CN111952585A - High-compaction-density rubidium-doped lithium battery positive electrode material and preparation method thereof - Google Patents
High-compaction-density rubidium-doped lithium battery positive electrode material and preparation method thereof Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
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- H01M4/625—Carbon or graphite
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a high compaction density rubidium-doped lithium battery positive electrode material and a preparation method thereof, wherein the preparation method comprises the following steps: s1) uniformly mixing a nickel source, a cobalt source, a manganese source, a lithium source, a rubidium source and a cesium source, and calcining at 600-1000 ℃ for 5-10 h to obtain a precursor material; s2) annealing the precursor material after high-temperature calcination, then mixing the coating agent and the conductive nano carbon material, and placing the mixture in a ball mill for ball milling for 0.5-2h to obtain the lithium battery anode material. On one hand, the particle size of material particles is reduced through high-temperature calcination and grinding, and the compaction density of the material is increased; on the other hand, rubidium/cesium ions are doped to replace part of lithium ions, so that the effect of increasing the particle size is achieved, gaps inside particles are reduced, and meanwhile, the rubidium/cesium ions are doped to enable edges and corners of the particles to be smoother, so that the compaction density of the material is increased.
Description
Technical Field
The invention belongs to the field of preparation of lithium battery materials, and particularly relates to a high-compaction-density rubidium-doped lithium battery positive electrode material and a preparation method thereof.
Background
The lithium ion battery has the advantages of high working voltage, large specific energy, light weight, small volume, long cycle life, no memory effect, quick charge and discharge, small environmental pollution and the like, is more and more widely applied to electric automobiles and hybrid electric automobiles, and is the most attractive energy storage mode at present.
The low compaction density of the lithium battery cathode material is always one of the main problems affecting the performance of the lithium battery. At present, the main methods for improving the compaction density of the lithium battery positive electrode material comprise: the amount of the conductive agent and the binder is reduced by coating, doping and the like so as to improve the compaction density. The doping modification is to improve the stability of the material structure, to improve the electronic conductivity and ionic conductivity of the material, to reduce the cation mixing and to increase the output power density of the battery by changing the lattice constant of the material or the valence state of some elements in the material. Patent application CN108023078A discloses a method for doping metal ions to prepare a high-nickel ternary cathode material with a single crystal morphology, which can enhance the cycle performance of the high-nickel ternary cathode material; however, the material prepared by the method has uneven particle size, unstable performance and low compaction density.
Disclosure of Invention
Aiming at the technical problem of low compaction density of the lithium battery positive electrode material in the prior art, the invention provides a high compaction density rubidium-doped lithium battery positive electrode material and a preparation method thereof, on one hand, the particle size of material particles is reduced through high-temperature calcination and grinding, and the compaction density of the material is increased; on the other hand, rubidium/cesium ions are selected to be doped to replace part of lithium ions, so that the effect of increasing the particle size is achieved, the gaps inside the particles are reduced, and the real density of the material is increased.
In order to achieve the purpose, the invention provides a high compaction density rubidium-doped lithium battery positive electrode material, which takes a ternary nickel-cobalt-manganese positive electrode material (NCM) as a matrix and is doped with a rubidium compound and a cesium compound.
In addition, the invention also provides a preparation method of the high-compaction-density rubidium-doped lithium battery positive electrode material, which comprises the following steps:
s1) uniformly mixing a nickel source, a cobalt source, a manganese source, a lithium source, a rubidium source and a cesium source, and calcining at 600-1000 ℃ for 5-10 h to obtain a precursor material;
s2) annealing the precursor material after high-temperature calcination, then mixing the coating agent and the conductive nano carbon material, and placing the mixture in a ball mill for grinding for 0.5-2h to obtain the high-compaction-density rubidium-doped lithium battery positive material;
s3) mixing the lithium battery positive electrode material prepared in the step S2) with a conductive agent and a binder according to the mass ratio of 5-6: 1-2: carrying out ultrasonic treatment for 2-4 h after 0.5-1 blending to obtain high-compaction-density rubidium-doped lithium battery anode material slurry;
s4) coating the lithium battery positive electrode material slurry prepared in the step S3) on the surface of an aluminum foil in a blade coating mode, and drying the aluminum foil in a vacuum environment at 80-120 ℃ for 8-12 hours to obtain the high-compaction-density rubidium-doped lithium battery positive electrode plate.
Preferably, the nickel source in step S1) is nickel nitrate (Ni (NO)3)2) Nickel sulfate (NiSO)4) Or nickel carbonate (NiCO)3) Etc.; the cobalt source is cobalt carbonate (CoCO)3) Cobalt sulfate (CoSO)4) Or cobalt nitrate (Co (NO)3)2) Etc.; the manganese source is manganese carbonate (MnCO)3) Cobalt nitrate (Mn (NO)3)2) Or manganese acetate (Mn (CH)3COO)2) Etc.; the lithium source is lithium hydroxide (LiOH) or lithium carbonate (Li)2CO3) Etc.; the rubidium source is rubidium hydroxide (RbOH) or rubidium carbonate (Rb)2CO3) Etc.; the cesium source is cesium carbonate (Cs)2CO3) Or cesium bicarbonate (CsHCO)3) And the like.
Preferably, the mass ratio of the nickel source, the cobalt source, the manganese source, the lithium source, the rubidium source, the cesium source, the coating agent and the conductive nano carbon material is 5-10: 2-4: 2-4: 1-3: 0.5-1: 0.3-0.7: 10-20: 0.5 to 2.
Preferably, the coating agent in the step S2) is a polyamide solution or a polyvinylpyrrolidone solution, the mass fraction is controlled within a range of 2 to 5 wt%, and N-methyl pyrrolidone is used as a solvent.
Preferably, the conductive nanocarbon material of step S2) consists of carbon nanotubes and conductive carbon black; the using amounts of the carbon nano tube and the conductive carbon black are respectively 0.02-0.04 wt% and 0.6-1.0 wt% of the total mass of the positive active substance; the total mass of the positive active material is the total mass of a nickel source, a cobalt source, a manganese source and a lithium source, and the total mass of the positive active material comprises 0.02-0.04 wt% of carbon nano tubes and 0.6-1.0 wt% of conductive carbon black in percentage by mass.
Preferably, the diameter of the carbon nano tube is 2-7 nm, and the length of the carbon nano tube is 2-15 um; the specific surface area of the conductive carbon black is 50-100 m2The particle diameter of the particles is 20-35 nm.
Preferably, the conductive agent is acetylene black or Super-P, etc.; the binder is polyvinylidene fluoride (PVDF) or sodium carboxymethyl cellulose (CMC) and the like.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects: on one hand, the particle size of material particles is reduced through high-temperature calcination and grinding, and the compaction density of the material is increased; on the other hand, rubidium/cesium ions are selected for doping to replace part of lithium ions, so that the effect of increasing the particle size is achieved, gaps inside particles are reduced, and meanwhile, the rubidium/cesium ions are doped to enable the edges and corners of the particles to be smoother, so that the compaction density of the material is increased.
Drawings
FIG. 1 is a graph showing the cycle charge and discharge curves of electrode sheets prepared according to example 1 of the present invention and comparative example 1, respectively.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
A preparation method of a high-compaction-density rubidium-doped lithium battery positive electrode material comprises the following specific steps:
s1) uniformly mixing 5 parts of nickel nitrate, 2 parts of cobalt carbonate, 2 parts of manganese carbonate, 1 part of lithium carbonate, 0.5 part of rubidium carbonate and 0.3 part of cesium carbonate according to parts by mass, and calcining the mixture in a tubular furnace at the high temperature of 600 ℃ for 10 hours to obtain a precursor material.
S2) annealing the precursor material calcined at high temperature in step S1), and then mixing 10 parts of polyamide solution (with N-methylpyrrolidone as a solvent) with a content of 2 wt% and 1 part of conductive nanocarbon material (the conductive nanocarbon material is composed of carbon nanotubes and conductive carbon black) based on the mass parts in step S1; the using amounts of the carbon nano tube and the conductive carbon black are respectively 0.02 wt% and 0.6 wt% of the total mass of the positive active material, and the total mass of the positive active material is the total mass of the nickel source, the cobalt source, the manganese source and the lithium source; wherein the diameter of the carbon nano tube is about 2nm, the length is about 2um, and the specific surface of the conductive carbon black is 50m2About/g, the particle size of the particles is about 20 nm), and placing the particles in a ball mill for grinding for 0.5h to obtain the high-compaction-density rubidium-doped lithium battery anode material;
s3) mixing the high-compaction-density rubidium doped lithium battery positive electrode material prepared in the step S2) with acetylene black and polyvinylidene fluoride according to the mass ratio of 5: 1: carrying out ultrasonic treatment for 2h after 0.5 blending to obtain high-compaction-density rubidium-doped lithium battery anode material slurry;
s4) uniformly coating the high-compaction-density rubidium-doped lithium battery positive electrode material slurry prepared in the step S3) on the surface of an aluminum foil in a blade coating mode, and then drying for 12 hours in a vacuum environment at 80 ℃ to obtain the high-compaction-density rubidium-doped lithium battery positive electrode plate.
The electrode plate obtained in the example 1 is rolled under the pressure of 30-40Mpa, the surface density of the rolled plate reaches 2.54g/cm3, the gram capacity of lithium iron phosphate is more than 165.2mAh/g, and the cycle performance is more than 93 percent (1000 cycles).
In addition, the electrode plate not doped with rubidium source is prepared as a comparison sample 1 according to the steps of the embodiment, and the electrode plate is pressed and molded under the pressure of 30-40MPa, and the surface density of the rolled electrode plate is 2.43g/cm3About 143.3mAh/g of lithium iron phosphate gram capacity, and the cycle performance is only kept about 84% (1000 cycles).
Example 2
A preparation method of a high-compaction-density rubidium-doped lithium battery positive electrode material comprises the following specific steps:
s1) uniformly mixing 10 parts of nickel sulfate, 4 parts of cobalt sulfate, 4 parts of manganese nitrate, 3 parts of lithium hydroxide, 1 part of rubidium hydroxide and 0.7 part of cesium bicarbonate according to the mass parts, and calcining for 5 hours in a tubular furnace at the high temperature of 1000 ℃ to obtain a precursor material.
S2) annealing the precursor material calcined at high temperature in the step S1), and then mixing 20 parts of polyvinylpyrrolidone solution (with N-methyl pyrrolidone as a solvent) with the content of 5 wt% and 1 part of conductive nanocarbon material (consisting of carbon nanotubes and conductive carbon black according to the mass part of the step S1); the using amounts of the carbon nano tube and the conductive carbon black are respectively 0.04 wt% and 1 wt% of the total mass of the positive active material, and the total mass of the positive active material is the total mass of the nickel source, the cobalt source, the manganese source and the lithium source; wherein the diameter of the carbon nano tube is about 7nm, the length is about 15um, and the specific surface of the conductive carbon black is 100m2About/g, the particle size is about 35 nm), and placing the mixture in a ball mill for grinding for 2 hours to obtain the high-compaction-density rubidium-doped lithium battery anode material;
s3) mixing the high-compaction-density rubidium-doped lithium battery positive electrode material prepared in the step S2) with Super-P and sodium hydroxymethyl cellulose according to the mass ratio of 6: 2: 1, carrying out ultrasonic treatment for 4 hours after blending to obtain the high-compaction-density rubidium-doped lithium battery anode material slurry.
S4) uniformly coating the high-compaction-density rubidium-doped lithium battery positive electrode material slurry prepared in the step S3) on the surface of an aluminum foil in a blade coating mode, and then drying for 8 hours in a vacuum environment at 120 ℃ to obtain the high-compaction-density rubidium-doped lithium battery positive electrode plate.
The electrode plate obtained in the example 2 is rolled under the pressure of 30-40Mpa, the surface density of the rolled plate reaches 2.56g/cm3, the gram capacity of lithium iron phosphate is more than 165.4mAh/g, and the cycle performance is more than 93 percent (1000 cycles).
In addition, the electrode plate not doped with rubidium source is prepared as a comparison sample 2 according to the steps of the embodiment, and the electrode plate is pressed and molded under the pressure of 30-40MPa, and the surface density of the rolled electrode plate is 2.45g/cm3About 143.7mAh/g of lithium iron phosphate gram capacity, and the cycle performance is only kept about 84% (1000 cycles).
Characteristics of the positive electrode plate of the rubidium-doped lithium battery prepared in examples 1-2 and comparative examples 1-2 are shown in table 1, and an overall result shows that the compaction density of the positive electrode material can be obviously increased by doping rubidium/cesium ions, and the ionic conductivity of the lithium battery composite diaphragm can be obviously improved.
TABLE 1
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The high-compaction density rubidium doped lithium battery positive electrode material is characterized in that a ternary nickel-cobalt-manganese positive electrode material is used as a matrix and is doped with a rubidium compound and a cesium compound.
2. The high tap density rubidium doped lithium battery positive electrode material as claimed in claim 1, wherein the rubidium source adopted by the rubidium compound is rubidium hydroxide or rubidium carbonate; the cesium compound adopts cesium source as cesium carbonate or cesium bicarbonate.
3. The preparation method of the high-compaction-density rubidium-doped lithium battery positive electrode material is characterized by comprising the following steps of:
s1) uniformly mixing a nickel source, a cobalt source, a manganese source, a lithium source, a rubidium source and a cesium source, and calcining at 600-1000 ℃ for 5-10 h to obtain a precursor material;
s2) annealing the precursor material after high-temperature calcination, then mixing the coating agent and the conductive nano carbon material, and placing the mixture in a ball mill for grinding for 0.5-2h to obtain the high-compaction-density rubidium-doped lithium battery positive material.
4. The preparation method according to claim 3, wherein the mass ratio of the nickel source, the cobalt source, the manganese source, the lithium source, the rubidium source, the cesium source, the coating agent and the conductive nanocarbon material is 5-10: 2-4: 2-4: 1-3: 0.5-1: 0.3-0.7: 10-20: 0.5 to 2.
5. The method of claim 3, further comprising the steps of:
s3) mixing the lithium battery positive electrode material prepared in the step S2) with a conductive agent and a binder according to the mass ratio of 5-6: 1-2: carrying out ultrasonic treatment for 2-4 h after 0.5-1 blending to obtain lithium battery anode material slurry;
s4) coating the lithium battery positive electrode material slurry prepared in the step S3) on the surface of an aluminum foil in a blade coating mode, and drying the aluminum foil in a vacuum environment at 80-120 ℃ for 8-12 hours to obtain the high-compaction-density rubidium-doped lithium battery positive electrode plate.
6. The method according to claim 5, wherein the conductive agent is acetylene black or Super-P; the binder is polyvinylidene fluoride or sodium hydroxymethyl cellulose.
7. The method according to claim 3, wherein the nickel source of step S1) is nickel nitrate, nickel sulfate or nickel carbonate; the cobalt source is cobalt carbonate, cobalt sulfate or cobalt nitrate; the manganese source is manganese carbonate, cobalt nitrate or manganese acetate; the lithium source is lithium hydroxide or lithium carbonate; the rubidium source is rubidium hydroxide or rubidium carbonate; the cesium source is cesium carbonate or cesium bicarbonate.
8. The preparation method according to claim 3, wherein the coating agent in step S2) is polyamide or polyvinylpyrrolidone solution, the mass fraction is 2-5 wt%, and N-methylpyrrolidone is used as a solvent.
9. The method according to claim 3, wherein the one part of the conductive nanocarbon material of step S2) consists of carbon nanotubes and conductive carbon black; the using amounts of the carbon nano tube and the conductive carbon black are respectively 0.02-0.04 wt% and 0.6-1.0 wt% of the total mass of the positive active substance; the total mass of the positive electrode active material is the total mass of the nickel source, the cobalt source, the manganese source and the lithium source.
10. The method of claim 9, wherein the carbon nanotubes have a diameter of 2 to 7nm and a length of 2 to 15 um; the specific surface area of the conductive carbon black is 50-100 m2The particle diameter of the particles is 20-35 nm.
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