CN114436238A - Preparation method of low-expansion silicon-carbon negative electrode material for lithium ion battery - Google Patents
Preparation method of low-expansion silicon-carbon negative electrode material for lithium ion battery Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- 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
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- 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
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Abstract
The invention discloses a preparation method of a low-expansion silicon-carbon negative electrode material for a lithium ion battery, which comprises the following steps of: adding silicon powder, a binder, a pore-forming agent and a solvent into a sand mill according to a certain proportion, and grinding to obtain silicon slurry; drying the obtained silicon slurry into powder to obtain a silicon-carbon precursor; and finally, placing the obtained silicon-carbon precursor in a nitrogen atmosphere protective furnace for sintering, and crushing and screening to obtain the silicon-carbon negative electrode material. According to the method, the pore-forming agent is subjected to full thermal decomposition pore-forming on the surface of silicon powder, a primary pore framework is realized, asphalt flows to coat the surface of the pore framework, a silicon carbon material which is porous inside and uniformly and compactly coated on the surface is formed, the internal porosity formed after carbonization can effectively buffer the volume expansion of silicon, meanwhile, the coating layer with the compact surface can realize low specific surface area, the interface is improved, and the silicon carbon cathode capacity, the first efficiency and the power performance can be greatly improved.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a low-expansion silicon-carbon negative electrode material for a lithium ion battery.
Background
The lithium ion battery has the characteristics of high working voltage, high energy density, wide working temperature, long cycle life, no memory effect, environmental friendliness and the like, and is widely applied to the fields of power batteries of automobiles, electric bicycles and the like, the fields of energy storage of power grids, industrial energy storage, household energy storage, communication energy storage and the like, and the fields of 3C digital codes of smart phones, notebook computers, intelligent wearable equipment, mobile power supplies and the like.
The current commercialized lithium battery negative electrode materials are mainly modified natural graphite and artificial graphite, although the preparation technology is quite mature, the theoretical specific capacity of the lithium battery negative electrode materials is only 372mAh/g, and the requirement of the market on a high-capacity lithium ion battery is difficult to meet, so that the current research and development of a silicon-carbon negative electrode with higher gram capacity are increased. Although the capacity of the silicon carbon negative electrode is high, the expansion is very large, and about 300% volume expansion can be achieved in the fully charged state. For example, the chinese invention patent CN109659551A discloses a preparation method of a silicon negative electrode material for a low expansion lithium ion battery, which comprises the steps of dispersing nano silicon powder in ultrapure water to prepare silicon slurry; adding benzenediol, formaldehyde and sodium carbonate into the silicon slurry to prepare silica sol; forming silica sol to obtain silica gel; aging and carbonizing the silica gel to obtain a carbonized material; crushing and grading the carbonized material to obtain a silicon-carbon composite material A; impregnating the silicon-carbon composite material A by adopting mesophase pitch, and coating the surface of the silicon-carbon composite material A to obtain a coating material B; and carbonizing and sieving the coating material B to obtain the silicon negative electrode material for the low-expansion lithium ion battery. The method has complex steps, multi-step heat treatment, high energy consumption and is not beneficial to industrialization.
Therefore, there is a need for an improved method for preparing silicon negative electrode materials for low expansion lithium ion batteries.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a low-expansion silicon-carbon negative electrode material for a lithium ion battery, which is simple in process and low in energy consumption, thereby further reducing the cost, facilitating popularization and application, and facilitating industrialization.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a low-expansion silicon-carbon negative electrode material for a lithium ion battery comprises the following steps:
(1) mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: (0.05-0.5): (0.05-0.1): (0.5-2.0) adding the mixture into a sand mill to be ground for 1-5h, wherein the grinding speed is 500-2500r/min, and obtaining silicon slurry;
(2) and (3) granulation: drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of spray drying is 150-;
(3) carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1100-1500 ℃ at the heating rate of 2-25 ℃/min, preserving the heat for 6-12 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
Preferably, the silicon powder D50 in the step (1) has a spherical morphology ranging from 20 nm to 100 nm.
Preferably, the binder in step (1) is one or a mixture of coal-based asphalt and oil-based asphalt, and the softening point of the binder is 50-200 ℃.
Preferably, the pore-forming agent in step (1) is one or more of ammonium bicarbonate, ammonium carbonate, ammonium oxalate, ammonium nitrate, ammonium phosphate and ammonium hydrogen phosphate.
Preferably, the solvent in step (1) is one or more of benzene, toluene and xylene.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
according to the method, a simple three-step method is adopted, the integrated preparation of pore forming and coating is realized, the pore forming agent is subjected to full thermal decomposition pore forming on the surface of silicon powder, a primary pore framework is realized, asphalt flows to coat the surface of the pore framework, a silicon carbon material which is porous inside and uniformly and densely coated on the surface is formed, the internal porosity formed after carbonization can effectively buffer the volume expansion of silicon, meanwhile, the coating layer with the dense surface can realize low specific surface area, the interface is improved, and the capacity, the first efficiency and the power performance of the silicon carbon cathode can be greatly improved. Moreover, the method has the advantages of simple process, simple operation and lower energy consumption, thereby further reducing the cost, being convenient for popularization and application and being beneficial to industrialization.
To more clearly illustrate the features and effects of the present invention, the present invention is described in detail below with reference to specific examples.
Detailed Description
The invention discloses a preparation method of a low-expansion silicon-carbon negative electrode material for a lithium ion battery, which comprises the following steps of:
(1) mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: (0.05-0.5): (0.05-0.1): (0.5-2.0) adding the mixture into a sand mill to be ground for 1-5h, wherein the grinding speed is 500-2500r/min, and obtaining silicon slurry; the silicon powder D50 is 20-100nm, and is spherical; the binder is one or a mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃; the pore-forming agent is one or more than two of ammonium bicarbonate, ammonium carbonate, ammonium oxalate, ammonium nitrate, ammonium phosphate and ammonium hydrogen phosphate; the solvent is one or more than two of benzene, toluene and xylene.
(2) And (3) granulation: and (2) drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of spray drying is 150-300 ℃, the air outlet temperature is 100-150 ℃, and the constant flow pump rotation rate is 50-100r/min, so as to obtain the silicon-carbon precursor.
(3) Carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1100-1500 ℃ at the heating rate of 2-25 ℃/min, preserving the heat for 6-12 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
The invention is illustrated in more detail below in the following examples:
example 1
(1) Mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: 0.05: 0.05: adding the silicon slurry into a sand mill according to the mass ratio of 0.5, and grinding for 1h at the grinding speed of 500r/min to obtain silicon slurry; the silicon powder D50 is 20-100nm and is spherical; the binder is coal-series asphalt with the softening point of 50-200 ℃; the pore-forming agent is ammonium bicarbonate; the solvent is benzene.
(2) And (3) granulation: drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of spray drying is 200 ℃, the air outlet temperature is 120 ℃, and the constant flow pump rotation speed is 80r/min, so as to obtain a silicon-carbon precursor;
(3) carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) into a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1200 ℃ at the heating rate of 20 ℃/min, preserving the heat for 8 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
Example 2
(1) Mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: 0.5: 0.1: 2.0, adding the mixture into a sand mill to be ground for 5 hours at the grinding speed of 2500r/min to obtain silicon slurry; the silicon powder D50 is 20-100nm and is spherical; the binder is oil-based asphalt with a softening point of 50-200 ℃; the pore-forming agent is ammonium carbonate; the solvent is toluene.
(2) And (3) granulation: and (2) drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of the spray drying is 180 ℃, the air outlet temperature is 140 ℃, and the constant flow pump rotation speed is 55r/min, so as to obtain the silicon-carbon precursor.
(3) Carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) into a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1250 ℃ at a heating rate of 15 ℃/min, preserving the heat for 10 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
Example 3
(1) Mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: 0.1: 0.08: 1, grinding for 3 hours by a sand mill at a grinding speed of 1500r/min to obtain silicon slurry; the silicon powder D50 is 20-100nm and is spherical; the binder is a mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃; the pore-forming agent is oxalic acid ammonium; the solvent is xylene.
(2) And (3) granulation: and (2) drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of spray drying is 150 ℃, the air outlet temperature is 100 ℃, and the constant flow pump rotation speed is 50r/min, so as to obtain the silicon-carbon precursor.
(3) Carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) into a nitrogen atmosphere protection furnace for sintering, raising the temperature to 1200 ℃ at the heating rate of 8 ℃/min, preserving the heat for 8 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
Example 4
(1) Mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: 0.2: 0.09: 1, grinding for 3 hours by a sand mill at the grinding speed of 500-; the silicon powder D50 is 20-100nm and is spherical; the binder is coal-series asphalt with the softening point of 50-200 ℃; the pore-forming agent is ammonium nitrate; the solvent is a mixture of benzene and toluene.
(2) And (3) granulation: and (2) drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of the spray drying is 300 ℃, the air outlet temperature is 150 ℃, and the constant flow pump rotation speed is 100r/min, so as to obtain the silicon-carbon precursor.
(3) Carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) into a nitrogen atmosphere protection furnace for sintering, raising the temperature to 1400 ℃ at a heating rate of 15 ℃/min, preserving the temperature for 10 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
(1) Mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: 0.2: 0.09: 1, grinding for 3 hours by adding a sand mill at the grinding speed of 12500r/min to obtain silicon slurry; the silicon powder D50 is 20-100nm and is spherical; the binder is coal-series asphalt with the softening point of 50-200 ℃; the pore-forming agent is ammonium phosphate; the solvent is benzene.
(2) And (3) granulation: and (2) drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of spray drying is 200 ℃, the air outlet temperature is 120 ℃, and the constant flow pump rotation speed is 80r/min, so as to obtain the silicon-carbon precursor.
(3) Carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) into a nitrogen atmosphere protection furnace for sintering, raising the temperature to 1100 ℃ at the heating rate of 2 ℃/min, preserving the heat for 6 hours, crushing and screening to obtain the silicon-carbon negative electrode material.
Example 6
(1) Mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: 0.2: 0.09: 1, grinding for 3 hours by a sand mill at a grinding speed of 1500r/min to obtain silicon slurry; the silicon powder D50 is 20-100nm and is spherical; the binder is coal-series asphalt with the softening point of 50-200 ℃; the pore-forming agent is ammonium hydrogen phosphate; the solvent is a mixture of benzene and toluene.
(2) And (3) granulation: and (2) drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of the spray drying is 300 ℃, the air outlet temperature is 120 ℃, and the constant flow pump rotation speed is 80r/min, so as to obtain the silicon-carbon precursor.
(3) Carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) into a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1500 ℃ at the heating rate of 25 ℃/min, preserving the heat for 12 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
Performance testing
The silicon-carbon negative electrode material prepared in each example and the silicon-carbon negative electrode material obtained in comparative example 1 without adding pore-forming agent were coated, and the performance of the silicon-carbon negative electrode material obtained in other steps which are the same as those of each example was tested, and the test performance is shown in table 1 below.
TABLE 1
As can be seen from Table 1, the prepared silicon-carbon negative electrode material has excellent capacity performance, cycle performance, first charge-discharge efficiency, low expansion performance and rate capability. The double-carbon-layer structure formed by the pore-forming agent and the binder plays a very critical role, realizes pore-forming buffer expansion, realizes low specific surface area, reduces interfacial resistance and improves performances in all aspects.
Test method
(1) The specific surface area of the material was measured using a Micromeritics TriStar II 3020 specific surface area apparatus from Mach instruments, USA;
(2) the anode material, SBR (solid content 50%), CMC and Super-p (weight ratio) of the above examples and comparative examples are mixed with a proper amount of deionized water to form slurry, the slurry is coated on a copper foil and dried in a vacuum drying oven for 12 hours to prepare an anode piece, electrolyte is 1M, LiPF is added6And the/EC + DEC + DMC is 1: 1, the polypropylene microporous membrane is a diaphragm, the counter electrode is a lithium sheet, and the battery is assembled. And (3) carrying out a constant-current charge and discharge experiment in the LAND battery test system, limiting the charge and discharge voltage to be 0.01-3.0V, carrying out data acquisition and control by using a charge and discharge cabinet controlled by a computer, and measuring the pole piece bounce under full power.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (5)
1. A preparation method of a low-expansion silicon-carbon negative electrode material for a lithium ion battery is characterized by comprising the following steps of: the method comprises the following steps:
(1) mixing materials: silicon powder, a binder, a pore-forming agent and a solvent are mixed according to the proportion of 1: (0.05-0.5): (0.05-0.1): (0.5-2.0) adding the mixture into a sand mill to be ground for 1-5h, wherein the grinding speed is 500-2500r/min, and obtaining silicon slurry;
(2) and (3) granulation: drying the silicon slurry obtained in the step (1) into powder by a spray dryer, wherein the air inlet temperature of spray drying is 150-;
(3) carbonizing: and (3) placing the silicon-carbon precursor obtained in the step (2) in a nitrogen atmosphere protective furnace for sintering, raising the temperature to 1100-1500 ℃ at the heating rate of 2-25 ℃/min, preserving the heat for 6-12 hours, and crushing and screening to obtain the silicon-carbon negative electrode material.
2. The preparation method of the low-expansion silicon-carbon negative electrode material for the lithium ion battery according to claim 1, characterized in that: the silicon powder D50=20-100nm in the step (1), and the shape of the silicon powder is spherical.
3. The preparation method of the low-expansion silicon-carbon negative electrode material for the lithium ion battery according to claim 1, characterized in that: the binder in the step (1) is one or a mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃.
4. The preparation method of the low-expansion silicon-carbon negative electrode material for the lithium ion battery according to claim 1, characterized in that: the pore-forming agent in the step (1) is one or more than two of ammonium bicarbonate, ammonium carbonate, ammonium oxalate, ammonium nitrate, ammonium phosphate and ammonium hydrogen phosphate.
5. The preparation method of the low-expansion silicon-carbon negative electrode material for the lithium ion battery according to claim 1, characterized in that: the solvent in the step (1) is one or more than two of benzene, toluene and xylene.
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