CN117650245A - Lithium battery anode material and preparation method and application thereof - Google Patents
Lithium battery anode material and preparation method and application thereof Download PDFInfo
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- CN117650245A CN117650245A CN202410120361.3A CN202410120361A CN117650245A CN 117650245 A CN117650245 A CN 117650245A CN 202410120361 A CN202410120361 A CN 202410120361A CN 117650245 A CN117650245 A CN 117650245A
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- anode material
- lithium battery
- battery anode
- silicon oxide
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- 239000010405 anode material Substances 0.000 title claims abstract description 50
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 43
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- 239000005011 phenolic resin Substances 0.000 claims description 8
- 229920001568 phenolic resin Polymers 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- 239000007773 negative electrode material Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 238000009830 intercalation Methods 0.000 description 6
- 230000002687 intercalation Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000009831 deintercalation Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012216 screening Methods 0.000 description 3
- 229910018557 Si O Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 2
- 229910052912 lithium silicate Inorganic materials 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
Abstract
The invention provides a lithium battery anode material and a preparation method and application thereof, and belongs to the technical field of lithium battery anode materials.
Description
Technical Field
The invention relates to the technical field of lithium battery anode materials, in particular to a lithium battery anode material, a preparation method and application thereof.
Background
The traditional lithium ion battery negative electrode materials are mostly graphite negative electrode materials, the theoretical reversible specific capacity of the traditional lithium ion battery negative electrode materials is only 372mAh/g, the battery energy density is difficult to break through 300Wh/kg, the application requirements of the lithium ion battery cannot be met, and therefore the negative electrode materials with more excellent performance are required to replace graphite.
Silica has a high theoretical specific capacity (about 2600 mAh/g), a low lithium intercalation potential (about 0.5V) and low cost, strong silicon oxygen bonds and lithium silicate, li, formed in the cycle 2 O imparts excellent cycle performance to the buffer of volume expansion, and is one of the preferred alternatives to graphite materials as the negative electrode. However, silicon oxide also has some drawbacks. Such as lithium silicate and Li 2 The formation of O increases the irreversible capacity at the first week of SiOx, and has problems such as large volume change during charge and discharge and poor self-conductivity. Currently, research in silicon-carbon materials has focused mainly on carbon coating of silicon-based materials. Although the carbon layer coating on the surface of the silicon oxide can relieve the volume change in the battery charging and discharging process to a certain extent, and improve the primary charging and discharging efficiency and the circulation stability. However, there is no chemical bond between the carbon atoms in the carbon coating and the silicon atoms in the silicon oxide, and the volume expansion of the silicon-based material during the repeated lithium ion intercalation and deintercalation process can lead to the falling of the carbon coating on the surface, so that the cycle life of the material is poor, and the simple physical carbon coating can not thoroughly solve the problems. Therefore, the method has great research significance on how to effectively relieve the volume expansion of silicon in the repeated intercalation and deintercalation process of lithium ions in the charge and discharge process and improve the cycle performance of the silicon oxide composite anode material.
Disclosure of Invention
The invention aims to provide a lithium battery anode material, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a lithium battery anode material, which comprises the following steps:
(1) Mixing a carbon source with silicon oxide, and stirring to obtain a mixture;
(2) And (3) sequentially carrying out heating treatment and sieving on the mixture obtained in the step (1) in an inert atmosphere to obtain the lithium battery anode material.
Preferably, the carbon source in the step (1) is one or more of furfural, citric acid and phenolic resin.
Preferably, in the step (1), the mass ratio of the carbon source to the silicon oxide is (1-99): (1-99).
Preferably, the stirring speed in the step (1) is 60-300 r/min, and the stirring time is 0.5-12 h.
Preferably, the inert atmosphere in step (2) is one of nitrogen, helium or argon.
Preferably, the temperature of the heating treatment in the step (2) is 600-1400 ℃, and the time of the heating treatment is 2-6 hours.
Preferably, the heating rate of the heating treatment in the step (2) is 1-4 ℃/min.
Preferably, the number of the screen meshes used for screening in the step (2) is 50-200 meshes.
The invention also provides the lithium battery anode material prepared by the preparation method.
The invention provides a preparation method of a lithium battery anode material, which comprises the steps of firstly mixing a carbon source with silicon oxide, stirring, and then heating, wherein the prepared lithium battery anode material is a silicon oxide composite anode material, so that chemical bonds are formed between carbon atoms and silicon atoms in the silicon oxide composite anode material, the uniformity of silicon-carbon distribution can be remarkably improved, the volume expansion of silicon in the repeated intercalation and deintercalation process of lithium ions in the charge and discharge process can be effectively relieved, the cycle performance of the silicon oxide composite anode material can be improved, and the preparation method provided by the invention is simple and can be used for industrial production.
Drawings
FIG. 1 is an SEM image of the negative electrode material CFTL-1 of a lithium battery prepared in example 1 of the invention;
FIG. 2 is an SEM image of the negative electrode material CFTL-2 of a lithium battery prepared in example 2 of the invention;
FIG. 3 is an SEM image of the negative electrode material CFTL-3 of a lithium battery prepared in example 3 of the invention;
fig. 4 is a graph showing cycle performance comparison of lithium batteries respectively assembled by the lithium battery anode materials prepared in examples 1 to 3 of the present invention and the SiOx anode materials prepared in comparative examples.
Detailed Description
The invention provides a preparation method of a lithium battery anode material, which comprises the following steps:
(1) Mixing a carbon source with silicon oxide, and stirring to obtain a mixture;
(2) And (3) sequentially carrying out heating treatment and sieving on the mixture obtained in the step (1) in an inert atmosphere to obtain the lithium battery anode material.
In the present invention, the raw materials used are all conventional commercial products in the art unless otherwise specified.
The invention mixes the carbon source and the silicon oxide, and then carries out stirring treatment to obtain a mixture.
In the present invention, the carbon source is preferably one or more of furfural, citric acid, phenolic resin.
In the invention, the mass ratio of the carbon source to the silicon oxide is preferably (1-99): (1-99). The invention controls the mass ratio of the carbon source to the silicon oxide in the range, promotes the full formation of chemical bonds between carbon atoms and silicon atoms in the raw materials, can obviously improve the uniformity of silicon-carbon distribution, and prepares the lithium battery anode material with better performance.
In the present invention, the stirring speed is preferably 60 to 300 r/min, more preferably 80 to 200 r/min. In the invention, the stirring treatment time is preferably 0.5-12 h, more preferably 1-10 h. The invention controls the speed and time of the stirring treatment in the above range so as to uniformly mix the components.
After the mixture is obtained, the invention sequentially carries out heating treatment and sieving on the mixture in inert atmosphere to obtain the lithium battery anode material.
In the present invention, the inert atmosphere is preferably one of nitrogen, helium or argon.
In the present invention, the temperature of the heating treatment is preferably 600 to 1400 ℃, more preferably 800 to 1200 ℃. In the present invention, the time of the heating treatment is preferably 2 to 6 hours, more preferably 3 to 5 hours. In the invention, the heating rate of the heating treatment is preferably 1-4 ℃/min, more preferably 2-3 ℃/min. The invention controls the temperature, time and heating rate of the heating treatment in the above range so as to promote the reaction to be fully carried out, so that chemical bonds are formed between carbon atoms and silicon atoms, the uniformity of silicon-carbon distribution can be obviously improved, the volume expansion of silicon in the repeated intercalation and deintercalation process of lithium ions in the charge and discharge process is effectively relieved, and the cycle performance of the lithium battery anode material is improved.
In the present invention, the number of the screen meshes used for the screening is preferably 50 to 200 mesh. The invention controls the number of the screen meshes used for screening in the range so as to adjust the particle size of the lithium battery anode material and obtain the lithium battery anode material with better performance.
The invention also provides the lithium battery anode material prepared by the preparation method.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the lithium battery anode material comprises the following steps:
(1) Mixing 50g of silicon oxide and 50g of carbon source phenolic resin, and stirring in a high-speed mixer at 120 r/min for 180min to obtain a mixture;
(2) Adding the mixture obtained in the step (1) into a reaction furnace, introducing nitrogen, heating at 950 ℃ for 3 hours in nitrogen atmosphere, and then sieving the heated product with a 150-mesh sieve to obtain the lithium battery anode material which is the silicon oxide composite anode material and named as CFTL-1.
Example 2
The preparation method of the lithium battery anode material comprises the following steps:
(1) 50g of silicon oxide and 25g of carbon source phenolic resin are mixed, and then stirred in a high-speed mixer at 120 r/min for 180min to obtain a mixture;
(2) Adding the mixture obtained in the step (1) into a reaction furnace, introducing nitrogen, heating at 950 ℃ for 3 hours in nitrogen atmosphere, and then sieving the heated product with a 150-mesh sieve to obtain the lithium battery anode material which is the silicon oxide composite anode material and named as CFTL-2.
Example 3
The preparation method of the lithium battery anode material comprises the following steps:
(1) 50g of silicon oxide and 10g of carbon source phenolic resin are mixed, and then stirred in a high-speed mixer at 120 r/min for 180min to obtain a mixture;
(2) Adding the mixture obtained in the step (1) into a reaction furnace, introducing nitrogen, heating at 950 ℃ for 3 hours in nitrogen atmosphere, and then sieving the heated product with a 150-mesh sieve to obtain the lithium battery anode material which is the silicon oxide composite anode material and named as CFTL-3.
As can be seen from comparison of examples 1 and 2, when phenolic resins of different masses are added, the structure of the obtained silica composite anode material is different; and when the silicon oxide composite negative electrode prepared from phenolic resin with different quality is subjected to the lithium battery cycle performance test, the thermal cycle performance of the obtained battery is different.
Comparative example
The preparation method of the SiOx anode material comprises the following steps:
(1) 50g of silicon oxide is stirred for 180min in a high-speed mixer at 120 r/min to obtain mixed powder;
(2) Adding the uniformly mixed powder obtained in the step (1) into a reaction furnace, introducing nitrogen, performing heating treatment at 950 ℃ for 3 hours in a nitrogen atmosphere, and then sieving the heated product with a 150-mesh sieve to obtain the SiOx anode material.
As can be seen from FIG. 1-3, the SEM images of CFTL-1, CFTL-2 and CFTL-3 are respectively obtained by observing the silicon oxide composite anode materials CFTL-1, CFTL-2 and CFTL-3 prepared in the embodiments 1-3 by adopting a scanning electron microscope, the silicon oxide composite anode materials with uniform Si-O-C distribution are obtained by the CFTL-2, the Si-O of the materials obtained by the CFTL-1 is distributed in the particles, the carbon materials are distributed outside the particles, the silicon oxide and the carbon materials of the CFTL-3 are distributed in a layered manner, the Si-O is distributed in the upper layer of the particles, the carbon materials are distributed in the lower layer of the particles, and the distribution is uneven.
The lithium batteries respectively assembled by the silicon oxide composite anode materials prepared in the examples 1-3 and the SiOx anode materials prepared in the comparative examples are respectively tested for the cycle performance of the lithium batteries assembled by the silicon oxide composite anode materials prepared in the examples 1-3 and the SiOx anode materials prepared in the comparative examples, and the obtained cycle performance comparison chart is shown in figure 4, and as can be seen from figure 4, the CFTL-2 remarkably improves the conductivity of the SiOx anode due to uniform internal Si-O-C distribution, relieves the structural profit and expansion, remarkably improves the cycle performance of the materials, and the capacity is remarkably higher than that of the CFTL-1, the CFTL-3 and the commercial silicon oxide materials when the batteries are cycled to 140 circles, as shown in figure 4.
In conclusion, when the silicon oxide composite anode material prepared in the embodiments 1-3 is used as the anode material of a lithium battery, the volume expansion of silicon in the repeated intercalation and deintercalation process of lithium ions in the charge and discharge process can be effectively avoided, and the silicon oxide composite anode material has excellent cycle performance.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (5)
1. The preparation method of the lithium battery anode material comprises the following steps:
(1) Mixing a carbon source with silicon oxide, and stirring to obtain a mixture;
the carbon source in the step (1) is one or more of furfural, citric acid and phenolic resin;
in the step (1), the mass ratio of the carbon source to the silicon oxide is (1-99): (1-99);
(2) Sequentially carrying out heating treatment and sieving on the mixture obtained in the step (1) in an inert atmosphere to obtain a lithium battery anode material;
the temperature of the heating treatment in the step (2) is 600-1400 ℃, and the time of the heating treatment is 2-6 hours;
the heating rate of the heating treatment in the step (2) is 1-4 ℃/min.
2. The preparation method according to claim 1, wherein the stirring treatment in the step (1) is performed at a speed of 60-300 r/min, and the stirring treatment time is 0.5-12 h.
3. The method of claim 1, wherein the inert atmosphere in step (2) is one of nitrogen, helium or argon.
4. The method according to claim 1, wherein the number of meshes used for sieving in the step (2) is 50 to 200.
5. The lithium battery anode material prepared by the preparation method of any one of claims 1-4.
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