CN109980206A - Preparation method, negative electrode material and the lithium ion battery of low bulk silicon-carbon cathode material - Google Patents
Preparation method, negative electrode material and the lithium ion battery of low bulk silicon-carbon cathode material Download PDFInfo
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- CN109980206A CN109980206A CN201910261020.7A CN201910261020A CN109980206A CN 109980206 A CN109980206 A CN 109980206A CN 201910261020 A CN201910261020 A CN 201910261020A CN 109980206 A CN109980206 A CN 109980206A
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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
- H01M4/362—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
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 embodiments relate to preparation method, negative electrode material and the lithium ion batteries of a kind of low bulk silicon-carbon cathode material, and nano-silicon powder, asphalt powder and surfactant are ground in sand mill, obtain the first suspension；Obtained the first suspension and carbon source material are stirred in high-speed shearing emulsion machine, obtain the second suspension, and deaeration processing is carried out to the second suspension；To deaeration, treated that the second suspension is stirred, and during stirring, and the second suspension is used centrifugal spray drying under the conditions of 120~270 DEG C, obtains dry pack；Dry pack is carbonized at 700~1300 DEG C, obtains finished product after cooling, screening.The present invention is compound using porous carbon source material and nano-silicon, cladding provides cushion space due to the presence of carbon source surface micropore, and to the violent silicon of volume expansion during cycle charging, therefore electrode or battery bulk expansion is available is effectively relieved.
Description
Technical field
The present invention relates to field of material technology more particularly to a kind of preparation methods of low bulk silicon-carbon cathode material, cathode
Material and lithium ion battery.
Background technique
Current world economy rapid development, energy and environment problem is also increasingly serious, and countries in the world also can by sight steering
Energy of persistent loop, such as wind energy, geothermal energy, tide energy etc., and these energy require to use energy storage device, it is in addition electronic
Automobile, digital product etc. are also required to use energy storage device.In these energy storage devices, generally based on lithium secondary battery, and it is current
The lithium secondary battery of industrialization has that energy density is low mainly using graphite as cathode.
To solve this problem, many experts, scholar begin one's study silicon-carbon composite cathode material, the theoretical capacity of pure silicon
4200mAh/g, but volume expansion of charging is violent, and meeting pulverization situation is severe after silicon materials circulation is multiple, and capacitance loss is huge.Cause
This, silicon materials are usually crushed to nanoscale and are coated with soft carbon by existing method, are being filled although silicon can be effectively relieved
Dusting in electric cyclic process, but partial volume can only be inhibited to expand, volume expansion is still violent, severe.
Summary of the invention
The purpose of the present invention is in view of the drawbacks of the prior art, provide a kind of preparation side of low bulk silicon-carbon cathode material
Method, negative electrode material and lithium ion battery, cladding compound using porous carbon source material and nano-silicon, during cycle charging, by
Cushion space is provided in the presence of carbon source surface micropore, and to the violent silicon of volume expansion, therefore electrode or battery are integrally swollen
It is swollen available to be effectively relieved.
In view of this, in a first aspect, the embodiment of the invention provides a kind of preparation method of low bulk silicon-carbon cathode material,
The described method includes:
Nano-silicon powder, asphalt powder and surfactant are ground in sand mill, obtain the first suspension；
Obtained first suspension and carbon source material are stirred in high-speed shearing emulsion machine, it is outstanding to obtain second
Supernatant liquid, and deaeration processing is carried out to second suspension；
To the deaeration, treated that the second suspension is stirred, and during stirring, by the second suspension
Centrifugal spray drying is used under the conditions of 120~270 DEG C, obtains dry pack；
The dry pack is carbonized at 700~1300 DEG C, obtains finished product after cooling, screening.
Preferably, the surface of the carbon source material is cellular, 0.01~0.10cm of Kong Rongwei3/ g, partial size Dv50 be 5~
30um。
It is further preferred that the carbon source material is that artificial graphite, natural graphite, carbonaceous mesophase spherules are one or more.
It is further preferred that the carbon source material and nano-silicon powder, asphalt powder, the weight ratio between surfactant
For 100:5~30:10~40:0.5~5.
Preferably, the surfactant is neopelex, sodium carboxymethylcellulose pyce, methylcellulose, poly- second
One of glycol is a variety of.
Preferably, the partial size Dv50 of the nano-silicon powder is 3~120nm.
Preferably, the partial size Dv50 of the asphalt powder be 1~20um, coking value be 30~80%, softening point be 50~
300℃。
Second aspect, the embodiment of the invention provides a kind of silicon prepared using preparation method described in above-mentioned first aspect
Carbon negative pole material.
The third aspect, the embodiment of the invention provides a kind of lithiums including silicon-carbon cathode material described in above-mentioned second aspect
Ion battery.
Preparation method, negative electrode material and the lithium-ion electric of a kind of low bulk silicon-carbon cathode material provided in an embodiment of the present invention
Pond, cladding compound using porous carbon source material and nano-silicon, during cycle charging, due to the presence of carbon source surface micropore,
And cushion space is provided to the violent silicon of volume expansion, therefore electrode or battery bulk expansion is available is effectively relieved.
Detailed description of the invention
Fig. 1 is a kind of preparation method flow chart of low bulk silicon-carbon cathode material provided in an embodiment of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of carbon source material surface topography used in the present invention.
Specific embodiment
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Fig. 1 is a kind of preparation method flow chart of low bulk silicon-carbon cathode material provided in an embodiment of the present invention, such as Fig. 1 institute
Show, which comprises
Step 101, nano-silicon powder, asphalt powder and surfactant are ground in sand mill, obtains the first suspension
Liquid.
Wherein, the partial size Dv50 of nano-silicon powder is 3~120nm.
The partial size Dv50 of asphalt powder is 1~20um, and coking value is 30~80%, and softening point is 50~300 DEG C.
Surfactant is one of neopelex, sodium carboxymethylcellulose pyce, methylcellulose, polyethylene glycol
Or it is a variety of.
It is ground specifically, nano-silicon powder, asphalt powder and surfactant are placed in sand mill, grinding
Effect is by force plus an external force is sufficiently mixed nano-silicon powder and asphalt powder under the action of surfactant
It is even, obtain the first suspension.
Step 102, obtained the first suspension and carbon source material are stirred in high-speed shearing emulsion machine, obtain
Two suspension, and deaeration processing is carried out to the second suspension.
Wherein, the surface of carbon source material is cellular, specifically as shown in Fig. 2, 0.01~0.10cm of Kong Rongwei3/ g, partial size
Dv50 is 5~30um.Carbon source material is that artificial graphite, natural graphite, carbonaceous mesophase spherules are one or more.
Further, carbon source material and nano-silicon powder, asphalt powder, the weight ratio between surfactant are 100:5
~30:1~40:0.5~5.
Specifically, the first suspension and carbon source material are stirred in high-speed shearing emulsion machine, thus by carbon source material
Material is distributed in the first suspension, obtains the second suspension.
After this, to the second suspension carry out vacuumizing and defoaming processing, vacuumizing and defoaming processing purpose be in order to from
Heart spray drying is prepared, and will cause spray head if there is bubble enters in pipeline and has one section of no liquid dry and cause sharply to rise
Temperature, after bubble section is gone out, the place that liquid segment flows to nozzle, which encounters high temperature, can be carbonized plug nozzle, and deaeration processing can avoid this
One the occurrence of.
Step 103, to deaeration, treated that the second suspension is stirred, and during stirring, second is hanged
Supernatant liquid uses centrifugal spray drying under the conditions of 120~270 DEG C, obtains dry pack.
The second suspension precipitates before the drying in order to prevent, is stirred, and during stirring, will
Second suspension uses centrifugal spray drying under the conditions of 120~270 DEG C, and aqueous solvent is all evaporated, carbon source material and nano-silicon
Powder is bonded by pitch, is coated togather, and a bulky grain, i.e. dry pack are formed.
It should be noted that according to charging rate and asphalt softening point difference, temperature is different.
In spray-drying process, asphalt powder softening point height is related with the nozzle temperature of spray drying, in order to make to drip
Melting state is in when blueness is at nozzle, temperature reduces after ejection, and just nano-silicon and carbon source material are bonded and coated, is formed
Composite particles, the above-mentioned coking value used is 30~80%, pitch that softening point is 50~300 DEG C.It is unfavorable if softening point is too low
It is crushed in pitch point, will appear hardened caking phenomenon under the pitch room temperature crushed；It is needed if softening point is too high, when spraying higher
Temperature makes asphalt melting, and heating energy consumption is high.
Step 104, dry pack is carbonized at 700~1300 DEG C, obtains finished product after cooling, screening.
At a temperature of 700~1300 DEG C, pitch loses volatile matter, forms soft carbon and coats carbon source material and nano-silicon to be formed
Composite particles, i.e. silicon-carbon composite cathode material.
The preparation method of low bulk silicon-carbon cathode material provided in an embodiment of the present invention provides one and silicon-carbon is effectively reduced
The approach of negative electrode material expansion, cladding compound using porous carbon source material and nano-silicon, due to the presence of carbon source surface micropore,
And cushion space is provided to the violent silicon of volume expansion.
Silicon-carbon composite cathode material made from the preparation method provided through the embodiment of the present invention, in cycle charging process
In, cushion space is provided due to the presence of carbon source surface micropore, and to the violent silicon of volume expansion, therefore electrode or battery are whole
Body expansion is available to be effectively relieved.
Negative electrode material provided in this embodiment can be used as the negative electrode material of lithium ion battery or as the one of its negative electrode material
Part, the expansion of elemental silicon is under soft carbon cladding and the collective effect of micropore, and battery bulk expansion effect reduces, and capacity is kept
Rate is improved, and is of great significance to battery energy density is improved.
In the following, by some specific embodiments, to the preparation process of silicon-carbon cathode material provided in an embodiment of the present invention
And the application of silicon-carbon cathode material obtained, performance are described in more detail.
Embodiment 1
Step 1, by 5nm nano-silicon powder, 5um asphalt powder (last coking value=70%, softening point=260 DEG C) and dodecane
Base benzene sulfonic acid sodium salt is ground in sand mill, obtains suspension I；
Step 2, by obtained suspension I and artificial graphite (Kong Rong=0.08cm3/ g) stirring in high-speed shearing emulsion machine
Suspension II is formed under the effect of mixing, and carries out deaeration processing, artificial graphite and nano-silicon powder, asphalt powder and surfactant
Weight ratio is respectively 100:25,100:40,100:5；
Step 3, during being kept stirring, suspension II is used into centrifugal spray drying under the conditions of 270 DEG C, is obtained
Dry pack I；
Step 4, mixture I is carbonized at 700 DEG C, obtains finished product after cooling screening.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
Embodiment 2
Step 1, by 30nm nano-silicon powder, 20um asphalt powder (last coking value=50%, softening point=200 DEG C) and methyl
Cellulose is ground in sand mill, obtains suspension I；
Step 2, by obtained suspension I and artificial graphite (Kong Rong=0.04cm3/ g) stirring in high-speed shearing emulsion machine
Suspension II is formed under the effect of mixing, and carries out deaeration processing, artificial graphite and nano-silicon powder, asphalt powder and surfactant
Weight ratio is respectively 100:15,100:25,100:4；
Step 3, during being kept stirring, suspension II is used into centrifugal spray drying under the conditions of 230 DEG C, is obtained
Dry pack I；
Step 4, mixture I is carbonized at 900 DEG C, obtains finished product after cooling screening.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
Embodiment 3
Step 1, by 60nm nano-silicon powder, 10um asphalt powder (last coking value=40%, softening point=120 DEG C) He Juyi
Glycol is ground in sand mill, obtains suspension I；
Step 2, by obtained suspension I and natural graphite (Kong Rong=0.02cm3/ g) stirring in high-speed shearing emulsion machine
Suspension II is formed under the effect of mixing, and carries out deaeration processing, artificial graphite and nano-silicon powder, asphalt powder and surfactant
Weight ratio is respectively 100:5,100:15,100:1；
Step 3, during being kept stirring, suspension II is used into centrifugal spray drying under the conditions of 180 DEG C, is obtained
Dry pack I；
Step 4, mixture I is carbonized at 1100 DEG C, obtains finished product after cooling screening.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
Embodiment 4
Step 1, by 120nm nano-silicon powder, 15um asphalt powder (last coking value=30%, softening point=80 DEG C) and methyl
Sodium cellulosate is ground in sand mill, obtains suspension I；
Step 2, by obtained suspension I and natural graphite (Kong Rong=0.06cm3/ g) stirring in high-speed shearing emulsion machine
Suspension II is formed under the effect of mixing, and carries out deaeration processing, artificial graphite and nano-silicon powder, asphalt powder and surfactant
Weight ratio is respectively 100:7,100:10,100:2.5；
Step 3, during being kept stirring, suspension II is used into centrifugal spray drying under the conditions of 120 DEG C, is obtained
Dry pack I；
Step 4, mixture I is carbonized at 1300 DEG C, obtains finished product after cooling screening.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
Comparative example 1
Comparative example 1 and embodiment 1 distinguish the carbon source for being that comparative example uses using the carbon source material of same particle size and material
Material surface is smooth non-porous, other steps, parameter are same as Example 1.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
Comparative example 2
Comparative example 2 and embodiment 2 distinguish the carbon source for being that comparative example uses using the carbon source material of same particle size and material
Material surface is smooth non-porous, other steps, parameter are same as Example 2.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
Comparative example 3
Comparative example 3 and embodiment 3 distinguish the carbon source for being that comparative example uses using the carbon source material of same particle size and material
Material surface is smooth non-porous, other steps, parameter are same as Example 3.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
Comparative example 4
Comparative example 4 and embodiment 4 distinguish the carbon source for being that comparative example uses using the carbon source material of same particle size and material
Material surface is smooth non-porous, other steps, parameter are same as Example 4.
Obtained finished product is made into 1.60g/cm3Pole piece and be assembled into full battery and tested, test result such as 1 institute of table
Show.
1 embodiment 1-4 of table and comparative example 1-4 raw material physical property and full electrical test results
Result is found out from table 1, and comparative example is suitable corresponding thereto with capacity for the first effect of each embodiment, and loop test
When capacity keeps 80%, embodiment cycle-index is slightly above comparative example.In addition, the full electric cubical expansivity of each embodiment pole piece is wanted
Significantly lower than its comparative example, this point mainly has benefited from part silicon volume expansion and offsets to micropore diffusion, therefore battery entirety
Bulking effect reduces.It can be seen that this method provides the approach that one is effectively reduced silicon-carbon cathode material expansion, it is obtained
Silicon-carbon cathode material is used for lithium ion battery, and under soft carbon cladding and the collective effect of micropore, battery is whole for the expansion of elemental silicon
Bulking effect reduces, and capacity retention ratio is improved, and is of great significance to battery energy density is improved.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of low bulk silicon-carbon cathode material, which is characterized in that the described method includes:
Nano-silicon powder, asphalt powder and surfactant are ground in sand mill, obtain the first suspension；
Obtained first suspension and carbon source material are stirred in high-speed shearing emulsion machine, obtain the second suspension
Liquid, and deaeration processing is carried out to second suspension；
To the deaeration, treated that the second suspension is stirred, and during stirring, by the second suspension 120
Centrifugal spray drying is used under the conditions of~270 DEG C, obtains dry pack；
The dry pack is carbonized at 700~1300 DEG C, obtains finished product after cooling, screening.
2. the preparation method of low bulk silicon-carbon cathode material according to claim 1, which is characterized in that the carbon source material
Surface be cellular, 0.01~0.10cm of Kong Rongwei3/ g, partial size Dv50 are 5~30um.
3. the preparation method of low bulk silicon-carbon cathode material according to claim 1 or 2, which is characterized in that the carbon source
Material is that artificial graphite, natural graphite, carbonaceous mesophase spherules are one or more.
4. the preparation method of low bulk silicon-carbon cathode material according to claim 3, which is characterized in that the carbon source material
Weight ratio between nano-silicon powder, asphalt powder, surfactant is 100:5~30:10~40:0.5~5.
5. the preparation method of low bulk silicon-carbon cathode material according to claim 1, which is characterized in that the surface-active
Agent is one of neopelex, sodium carboxymethylcellulose pyce, methylcellulose, polyethylene glycol or a variety of.
6. the preparation method of low bulk silicon-carbon cathode material according to claim 1, which is characterized in that the nano silica fume
The partial size Dv50 at end is 3~120nm.
7. the preparation method of low bulk silicon-carbon cathode material according to claim 1, which is characterized in that the asphalt powder
Partial size Dv50 be 1~20um, coking value be 30~80%, softening point be 50~300 DEG C.
8. a kind of silicon-carbon cathode material using any preparation method preparation of the claims 1-7.
9. a kind of lithium ion battery including silicon-carbon cathode material described in the claims 8.
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| CN111668472A (en) * | 2020-06-28 | 2020-09-15 | 贝特瑞新材料集团股份有限公司 | Silicon-based composite negative electrode material, preparation method thereof and lithium ion battery |
| CN115064688A (en) * | 2022-08-15 | 2022-09-16 | 溧阳紫宸新材料科技有限公司 | Preparation method of silicon-carbon composite negative electrode material with micropore pores inside |
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