CN110620227A - Lithium ion battery positive electrode material, preparation method and application thereof - Google Patents
Lithium ion battery positive electrode material, preparation method and application thereof Download PDFInfo
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery anode material, and a preparation method and application thereof. The lithium ion battery positive electrode material comprises: a ternary material; and a coating layer coated on the outer surface of the ternary material; the coating layer includes vitamin C and a sulfur-based compound. The sulfur-based compound can form a layer of stable interfacial film on the surface of the ternary material, and the cycling stability of the ternary material under high voltage is remarkably improved. The VC additive can reduce the decomposition of the electrolyte solvent on the surface of the negative electrode, so that VC can form a stable interface film on the surface of the negative electrode. In conclusion, the BDTT and VC are matched for use, so that the interface of the positive electrode and the negative electrode can be stabilized simultaneously, the polarization in the charge and discharge process is reduced, and the cycle performance of the lithium ion battery is obviously improved. The lithium ion battery prepared from the lithium ion battery anode material has high first discharge specific capacity and excellent cycle performance.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery anode material, and a preparation method and application thereof.
Background
In order to meet the increasing demand for high energy density of lithium ion batteries in recent years, cathode materials have also been developed in two directions: 1) the nickel content is high, and higher Ni content can bring higher capacity; 2) the high voltage, the improvement of voltage can promote the capacity of material on the one hand, on the other hand also can promote the voltage platform of material. However, the stability of the positive electrode material/electrolyte interface is reduced with the increase of the charging voltage, so that the side reaction is increased, and the cycle performance of the lithium ion battery is seriously influenced. In order to solve the problem of poor stability of ternary materials under high voltage, surface coating, single crystals and electrolyte additives are the most common methods. The effective surface coating can obviously improve the comprehensive performance of the material, and the comprehensive performance of the material obtained by surface coating in the prior art needs to be improved.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a lithium ion battery cathode material, a preparation method and an application thereof, and a lithium ion battery prepared from the lithium ion battery cathode material has a better cycle performance.
The invention provides a lithium ion battery anode material, which comprises the following components:
a ternary material;
and a coating layer coated on the outer surface of the ternary material;
the coating layer includes vitamin C and a sulfur-based compound.
Preferably, the ternary material has the general formula: lixNi1-y-zCoyMnzO2(ii) a Wherein 1 is<x≤1.15,0≤y≤1/3,0≤z≤1/3。
Preferably, the ternary material is Li1.05Ni0.5Co0.2Mn0.3O2、Li1.07Ni0.5Co0.2Mn0.3O2、Li1.10Ni0.5Co0.2Mn0.3O2 OrLi1.12Ni0.6Co0.2Mn0.2O2。
Preferably, the sulfur-based compound is BDTT.
The invention also provides a preparation method of the lithium ion battery anode material, which comprises the following steps:
and (3) mixing the ternary material powder, the vitamin C and the sulfur-based compound at a high speed to obtain the lithium ion battery anode material.
Preferably, the mass ratio of the ternary material powder to the vitamin C to the sulfur-based compound is 100: 0.1-0.3: 0.1 to 0.3.
Preferably, the particle size of the ternary material powder is 3-15 μm.
Preferably, the rotation speed of the high-speed mixing is 300-500 rpm.
Preferably, after the high-speed mixing, the method further comprises:
the compound obtained by high speed mixing is sieved by a 300 mesh sieve.
The invention also provides a lithium ion battery which comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, and is characterized in that the positive electrode comprises the lithium ion battery positive electrode material or the lithium ion battery positive electrode material prepared by the preparation method.
The invention provides a lithium ion battery anode material, which comprises the following components: a ternary material; and a coating layer coated on the outer surface of the ternary material; the coating layer includes vitamin C and a sulfur-based compound. In the lithium ion battery anode material provided by the invention, the vitamin C and the sulfur-based compound are coated on the surface of the ternary material, and the sulfur-based compound can form a layer of stable interface film on the surface of the ternary material, so that the side reaction on the surface of the anode under high voltage is reduced, the decomposition of electrolyte on the surface of the anode is inhibited, and the cycle stability of the ternary material under high voltage is obviously improved; the VC additive can reduce the decomposition of the electrolyte solvent on the surface of the negative electrode, so that VC can form a stable interfacial film on the surface of the negative electrode. In conclusion, the BDTT and VC are matched for use, so that the interface of the positive electrode and the negative electrode can be stabilized simultaneously, the polarization in the charge and discharge process is reduced, and the cycle performance of the lithium ion battery is obviously improved. Therefore, the lithium ion battery prepared from the lithium ion battery cathode material has higher first discharge specific capacity and better cycle performance.
The performance of the prepared lithium ion battery is tested, and the voltage testing range is 3.0-4.2V. Experimental results show that the lithium ion battery prepared from the lithium ion battery anode material provided by the invention has the first discharge capacity higher than 156mAh/g, the retention rate of the 2500-time circulation capacity higher than 83%, and the BET (BET) not lower than 0.53m2(ii)/g, the total content of Li (surface free lithium ion content) does not exceed 0.030%.
Drawings
Fig. 1 is an SEM image of the positive electrode material for a lithium ion battery prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a lithium ion battery anode material, which comprises the following components:
a ternary material;
and a coating layer coated on the outer surface of the ternary material;
the coating layer includes vitamin C and a sulfur-based compound.
In certain embodiments of the present invention, the ternary material has the general formula: lixNi1-y-zCoyMnzO2(ii) a Wherein 1 is<x is less than or equal to 1.15, y is less than or equal to 1/3 and z is less than or equal to 1/3 and is more than or equal to 0. In certain embodiments of the present invention, the ternary material is Li1.05Ni0.5Co0.2Mn0.3O2、Li1.07Ni0.5Co0.2Mn0.3O2、Li1.10Ni0.5Co0.2Mn0.3O2 OrLi1.12Ni0.6Co0.2Mn0.2O2。
In certain embodiments of the invention, the sulfur-based compound is BDTT ([4,4-bi (1,3,2-dioxathiolane) ]2,2,2, 2-tetraoxide).
The particle size of the lithium ion battery anode material is not particularly limited, and can be adjusted according to actual needs.
In the lithium ion battery anode material provided by the invention, the vitamin C and the sulfur-based compound are coated on the surface of the ternary material, and the sulfur-based compound can form a layer of stable interface film on the surface of the ternary material, so that the side reaction on the surface of the anode under high voltage is reduced, the decomposition of electrolyte on the surface of the anode is inhibited, and the cycle stability of the ternary material under high voltage is obviously improved; the VC additive can reduce the decomposition of the electrolyte solvent on the surface of the negative electrode, so that VC can form a stable interfacial film on the surface of the negative electrode. In conclusion, the BDTT and VC are matched for use, so that the interface of the positive electrode and the negative electrode can be stabilized simultaneously, the polarization in the charge and discharge process is reduced, and the cycle performance of the lithium ion battery is obviously improved. Therefore, the lithium ion battery prepared from the lithium ion battery cathode material has higher first discharge specific capacity and better cycle performance.
The invention also provides a preparation method of the lithium ion battery anode material, which comprises the following steps:
and (3) mixing the ternary material powder, the vitamin C and the sulfur-based compound at a high speed to obtain the lithium ion battery anode material.
In certain embodiments of the present invention, the ternary material has the general formula: lixNi1-y-zCoyMnzO2(ii) a Wherein 1 is<x is less than or equal to 1.15, y is less than or equal to 1/3 and z is less than or equal to 1/3 and is more than or equal to 0. In certain embodiments of the present invention, the ternary material is Li1.05Ni0.5Co0.2Mn0.3O2、Li1.07Ni0.5Co0.2Mn0.3O2、Li1.10Ni0.5Co0.2Mn0.3O2Or Li1.12Ni0.6Co0.2Mn0.2O2. The source of the ternary material is not particularly limited in the present invention, and may be generally commercially available.
In some embodiments of the invention, the ternary material powder is prepared according to the following method:
and (4) crushing the ternary material to obtain ternary material powder.
The method of pulverization in the present invention is not particularly limited, and pulverization methods known to those skilled in the art can be used.
In some embodiments of the invention, the particle size of the ternary material powder is 3-15 μm. In certain embodiments, the ternary material powder has a particle size of 10.2 μm, 10.8 μm, 11 μm, 10.6 μm, or 10.5 μm.
In certain embodiments of the invention, the sulfur-based compound is BDTT ([4,4-bi (1,3,2-dioxathiolane) ]2,2,2, 2-tetraoxide). The source of the BDTT is not particularly limited in the invention, and the BDTT can be generally commercially available.
In some embodiments of the present invention, the mass ratio of the ternary material powder, the vitamin C, and the sulfur-based compound is 100: 0.1-0.3: 0.1 to 0.3. In some embodiments of the present invention, the mass ratio of the ternary material powder, the vitamin C, and the sulfur-based compound is 100: 0.1: 0.1, 100: 0.15: 0.15, 100: 0.2: 0.2.
in some embodiments of the present invention, the high speed mixing is performed at a speed of 300 to 500 rpm. In certain embodiments, the high speed mixing is at a speed of 400 rpm.
After the ternary material powder, the vitamin C and the sulfur-based compound are mixed at a high speed, the vitamin C and the sulfur-based compound are coated on the surface of the ternary material powder, and a stable interfacial film is formed on the surface of the ternary material, so that a coating layer is obtained, and the comprehensive performance of the material is improved.
In some embodiments of the present invention, after the high speed mixing, further comprising:
the compound obtained by high speed mixing is sieved by a 300 mesh sieve.
The effect of passing the composite obtained by high speed mixing through a 300 mesh screen was to remove any sagger impurities that may remain in the material.
The invention also provides a lithium ion battery which comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the positive electrode comprises the lithium ion battery positive electrode material or the lithium ion battery positive electrode material prepared by the preparation method.
The invention has no special limitation to the types of the negative electrode, the diaphragm and the electrolyte, and specifically, the negative electrode, the diaphragm and the electrolyte can be:
the lithium ion battery positive electrode material (or the lithium ion battery positive electrode material prepared by the preparation method) is used as a positive electrode, graphite is used as a negative electrode, polyvinylidene fluoride is used as a polar plate binder, a positive plate and a negative plate of the lithium ion battery are respectively prepared, a polypropylene microporous membrane is used as an electrode diaphragm, and 1mol/L lithium hexafluorophosphate is used as an electrolyte (wherein dimethyl carbonate, diethyl carbonate and ethylene carbonate are in a volume ratio of 1: 1: 1) to assemble the lithium ion battery.
The performance of the prepared lithium ion battery is tested, and the voltage testing range is 3.0-4.2V. Experimental results show that the lithium ion battery prepared from the lithium ion battery anode material provided by the invention has the first discharge capacity higher than 156mAh/g, the retention rate of the 2500-time circulation capacity higher than 83%, and the BET (BET) not lower than 0.53m2(ii)/g, the total content of Li (surface free lithium ion content) does not exceed 0.030%.
In order to further illustrate the present invention, the following examples are provided to describe the lithium ion battery cathode material, the preparation method and the application thereof in detail, but they should not be construed as limiting the scope of the present invention.
The starting materials used in the following examples are all generally commercially available.
Example 1
Mixing ternary material Li1.05Ni0.5Co0.2Mn0.3O2Crushing, wherein the particle size of the crushed particles is 10.2 mu m, then adding vitamin C and a sulfur-based compound BDTT for high-speed mixing (the rotation speed of the high-speed mixing is 400rpm), and sieving the obtained compound with a 300-mesh sieve to obtain the lithium ion battery anode material; the mass ratio of the crushed ternary material to the vitamin C to the sulfur-based compound is 100: 0.1: 0.1.
scanning electron microscope scanning analysis is carried out on the obtained lithium ion battery cathode material, the result is shown in fig. 1, fig. 1 is an SEM image of the lithium ion battery cathode material prepared in the embodiment 1 of the invention, and as can be seen from fig. 1, the lithium ion battery cathode material prepared in the embodiment 1 is in the shape of secondary spherical particles, a coating layer is clear and visible, the size of primary particles is uniform, and the sphericity is good.
Example 2
Mixing ternary material Li1.05Ni0.5Co0.2Mn0.3O2Crushing, wherein the particle size of the crushed particles is 10.8 mu m, then adding vitamin C and a sulfur-based compound BDTT for high-speed mixing (the rotation speed of the high-speed mixing is 400rpm), and sieving the obtained compound with a 300-mesh sieve to obtain the lithium ion battery anode material; the mass ratio of the crushed ternary material to the vitamin C to the sulfur-based compound is 100: 0.15: 0.15.
example 3
Mixing ternary material Li1.07Ni0.5Co0.2Mn0.3O2Crushing, wherein the particle size of the crushed particles is 11 microns, then adding vitamin C and a sulfur-based compound BDTT for high-speed mixing (the rotation speed of the high-speed mixing is 400rpm), and sieving the obtained compound with a 300-mesh sieve to obtain the lithium ion battery anode material; the pulverized ternary material and vitaminsThe mass ratio of the element C to the sulfur-based compound is 100: 0.15: 0.15.
example 4
Mixing ternary material Li1.10Ni0.5Co0.2Mn0.3O2Crushing, wherein the particle size of the crushed particles is 10.6 mu m, then adding vitamin C and a sulfur-based compound BDTT for high-speed mixing (the rotation speed of the high-speed mixing is 400rpm), and sieving the obtained compound with a 300-mesh sieve to obtain the lithium ion battery anode material; the mass ratio of the crushed ternary material to the vitamin C to the sulfur-based compound is 100: 0.2: 0.2.
example 5
Mixing ternary material Li1.12Ni0.6Co0.2Mn0.2O2Crushing, wherein the particle size of the crushed particles is 10.5 mu m, then adding vitamin C and a sulfur-based compound BDTT for high-speed mixing (the rotation speed of the high-speed mixing is 400rpm), and sieving the obtained compound with a 300-mesh sieve to obtain the lithium ion battery anode material; the mass ratio of the crushed ternary material to the vitamin C to the sulfur-based compound is 100: 0.2: 0.2.
comparative example 1
Mixing ternary material Li1.12Ni0.6Co0.2Mn0.2O2And (3) crushing, wherein the particle size of the crushed particles is 10.5 mu m, and sieving the particles with a 300-mesh sieve to obtain the lithium ion battery anode material.
The lithium ion battery is assembled by taking the lithium ion battery anode material as an anode, graphite as a cathode and polyvinylidene fluoride as a polar plate binder, respectively preparing an anode plate and a cathode plate of the lithium ion battery, taking a polypropylene microporous membrane as an electrode diaphragm and taking 1mol/L lithium hexafluorophosphate as an electrolyte (wherein dimethyl carbonate, diethyl carbonate, ethylene carbonate, vitamin C and BDTT are 1: 1: 1: 0.1: 0.1 (volume ratio)).
Example 6
In the embodiment, the positive electrode material of the lithium ion battery (respectively selected from the positive electrode materials of the lithium ion batteries in the embodiments 1 to 5) is used as a positive electrode, graphite is used as a negative electrode, polyvinylidene fluoride is used as a polar plate binder, and a positive plate and a negative plate of the lithium ion battery are respectively prepared, a polypropylene microporous membrane is used as an electrode diaphragm, and 1mol/L lithium hexafluorophosphate is used as an electrolyte (wherein dimethyl carbonate: diethyl carbonate: ethylene carbonate: 1: 1 (volume ratio)) to assemble 5 groups of lithium ion batteries (the lithium ion battery cathode material in example 1 corresponds to battery No. 1, the lithium ion battery cathode material in example 2 corresponds to battery No. 2, the lithium ion battery cathode material in example 3 corresponds to battery No. 3, the lithium ion battery cathode material in example 4 corresponds to battery No. 4, and the lithium ion battery cathode material in example 5 corresponds to battery No. 5).
The performance test of the lithium ion batteries prepared from the lithium ion battery cathode materials of examples 1 to 5 was performed, and the performance test of the lithium ion battery prepared in comparative example 1 (corresponding to battery No. 6) was also performed, wherein the voltage test range was 3.0 to 4.2V, and the results are shown in table 1.
Table 1 results of performance tests of the lithium ion battery obtained in example 6 and the lithium ion battery obtained in comparative example 1
As can be seen from Table 1, the lithium ion battery prepared by the embodiment of the invention has the first discharge capacity of 156.5-164.5 mAh/g, the retention rate of the 2500-time circulation capacity of 83.2-85.8% and the BET of 0.53-0.58 m2The amount of Li (surface free lithium ion content) is 0.016 to 0.030%. The lithium ion battery prepared in comparative example 1 had a first discharge capacity of 164.0mAh/g, a retention rate of 2500 cycle capacity of 72.1%, and a BET of 0.52m2Per g, the total% of Li (the content of free lithium ions on the surface) was 0.031%. The cycle performance of the lithium ion battery prepared by the invention is obviously better than that of the lithium ion battery prepared by the comparative example 1.
Experimental results show that the lithium ion battery prepared from the lithium ion battery cathode material prepared by the invention has the first discharge capacity higher than 156mAh/g, the 2500-time circulation capacity retention rate higher than 83%, and the BET (BET) value not less than 0.53m2(ii)/g, the total content of Li (surface free lithium ion content) does not exceed 0.030%.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A lithium ion battery positive electrode material comprising:
a ternary material;
and a coating layer coated on the outer surface of the ternary material;
the coating layer includes vitamin C and a sulfur-based compound.
2. The lithium ion battery cathode material according to claim 1, wherein the ternary material has a general formula: lixNi1-y-zCoyMnzO2(ii) a Wherein 1 is<x≤1.15,0≤y≤1/3,0≤z≤1/3。
3. The lithium ion battery cathode material according to claim 2, wherein the ternary material is Li1.05Ni0.5Co0.2Mn0.3O2、Li1.07Ni0.5Co0.2Mn0.3O2、Li1.10Ni0.5Co0.2Mn0.3O2Or Li1.12Ni0.6Co0.2Mn0.2O2。
4. The lithium ion battery positive electrode material of claim 1, wherein the sulfur-based compound is BDTT.
5. A preparation method of a lithium ion battery anode material comprises the following steps:
and (3) mixing the ternary material powder, the vitamin C and the sulfur-based compound at a high speed to obtain the lithium ion battery anode material.
6. The preparation method according to claim 1, wherein the mass ratio of the ternary material powder to the vitamin C and the sulfur-based compound is 100: 0.1-0.3: 0.1 to 0.3.
7. The preparation method according to claim 1, wherein the particle size of the ternary material powder is 3-15 μm.
8. The method according to claim 1, wherein the high-speed mixing is performed at a rotation speed of 300 to 500 rpm.
9. The method of claim 1, further comprising, after the high speed mixing:
the compound obtained by high speed mixing is sieved by a 300 mesh sieve.
10. A lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and an electrolyte, and is characterized in that the positive electrode comprises the lithium ion battery positive electrode material of any one of claims 1 to 4 or the lithium ion battery positive electrode material prepared by the preparation method of any one of claims 5 to 9.
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