pole piece according to the compaction density, performing rolling treatment, cutting the rolled pole piece into pole pieces with uniform thickness and diameter of 12 mm by using a cutting machine, and assembling the pole pieces into the button cell in a vacuum glove box, wherein the lithium piece is used as a counter electrode, a diaphragm of Celgard 2300 type is adopted, and LiFP is adopted6A base electrolyte.
The nickel-cobalt-manganese single crystal ternary materials in example 1 and experimental comparative example 1 were subjected to electrochemical performance test (the test method is charging) and an electrochemical specific capacity curve was obtained, and the results are shown in fig. 2 and fig. 3, and the test results are shown in table 1:
| performance of | Comparative example 1 | Example 1 |
| 0.2C capacity (mAh/g) | >200 | >200 |
| 1C Capacity (mAh/g) | >200 | >200 |
| |
47.5 | 78.4 |
As can be seen from table 1, the capacity retention rate of the nickel-cobalt-manganese single-crystal ternary material prepared by the method of example 1 in the present example after being cycled for 500 times at a rate of 1C is superior to that of comparative example 1 in the experiment, and through testing, the performance of the nickel-cobalt-manganese single-crystal ternary material is significantly improved by the method of example 1 in the present example, and the method is very suitable for industrial scale-up production, and as shown in fig. 1, it can be seen that the nickel-cobalt-manganese single-crystal ternary material prepared by the method of example 1 in the present example has a uniform wavy coating on the surface, and basically realizes full surface coating.
Claims (6)
1. A preparation method of a high-nickel single crystal ternary material with a fully-coated surface is characterized by comprising the following steps:
1) uniformly mixing the high-nickel ternary precursor and a lithium source according to a molar ratio of 1.0-1.06 to obtain a mixture, wherein the mixing speed is 200 r/min-300 r/min, and the mixing time is 30 min-120 min;
2) calcining the mixture obtained in the step 1) in an oxygen atmosphere to obtain high-nickel single crystal ternary material matrix particles, 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 5 hours, and 750-900 ℃ is kept for 15 hours;
3) crushing and sieving the base material obtained in the step 2) to obtain high-nickel single crystal ternary material single crystal particles with uniformly dispersed particle sizes, wherein a sieving screen is 300-500 meshes, and the particle size of the crushed high-nickel single crystal ternary material particles is 2-3.5 um;
4) dispersing the high-nickel single crystal ternary material particles obtained in the step 3) in absolute ethyl alcohol, adding a solution containing reducing boron hydride into the ethanol by using a peristaltic pump, and performing adsorption, filtration, drying and calcination on the solution containing reducing boron hydride to obtain a high-nickel single crystal ternary material with a fully-coated surface, wherein the mass ratio of the high-nickel single crystal ternary material particles to the absolute ethyl alcohol is 1: 10 to 20 percent, the mass ratio of the solution containing the reducing boron compound to the high-nickel monocrystal ternary material monocrystal particles is 0.5 to 3 percent, the concentration is 0.078M to 0.1M,
the liquid injection amount of the peristaltic pump is 10 ml/min-120ml/min, the stirring speed is 20 r/min-100 r/min, the stirring time is 1 h-3 h, the drying temperature is 80-120 ℃, the drying time is 12 h, the calcination temperature and the calcination time are 500 ℃, the temperature is kept for 120 min, and the atmosphere is argon.
2. The method for preparing the surface-fully-coated high-nickel single-crystal ternary material according to claim 1, wherein the high-nickel ternary precursor in the step 1) is nickel-cobalt-manganese or nickel-cobalt-aluminum hydroxide with a molecular formula of NixCoyM1-x-y(OH)2Wherein x is 0.65-0.95, and y is 0.01-0.2.
3. The method for preparing the surface-fully-coated high-nickel single-crystal ternary material according to claim 1, wherein the lithium source in the step 1) is one or more of lithium hydroxide or lithium carbonate.
4. The method for preparing the surface-fully-coated high-nickel single-crystal ternary material according to claim 1, wherein the reducing boron-containing compound in the step 4) is one or more of sodium borohydride, potassium borohydride or lithium borohydride.
5. The surface-fully-coated high-nickel single-crystal ternary material prepared by the preparation method of the surface-fully-coated high-nickel single-crystal ternary material according to any one of claims 1 to 4.
6. The use of the surface-fully-coated high-nickel single-crystal ternary material of claim 5 in a positive electrode material of a lithium ion battery.
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| CN115465901A (en) * | 2022-11-01 | 2022-12-13 | 贺州学院 | Method for completely coating surface of lithium ion battery anode material |
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