CN109585820A - Si-C composite material, preparation method, application and negative electrode of lithium ion battery - Google Patents
Si-C composite material, preparation method, application and negative electrode of lithium ion battery Download PDFInfo
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- CN109585820A CN109585820A CN201811403672.1A CN201811403672A CN109585820A CN 109585820 A CN109585820 A CN 109585820A CN 201811403672 A CN201811403672 A CN 201811403672A CN 109585820 A CN109585820 A CN 109585820A
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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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/58—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
Abstract
The present invention relates to battery cathode related fieldss, and in particular to Si-C composite material, preparation method, application and negative electrode of lithium ion battery.The Si-C composite material, including surface oxidation are SiOxSilicon powder, graphite composite material, the organic carbon source, surfactant of (x=1 or 2)；The surface oxidation is SiOxThe order of magnitude of partial size of silicon powder be 102nm‑103nm；The graphite composite material includes the graphite of 60%-80% weight percent and the graphene of 20%-40% weight percent；The organic carbon source is pitch or glucose.The capacity boost of the application Si-C composite material, preparation method, application and negative electrode of lithium ion battery, gained composite material is obvious, can preferably be applied to prepare negative electrode of lithium ion battery.
Description
Technical field
The present invention relates to battery cathode related fieldss, and in particular to Si-C composite material, preparation method, application and lithium ion
Battery cathode.
Background technique
Lithium battery can be divided into lithium metal battery and lithium ion battery at present, and wherein the application range of lithium ion battery is wider,
Such as the electronic devices such as calculator, notebook, mobile communication equipment.
Lithium ion battery is usually to use lithium ion as anode, therein using carbon material as battery cathode
Carbon material can be the materials such as graphite, carbon fiber.Graphite therein is since raw material are easy to get, and cost is relatively low, typically as
The negative electrode material of lithium ion battery uses, but since graphite material itself limits, relatively low capacity gradually cannot
Meets the needs of today's society is to high-capacity battery.Therefore, usually there is Surface Oxygen to the processing method that graphite is modified at present
Change, surface cladding etc., but also have certain limitation to the promotion effect of its capacity.
Summary of the invention
In view of this, the application provides a kind of Si-C composite material, preparation method, application and negative electrode of lithium ion battery,
The capacity boost of gained composite material is obvious, can preferably be applied to prepare negative electrode of lithium ion battery.
In view of the deficiencies of the prior art, the present invention provides the technical solutions of first aspect, i.e. Si-C composite material, including
Surface oxidation is SiOxSilicon powder, graphite composite material, organic carbon source, surfactant；X=1 or 2；
The surface oxidation is SiOxThe order of magnitude of partial size of silicon powder be 102nm-103nm；
The graphite composite material includes the graphite and 20%-40% weight hundred of 60%-80% weight percent
Divide the graphene of ratio；
The organic carbon source is pitch or glucose.
Optionally, the particle size of the graphite is 5 μm -200 μm.
The application also provides the technical solution of second aspect, the i.e. preparation method of Si-C composite material, comprising the following steps:
1) after metallic silicon power being mixed with solvent, be added zirconia ball carry out ball milling, filter surface oxidation be SiOx's
Silicon powder；X=1 or 2；
2) through ball milling after being mixed in a certain ratio graphite and grinding aid, dispersing agent, while a period of time is stirred by ultrasonic, obtains
Obtain mixed slurry；The ratio of graphite and grinding aid is (1-4): 1, the concentration that graphite and grinding aid are formed in dispersing agent is 2mg/
mL-5mg/mL；Gained mixed slurry is placed in natural cooling under 15 DEG C -20 DEG C of temperature environment, after be freeze-dried, obtain
Graphite composite material；
It 3) is SiO by surface oxidation obtained by step 1)xSilicon powder and step 2) obtained by graphite composite material it is mixed
Conjunction, after organic carbon source, surfactant is added, ultrasonic agitation obtains Si-C composite material after dry cracking.
Optionally, the purity of metallic silicon power described in step 1) is 99% or more, and the solvent is organic solvent.
Optionally, gained surface oxidation is SiO in step 1)xSilicon powder, surface at least 90% or more is oxidized to SiOx。
Optionally, grinding aid described in step 2) is more fragrant type organics.
Optionally, grinding aid described in step 2) is N- methyl-pyrrolidon NMP or n,N-Dimethylformamide DMF.
Optionally, dispersing agent described in step 2) is water.
It optionally, is 1h-8h for a period of time described in step 2).
Optionally, in step 2) time of natural cooling be for 24 hours -48h, the time of freeze-drying be 20h-24h.
Optionally, surface oxidation is SiO in step 3)xSilicon powder, graphite composite material, organic carbon source, surface
The mixed proportion of activating agent is 10:(5-10 by weight): (2-3): (1-2).
The application also provides the technical solution of the third aspect, i.e. Si-C composite material, according to aforementioned any system
Preparation Method is prepared.
Optionally, including surface oxidation is SiOxSilicon powder, graphite composite material, organic carbon source, surface-active
Agent；X=1 or 2；
The surface oxidation is SiOxThe order of magnitude of partial size of silicon powder be 102nm-103nm；
The graphite composite material includes the graphite and 20%-40% weight hundred of 60%-80% weight percent
Divide the graphene of ratio；
The organic carbon source is pitch or glucose.
Optionally, the particle size of the graphite is 5 μm -200 μm.
The application also provides the technical solution of fourth aspect, i.e., aforementioned any Si-C composite material prepare lithium from
The application of sub- battery cathode.
The application also provides the technical solution of the 5th aspect, i.e. negative electrode of lithium ion battery, using aforementioned any silicon
Carbon composite is prepared.
Scheme provided by the present invention is mainly by using Si-C composite material, preparation method, application and lithium ion battery
Cathode, gained composite material use surface oxidation for SiOxSilicon powder and graphite composite material based on carry out it is compound,
Improve its capacitance, hence it is evident that higher than the capacitance of graphite itself, can preferably be applied to prepare negative electrode of lithium ion battery.
Material or component used by the application are routinely component, can buy acquisition in the market.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 gained Si-C composite material of embodiment；
Fig. 2 is the XRD spectrum of 1 gained Si-C composite material (Si/C) of embodiment；
Fig. 3 is the charge and discharge song that 1 gained Si-C composite material of embodiment is applied to the negative electrode of lithium ion battery being prepared
Line chart；
Fig. 4 is that 1 gained Si-C composite material (Si/C) of embodiment is respectively applied to prepare with natural graphite (Graphite)
The 1C charge-discharge performance comparison diagram of obtained negative electrode of lithium ion battery.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with embodiment of the present invention,
Technical solution in embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only this
Invent a part of embodiment, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.In the absence of conflict, the feature in the embodiment and embodiment in the present invention can mutual any combination.
Si-C composite material and negative electrode of lithium ion battery described herein can be used in following every embodiment not
The Si-C composite material and negative electrode of lithium ion battery of each embodiment are obtained with preparation method.
Embodiment one
According to the following steps and the parameters of table 1 prepare the Si-C composite material of each embodiment respectively.
1) after mixing the metallic silicon power that purity is x/% with solvent C (such as ethyl alcohol organic solvent or water), oxidation is added
Zirconium ball carry out ball milling, filter surface oxidation be SiOxSilicon powder, gained surface oxidation be SiOxThe particle size of silicon powder be n*
102nm-103nm；The mass ratio of zirconia ball, metallic silicon power and solvent C is (1-20): (1-2): 1, Ball-milling Time is 15min-
2h etc.；X=1 or 2；
2) through ball milling after being mixed in a certain ratio graphite and grinding aid, dispersing agent, while a period of time T1/ is stirred by ultrasonic
H obtains mixed slurry；The ratio of graphite and grinding aid A are D1, and graphite is with the grinding aid A concentration formed in dispersant B
D2/mg/mL；Gained mixed slurry is placed in natural cooling T2/h in the environment of t/ DEG C of temperature, after carry out freeze-drying T3/h, obtain
To graphite-graphene composite material；
It 3) is SiO by surface oxidation obtained by step 1)xSilicon powder and step 2) obtained by graphite composite material it is mixed
It closes, (carbonaceous organic materials such as pitch or glucose, surface-active can be used in organic carbon source after addition organic carbon source, surfactant
Neopelex SDBS etc. can be used in agent), ultrasonic agitation obtains Si-C composite material after dry cracking.
3) Si-C composite material of resulting each embodiment is used to prepare negative electrode of lithium ion battery, it is normal that this field can be used
Regulation Preparation Method, and gained Si-C composite material is subjected to UV absorbance detection, obtain its ingredient relative amount value, including stone
The weight percent L2/% and silicon-carbon of the weight percent L1/% of graphite and graphene are multiple in ink/graphene composite material
Surface oxidation is SiO in condensation materialxSilicon powder, graphite composite material, the weight between organic carbon source and surfactant
Measure portion rate y, wherein the particle size of graphite is h/ μm, while by the negative electrode of lithium ion battery being accordingly prepared with other
Lithium ion battery is made in conventional material, measures first charge-discharge capacity Q1/mAhg under its cathode 1C-1, recycle at 1C it is several
Secondary charge/discharge capacity Q2/mAhg-1, 100 charge/discharge capacity Q3/mAhg are recycled at 1C-1, gained measured value is such as
Table 2.
Table 1
| Embodiment | X/% | n | A | B | T1/h | D1 | D2/mg/mL | t/℃ | T2/h | T3/h |
| 1 | 95 | 9 | NMP | Water | 1 | 1:1 | 2 | 20 | 24 | 20 |
| 2 | 97 | 8 | NMP | Water | 8 | 4:1 | 3 | 18 | 30 | 21 |
| 3 | 98 | 5 | NMP | Water | 5 | 2:1 | 4 | 17 | 40 | 22 |
| 4 | 99 | 2 | NMP | Water | 6 | 3:1 | 5 | 15 | 48 | 24 |
| 5 | 95 | 9 | DMF | Water | 1 | 1:1 | 2 | 20 | 24 | 20 |
| 6 | 97 | 8 | DMF | Water | 8 | 4:1 | 3 | 18 | 30 | 21 |
| 7 | 98 | 5 | DMF | Water | 5 | 2:1 | 4 | 17 | 40 | 22 |
| 8 | 99 | 2 | DMF | Water | 6 | 3:1 | 5 | 15 | 48 | 24 |
Table 2
| Embodiment | L1/% | L2/% | y | h/μm | Q1/mAh·g-1 | Q2/mAh·g-1 | Q3/mAh·g-1 |
| 1 | 60 | 40 | 10:5:3:2 | 200 | 552 | 601 | 600 |
| 2 | 70 | 30 | 10:8:3:2 | 100 | 559 | 609 | 608 |
| 3 | 80 | 20 | 10:10:3:2 | 50 | 569 | 616 | 614 |
| 4 | 80 | 20 | 10:10:2:1 | 5 | 572 | 621 | 620 |
| 5 | 60 | 40 | 10:5:3:2 | 200 | 552 | 601 | 600 |
| 6 | 70 | 30 | 10:8:3:2 | 100 | 559 | 609 | 608 |
| 7 | 80 | 20 | 10:10:3:2 | 50 | 569 | 616 | 614 |
| 8 | 80 | 20 | 10:10:2:1 | 5 | 572 | 621 | 620 |
It can be concluded that, the embodiment in table 1 and table 2 uses system described herein from above table and subsequent drawings
Preparation Method, for gained composite material after being applied to prepare negative electrode of lithium ion battery, charge/discharge capacity is apparently higher than graphite material
Negative electrode of lithium ion battery prepared by matter, while for the more material of graphene, the application composite material is multiple
Under recycling, charge/discharge capacity is more stable.
Shown in the drawings, Fig. 1 is the scanning electron microscope (SEM) photograph of 1 gained Si-C composite material of embodiment；Fig. 2 is 1 institute of embodiment
Obtain the XRD spectrum of Si-C composite material (Si/C)；Fig. 3 is that 1 gained Si-C composite material of embodiment is applied to the lithium being prepared
The charging and discharging curve figure of ion battery cathode；Fig. 4 is 1 gained Si-C composite material (Si/C) of embodiment and natural graphite
(Graphite) it is respectively applied to the 1C charge-discharge performance comparison diagram for the negative electrode of lithium ion battery being prepared.From attached drawing
It can also clearly obtain, Si-C composite material described herein can more preferably be obtained using the application preparation method, and
For gained composite material after being applied to prepare negative electrode of lithium ion battery, charge/discharge capacity is substantially better than filling for graphite material itself
Discharge capacity, and the stability of its charge/discharge capacity is also apparently higher than graphite material itself.
The above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
Limitation of the invention, protection scope of the present invention should be defined by the scope defined by the claims..For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change
It also should be regarded as protection scope of the present invention into retouching.
Claims (10)
1. Si-C composite material, it is characterised in that: including surface oxidation be SiOxSilicon powder, graphite composite material, have
Machine carbon source, surfactant；X=1 or 2；
The surface oxidation is SiOxThe order of magnitude of partial size of silicon powder be 102nm-103nm；
The graphite composite material includes the graphite and 20%-40% weight percent of 60%-80% weight percent
Graphene；
The particle size for stating graphite is 5 μm -200 μm；
The organic carbon source is pitch or glucose.
2. the preparation method of Si-C composite material, which comprises the following steps:
1) after metallic silicon power being mixed with solvent, be added zirconia ball carry out ball milling, filter surface oxidation be SiOxSilicon powder；x
=1 or 2；
2) through ball milling after being mixed in a certain ratio graphite and grinding aid, dispersing agent, while a period of time is stirred by ultrasonic, is mixed
Close slurry；The ratio of graphite and grinding aid is (1-4): 1, the concentration that graphite and grinding aid are formed in dispersing agent is 2mg/mL-
5mg/mL；Gained mixed slurry is placed in natural cooling under 15 DEG C -20 DEG C of temperature environment, after be freeze-dried, obtain stone
Ink/graphene composite material；
It 3) is SiO by surface oxidation obtained by step 1)xSilicon powder and step 2) obtained by graphite composite material mixing, be added
After organic carbon source, surfactant, ultrasonic agitation obtains Si-C composite material after dry cracking.
3. preparation method according to claim 2, it is characterised in that: the purity of metallic silicon power described in step 1) is 99%
More than, the solvent is organic solvent；
Grinding aid described in step 2) is N- methyl-pyrrolidon NMP or n,N-Dimethylformamide DMF.
4. preparation method according to claim 2, it is characterised in that: gained surface oxidation is SiO in step 1)xSilicon powder,
Its surface at least 90% or more is oxidized to SiOx。
5. preparation method according to claim 2, it is characterised in that: be 1h-8h for a period of time described in step 2)；Step
2) in the time of natural cooling be for 24 hours -48h, the time of freeze-drying be 20h-24h.
6. preparation method according to claim 2, it is characterised in that: surface oxidation is SiO in step 3)xSilicon powder, stone
Ink/graphene composite material, organic carbon source, surfactant mixed proportion be by weight 10:(5-10): (2-3):
(1-2)。
7. Si-C composite material, it is characterised in that: it is prepared according to preparation method described in power 2.
8. Si-C composite material according to claim 7, it is characterised in that: including surface oxidation be SiOxSilicon powder, stone
Ink/graphene composite material, organic carbon source, surfactant；X=1 or 2；
The surface oxidation is SiOxThe order of magnitude of partial size of silicon powder be 102nm-103nm；
The graphite composite material includes the graphite and 20%-40% weight percent of 60%-80% weight percent
Graphene；
The organic carbon source is pitch or glucose.
9. any Si-C composite material of power 1, power 8 is in the application for preparing negative electrode of lithium ion battery.
10. negative electrode of lithium ion battery, it is characterised in that: formed using power 1, any preparation of silicon carbon composite materials of power 8.
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Application publication date: 20190405 |