CN110690432A - Lithium silicon carbon composite material for lithium ion battery and preparation method and application thereof - Google Patents
Lithium silicon carbon composite material for lithium ion battery and preparation method and application thereof Download PDFInfo
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- CN110690432A CN110690432A CN201910981716.7A CN201910981716A CN110690432A CN 110690432 A CN110690432 A CN 110690432A CN 201910981716 A CN201910981716 A CN 201910981716A CN 110690432 A CN110690432 A CN 110690432A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 lithium silicon carbon composite material for a lithium ion battery, which comprises the following raw materials in percentage by weight: 5-30% of lithium metal, 10-50% of silicon material and 20-85% of carbon material. The invention also provides a preparation method and application of the lithium silicon carbon composite material for the lithium ion battery. Compared with the traditional silicon-carbon material, the lithium silicon-carbon composite material for the lithium ion battery prepared by the invention obviously improves the first charge-discharge efficiency and improves the cycle and expansion.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lithium silicon carbon composite material for a lithium ion battery, and a preparation method and application thereof.
Background
Lithium ion batteries have the advantages of high voltage, high energy density, and long cycle life, and thus are one of the most widely used secondary batteries. However, with the miniaturization and continuous development of long standby time of portable electronic devices and the use of high-power and high-energy devices such as electric bicycles and electric automobiles, higher and higher requirements are made on the energy density of lithium ion batteries as energy storage power sources. For the current commercial graphite material, the utilization rate and the approach to the limit are adopted, new materials are continuously developed to make up the defects of the graphite material, and the existing silicon-carbon material has the problems of low first charge-discharge efficiency, large volume expansion and serious cycle attenuation, so that the mass production cannot be realized at a later time.
In addition, due to the limitation of the prior art, the ultrathin lithium strip can only be manufactured to 20 micrometers, while the graphite (negative electrode) only needs 3 micrometers, and the prior art is easy to cause excessive lithium supplement. The lithium powder has high activity and is easy to react with a solvent; and the lithium powder has large specific surface area, is easy to react with water in the environment, causes the failure of the material, and has high requirements on the production environment. And the high activity of lithium metal is not beneficial to homogenate coating.
Disclosure of Invention
In view of the above, the main objective of the present invention is to provide a lithium silicon carbon composite material for lithium ion batteries, and a preparation method and applications thereof.
In order to achieve the above purpose, in one aspect, the present invention provides a lithium silicon carbon composite material for a lithium ion battery, which comprises the following raw materials by weight: 5-30% of lithium metal, 10-50% of silicon material and 20-85% of carbon material.
Further, the lithium silicon carbon composite material for the lithium ion battery comprises the following raw materials in percentage by weight: 10-20% of lithium metal, 10-30% of silicon material and 55-80% of carbon material.
Further wherein the lithium metal comprises one of a lithium ribbon or a passivated lithium powder.
Further wherein the thickness of the lithium ribbon is less than or equal to 30 μm.
Further, the silicon material comprises at least one of silicon nanowires, silicon monoxide or silicon nanospheres, and the particle size of the silicon material is 1-10000 nm.
Further, the grain size of the silicon material is 200-5000 nm. The product with different particle sizes can be selected according to different requirements, for example, the particle size can be selected to be lower for manufacturing a high-power battery, and the particle size can be selected to be larger for manufacturing a high-energy density battery.
Further, the carbon material comprises at least one of artificial graphite and derivatives thereof, natural graphite and derivatives thereof, mesocarbon microbeads and derivatives thereof, soft carbon and derivatives thereof, and hard carbon and derivatives thereof, and has a particle size of 0.1-200 μm.
Further, wherein the particle size of the carbon material is 5 to 80 μm. Products with different particle sizes are selected according to different requirements, for example, the particle size of the product for manufacturing a high-power battery can be selected to be lower; the particle size can be selected to be larger for making a high energy density battery.
In order to achieve the above object, another aspect of the present invention provides a method for preparing the lithium-silicon-carbon composite material for the lithium ion battery, including the following steps:
mixing silicon material with carbon material, and grinding to obtain a first mixture;
adding lithium metal into the first mixture, heating, and grinding while introducing inert gas to obtain a second mixture;
spray drying and granulating the second mixture to obtain a granular material;
and cooling the particle material to room temperature in an inert gas environment to obtain the lithium-silicon-carbon composite material.
Further wherein the preparation method comprises the steps of:
sequentially adding the silicon material and the carbon material into a high-energy ball mill (30-35r/min) for mixing, and carrying out ball milling for 2-20 h to obtain a first mixture;
adding lithium metal into the first mixture of the high-energy ball mill, heating the ball mill at the temperature of 180 ℃ and 500 ℃, and simultaneously performing ball milling (30-35r/min) for 2-20 h by using inert gas to obtain a second mixture;
and adding the second mixture into a spray drying device (5000-30000rpm), and performing spray drying granulation at the temperature of 180-500 ℃ to obtain the granular material.
Further, wherein the preparation method further comprises: and cooling the granular material to room temperature in an inert gas environment, and sieving the granular material by using a sieve with 80-300 meshes to obtain the lithium silicon carbon composite material.
Further wherein the rotational speed of the spray drying apparatus is 15000 rpm; the specification of the screen is 200 meshes.
Further, the method also comprises the step of packaging after screening.
Further wherein the inert gas is selected from one of argon, nitrogen, helium, neon or xenon.
In order to achieve the above object, a further aspect of the present invention provides a lithium ion secondary battery comprising an anode including the above lithium silicon carbon composite.
Further, the lithium ion secondary battery further comprises a positive electrode matched with the negative electrode, and the positive electrode is selected from at least one of lithium iron phosphate, nickel-cobalt-manganese ternary materials and lithium-rich manganese-based materials.
In order to achieve the above object, the present invention provides an electric vehicle including a power source, the power source being a lithium ion secondary battery including a negative electrode, the negative electrode including the lithium silicon carbon composite material described above.
Further, the electric vehicle is an electric bicycle or an electric automobile.
The invention has the following beneficial effects:
according to the lithium-silicon-carbon composite material for the lithium ion battery, the active lithium metal is compounded with the silicon-carbon material in advance, so that the activity of the lithium metal is reduced, and the homogenate coating is possible, namely, the homogenate coating can be carried out by using the production equipment of the existing power battery, and under the condition of not changing the equipment and the process, the capacity and the energy density of a single battery are improved, the endurance mileage of an electric automobile is further improved, and the production cost of the single battery is reduced; if the previous lithium powder or lithium ribbon is used, the slurry coating is impossible due to the high activity of lithium metal; on the other hand, after the material is assembled into a battery for liquid injection, the material has a remarkable lithium supplementing effect; compared with the traditional silicon-carbon material, the first charge-discharge efficiency is obviously improved, the cycle is improved, the expansion is controlled, and a foundation is laid for the development of a subsequent battery with higher energy density; compared with the traditional lithium supplement method, the method overcomes the problem of environmental temperature and humidity control caused by a lithium powder coating method, and solves the problem of excessive lithium supplement caused by lithium supplement of an ultrathin lithium belt; aiming at batteries with different energy densities, the method can optimize materials and realize product diversification, is simple to operate and is suitable for large-scale production.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Materials, reagents and the like used in the following examples are commercially available.
Example 1: adding silicon material with the particle size of 500nm and carbon material with the particle size of 20 mu m (the mass ratio is 10%: 80%) into a high-energy ball mill (the rotating speed is 32r/min) for mixing, wherein the ball milling time is 5 h; adding passivated lithium powder (the mass ratio of the passivated lithium powder to the carbon material is 10%: 80%) into a high-energy ball mill, heating the ball mill at 200 ℃ to ensure that lithium metal is in a molten state, and carrying out ball milling under the protection of argon, wherein the ball milling time is 6 hours, and the rotating speed is 32 r/min; adding the ball-milled mixture into spray drying equipment, and performing spray drying granulation (the rotating speed is 15000rpm) at 220 ℃; the resulting particulate material was cooled to room temperature (25-30 ℃) in an inert gas (argon) atmosphere, and sieved with a 120-mesh sieve in a sieving machine to obtain a lithium silicon carbon composite material. And then, carrying out normal procedures such as homogenization and coating on the lithium silicon carbon composite material, and then forming a button cell with a lithium sheet to test the capacity, the first efficiency and the cycle performance.
Example 2: adding silicon material with the particle size of 800nm and carbon material with the particle size of 80 mu m (mass ratio is 30%: 55%) into a high-energy ball mill (rotating speed is 32r/min) for mixing, wherein the ball milling time is 7 h; adding passivated lithium powder (the mass ratio of the passivated lithium powder to the carbon material is 15%: 55%) into a high-energy ball mill, heating the ball mill at 250 ℃ to ensure that lithium metal is in a molten state, and carrying out ball milling under the protection of helium, wherein the ball milling time is 5h, and the rotating speed is 32 r/min; putting the ball-milled mixture into spray drying equipment, and performing spray drying granulation (the rotating speed is 15000rpm) at 300 ℃; cooling the obtained particle material to room temperature (25-30 ℃) in an inert gas (helium) environment, and screening the particle material by using a 160-mesh screen in a screening machine to obtain the lithium-silicon-carbon composite material; and then, carrying out normal procedures such as homogenization and coating on the lithium silicon carbon composite material, and then forming a button cell with a lithium sheet to test the capacity, the first efficiency and the cycle performance.
Example 3: putting a silicon material with the particle size of 1000nm and a carbon material with the particle size of 150 mu m (the mass ratio is 20%: 60%) into a high-energy ball mill (the rotating speed is 32r/min) for mixing, wherein the ball milling time is 10 h; cutting the ultrathin lithium belt (the mass ratio of the ultrathin lithium belt to the carbon material is 20%: 60%) into small sections (about 3cm x 3cm, the thickness is less than or equal to 30 microns), adding the small sections into a high-energy ball mill, heating the ball mill at the temperature of 300 ℃ to ensure that lithium metal is in a molten state, and carrying out ball milling under the protection of xenon for 5 hours; the rotating speed is 32 r/min; adding the ball-milled mixture into spray drying equipment, and performing spray drying granulation at 300 ℃ (the rotating speed is 20000 rpm); cooling the obtained granular material to room temperature (25-30 ℃) in an inert gas (xenon) environment, and screening the granular material by using a 160-mesh screen in a screening machine to obtain the lithium-silicon-carbon composite material; and then, carrying out normal procedures such as homogenization and coating on the lithium silicon carbon composite material, and then forming a button cell with a lithium sheet to carry out tests on capacity, first efficiency, cycle performance, rate performance and electrode sheet expansion.
Comparative example 1: and (3) carrying out normal procedures such as homogenizing and coating on a silicon-carbon (mass ratio of 15% to 85%) material, and then forming a button cell with a lithium sheet to test the capacity, the first efficiency, the cycle performance, the rate performance and the expansion of the electrode sheet.
Comparative example 2: after normal processes such as homogenizing and coating, the silicon-carbon (mass ratio of 15% to 85%) material is compounded with an ultrathin lithium belt (thickness is less than or equal to 30 μm) for lithium supplement, and after the lithium supplement operation is finished, the silicon-carbon material and a lithium sheet form a button cell for testing capacity, first efficiency, cycle performance, rate performance and sheet expansion.
The preparation method of the button cell batteries of the above embodiments 1 to 3 and the comparative example 1 specifically comprises the following steps:
s1, adding the lithium silicon carbon material (or the silicon carbon material in the comparative example 1) in any one of the embodiments 1-3, a conductive agent (graphene, conductive carbon black or carbon nano tube) and a binder (styrene butadiene rubber) into a solvent (benzene or ether) according to a mass ratio of 90:5:5, and uniformly stirring for 4 hours generally;
s2, performing single-side coating on the stirred slurry on a copper foil through experimental coating equipment, and controlling the coating speed and the coating thickness to be 30-60 mu m;
s3, putting the coated pole piece into an oven at 80-100 ℃ for drying for 6-16 h;
s4, placing the dried pole piece on rolling equipment for rolling, and ensuring that the thickness after rolling is 15-30 mu m;
s5, pressing the rolled pole pieces out of small round pieces (the diameter is 32 mm) through a button cell tablet press, then putting the small round pieces into a glove box to prepare button cell assembly, wherein the humidity in the glove box needs to be controlled to be lower than 5%, and helium gas is used for protection (because the lithium activity in the small round pieces is high);
s6, assembling the small round sheet, the diaphragm (polyethylene or polypropylene), the lithium sheet (with the diameter of 20 mm and the thickness of 50 microns), 1mol/L electrolyte (dimethyl carbonate, diethyl carbonate and ethylene carbonate in the volume ratio of 1:1:1, and the solute is lithium hexafluorophosphate) and the shell of the button cell (commercially available CR2016 phi 20 + 1.6mm and 304# stainless steel) in a certain sequence, and compacting the shell by button cell equipment to obtain the button cell.
The preparation method of the button cell of the comparative example 2 specifically comprises the following steps:
steps S1 to S3 are the same as steps S1 to S3 of examples 1 to 3 and comparative example 1, and steps S4 to S6 are as follows:
s4, placing the dried pole piece and the ultrathin lithium belt (the thickness is less than or equal to 30 mu m, the width is the same as that of the pole piece) on rolling equipment for rolling, and ensuring that the rolled thickness is 15-30 mu m;
s5, pressing the rolled pole piece and the ultrathin lithium belt out of a small wafer (the diameter is 32 mm) through a button cell tablet press, then putting the small wafer into a glove box to prepare button cell assembly, wherein the humidity in the glove box needs to be controlled to be lower than 5%, and helium gas is used for protection (because the lithium activity in the small wafer is high);
s6, assembling the small round sheet, the diaphragm (polyethylene or polypropylene), the lithium sheet (with the diameter of 20 mm and the thickness of 50 microns), 1mol/L electrolyte (dimethyl carbonate, diethyl carbonate and ethylene carbonate in the volume ratio of 1:1:1, and the solute is lithium hexafluorophosphate) and the shell of the button cell (commercially available CR2016 phi 20 + 1.6mm and 304# stainless steel) in a certain sequence, and compacting the shell by button cell equipment to obtain the button cell.
And standing the assembled button cell for 10-20h, and testing the capacity, the first efficiency, the cycle performance, the rate performance and the expansion of a pole piece.
And (3) capacity testing process: the voltage setting range is 0-2.0V, the current is set to be 0.01C, the cycle is twice, the equipment automatically records the first charge-discharge capacity and the second charge-discharge capacity, and the first efficiency (the ratio of the first charge capacity to the first discharge capacity) is calculated through twice data;
the cycle performance test process: the voltage setting range is 0-2.0V, the charging and discharging current is set to be 0.05C, and the equipment automatically records the capacity of each cycle;
discharge rate test flow: setting the assembled button type electric voltage range to be 0-2V, setting the charging current to be 0.1C, and discharging to cut-off voltage by using 1C current after full charge; then the battery is fully charged by 0.1C; discharging to cut-off voltage by using 2C current after full charge;
expansion ratio calculation process: disassembling the assembled battery in a drying room after the assembled battery is fully charged, measuring the thickness of a pole piece by using a micrometer, and comparing the thickness with the pole piece of the battery which is not assembled to calculate the expansion rate;
TABLE 1 comparison of first Charge-discharge efficiency and cycle Retention ratio between inventive examples 1-3 and comparative examples 1-2
As can be seen from the test data in table 1, the lithium silicon carbon negative electrode material prepared in examples 1 to 3 of the present invention not only can improve the first charge and discharge efficiency, but also can significantly improve the problem of poor cycle of the original silicon carbon negative electrode, although comparative example 2 also improves the first charge and discharge efficiency and cycle performance after ultra-thin lithium ribbon compounding, since the lithium supplement is excessive, the battery is short-circuited and the capacity becomes 0 when the cycle is performed between 100 and 200 times, because the excessive lithium cannot react with the negative electrode, is precipitated on the surface of the negative electrode, becomes a lithium-philic active site during the cycle, and causes lithium dendrites to grow along the direction of the separator, and the lithium dendrites pierce the separator to cause the battery short-circuit and fail when the cycle is performed for a certain number of times; on one hand, the invention improves the first charge-discharge efficiency and improves the cycle, on the other hand, the invention avoids the problem of lithium precipitation caused by compounding the traditional lithium belt, and has simple operation and easy large-scale production.
TABLE 2 discharge Rate and expansion comparison of inventive examples 1-3 and comparative examples 1-2
As can be seen from the test data in table 2, the lithium silicon carbon composite materials for lithium ion batteries prepared in examples 1 to 3 of the present invention are superior to those of comparative examples 1 to 2 in the index of rate and full-current expansion; although comparative example 1 was improved in full electrical expansion as compared with comparative example 2, it was increased in full electrical expansion as compared with examples 1-3 because the recombination of the lithium ribbon itself and the negative electrode was on the surface of the negative electrode sheet, and the bonding with the negative electrode was not uniform; in the case of examples 1 to 3, since the lithium intercalation of the composite material was completed before the battery was used normally, the full-charge expansion was reduced, and the energy density and capacity of the battery were improved within the same volume.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (13)
1. The lithium silicon carbon composite material for the lithium ion battery is characterized by comprising the following raw materials in percentage by weight: 5-30% of lithium metal, 10-50% of silicon material and 20-85% of carbon material.
2. The lithium silicon carbon composite material for the lithium ion battery according to claim 1, wherein the lithium silicon carbon composite material for the lithium ion battery comprises the following raw materials in percentage by weight: 10-20% of lithium metal, 10-30% of silicon material and 55-80% of carbon material.
3. The lithium silicon carbon composite for a lithium ion battery according to claim 1 or 2, wherein the lithium metal comprises one of a lithium ribbon or a passivated lithium powder.
4. The lithium silicon carbon composite material for a lithium ion battery according to claim 3, wherein the thickness of the lithium ribbon is 30 μm or less.
5. The lithium silicon carbon composite material for a lithium ion battery according to claim 1 or 2, wherein the silicon material comprises at least one of silicon nanowires, silicon monoxide or silicon nanospheres, and has a particle size of 1 to 10000 nm.
6. The lithium silicon carbon composite material for the lithium ion battery as claimed in claim 5, wherein the particle size of the silicon material is 200-5000 nm.
7. The lithium silicon carbon composite material for a lithium ion battery according to claim 1 or 2, wherein the carbon material comprises at least one of artificial graphite and derivatives thereof, natural graphite and derivatives thereof, mesocarbon microbeads and derivatives thereof, soft carbon and derivatives thereof, and hard carbon and derivatives thereof, and has a particle size of 0.1 to 200 μm.
8. The lithium silicon carbon composite material for a lithium ion battery according to claim 7, wherein the particle size of the carbon material is 5 to 80 μm.
9. A method for preparing a lithium silicon carbon composite material for a lithium ion battery according to any one of claims 1 to 8, comprising the steps of:
mixing silicon material with carbon material, and grinding to obtain a first mixture;
adding lithium metal into the first mixture, heating, and grinding while introducing inert gas to obtain a second mixture;
spray drying and granulating the second mixture to obtain a granular material;
and cooling the particle material to room temperature in an inert gas environment to obtain the lithium-silicon-carbon composite material.
10. The method of claim 9, comprising the steps of:
sequentially adding the silicon material and the carbon material into a high-energy ball mill for mixing, and carrying out ball milling for 2-20 h to obtain a first mixture;
adding lithium metal into the first mixture of the high-energy ball mill, heating the ball mill at the temperature of 180 ℃ to 500 ℃, and performing ball milling for 2-20 h while passing through inert gas to obtain a second mixture;
and adding the second mixture into a spray drying device, and carrying out spray drying granulation at 180-500 ℃ to obtain the granular material.
11. The method of claim 10, further comprising:
and cooling the granular material to room temperature in an inert gas environment, and sieving the granular material by using a sieve with 80-300 meshes to obtain the lithium silicon carbon composite material.
12. A lithium ion secondary battery, characterized in that a negative electrode of the lithium ion secondary battery comprises the lithium silicon carbon composite material according to any one of claims 1 to 8.
13. An electric vehicle comprising a power source, wherein the power source is a lithium ion secondary battery, and wherein a negative electrode of the lithium ion secondary battery comprises the lithium silicon carbon composite material according to any one of claims 1 to 8.
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