CN117174845A - Preparation method of silicon-carbon composite graphite quick-charge anode material - Google Patents
Preparation method of silicon-carbon composite graphite quick-charge anode material Download PDFInfo
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- CN117174845A CN117174845A CN202310379160.0A CN202310379160A CN117174845A CN 117174845 A CN117174845 A CN 117174845A CN 202310379160 A CN202310379160 A CN 202310379160A CN 117174845 A CN117174845 A CN 117174845A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 46
- 239000010439 graphite Substances 0.000 title claims abstract description 45
- 239000010405 anode material Substances 0.000 title claims abstract description 25
- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 229910003481 amorphous carbon Inorganic materials 0.000 claims abstract description 18
- 238000007873 sieving Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000003763 carbonization Methods 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000013508 migration Methods 0.000 claims abstract description 8
- 230000005012 migration Effects 0.000 claims abstract description 8
- 239000007833 carbon precursor Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 6
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 5
- 239000010426 asphalt Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 239000007849 furan resin Substances 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 8
- 239000011856 silicon-based particle Substances 0.000 abstract description 4
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003575 carbonaceous material Substances 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 abstract 1
- 239000007773 negative electrode material Substances 0.000 description 11
- 230000014759 maintenance of location Effects 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000009818 secondary granulation Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a silicon-carbon composite graphite quick-charge anode material, which belongs to the technical field of composite materials and comprises the following specific steps: 1) Grinding and sieving graphite powder, and controlling the particle size to be 5-30 μm; 2) Mixing the graphite powder obtained in the step 1) with nano silicon powder according to a certain proportion, uniformly putting into a high-speed migration equipment, and planting the nano silicon powder on the surface of graphite to obtain a precursor; 3) Mixing the precursor and the amorphous carbon precursor according to a certain proportion, and then putting the mixture into amorphous carbon coating and secondary granulating equipment for carbonization heat treatment; 4) And cooling to room temperature after carbonization heat treatment, and mixing and sieving to obtain the anode material. The invention can improve the energy density of the cathode material, effectively inhibit the expansion and crushing of silicon particles and ensure the structural stability of the silicon-carbon material.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method of a silicon-carbon composite graphite fast-charging anode material.
Background
In recent years, graphite has been used as a main current negative electrode material of a lithium ion battery, however, the gram specific capacitance of the current commercial high-quality graphite is 360mAh/g, the theoretical value of the gram specific capacitance of the current commercial high-quality graphite is close to 372mAh/g, the energy density in the whole battery reaches a ceiling, and the current requirements of various electronic devices, especially energy storage devices and electric automobiles, on the energy density cannot be met, so that the development of the negative electrode material with higher energy density is one of the current research emphasis. Silicon is taken as a negative electrode material of a lithium ion battery, and is considered to be the lithium battery negative electrode material with the most commercialized prospect because of the advantages of high theoretical specific capacity of 4200mAh/g and rich storage capacity, and the silicon rapidly enters the eyes of people, and is the key point of research at the present stage. However, it is found that the volume of the silicon particles can be severely expanded and contracted in the charge-discharge cycle process, and the volume expansion can reach 300%, so that the crushing of the silicon particles and the cracking of the SEI film greatly influence the cycle performance of the battery, thereby influencing the service performance of the battery.
In order to integrate the properties of graphite and silicon materials, silicon carbon composites have been developed. The existing silicon-carbon composite material uses secondary particles formed by granulating nano silicon, graphite and carbon, but as the nano silicon and the graphite have 2 orders of magnitude difference in particle size, and the higher surface energy of the nano silicon is easy to agglomerate, so that the nano silicon and the graphite are difficult to uniformly disperse, the nano silicon can agglomerate on the surface of the graphite or concentrate on one position, the local volume expansion of the particles is caused, the graphite substrate cannot well absorb and relieve the expansion of the silicon, the composite structure is finally damaged and disintegrated, the nano silicon falls off from the surface of the graphite, and meanwhile, the cyclic rate performance is poor due to limited loading capacity and unstable structure. Therefore, the preparation method for the lithium battery anode material, which can improve the energy density of the anode material, effectively inhibit the expansion and crushing of silicon particles and ensure the structural stability of the silicon-carbon material, is very important.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a silicon-carbon composite graphite fast-charging anode material, which comprises the following specific steps:
1) Grinding and sieving graphite powder, and controlling the particle size to be 5-30 μm;
2) Mixing the graphite powder obtained in the step 1) with nano silicon powder according to a certain proportion, uniformly putting into a high-speed migration equipment, and planting the nano silicon powder on the surface of graphite to obtain a precursor;
3) Mixing the precursor and the amorphous carbon precursor according to a certain proportion, and then putting the mixture into amorphous carbon coating and secondary granulating equipment for carbonization heat treatment;
4) And cooling to room temperature after carbonization heat treatment, and mixing and sieving to obtain the anode material.
Preferably, the graphite in the step 1) is one or a mixture of more than one of natural graphite, artificial graphite and mesophase carbon microspheres.
Preferably, in the step 2), the mass ratio of the graphite powder to the nano silicon powder is 70-97:3-30.
Preferably, the nano silicon powder in the step 2) is one or a mixture of more of nano silicon, silicon oxide and silicon carbide.
Preferably, the amorphous carbon precursor in the step 3) is one or a mixture of more than one of petroleum asphalt, coal asphalt, phenolic resin and furan resin.
Preferably, the mass ratio of the precursor to the amorphous carbon precursor in step 3) is 19:1.
preferably, the heating rate of the carbonization heat treatment in the step 3) is 1-10 ℃/min, the heat treatment temperature is 800-1200 ℃, the heat treatment temperature is 900-1100 ℃ preferably, and the time is 1-15 hours.
Preferably, the size of the anode material after sieving in step 4) is 11-15 μm.
Compared with the prior art, the invention has the following advantages:
the nano silicon powder is planted on the surface of graphite through the high-speed migration equipment, after the nano silicon powder is carbonized through the amorphous carbon coating and the heat treatment of the secondary granulation equipment, the nano silicon can be tightly coated on the surface of graphite particles, the particles are perfectly combined, the nano silicon has a complete nucleocapsid structure, the nano silicon can not be cracked or broken from the graphite due to too large expansion under the condition of rapid charging, the performance of rapid charging and discharging cycle life is reduced, the rapid charging characteristic can be fully exerted, and the charging and discharging performance of the lithium ion battery is improved. Meanwhile, as the amorphous carbon has large interlayer spacing, the lithium ions can be more smoothly fed in and fed out, the reaction of the amorphous carbon on electrolyte is more stable, the amorphous carbon has better charge-discharge cycle performance, the cycle stability and the capacitance retention rate can be maintained under higher charge current, and the capacitance retention rate can reach more than 90% under 300 charge-discharge cycles.
Drawings
FIG. 1 is a schematic diagram of a process of planting nano-silicon on the surface of graphite according to the invention;
FIG. 2 is a schematic diagram of an amorphous carbon coating and secondary granulation process according to the present invention;
FIG. 3 is a scanning electron microscope image of the material after the nano-silicon of the present invention is planted on the graphite surface;
FIG. 4 is a scanning electron microscope image of a negative electrode material of the present invention;
FIG. 5 is a graph showing the charge capacity of the negative electrode materials A1, A2, A3 under the conditions of 0.2C, 0.5C, 1C,2C, 5C;
fig. 6 is a graph showing the capacity retention ratio of the negative electrode materials A1, A2, A3 at 300 cycles under a 5C charge-discharge flow.
Description of the embodiments
The present invention will be described in further detail with reference to specific examples.
Examples
A preparation method of a silicon-carbon composite graphite fast-charging anode material comprises the following specific steps:
1) Grinding and sieving artificial graphite powder, and controlling the particle size to be 5-30 μm;
2) Mixing the graphite powder obtained in the step 1) with nano silicon powder according to the mass ratio of 80:20, uniformly putting into a high-speed migration equipment machine, and planting the nano silicon powder on the surface of graphite to obtain a precursor;
3) Mixing the precursor and petroleum asphalt according to the mass ratio of 19:1, and then adding amorphous carbon coating and secondary granulating equipment after uniformly mixing, and performing carbonization heat treatment, wherein the heating rate of the carbonization heat treatment is 10 ℃/min, and the heat treatment temperature is 1100 ℃ and the time is 15 hours;
4) And cooling to room temperature after carbonization heat treatment, mixing and sieving to obtain the anode material A3 with the size of 11-15 mu m.
Comparative example 1
A preparation method of a silicon-carbon composite graphite fast-charging anode material comprises the following specific steps:
1) Grinding and sieving artificial graphite powder, and controlling the particle size to be 5-30 μm;
2) Mixing the graphite powder obtained in the step 1) with the nano silicon powder according to the mass ratio of 80:20, and uniformly putting into V
And (3) uniformly mixing the nano silicon powder and the graphite powder in a mixing device, and sieving to obtain the negative electrode material A1, wherein the size of the nano silicon powder is 11-15 mu m.
Comparative example 2
A preparation method of a silicon-carbon composite graphite fast-charging anode material comprises the following specific steps:
1) Grinding and sieving artificial graphite powder, and controlling the particle size to be 5-30 μm;
2) Mixing the graphite powder obtained in the step 1) with nano silicon powder according to the mass ratio of 80:20, uniformly putting into a high-speed migration equipment machine, and planting the nano silicon powder on the surface of graphite to obtain a precursor;
3) Carbonizing the precursor at the heating rate of 10 ℃/min and the heat treatment temperature of 1100 ℃ for 15 hours;
4) And cooling to room temperature after carbonization heat treatment, mixing and sieving to obtain the anode material A2 with the size of 11-15 mu m.
Powder of negative electrode materials A1, A2 and A3 is used as negative electrode materials of lithium ion batteries to be coated:
1) Mixing 0.1wt% of trace oxalic acid and 10wt% of polyvinylidene fluoride binder into N-methyl pyrrolidone solvent, and uniformly stirring for 20 minutes to enable the polyvinylidene fluoride to be uniformly dispersed in the mixed solution of the solvent;
2) Putting the negative electrode materials A1, A2 and A3 into the uniformly stirred mixed solution, and continuously stirring for 20 minutes;
3) And (3) forming slurry by the mixed solution, uniformly coating the slurry on the copper foil by using a 130 mu m scraper, drying at 100 ℃ to remove residual solvent, rolling at 25% rolling rate, and drying at 150 ℃.
And (3) battery assembly:
1) Cutting the completely coated negative electrode plate into circular plates with the diameter of 13mm, and adopting a lithium metal foil as a positive electrode;
2) The components required for the coin-shaped battery were assembled sequentially in a dry atmosphere control chamber, and an electrolyte solution (1M lithium hexafluorophosphate (LiPF) 6 ) (solute) -Ethylene Carbonate (EC)/ethylmethyl carbonate (EMC) (solvent) (Volume 1: 2)), a coin-shaped battery is completed;
3) The assembled coin-type battery was subjected to continuous charge/discharge performance test at charge/discharge rates of 0.2C, 0.5C, 1C,2C,5C, and constant current density for 5 times, and a charge cut-off voltage of 2V (vs Li/Li) + ) The discharge cut-off voltage was 0.005V (vs. Li/Li + )。
As can be seen from FIG. 5, the charging capacities of A1, A2 and A3 of 0.2C are respectively 434.7 mAh/g, 431.2mAh/g and 430.3 mAh/g, which are equivalent to each other, when the charging capacities of A1, A2 and A3 are increased to 0.5C, 1C,2C and 5C, the charging capacities of A3 are respectively 426.1mAh/g, 415.2mAh/g, 405.7mAh/g and 390.8mAh/g, the charging capacities of A2 are respectively 415.9mAh/g, 400.2mAh/g, 355.2mAh/g and 300.3mAh/g, and the charging capacities of A1 are respectively 410.7mAh/g, 389.3mAh/g, 305.7mAh/g and 260.5mAh/g, so that the charging and discharging amounts of A3 are obviously better than those of A1 and A2. Therefore, it can be found that in the amorphous carbon coating and secondary granulating device, the nano silicon material is completely and tightly sealed in the composite graphite particles, so that the composite graphite particles have a complete core-shell structure, and the nano silicon particles are not easy to expand and crack under the condition of increasing charging current, so that the nano silicon particles completely exert quick charging characteristics, however, compared with A1 and A2, the charging capacity of the A2 for planting the nano silicon powder on the whole graphite surface through the high-speed migration device is better than that of A1, because the nano silicon particles can uniformly disperse the graphite surface through the high-speed migration device and are tightly combined with the graphite, the nano silicon particles are not easy to fall off, and the expansion change of silicon can be restrained.
From the graph of fig. 6, it can be seen that the capacity retention rates of the graphite composites A1, A2, A3 in 300 cycles under 5C charge-discharge flow are compared, and it is shown that the capacity retention rates A3 in 300 cycles of the graphite composites A1, A2, A3 are larger than those of A1 and A2, so that it is known that the effect of the graphite composite A3 after the amorphous carbon coating and the secondary granulation heat treatment is due to the fact that the nano silicon material is completely and tightly enclosed inside the composite graphite particles, and besides the effect of filling the nano silicon particles on the surface of the graphite composite, the granulation effect is further smooth, so that the cycle stability and the capacity retention rate under such high charge current are maintained, and the efficiency of the nano silicon material can reach 90% or more for 300 times.
The foregoing is merely exemplary embodiments of the present invention, and it should be noted that various changes, modifications, substitutions and alterations can be made herein by those skilled in the art without departing from the technical principles of the present invention, which are also intended to be regarded as the scope of the invention.
Claims (8)
1. The preparation method of the silicon-carbon composite graphite fast-charging anode material is characterized by comprising the following specific steps:
1) Grinding and sieving graphite powder, and controlling the particle size to be 5-30 μm;
2) Mixing the graphite powder obtained in the step 1) with nano silicon powder according to a certain proportion, uniformly putting into a high-speed migration equipment, and planting the nano silicon powder on the surface of graphite to obtain a precursor;
3) Mixing the precursor and the amorphous carbon precursor according to a certain proportion, and then putting the mixture into amorphous carbon coating and secondary granulating equipment for carbonization heat treatment;
4) And cooling to room temperature after carbonization heat treatment, and mixing and sieving to obtain the anode material.
2. The preparation method of the silicon-carbon composite graphite fast-charging anode material according to claim 1, wherein the graphite in the step 1) is one or a mixture of more than one of artificial graphite, natural graphite and mesophase carbon microspheres.
3. The preparation method of the silicon-carbon composite graphite fast-charging anode material according to claim 1, wherein the mass ratio of the graphite powder to the nano silicon powder in the step 2) is 70-97:3-30.
4. The preparation method of the silicon-carbon composite graphite fast-charging anode material according to claim 1, wherein the nano silicon powder in the step 2) is one or a mixture of a plurality of nano silicon and silicon oxide.
5. The preparation method of the silicon-carbon composite graphite fast-charging anode material according to claim 1, wherein the amorphous carbon precursor in the step 3) is one or a mixture of more of petroleum asphalt, coal asphalt, phenolic resin and furan resin.
6. The method for preparing the silicon-carbon composite graphite fast-charging anode material according to claim 1, wherein the mass ratio of the precursor to the amorphous carbon precursor in the step 3) is 19:1.
7. the method for preparing the silicon-carbon composite graphite fast-charging anode material according to claim 1, wherein the heating rate of the carbonization heat treatment in the step 3) is 1-10 ℃/min, the heat treatment temperature is 800-1200 ℃, the heat treatment temperature is 900-1100 ℃ preferably, and the time is 1-15 hours.
8. The method for preparing the silicon-carbon composite graphite fast-charging anode material according to claim 1, wherein the size of the anode material after sieving in the step 4) is 11-15 μm.
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