CN109192937A - A kind of preparation method of silicon-carbon cathode material - Google Patents
A kind of preparation method of silicon-carbon cathode material Download PDFInfo
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- CN109192937A CN109192937A CN201810837167.1A CN201810837167A CN109192937A CN 109192937 A CN109192937 A CN 109192937A CN 201810837167 A CN201810837167 A CN 201810837167A CN 109192937 A CN109192937 A CN 109192937A
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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
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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
- 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
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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
- H01M4/58—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
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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 invention discloses a kind of preparation methods of silicon-carbon cathode material.The following steps are included: (1) is by silicon powder or nano-silicon and deionized water according to molar ratio 1:(0.7-1.7) mixing and ball milling 4-48h；(2) step (1) gains are dry, 1-4h is then calcined, Si/SiO is obtainedXCombination product；(3) Si/SiO is takenXCombination product and carbon source, ball milling 4-48h；(4) mixture of step (3) is carbonized, is then cooled to room temperature, continued ball milling and refine 6h；(5) powder for taking step (4) to obtain HF corrodes 4-48h, is then centrifuged 3-30 minutes under the conditions of 5000-10000rpm, up to silicon-carbon cathode material after drying.Silicon-carbon cathode material of the invention is provided simultaneously with the high circulation stability of high storage the lithium characteristic and Carbon materials of silicon class material, and specific capacity is high, good cycling stability；The case where active material causes pole piece to lose powder because of expansion is efficiently solved, the cycle performance of lithium ion battery is improved, is had a good application prospect on lithium ion battery.
Description
Technical field
The present invention relates to a kind of lithium ion battery negative material, the preparation method of specifically a kind of silicon-carbon cathode material.
Background technique
Due to the fast development and extensive use of portable electronic device and electric car, for high-energy-density, long circulating
The demand of the lithium ion battery in service life is very urgent.The lithium ion battery used is commercialized at present mainly uses graphite as cathode
Material still since the theoretical specific capacity of graphite is only 372mAh/g, limits further mentioning for lithium ion battery specific energy
It is high.Silicon because its with the high embedding lithium specific capacity of theory (4200mAh/g, much higher than current other all negative electrode materials), compared with
Low storage lithium current potential and cause great concern, be one of ideal candidates material of novel high-capacity lithium storage materials.
But silicon materials, during removal lithium embedded, there are serious volume changes, be easy to cause the dusting of silicon particle, make
Electrode slice is loose, and active material is caused to fall off from collector, leads to the cyclical stability sharp fall of electrode.For the body of silicon
Product effect, carries out the compound bulk effect to buffer silicon for the carbon of silicon, is the effective means for improving silica-base material.Although carbon material
Theoretical capacity it is relatively low, but carbon material has relatively good elasticity, is good lithium ion conductor, itself has certain embedding
Lithium capacity, and removal lithium embedded volume change very little, the stability of cycle performance are good.
Improve the method for the cycle performance of silica-base material at present by sol-gel method, silicon-carbon composite algorithm, doping and surface
Cladding process etc..However, there is also certain shortcomings, for example, one in these existing silicon-carbon cathode material preparation methods
The organic solvents such as acetone, butanone can be used in a little sol-gel methods, not only increase production cost, also to operator and environment
Bring adverse effect；And the organic solvents such as acetone, butanone are difficult to completely remove in process of production, and the impurity of trace will affect
The efficiency for charge-discharge of battery and service life.In addition, only tentatively solving silicon substrate using the material of the processing such as sol-gel method
The expansion issues of material；However, will appear the problem of being easy picking after being prepared into electrode slice since silicon materials are hard, crisp.Meanwhile electricity
The service life in pond is low.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of silicon-carbon cathode material, to solve to mention in above-mentioned background technique
Out the problem of.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of silicon-carbon cathode material, comprising the following steps:
(1) by silicon powder or nano-silicon and deionized water according to molar ratio 1:(0.7-1.7) mixing and ball milling 4-48h；
(2) step (1) gains are dry, 1-4h is then calcined, Si/SiO is obtainedXCombination product；
(3) Si/SiO is takenXCombination product and carbon source, ball milling 4-48h；
(4) mixture of step (3) is carbonized, is then cooled to room temperature, continued ball milling and refine 6h；
(5) powder for obtaining step (4) corrodes, up to silicon-carbon cathode material after drying.
As a further solution of the present invention: calcination temperature is 700-1000 DEG C in the step (2).
As a further solution of the present invention: the carbon source in the step (3) is pitch, sucrose, glucose and phenolic aldehyde tree
Any one in rouge.
As a further solution of the present invention: Si/SiO in the step (3)XThe weight ratio of combination product and carbon source is
(1-9): 1.
As a further solution of the present invention: carburizing temperature is 600-1500 DEG C in the step (4).
As a further solution of the present invention: the powder for taking step (4) to obtain in the step (5) is with mass concentration
Corrode 4-48h under the HF ultrasound condition of 4%-20%.
As a further solution of the present invention: the step (5) further includes rotary process: the gains after corrosion exist
It is centrifuged 3-30 minutes under the conditions of 5000-10000rpm.
As a further solution of the present invention: the step (5) further includes washing step: before dry, gains first being used
Deionized water is washed to neutrality.
Compared with prior art, the beneficial effects of the present invention are:
Silicon-carbon cathode material of the invention is provided simultaneously with the high circulation stability of high storage the lithium characteristic and Carbon materials of silicon class material,
Specific capacity is high, good cycling stability；Efficiently solve the case where active material causes pole piece to lose powder because of expansion, improve lithium from
The cycle performance of sub- battery, method is simple to operation, easily realization industrialization, before having application well on lithium ion battery
Scape.
Detailed description of the invention
Fig. 1 is the XRD diagram of silicon-carbon cathode material prepared by embodiment 1, embodiment 2 and embodiment 3.Wherein, (a) is corresponding
Embodiment 1, (b) corresponding embodiment 2, (c) corresponding embodiment 3.It (d) is the XRD diagram of pure silicon.
Fig. 2 is the SEM figure of silicon-carbon cathode material prepared by embodiment 1.
Fig. 3 is the SEM figure of silicon-carbon cathode material prepared by embodiment 2.
Fig. 4 is the SEM figure of silicon-carbon cathode material prepared by embodiment 3.
Fig. 5 is the cycle performance figure of silicon-carbon cathode material prepared by embodiment 4.
Fig. 6 is the high rate performance figure of silicon-carbon cathode material prepared by embodiment 5.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
It takes silicon powder or nano-silicon and water to be put into ball milling 12h in ball grinder according to molar ratio for 1:1.3, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 3h at 900 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and sucrose
It is in mass ratio 1:1 mixing and ball milling 10h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 200 DEG C, 400 DEG C then are warming up to 0.6 DEG C/min, is then warming up to 700 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, is added concentration 5mol/L's
In NaOH, ultrasonic 12h corrosion；Then it is washed with water to neutrality, then is dried to get silicon-carbon cathode material.
Embodiment 2
It takes silicon powder or nano-silicon and water to be put into ball milling 36h in ball grinder according to molar ratio for 1:0.8, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 3h at 900 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and pitch
It is in mass ratio 1:1 mixing and ball milling 12h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 300 DEG C, 600 DEG C then are warming up to 2 DEG C/min, is then warming up to 1200 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and mass concentration 10% is added
Ultrasound 12 hours in HF；Then it is washed with water to neutrality, then is dried to get silicon-carbon cathode material.
Embodiment 3
It takes silicon powder or nano-silicon and water to be put into ball milling 12h in ball grinder according to molar ratio for 1:1.3, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 3h at 900 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and pitch
It is in mass ratio 4:1 mixing and ball milling 15h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 300 DEG C, 600 DEG C then are warming up to 2 DEG C/min, is then warming up to 1400 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and mass concentration 10% is added
Ultrasound 12 hours in HF；Then it is washed with water to neutrality, then is dried to get silicon-carbon cathode material.
Embodiment 4
Take silicon powder or nano-silicon and water to be put into ball milling in ball grinder according to molar ratio for 1:1.6 for 24 hours, will pour into after gains drying
In crucible, it is put into Muffle furnace the calcining 3h at 800 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and sucrose
It is in mass ratio 1:1 mixing and ball milling 18h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 200 DEG C, 400 DEG C then are warming up to 0.6 DEG C/min, is then warming up to 700 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and mass concentration 10% is added
Ultrasound 24 hours in HF；Then it is washed with water to neutrality, then is dried to get silicon-carbon cathode material.
Embodiment 5
It takes silicon powder or nano-silicon and water to be put into ball milling 12h in ball grinder according to molar ratio for 1:1.3, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 3h at 900 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and sucrose
It is in mass ratio 9:1 mixing and ball milling 20h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 200 DEG C, 400 DEG C then are warming up to 0.6 DEG C/min, is then warming up to 700 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and mass concentration 10% is added
Ultrasound 36 hours in HF；Then it is washed with water to neutrality, then is dried to get silicon-carbon cathode material.
Embodiment 6
It takes silicon powder or nano-silicon and water to be put into ball milling 48h in ball grinder according to molar ratio for 1:1.3, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 3h at 900 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and pitch
It is in mass ratio 1:1 mixing and ball milling 25h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 300 DEG C, 600 DEG C then are warming up to 2 DEG C/min, is then warming up to 1200 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and mass concentration 10% is added
Ultrasound 12 hours in HF；Then it is washed with water to neutrality, then is dried to get silicon-carbon cathode material.
Embodiment 7
It takes silicon powder or nano-silicon and water to be put into ball milling 48h in ball grinder according to molar ratio for 1:1.3, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 3h at 900 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and pitch
It is in mass ratio 4:1 mixing and ball milling 15h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 300 DEG C, 600 DEG C then are warming up to 2 DEG C/min, is then warming up to 1200 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and mass concentration 10% is added
Ultrasound 48 hours in HF；Then it is washed with water to neutrality, then is dried to get silicon-carbon cathode material.
The electrode of lithium ion battery is made in the material made from above-mentioned steps, and just extremely lithium piece, electrolyte are silicon carbon material
Electrolyte is made into button cell, and test macro is blue electrical measurement test system, and test charging and discharging currents density is 0.1mA, ends charge and discharge
Piezoelectric voltage is 0.01-3V.
Embodiment 8
It takes silicon powder or nano-silicon and water to be put into ball milling 4h in ball grinder according to molar ratio for 1:0.7, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 1h at 700 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and sucrose
It is in mass ratio 1:1 mixing and ball milling 4h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 200 DEG C, 400 DEG C then are warming up to 0.6 DEG C/min, is then warming up to 600 DEG C and constant temperature 2h with 5 DEG C/min, carbonization is wrapped up,
It is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and the HF that concentration is 4% is added
In, ultrasonic 4h corrosion；Then it is centrifuged 3 minutes under the conditions of 5000rpm；Then it is washed with deionized to neutrality；Place into 50
DEG C baking oven in drying to get silicon-carbon cathode material.
Embodiment 9
It takes silicon powder or nano-silicon and water to be put into ball milling 48h in ball grinder according to molar ratio for 1:1.7, will be poured into after gains drying
In crucible, it is put into Muffle furnace the calcining 4h at 1000 DEG C and obtains Si/SiOXCombination product；By Si/SiOXCombination product and sucrose
It is in mass ratio 1:9 mixing and ball milling 48h；Then gains are poured into quartz boat, be put into tube furnace with 5 DEG C/min by room temperature liter
To 200 DEG C, 400 DEG C then are warming up to 0.6 DEG C/min, is then warming up to 1500 DEG C and constant temperature 2h with 5 DEG C/min, carbonization packet
It wraps up in, is then cooled to room temperature；By obtained product, ball milling refines 6h in the ball mill, is put into beaker, and it is 20% that concentration, which is added,
In HF, ultrasonic 48h corrosion；Then it is centrifuged 30 minutes under the conditions of 10000rpm；Then it is washed with deionized to neutrality；It puts again
Enter in 120 DEG C of baking oven and dries to get silicon-carbon cathode material.
Embodiment 10
As different from Example 9, sucrose therein is replaced with into glucose.
Embodiment 11
As different from Example 9, sucrose therein is replaced with into phenolic resin.
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective
Various changes can be made.
Claims (8)
1. a kind of preparation method of silicon-carbon cathode material, which comprises the following steps:
(1) by silicon powder or nano-silicon and deionized water according to molar ratio 1:(0.7-1.7) mixing and ball milling 4-48h；
(2) step (1) gains are dry, 1-4h is then calcined, Si/SiO is obtainedXCombination product；
(3) Si/SiO is takenXCombination product and carbon source, ball milling 4-48h；
(4) mixture of step (3) is carbonized, is then cooled to room temperature, continued ball milling and refine 6h；
(5) powder for obtaining step (4) corrodes, up to silicon-carbon cathode material after drying.
2. the preparation method of silicon-carbon cathode material according to claim 1, which is characterized in that calcining in the step (2)
Temperature is 700-1000 DEG C.
3. the preparation method of silicon-carbon cathode material according to claim 1, which is characterized in that the carbon in the step (3)
Source is any one in pitch, sucrose, glucose and phenolic resin.
4. the preparation method of silicon-carbon cathode material according to claim 1, which is characterized in that Si/ in the step (3)
SiOXThe weight ratio of combination product and carbon source is (1-9): 1.
5. the preparation method of silicon-carbon cathode material according to claim 1, which is characterized in that carbonization in the step (4)
Temperature is 600-1500 DEG C.
6. the preparation method of silicon-carbon cathode material according to claim 1, which is characterized in that take step in the step (5)
Suddenly corrode 4-48h under the HF ultrasound condition that the powder that (4) obtain is 4%-20% with mass concentration.
7. the preparation method of silicon-carbon cathode material according to claim 1, which is characterized in that the step (5) further includes
Rotary process: the gains after corrosion are centrifuged 3-30 minutes under the conditions of 5000-10000rpm.
8. the preparation method of silicon-carbon cathode material according to claim 7, which is characterized in that the step (5) further includes
Washing step: before dry, gains are first washed with deionized to neutrality.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110783531A (en) * | 2018-07-31 | 2020-02-11 | 纳米及先进材料研发院有限公司 | Method for preparing electrode active material and battery electrode |
| CN111900347A (en) * | 2020-07-14 | 2020-11-06 | 中国科学院山西煤炭化学研究所 | Method for preparing silicon-carbon composite material based on ball milling method in air atmosphere and application thereof |
| CN113471436A (en) * | 2021-06-07 | 2021-10-01 | 四川启睿克科技有限公司 | In-situ coated silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| CN116516522A (en) * | 2023-04-03 | 2023-08-01 | 苏州大学 | Lithium ion self-supporting silicon-carbon composite nanofiber negative electrode material and preparation method and application thereof |
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| CN104953122A (en) * | 2015-06-30 | 2015-09-30 | 深圳清华大学研究院 | Nanometer silicon and carbon composite negative electrode material and preparation method and lithium ion battery thereof |
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| CN103107317A (en) * | 2013-01-17 | 2013-05-15 | 奇瑞汽车股份有限公司 | Si-C composite material and preparation method thereof and lithium ion battery containing same |
| CN103779546A (en) * | 2014-01-21 | 2014-05-07 | 南京安普瑞斯有限公司 | Hollow structure material as well as preparation method and use thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110783531A (en) * | 2018-07-31 | 2020-02-11 | 纳米及先进材料研发院有限公司 | Method for preparing electrode active material and battery electrode |
| CN111900347A (en) * | 2020-07-14 | 2020-11-06 | 中国科学院山西煤炭化学研究所 | Method for preparing silicon-carbon composite material based on ball milling method in air atmosphere and application thereof |
| CN113471436A (en) * | 2021-06-07 | 2021-10-01 | 四川启睿克科技有限公司 | In-situ coated silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| CN113471436B (en) * | 2021-06-07 | 2022-10-14 | 四川启睿克科技有限公司 | In-situ coated silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| CN116516522A (en) * | 2023-04-03 | 2023-08-01 | 苏州大学 | Lithium ion self-supporting silicon-carbon composite nanofiber negative electrode material and preparation method and application thereof |
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Application publication date: 20190111 |
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| RJ01 | Rejection of invention patent application after publication |