CN113506864B - Silicon monoxide composite material for lithium ion battery and preparation method thereof - Google Patents
Silicon monoxide composite material for lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The invention provides a silicon monoxide composite material for a lithium ion battery and a preparation method thereof, and relates to the technical field of battery composite materials. According to the silicon monoxide composite material for the lithium ion battery, the porous carbon material is used for coating the silicon monoxide powder, so that a three-dimensional network frame space is provided for the expansion of the silicon monoxide, and the polyvinyl chloride is used for coating the silicon monoxide, so that the volume effect of silicon monoxide particles in the charging and discharging processes of the battery is effectively inhibited, the silicon monoxide and graphite are prevented from agglomerating, the cycle stability is improved, and the silicon monoxide composite material has good specific capacity as a lithium ion battery cathode material; the preparation method effectively promotes the adsorption and coating of the silicon monoxide, and ensures the cycling stability and specific capacity of the cathode material.
Description
Technical Field
The invention relates to the technical field of battery composite materials, in particular to a silicon monoxide composite material for a lithium ion battery and a preparation method thereof.
Background
At present, graphite carbon materials are mostly adopted as negative electrode materials of lithium ion batteries, and the graphite carbon materials have the characteristics of good cycle stability, long service life, low cost, excellent conductivity and the like, but the capacity is close to the theoretical value of 372 mA.h/g, the increasing requirements of the current market on the high-energy-density lithium ion batteries cannot be met, the development of novel high-energy-density and high-performance negative electrode materials is urgent, the theoretical capacity of silicon reaches 4200 mA.h/g, a lithium removal potential platform is low, lithium precipitation is not easy to generate, the safety performance is better, and the graphite carbon materials become one of the negative electrode materials of the lithium ion batteries with the development potential at present.
The application No. 201310103828.5 discloses a silicon monoxide composite negative electrode material for a lithium ion battery and a preparation method thereof, which comprises 10-30% of composite particle material and 70-90% of natural graphite or artificial graphite by mass percentage, wherein the composite particle material is silicon monoxide coated with a carbon nano tube and an amorphous carbon coating layer; by coating the cracked carbon on the surface of the silicon oxide particles, the volume effect of the silicon oxide particles in the charging and discharging processes of the battery is effectively inhibited, and the silicon oxide particles have good cycle performance. The technical problem is that the adsorption and coating of the SiO can not be effectively promoted so as to further improve the cycling stability and specific capacity of the SiO composite material as the cathode material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a silicon monoxide composite material for a lithium ion battery and a preparation method thereof.
The invention solves the technical problems through the following technical means:
the invention provides a silicon monoxide composite material for a lithium ion battery, which is prepared by mixing 30-45 parts by weight of silicon monoxide powder, 65-80 parts by weight of a porous carbon material and 550-700 parts by weight of an organic silicon solution to obtain slurry, spray drying, primary calcining and cooling the slurry to obtain mixed particles, and mixing the mixed particles with polyvinyl chloride through ball milling, coating and granulating, and mixing with graphite after secondary calcining.
According to the silicon monoxide composite material for the lithium ion battery, the porous carbon material is used for coating the silicon monoxide powder, a three-dimensional network frame space is provided for the expansion of the silicon monoxide, and the polyvinyl chloride is used for coating the silicon monoxide, so that the volume effect of silicon monoxide particles in the charging and discharging processes of the battery is effectively inhibited, the silicon monoxide and graphite are prevented from agglomerating, the cycle stability is improved, and the silicon monoxide composite material has good specific capacity as a lithium ion battery cathode material.
As a further improved scheme of the invention, the porous carbon material is one or a mixture of more of porous artificial graphite, porous natural graphite, porous hard carbon, porous soft carbon and porous meso-carbon microspheres; the organic silicon solution is obtained by uniformly mixing halogenated silane or ethyl orthosilicate and a solvent according to the mass ratio of 1: 3-6, wherein the solvent is one or a mixture of more of N-hexane, N-heptane, toluene, N-pentane, ethyl acetate and N, N-dimethylformamide.
The invention also provides a preparation method of the silicon monoxide composite material for the lithium ion battery, which comprises the following steps:
s100, slurry preparation: mixing 30-45 parts by weight of silicon monoxide powder and 65-80 parts by weight of porous carbon material, adding 550-700 parts by weight of organic silicon solution, and stirring and mixing uniformly to obtain slurry;
S200, spray drying and primary calcining: after the slurry is subjected to spray drying, calcining for the first time in a protective atmosphere, raising the temperature to 720-750 ℃ at a speed of 2-4 ℃, cooling to 200-250 ℃ by air cooling, and naturally cooling to room temperature to obtain mixed particles;
s300, coating granulation and secondary calcination: and carrying out ball milling and mixing on the mixed particles and polyvinyl chloride, coating and granulating after mixing, then carrying out secondary calcination, crushing to the particle size of 0.6-1.5 mu m after calcination, mixing with graphite according to the mass ratio of 1: 2.5-3.5, and stirring to obtain the silicon monoxide composite material for the lithium ion battery.
The preparation method of the silicon monoxide composite material for the lithium ion battery comprises the steps of slurry preparation, spray drying, primary calcination, coating granulation and secondary calcination, wherein after the silicon monoxide powder and the porous carbon material are dispersed in the organic silicon solution, the adsorption of the porous carbon material on the silicon monoxide is promoted in the stirring process; the preparation method effectively promotes the silicon monoxide to be adsorbed and coated, and ensures the cycling stability performance and specific capacity of the negative electrode material.
As a further improvement scheme of the invention, the porous carbon material is one or a mixture of more of porous artificial graphite, porous natural graphite, porous hard carbon, porous soft carbon and porous meso-carbon microspheres.
According to a further improved scheme of the invention, the organic silicon solution is obtained by uniformly mixing halogenated silane or ethyl orthosilicate and a solvent according to a mass ratio of 1: 3-6, wherein the solvent is one or a mixture of N-hexane, N-heptane, toluene, N-pentane, ethyl acetate and N, N-dimethylformamide.
As a further improved scheme of the invention, the inlet temperature of spray drying in the step b is 160-180 ℃, the outlet temperature is 100-115 ℃, and the heating power is 12 kw.
As a further improvement scheme of the invention, the protective atmosphere in the step b is one or a mixture of argon and hydrogen; the heat preservation time of the first calcination is 4-6 hours.
As a further improved scheme of the invention, the mass ratio of the mixed particles to the polyvinyl chloride in the step c is 3-5: 1, and a mixed gas of hydrogen and argon with a volume ratio of 1.5-2: 25 is introduced in the coating and granulating process.
As a further improved scheme of the present invention, the second calcination in step c specifically comprises: heating to 860-880 ℃ at the rate of 1.5-3 ℃, and preserving heat for 3-5 hours.
As a further improved scheme of the invention, the stirring and uniformly mixing in the step a is stirring for 30-50 min at the rotating speed of 200-400 rpm.
The invention has the beneficial effects that:
(1) according to the silicon monoxide composite material for the lithium ion battery, the porous carbon material is used for coating the silicon monoxide powder, a three-dimensional network frame space is provided for the expansion of the silicon monoxide, and the polyvinyl chloride is used for coating the silicon monoxide, so that the volume effect of silicon monoxide particles in the charging and discharging processes of the battery is effectively inhibited, the silicon monoxide and graphite are prevented from agglomerating, the cycle stability is improved, and the silicon monoxide composite material has good specific capacity as a lithium ion battery cathode material.
(2) According to the preparation method of the silicon monoxide composite material for the lithium ion battery, after the silicon monoxide powder and the porous carbon material are dispersed in the organic silicon solution, the adsorption of the porous carbon material to the silicon monoxide is promoted in the stirring process; the preparation method effectively promotes the silicon monoxide to be adsorbed and coated, and ensures the cycling stability performance and specific capacity of the negative electrode material.
Drawings
FIG. 1 is a flow chart of a method for preparing a SiO composite material for Li-ion batteries.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. 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.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
Example 1
As shown in fig. 1, in the present example, 42 parts by weight of a silicon monoxide composite material for a lithium ion battery is mixed with 76 parts by weight of a porous carbon material and 650 parts by weight of an organic silicon solution to obtain a slurry, the slurry is subjected to spray drying, primary calcination and cooling to obtain mixed particles, and the mixed particles are ball-milled and mixed with polyvinyl chloride, coated and granulated, and subjected to secondary calcination and mixed with graphite to obtain the silicon monoxide composite material for a lithium ion battery.
The preparation method of the silicon monoxide composite material for the lithium ion battery comprises the following steps:
s100, preparing slurry: mixing 42 parts of silicon monoxide powder and 76 parts of porous carbon material according to parts by weight, adding 650 parts of organic silicon solution, and stirring and uniformly mixing to obtain slurry;
s200, spray drying and primary calcining: after the slurry is spray-dried, the slurry is calcined for the first time in a protective atmosphere, the temperature is raised to 740 ℃ at the speed of 3 ℃, the temperature is reduced to 235 ℃ by air cooling, and then the slurry is naturally cooled to the room temperature to obtain mixed particles;
s300, coating granulation and secondary calcination: and performing ball milling and mixing on the mixed particles and polyvinyl chloride, coating and granulating after mixing, performing secondary calcination, crushing to obtain the particle size of 1.2 mu m after the calcination is finished, mixing the particles and graphite according to the mass ratio of 1:3, and stirring to obtain the silicon monoxide composite material for the lithium ion battery.
Wherein the porous carbon material is porous mesocarbon microbeads. The organic silicon solution is obtained by uniformly mixing halogenated silane or ethyl orthosilicate and a solvent according to the mass ratio of 1:5, wherein the solvent is n-heptane. And d, uniformly stirring in the step a for 45min at the rotating speed of 360 rpm. The inlet temperature of the spray drying in step b was 175 ℃, the outlet temperature was 110 ℃ and the heating power was 12 kw. In the step b, the protective atmosphere is one or a mixture of argon and hydrogen; the holding time for the first calcination was 5.5 hours. And c, the mass ratio of the mixed particles to the polyvinyl chloride in the step c is 4.5:1, and mixed gas of hydrogen and argon in the volume ratio of 1.8:25 is introduced in the coating and granulating process. The second calcination in the step c is specifically as follows: the temperature is raised to 875 ℃ at the rate of 2.5 ℃ and the temperature is kept for 4.5 hours.
The prepared silicon monoxide composite material is used as a research electrode, a metal lithium sheet is used as a counter electrode, the silicon monoxide composite material is assembled into an experimental button type lithium ion battery in a glove box filled with argon, charge and discharge circulation is carried out within a potential range of 0.01-3.0V at a multiplying power of 0.1C, the first charge capacity is 1758.7mAh/g, the discharge capacity is 1395.6mAh/g, and the capacity retention rate after 100 weeks of circulation is 93.8%.
Example 2
As shown in fig. 1, in the present embodiment, 38 parts by weight of a silicon monoxide composite material for a lithium ion battery is mixed with 78 parts by weight of a porous carbon material and 680 parts by weight of an organic silicon solution to obtain a slurry, the slurry is subjected to spray drying, primary calcination and cooling to obtain mixed particles, and the mixed particles are ball-milled and mixed with polyvinyl chloride, coated and granulated, and subjected to secondary calcination, and then mixed with graphite to obtain the silicon monoxide composite material for the lithium ion battery.
The preparation method of the silicon monoxide composite material for the lithium ion battery comprises the following steps:
s100, preparing slurry: mixing 38 parts of silicon monoxide powder and 78 parts of porous carbon material according to parts by weight, adding 680 parts of organic silicon solution, and stirring and uniformly mixing to obtain slurry;
s200, spray drying and primary calcining: after the slurry is spray-dried, the slurry is calcined for the first time in a protective atmosphere, the temperature is raised to 740 ℃ at the speed of 4 ℃, the temperature is reduced to 240 ℃ by air cooling, and then the slurry is naturally cooled to the room temperature to obtain mixed particles;
S300, coating granulation and secondary calcination: and performing ball milling and mixing on the mixed particles and polyvinyl chloride, coating and granulating after mixing, performing secondary calcination, crushing to obtain the particle size of 1.2 mu m after the calcination is finished, mixing the particles and graphite according to the mass ratio of 1:3.2, and stirring to obtain the silicon monoxide composite material for the lithium ion battery.
Wherein the porous carbon material is porous artificial graphite. The organic silicon solution is obtained by uniformly mixing halogenated silane or ethyl orthosilicate and a solvent according to the mass ratio of 1:5, wherein the solvent is toluene. The stirring and blending in the step a is stirring for 46min at the rotating speed of 360 rpm. The inlet temperature of the spray drying in step b was 175 ℃, the outlet temperature was 108 ℃ and the heating power was 12 kw. In the step b, the protective atmosphere is one or a mixture of argon and hydrogen; the holding time for the first calcination was 4.8 hours. And c, the mass ratio of the mixed particles to the polyvinyl chloride in the step c is 4.5:1, and mixed gas of hydrogen and argon in the volume ratio of 1.8:25 is introduced in the coating and granulating process. The second calcination in the step c is specifically as follows: the temperature is raised to 875 ℃ at the rate of 2.6 ℃ and the temperature is kept for 4.8 hours.
The prepared silicon monoxide composite material is used as a research electrode, a metal lithium sheet is used as a counter electrode, the silicon monoxide composite material is assembled into an experimental button type lithium ion battery in a glove box filled with argon, charge and discharge circulation is carried out within a potential range of 0.01-3.0V at a multiplying power of 0.1C, the first charge capacity is 1733.5mAh/g, the discharge capacity is 1397.5mAh/g, and the capacity retention rate after 100 weeks of circulation is 95.2%.
Example 3
As shown in fig. 1, in the present example, 42 parts by weight of a silicon monoxide composite material for a lithium ion battery is mixed with 75 parts by weight of a porous carbon material and 670 parts by weight of an organic silicon solution to obtain a slurry, the slurry is subjected to spray drying, primary calcination and cooling to obtain mixed particles, and the mixed particles are ball-milled and mixed with polyvinyl chloride, coated and granulated, and subjected to secondary calcination and mixed with graphite to obtain the silicon monoxide composite material for a lithium ion battery.
The preparation method of the silicon monoxide composite material for the lithium ion battery comprises the following steps:
s100, preparing slurry: mixing 42 parts of silicon monoxide powder and 75 parts of porous carbon material according to parts by weight, adding 670 parts of organic silicon solution, and stirring and uniformly mixing to obtain slurry;
s200, spray drying and primary calcining: after the slurry is spray-dried, the slurry is calcined for the first time in a protective atmosphere, the temperature is raised to 740 ℃ at the speed of 3.8 ℃, the temperature is reduced to 240 ℃ by air cooling, and then the slurry is naturally cooled to the room temperature to obtain mixed particles;
s300, coating granulation and secondary calcination: and carrying out ball milling and mixing on the mixed particles and polyvinyl chloride, coating and granulating after mixing, then carrying out secondary calcination, crushing to obtain particles with the particle size of 1.4 mu m after the calcination is finished, mixing the particles with graphite according to the mass ratio of 1:3.4, and stirring to obtain the silicon monoxide composite material for the lithium ion battery.
Wherein the porous carbon material is porous natural graphite. The organic silicon solution is obtained by uniformly mixing halogenated silane or tetraethoxysilane and a solvent according to the mass ratio of 1:5.5, wherein the solvent is toluene. The stirring and uniformly mixing in the step a is stirring for 48min at the rotating speed of 380 rpm. The inlet temperature of the spray drying in the step b is 172 ℃, the outlet temperature is 108 ℃, and the heating power is 12 kw. In the step b, the protective atmosphere is one or a mixture of argon and hydrogen; the holding time for the first calcination was 5.5 hours. And c, the mass ratio of the mixed particles to the polyvinyl chloride in the step c is 4.6:1, and mixed gas of hydrogen and argon in the volume ratio of 1.9:25 is introduced in the coating and granulating process. The second calcination in the step c is specifically as follows: the temperature is raised to 875 ℃ at the rate of 2.6 ℃ and the temperature is kept for 4.2 hours.
The prepared silicon monoxide composite material is used as a research electrode, a metal lithium sheet is used as a counter electrode, the silicon monoxide composite material is assembled into an experimental button type lithium ion battery in a glove box filled with argon, charge and discharge circulation is carried out within a potential range of 0.01-3.0V at a multiplying power of 0.1C, the first charge capacity is 1769.8mAh/g, the discharge capacity is 1407.6mAh/g, and the capacity retention rate after 100 weeks of circulation is 94.3%.
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. The preparation method of the silicon monoxide composite material for the lithium ion battery is characterized by comprising the following steps:
s100, slurry preparation: mixing 30-45 parts by weight of silicon monoxide powder and 65-80 parts by weight of porous carbon material, adding 550-700 parts by weight of organic silicon solution, and stirring and mixing uniformly to obtain slurry;
s200, spray drying and primary calcining: after spray drying, calcining the slurry for the first time in a protective atmosphere, heating to 720-750 ℃ at the speed of 2-4 ℃, cooling to 200-250 ℃ by air cooling, and naturally cooling to room temperature to obtain mixed particles;
s300, coating granulation and secondary calcination: ball-milling and mixing the mixed particles and polyvinyl chloride, coating and granulating after mixing, then carrying out secondary calcination, crushing to the particle size of 0.6-1.5 mu m after calcination, mixing the particles and graphite according to the mass ratio of 1: 2.5-3.5, and stirring to obtain the silicon monoxide composite material for the lithium ion battery;
The organic silicon solution is obtained by uniformly mixing halogenated silane or tetraethoxysilane with a solvent according to the mass ratio of 1: 3-6, wherein the solvent is one or a mixture of N-hexane, N-heptane, toluene, N-pentane, ethyl acetate and N, N-dimethylformamide;
in the step S200, the inlet temperature of spray drying is 160-180 ℃, the outlet temperature is 100-115 ℃, and the heating power is 12 kw;
in the step S300, the mass ratio of the mixed particles to the polyvinyl chloride is 3-5: 1, and mixed gas of hydrogen and argon with the volume ratio of 1.5-2: 25 is introduced in the coating and granulating process;
the secondary calcination in step S300 specifically includes: heating to 860-880 ℃ at the rate of 1.5-3 ℃, and preserving heat for 3-5 hours.
2. The method for preparing the silicon monoxide composite material for the lithium ion battery according to claim 1, wherein the porous carbon material is one or more of porous artificial graphite, porous natural graphite, porous hard carbon and porous soft carbon.
3. The method for preparing the SiO composite for Li-ion battery according to claim 1, wherein the protective atmosphere in step S200 is one or a mixture of argon and hydrogen; the heat preservation time of the primary calcination is 4-6 hours.
4. The preparation method of the silicon monoxide composite material for the lithium ion battery according to claim 1, wherein the step S100 of uniformly stirring is to stir at a rotation speed of 200-400 rpm for 30-50 min.
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| CN111689500A (en) * | 2020-04-27 | 2020-09-22 | 万向一二三股份公司 | Preparation method of low-expansibility SiO/graphite composite electrode material |
| CN112635733A (en) * | 2020-12-21 | 2021-04-09 | 江苏集芯半导体硅材料研究院有限公司 | Negative electrode material of lithium ion battery, preparation method of negative electrode material and lithium ion battery |
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