CN114275785A - High-first-efficiency silicon monoxide negative electrode and preparation method thereof - Google Patents
High-first-efficiency silicon monoxide negative electrode and preparation method thereof Download PDFInfo
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 229910000103 lithium hydride Inorganic materials 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000012298 atmosphere Substances 0.000 claims abstract description 8
- 239000005539 carbonized material Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000010000 carbonizing Methods 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 230000004927 fusion Effects 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 5
- 239000007790 solid phase Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 12
- 239000007773 negative electrode material Substances 0.000 abstract description 12
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 2
- 239000011232 storage material Substances 0.000 abstract description 2
- 238000003763 carbonization Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses a high-first-effect silicon monoxide negative electrode and a preparation method thereof, relates to the technical field of energy storage materials, and aims to solve the problems that the first-effect or capacity performance of a silicon monoxide negative electrode material is poor, and the popularization and the use of the silicon monoxide negative electrode are seriously restricted; physically mixing carbon-coated silicon monoxide and lithium hydride in an inert gas atmosphere; transferring the mixed materials into a heating device, and heating and carbonizing the materials in an inert gas atmosphere; scattering the carbonized materials; the method has the advantages of simple process, low cost and easy industrialization, the first effect of the silicon oxide negative electrode material can be obviously improved by the strong reducing agent lithium hydride, the reduction speed of the strong reducing agent lithium hydride can be controlled by carbon coating before reduction, the grain size of silicon is effectively reduced, the chemical expansion of the material is reduced, and the cycle performance is greatly improved.
Description
Technical Field
The invention relates to the technical field of energy storage materials, in particular to a high-first-efficiency silicon monoxide negative electrode and a preparation method thereof.
Background
In recent years, with the wide application of lithium ion batteries, the energy density of lithium ion batteries is increasingly required by markets such as power, digital and electric tools, and in the aspect of negative electrode materials, the energy density of traditional graphite negative electrodes is close to that of ceilings, so that the requirement of high-energy-density batteries is difficult to meet. The silicon-based material is concerned about the theoretical specific capacity as high as 4200mAh/g, but the volume expansion is as high as 300 percent in the charging and discharging processes, so that the reversible capacity is low, the cycle performance is poor, and no good method is provided for solving the problems at present.
The silicon oxide negative electrode material is concerned by high specific capacity and low volume expansion (150-. The existence of silica in the silicon oxide relieves the volume expansion of silicon in the lithium intercalation process to a certain extent, but the practical first effect of the silicon oxide is influenced because the silica can form irreversible lithium silicate in the first charge-discharge process. At present, the first effect of common silicon oxide is generally about 75 percent, and is lower than that of graphite 94 percent, so that the popularization and the use of the silicon oxide negative electrode are seriously restricted.
At present, researchers mainly add lithium salt or metal reducing agent to generate silicate from silicon dioxide or reduce silicon dioxide into silicon simple substance in advance to improve the first effect aiming at the problems. For example, the invention is disclosed as CN110993900A and named as magnesium silicate-carbon coated silicon oxide composite negative electrode material and a preparation method thereof, wherein magnesium silicate is generated by adding magnesium powder and magnesium oxide to improve the first effect, the first effect can reach 90 percent, but the capacity can only be improved to 700mAh/g even after graphite is compounded; for another example, the invention application with publication number CN111900369A, entitled "a prelithiation silicon oxide/carbon composite material and its preparation method and application", which carries out prelithiation by adding lithium compound, and then carries out gas phase coating, but the first effect can only reach 82%. In addition, in order to solve the above problems, a complicated or long-flow method is often required; therefore, a high-efficiency silica negative electrode and a preparation method thereof are needed to solve the problem.
Disclosure of Invention
The invention aims to provide a high-first-effect silicon monoxide negative electrode and a preparation method thereof, and aims to solve the problems that the first-effect or capacity performance of a silicon monoxide negative electrode material is poor, and the popularization and the use of the silicon monoxide negative electrode are seriously restricted.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-first-efficiency silicon monoxide negative electrode comprises the following specific steps:
s1, physically mixing the carbon-coated silicon monoxide and lithium hydride in an inert gas atmosphere;
s2, transferring the mixed materials into a heating device, and heating and carbonizing the mixed materials in an inert gas atmosphere;
and S3, scattering the carbonized materials.
Preferably, in step S1, the carbon-coated silica D50 is 0.1 to 10 μm and is coated in one or more of a solid phase, a gas phase, and a liquid phase.
Preferably, in step S1, the purity of lithium hydride is more than or equal to 95%; the proportion of lithium hydride added is between 2 and 20 wt.%.
Preferably, in step S1, the mixing device is one of a VC machine, a three-dimensional mixer, and a fusion machine; the inert gas is one or more of nitrogen, argon and helium.
Preferably, in step S2, the heating device is a roller kiln, a rotary kiln, a pusher kiln, a hot pot kettle, a fusion or VC machine with a heating device; the heating temperature is 600-1000 ℃, the heating time is 0.5-12 hours, and the inert gas is one or more of nitrogen, argon and helium.
Preferably, in step S3, the breaking device is a mechanical pulverizer, a shaper, a jet mill, a VC machine, or a fusion machine; the granularity of the scattered material is 2-15 mu m.
The invention provides another technical scheme that: a high-first-efficiency silicon monoxide negative electrode is prepared by adopting the preparation method in any scheme.
Preferably, the capacity of the high first-efficiency silicon monoxide negative electrode is more than 1200.0mAh/g, and the first efficiency is more than 90.00%.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the high-first-effect silicon monoxide negative electrode and the preparation method thereof, lithium hydride is used as a strong reducing agent, the chemical activity is high, and the first effect of the silicon monoxide negative electrode material can be remarkably improved.
2. According to the high-first-efficiency silicon monoxide negative electrode and the preparation method thereof, the carbon-coated silicon monoxide is used as a raw material, and compared with uncoated silicon monoxide, the carbon coating layer is used as a physical barrier, so that the reduction speed of lithium hydride serving as a strong reducing agent can be simply and effectively controlled, the grain size of silicon can be effectively reduced, the chemical expansion of the material can be reduced, the cycle performance can be greatly improved, the first capacity and efficiency of the negative electrode prepared by the method can reach 1244.0mAh/g and 90.27%, the cycle of a button cell can be 100 weeks, and the capacity retention rate can reach 90.5%.
3. The high-first-efficiency silicon monoxide negative electrode and the preparation method thereof have the advantages of simple process, low cost and easy industrialization.
Drawings
FIG. 1 is an SEM image of a high-efficiency silica negative electrode material prepared in example 2;
fig. 2 is a charging-down first cycle charge-discharge diagram of example 2 and comparative example 1.
Detailed Description
The inventor of the present invention has made a lot of experiments and analyses to solve the problems mentioned in the background art, and has encountered great difficulties in the proceeding process, and although a good reduction effect is obtained after lithium hydride, which is a strong reducing agent, and excellent first-effect performance can be brought, there is no way to guarantee capacity performance, until carbon coating is tried first, and unexpected effect is obtained on capacity performance, except that the first-effect is not greatly reduced, which is ideal compared with the previous experimental results, and on the basis, the inventor has performed detail optimization and improvement to control each key point, and finally has obtained the following excellent scheme:
firstly, physically mixing carbon-coated silicon monoxide and lithium hydride in an inert gas atmosphere; wherein, the carbon-coated silicon monoxide D50 is preferably controlled to be 0.1-10 μm, and the coating mode can be selected from solid phase, gas phase and liquid phase; in addition, the purity of lithium hydride is preferably not less than 95%, and the addition ratio thereof may be 2-20 wt%; the mixing device adopted by the physical mixing can be a VC machine, a three-dimensional mixing machine or a fusion machine and the like; the inert gas is one or more of nitrogen, argon and helium;
transferring the mixed materials into a heating device, and heating and carbonizing the materials in an inert gas atmosphere; the heating device can be roller kiln, rotary kiln, pushed slab kiln, hot ladle kettle, fusion with heating device or VC machine, etc., the heating condition is preferably 600-1000 deg.C, the time is 0.5-12 hours, the inert gas is one or more of nitrogen, argon and helium;
finally, the carbonized materials are scattered, and the scattering device can be a mechanical crusher, a shaping machine, an airflow crusher, a VC machine, a fusion machine and the like; the granularity of the scattered material is preferably controlled to be 2-15 mu m.
The following are 2 preferred examples, optionally selected by the inventors in numerous experiments, and comparative examples using the general method:
example 1
(1) The gas-phase coated silica and a strong reducing agent lithium hydride were charged into a VC machine and physically mixed under an argon atmosphere, wherein the amount of lithium hydride charged was 12 wt%, the mixing parameters were 300rpm for 30 minutes, and the silica D50 was 8 μm.
(2) And putting the mixed materials into a roller kiln for carbonization under nitrogen atmosphere, wherein the carbonization temperature is 850 ℃ and the carbonization time is 8 hours.
(3) And (3) scattering the carbonized materials to obtain a finished product, wherein the scattering device is a VC machine, and the technological parameters are 400rpm for 30 minutes.
And (3) detection results: the capacity of the finally obtained high-first-efficiency silicon monoxide negative electrode material is 1244.0mAh/g, the first efficiency is 90.27%, and D50 is 8.5 mu m. The button cell battery is cycled for 100 weeks, and the capacity retention rate is 90.5%.
Example 2
(1) Solid phase coated silica and lithium hydride, a strong reducing agent, were added to a fusion machine and physically mixed under a nitrogen atmosphere, wherein the amount of lithium hydride added was 7 wt%, the mixing parameters were 300rpm for 40 minutes, and the silica D50 was 5 μm.
(2) And putting the mixed materials into a rotary furnace under nitrogen atmosphere for carbonization, wherein the carbonization temperature is 900 ℃, and the carbonization time is 6 hours.
(3) And (3) scattering the carbonized materials to obtain a finished product, wherein the adopted scattering device is a fusion machine, and the technological parameters are 500rpm and 30 minutes.
And (3) detection results: the capacity of the finally obtained high-first-efficiency silicon monoxide negative electrode material is 1278.5mAh/g, the first efficiency is 90.09%, and D50 is 6.1 mu m. The button cell battery is cycled for 100 weeks, and the capacity retention rate is 88.9%.
Comparative example 1
(1) Solid phase silica having a particle size of 5 μm in D50 was carbonized in a rotary kiln at 900 ℃ for 6 hours under a nitrogen atmosphere.
(2) And (3) scattering the carbonized materials to obtain a finished product, wherein the adopted scattering device is a fusion machine, and the technological parameters are 500rpm and 30 minutes.
And (3) detection results: the capacity of the finally obtained silicon oxide negative electrode material is 1541mAh/g, the first effect is 75.3%, and D50 is 5.1 μm. The button cell battery is cycled for 100 weeks, and the capacity retention rate is 80.1%.
As can be seen from the above examples and comparative examples, the negative electrode material prepared by the method of the present invention has a slightly lower capacity than that of the conventional method, but has a higher first efficiency and more excellent cycle performance, and is relatively more suitable as a battery material.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (8)
1. A preparation method of a high-first-efficiency silicon monoxide negative electrode is characterized by comprising the following specific steps:
s1, physically mixing the carbon-coated silicon monoxide and lithium hydride in an inert gas atmosphere;
s2, transferring the mixed materials into a heating device, and heating and carbonizing the mixed materials in an inert gas atmosphere;
and S3, scattering the carbonized materials.
2. The method for preparing a high-efficiency silicon monoxide negative electrode according to claim 1, wherein the method comprises the following steps: in the step S1, the carbon-coated silica D50 is 0.1 to 10 μm, and the coating method is one or more of a solid phase, a gas phase, and a liquid phase.
3. The method for preparing a high-efficiency silicon monoxide negative electrode according to claim 1, wherein the method comprises the following steps: in the step S1, the purity of the lithium hydride is more than or equal to 95 percent; the proportion of lithium hydride added is between 2 and 20 wt.%.
4. The method for preparing a high-efficiency silicon monoxide negative electrode according to claim 1, wherein the method comprises the following steps: in the step S1, the mixing device is one of a VC machine, a three-dimensional mixer, and a fusion machine; the inert gas is one or more of nitrogen, argon and helium.
5. The method for preparing a high-efficiency silicon monoxide negative electrode according to claim 1, wherein the method comprises the following steps: in the step S2, the heating device is a roller kiln, a rotary kiln, a pusher kiln, a hot-pack kettle, a fusion or VC machine with a heating device; the heating temperature is 600-1000 ℃, the heating time is 0.5-12 hours, and the inert gas is one or more of nitrogen, argon and helium.
6. The method for preparing a high-efficiency silicon monoxide negative electrode according to claim 1, wherein the method comprises the following steps: in the step S3, the breaking device is a mechanical crusher, a shaping machine, an airflow crusher, a VC machine and a fusion machine; the granularity of the scattered material is 2-15 mu m.
7. A high-first-efficiency negative electrode of silica, characterized by being produced by the production method according to any one of claims 1 to 6.
8. A high-efficiency silicon monoxide negative electrode as recited in claim 7, wherein: the capacity of the high first-efficiency silicon monoxide negative electrode is more than 1200.0mAh/g, and the first efficiency is more than 90.00%.
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