CN108400293A - Nitrogen-doped carbon-coated silicon nanomaterial and preparation method and application thereof - Google Patents
Nitrogen-doped carbon-coated silicon nanomaterial and preparation method and application thereof Download PDFInfo
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- CN108400293A CN108400293A CN201810077349.3A CN201810077349A CN108400293A CN 108400293 A CN108400293 A CN 108400293A CN 201810077349 A CN201810077349 A CN 201810077349A CN 108400293 A CN108400293 A CN 108400293A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 75
- 239000010703 silicon Substances 0.000 title claims abstract description 75
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 238000005253 cladding Methods 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 15
- 239000012530 fluid Substances 0.000 claims description 15
- 229920000128 polypyrrole Polymers 0.000 claims description 15
- 239000013049 sediment Substances 0.000 claims description 14
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 7
- 229910001416 lithium ion Inorganic materials 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007773 negative electrode material Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims 1
- 230000000802 nitrating effect Effects 0.000 claims 1
- 150000003233 pyrroles Chemical class 0.000 claims 1
- 235000019698 starch Nutrition 0.000 claims 1
- 239000008107 starch Substances 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 10
- 239000011148 porous material Substances 0.000 abstract description 3
- 239000002210 silicon-based material Substances 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 abstract 2
- 239000000463 material Substances 0.000 description 17
- 238000000034 method Methods 0.000 description 6
- 229910005321 Li15Si4 Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical group [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a nitrogen-doped carbon-coated silicon nano material, wherein the nitrogen content of the nitrogen-doped carbon-coated silicon nano material is 4.0-4.2 wt%. The invention also discloses a preparation method and application of the nitrogen-doped carbon-coated silicon nano material. The nitrogen-doped carbon-coated silicon nano material prepared by the invention has the characteristics of high nitrogen doping amount, large specific surface area and diversified pore diameters, and can be used for regulating and controlling polymerizationThe thickness of the coated carbon is controlled by the amount of pyrrole, the expansion of the silicon material is effectively controlled, the flexibility is high, the whole preparation process is simple and easy to operate, and the preparation method is suitable for low cost. Experiments prove that the specific surface area of the nitrogen-doped carbon-coated silicon nano material is obviously larger than that of the silicon nano material before coating, and reaches 242.7m2(ii)/g; the nitrogen-doped carbon-coated silicon nano material has the aperture within the range of 2-10nm and has diversified aperture structures.
Description
Technical field
The present invention relates to silicon nano material technical fields, and in particular to nitrogen-doped carbon coats silicon nano material and its preparation side
Method and application.
Background technology
The course continuation mileage of power electric motor car is related to the variation of people's demand and the development of future automobile industry.In order to realize
The energy density of power battery 300wh/kg substitutes the LiFePO4 of the marketization, cobalt acid lithium as lithium-ion electric using ternary material
The positive electrode in pond is inevitable choice.At the same time, graphite cathode is substituted with silicon carbon material, the energy of promotion battery at double
Density is the inexorable trend of new-energy automobile industry development.This, which is primarily due to silicon, has lower plateau potential, the reason of superelevation
By capacity (3800mAh/g, Li15Si4；4200mAh/g, Li15Si4, it is nearly 10 times of market graphite capacity), high surface area,
High-tap density and the advantages that simple is prepared, therefore there is great application prospect.But silicon materials exist as negative material
Huge volume change can occur in charge and discharge process, cause the decaying of battery performance drastically.Currently, it is steady to improve silicon materials cycle
Qualitative mode has very much, common are carbon coating and hollow two ways.Wherein, the method that carbon coating prepares silicon nano material
Have very much, Chun-Sing Lee professors are obtained using glucose as organic carbon source by template and mild liquid-phase reduction process
The Si/C materials with nucleocapsid were obtained, conductive carbon-coating and hollow structure provide excellent lithium electrical property for material；
But its complex step and preparation method seriously constrain the yield of material.The Chen Zhongwei of University of Alberta is taught
Carbon-coating is equably grown in surface of silicon nanowires by the method that original flavor is grown, greatly improves the electric conductivity and machine of material
Tool stability, while material also shows considerable capacity and cycle performance.But due to the limitation of operating condition, pole
The earth improves production cost, is not suitable for large-scale production requirement.
Invention content
Technical problems based on background technology, the present invention propose a kind of nitrogen-doped carbon cladding silicon nano material and its
Preparation method and application, nitrogen-doped carbon cladding silicon nano material of the present invention have high nitrogen, large specific surface area and porous structure
Feature, greatly improve the performance of the battery as negative material.
The present invention proposes a kind of nitrogen-doped carbon cladding silicon nano material, and the nitrogen-doped carbon cladding silicon nano material is mixed
Nitrogen quantity is 4.0-4.2wt%.
The present invention also proposes a kind of preparation method of the nitrogen-doped carbon cladding silicon nano material, includes the following steps：
S1, silicon nano dispersion fluid is placed in water-bath in water bath device, adjusts pH, then stirring adds under stirring conditions
Enter polypyrrole, continues to stir, obtain mixed liquor；
S2, mixed liquor is filtered, obtains sediment, sediment is washed with deionized, it is dry；Under nitrogen atmosphere,
By sediment high temperature cabonization, nitrogen-doped carbon cladding silicon nano material is obtained.
Preferably, in S1, a concentration of 39-41wt% of the silicon nano dispersion fluid.
Preferably, in S1, the adjusting pH is added dropwise ammonium hydroxide for use and is adjusted.
Preferably, in S1, pH to 9.5-10.5 is adjusted.
Preferably, in S1,25-35min is stirred after adjusting pH.
Preferably, in S1, continue to stir 5-7h after polypyrrole is added.
Preferably, in S1, the temperature of the water-bath remains 0 DEG C.
Preferably, in S1, the volume ratio of the silicon nano dispersion fluid and polypyrrole is 10：0.5-1.5.
Preferably, in S2, the temperature of the carbonization is to be warming up to 880-920 DEG C with 3 DEG C/min, and keep temperature 2.5-
3.5h。
The present invention also proposes a kind of nitrogen-doped carbon coated Si applications to nanostructures, is applied to negative electrode of lithium ion battery material
Material.
The thickness of carbon coated can be controlled in the present invention by regulating and controlling the amount of polypyrrole.
Compared with prior art, beneficial effects of the present invention are as follows：
1) present invention improves the electric conductivity of material in carbon-coated silicon nanosphere by being doped with nitrogen, increases the ratio of material
Surface area, and provide porous structure and Li is built with this+Fast transferring channel so that silicon nano material be applied to lithium ion
When cell negative electrode material, the electric conductivity of battery can be also dramatically improved, and then improves its chemical property.
2) the present invention provides a kind of preparation methods of the carbon-coated silicon nano material of N doping, can apply to a variety of silicon and receive
Rice material, adaptability are good.
3) preparation method process of the present invention is simple to operation, and cost is relatively low, suitable for mass production.
Description of the drawings
A is the BET that nitrogen-doped carbon coats silicon nano material before silicon nano material and cladding in the embodiment of the present invention 1 in Fig. 1
Figure, b are the graph of pore diameter distribution that nitrogen-doped carbon coats silicon nano material in the embodiment of the present invention 1；
Fig. 2 is the TEM figures that nitrogen-doped carbon coats silicon nano material in the embodiment of the present invention 1.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of nitrogen-doped carbon cladding silicon nano material, the itrogen content of getter with nitrogen doped that the nitrogen-doped carbon coats silicon nano material are
4.1wt%.
The preparation method of the nitrogen-doped carbon cladding silicon nano material, includes the following steps：
S1, silicon nano dispersion fluid is placed in water-bath in water bath device, adjusts pH, then stirring adds under stirring conditions
Enter polypyrrole, continues to stir, obtain mixed liquor；
S2, mixed liquor is filtered, obtains sediment, sediment is washed with deionized, it is dry；Under nitrogen atmosphere,
By sediment high temperature cabonization, nitrogen-doped carbon cladding silicon nano material is obtained；
Wherein, in S1, a concentration of 40wt% of the silicon nano dispersion fluid；In S1, the adjusting pH is to use to add dropwise
Enter ammonium hydroxide to be adjusted；In S1, pH to 10 is adjusted；In S1,30min is stirred after adjusting pH；In S1, continue after polypyrrole is added
Stir 6h；In S1, the temperature of the water-bath remains 0 DEG C；In S1, the volume ratio of the silicon nano dispersion fluid and polypyrrole is
10：1；In S2, the temperature of the carbonization is to be warming up to 900 DEG C with 3 DEG C/min, and keep temperature 3h.
The nitrogen-doped carbon coated Si applications to nanostructures is applied to lithium ion battery negative material.
Embodiment 2
A kind of nitrogen-doped carbon cladding silicon nano material, the itrogen content of getter with nitrogen doped that the nitrogen-doped carbon coats silicon nano material are
4.2wt%.
The preparation method of the nitrogen-doped carbon cladding silicon nano material, includes the following steps：
S1, silicon nano dispersion fluid is placed in water-bath in water bath device, adjusts pH, then stirring adds under stirring conditions
Enter polypyrrole, continues to stir, obtain mixed liquor；
S2, mixed liquor is filtered, obtains sediment, sediment is washed with deionized, it is dry；Under nitrogen atmosphere,
By sediment high temperature cabonization, nitrogen-doped carbon cladding silicon nano material is obtained；
Wherein, in S1, a concentration of 39wt% of the silicon nano dispersion fluid；In S1, the adjusting pH is to use to add dropwise
Enter ammonium hydroxide to be adjusted；In S1, pH to 10.5 is adjusted；In S1,25min is stirred after adjusting pH；In S1, it is subsequent that polypyrrole is added
Continuous stirring 7h；In S1, the temperature of the water-bath remains 0 DEG C；In S1, the volume ratio of the silicon nano dispersion fluid and polypyrrole
It is 10：0.5；In S2, the temperature of the carbonization is to be warming up to 920 DEG C with 3 DEG C/min, and keep temperature 2.5h.
The nitrogen-doped carbon coated Si applications to nanostructures is applied to lithium ion battery negative material.
Embodiment 3
A kind of nitrogen-doped carbon cladding silicon nano material, the itrogen content of getter with nitrogen doped that the nitrogen-doped carbon coats silicon nano material are
4.0wt%.
The preparation method of the nitrogen-doped carbon cladding silicon nano material, includes the following steps：
S1, silicon nano dispersion fluid is placed in water-bath in water bath device, adjusts pH, then stirring adds under stirring conditions
Enter polypyrrole, continues to stir, obtain mixed liquor；
S2, mixed liquor is filtered, obtains sediment, sediment is washed with deionized, it is dry；Under nitrogen atmosphere,
By sediment high temperature cabonization, nitrogen-doped carbon cladding silicon nano material is obtained；
Wherein, in S1, a concentration of 41wt% of the silicon nano dispersion fluid；In S1, the adjusting pH is to use to add dropwise
Enter ammonium hydroxide to be adjusted；In S1, pH to 9.5 is adjusted；In S1,35min is stirred after adjusting pH；In S1, continue after polypyrrole is added
Stir 5h；In S1, the temperature of the water-bath remains 0 DEG C；In S1, the volume ratio of the silicon nano dispersion fluid and polypyrrole is
10：1.5；In S2, the temperature of the carbonization is to be warming up to 880 DEG C with 3 DEG C/min, and keep temperature 3.5h.
The nitrogen-doped carbon coated Si applications to nanostructures is applied to lithium ion battery negative material.
Test example 1
BET, TEM inspection are carried out respectively to silicon nano material before nitrogen-doped carbon cladding silicon nano material, cladding in embodiment 1
It surveys, obtains Fig. 1-2.
A is the BET that nitrogen-doped carbon coats silicon nano material before silicon nano material and cladding in the embodiment of the present invention 1 in Fig. 1
Figure, b are the graph of pore diameter distribution that nitrogen-doped carbon coats silicon nano material in the embodiment of the present invention 1；Fig. 2 is in the embodiment of the present invention 1
Nitrogen-doped carbon coats the TEM figures of silicon nano material.
The electric conductivity of the invention that material is improved by nitrogen doped is can be seen that according to Fig. 1, Fig. 2；Nitrogen of the present invention
The specific surface area of doped carbon cladding silicon nano material is significantly greater than uncoated preceding silicon nano material, reaches 242.7m2/g；This hair
The aperture of bright nitrogen-doped carbon cladding silicon nano material is 2-10nm, has diversified aperture structure.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of nitrogen-doped carbon coats silicon nano material, which is characterized in that the nitrating of the nitrogen-doped carbon cladding silicon nano material
Amount is 4.0-4.2wt%.
2. a kind of preparation method coating silicon nano material based on nitrogen-doped carbon described in claim 1, which is characterized in that including such as
Lower step：
S1, silicon nano dispersion fluid is placed in water-bath in water bath device, adjusts pH, then stirring is added poly- under stirring conditions
Pyrroles continues to stir, obtains mixed liquor；
S2, mixed liquor is filtered, obtains sediment, sediment is washed with deionized, it is dry；Under nitrogen atmosphere, it will sink
Starch high temperature cabonization obtains nitrogen-doped carbon cladding silicon nano material.
3. the preparation method of nitrogen-doped carbon cladding silicon nano material according to claim 2, which is characterized in that described in S1
A concentration of 39-41wt% of silicon nano dispersion fluid.
4. the preparation method of nitrogen-doped carbon cladding silicon nano material according to claim 2, which is characterized in that described in S1
It is to be adjusted using ammonium hydroxide to adjust pH；Preferably, in S1, pH to 9.5-10.5 is adjusted.
5. the preparation method of nitrogen-doped carbon cladding silicon nano material according to claim 2, which is characterized in that in S1, adjust
25-35min is stirred after pH.
6. the preparation method of nitrogen-doped carbon cladding silicon nano material according to claim 2, which is characterized in that in S1, be added
Continue to stir 5-7h after polypyrrole.
7. the preparation method of nitrogen-doped carbon cladding silicon nano material according to claim 2, which is characterized in that described in S1
The temperature of water-bath remains 0 DEG C.
8. the preparation method of nitrogen-doped carbon cladding silicon nano material according to claim 2, which is characterized in that described in S1
The volume ratio of silicon nano dispersion fluid and polypyrrole is 10：0.5-1.5.
9. the preparation method of nitrogen-doped carbon cladding silicon nano material according to claim 2, which is characterized in that described in S2
The temperature of carbonization is to be warming up to 880-920 DEG C with 3 DEG C/min, and keep temperature 2.5-3.5h.
10. it is a kind of according to any one of the claim 1-9 nitrogen-doped carbon coated Si applications to nanostructures, it is applied to lithium ion
Cell negative electrode material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109494360A (en) * | 2018-10-26 | 2019-03-19 | 合肥国轩高科动力能源有限公司 | Silicon monoxide composite material and preparation method thereof |
| CN111048747A (en) * | 2018-10-15 | 2020-04-21 | 通用汽车环球科技运作有限责任公司 | Method of making silicon-containing composite electrodes for lithium-based batteries |
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| CN109494360A (en) * | 2018-10-26 | 2019-03-19 | 合肥国轩高科动力能源有限公司 | Silicon monoxide composite material and preparation method thereof |
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Application publication date: 20180814 |