CN107946570A - Shelly texture silicon-carbon composite electrode material - Google Patents
Shelly texture silicon-carbon composite electrode material Download PDFInfo
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- CN107946570A CN107946570A CN201711156639.9A CN201711156639A CN107946570A CN 107946570 A CN107946570 A CN 107946570A CN 201711156639 A CN201711156639 A CN 201711156639A CN 107946570 A CN107946570 A CN 107946570A
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/364—Composites as mixtures
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The present invention proposes a kind of shelly texture silicon-carbon composite electrode material, it is made of redox graphene, nano silicon particles and carbon nanotubes, nano silicon particles are scattered in the redox graphene interlayer of multilayer, and there is gap between nano silicon particles and redox graphene, the carbon nanotubes supports the redox graphene, redox graphene piece is included nano silicon particles as shell.The present invention also proposes the preparation and application of the shelly texture silicon-carbon composite electrode material.Cell negative electrode material proposed by the present invention, redox graphene layer constitutes " conchoidal " structure, and carbon nanotubes provides support in redox graphene interlayer, space interval is provided for nano silicon particles, headspace is provided for silicon volumetric expansion during charging, discharging electric batteries, is conducive to keep the structural integrity of negative active core-shell material, so as to, the capacity of battery is high and is not easy to decay, and cyclicity is good, service life length.
Description
Technical field
The invention belongs to battery material field, and in particular to a kind of carbon silicon combination electrode material, its preparation method and application.
Background technology
Lithium ion battery due to have the advantages that open-circuit voltage is high, energy density is big, self-discharge rate is small and it is pollution-free and
It is widely used in the fields such as electronic equipment, electronic traffic, aerospace, military affairs, medicine.The discharge and recharge of lithium ion battery
Journey, the embedded and deintercalation repeatedly based on lithium ion between positive and negative pole material.At present, commercialized lithium ion battery mainly uses
Carbon materials has obtained widest answer beneficial to insertion and the abjection of lithium ion as anode, graphite due to its layer structure
With.It is relatively low but the theoretical specific capacity of graphite is only 372mAh/g, it can not meet growing high power capacity, height
Power demand.Therefore, the material of new height ratio capacity is found, becomes the important probing direction of negative electrode of lithium ion battery research.
In non-carbon material, silicon is due to its higher theoretical specific capacity (4200mAh/g) and discharge potential is low, natural reserves
The advantage such as abundant, becomes the most potential lithium ion battery negative material for substituting graphite.However, body silicon materials are embedding in lithium ion
During entering and deviating from, up to 300% volume change is had, this can cause electrode structure to destroy, be electrically connected failure, active material
The problems such as material persistently consumes, ultimately results in battery capacity and decays rapidly, and cycle performance deteriorates.
At present, a kind of main method for improving silicium cathode is by silicon materials nanosizing, such as nano thin-film, nano wire, nanometer
Particle etc., the silicon of nanosizing can preferably discharge the stress of volume change generation, while provide the space of volumetric expansion, but
Since the intrinsic conductivity of silicon is low, the silicon of nanosizing still suffers from obvious capacity attenuation, and battery work(over numerous cycles
Rate density is relatively low.M.Holzapfel, N.Liu etc. are not only led using silicon and the composite material of carbon beneficial to the electronics of reinforcing material
Electrically, while the light weight of carbon material, ductile characteristic are also beneficial to stress release.But traditional carbon material is in silicon cycling
During, easy fragmentation, causes the capacity attenuation after more cycle-index to accelerate, and unbodied carbon material limits electronics
Conduction velocity.
Therefore, the material of lithium ion battery is prepared up for further research.Graphene has good as two-dimentional carbon material
Good electric conductivity and mechanical strength, can be good at helping releasing for stress by the use of graphene as the carbon material compound with silicon materials
Put；Carbon nanotubes has high mechanical strength in the axial direction, and electronics can be helped quickly to be transmitted axial, is good bone
Frame material.Therefore, graphene, carbon nanotubes and silicon materials are effectively combined, it is steady that lithium ion battery circulation can greatly be improved
Qualitative and power-performance.
The content of the invention
It is contemplated that at least solve one of technical problem existing in the prior art.For this reason, one object of the present invention
It is the lithium ion battery negative material for proposing that a kind of specific discharge capacity is high, cyclicity is good, service life is long and power is high, it has
There is the shelly texture similar to pearl shell.
Second object of the present invention is to propose a kind of preparation method of shelly texture silicon-carbon composite electrode material.
Third object of the present invention is to propose the application of the shelly texture silicon-carbon composite electrode material.
The technical solution for realizing the object of the invention is：
A kind of shelly texture silicon-carbon composite electrode material, by redox graphene, nano silicon particles and carbon nanotubes
Form, nano silicon particles are scattered in the redox graphene interlayer of multilayer, and nano silicon particles and redox graphene it
Between have gap, the carbon nanotubes supports the redox graphene, redox graphene piece is wrapped as shell
Silicon-containing nano particle.
Wherein, the particle diameter of the nano silicon particles is 30-50nm, the diameter 8-10nm of the carbon nanotubes, length 8-15 μ
M, the spacing of two layers of redox graphene comprising nano silicon particles is 100nm-1000nm.
Wherein, the shelly texture silicon-carbon composite electrode material, by 56-20 mass parts redox graphene, 28-
66 mass parts nano silicon particles and 6-18 mass parts carbon nanotubes are formed.Preferably, by 30-20 mass parts reduction-oxidation graphite
Alkene, 62-66 mass parts nano silicon particles and 6-10 mass parts carbon nanotubes are formed.
The preparation method of shelly texture silicon-carbon composite electrode material of the present invention, it is characterised in that including step：
(1) graphene, carbon nanotubes, (GO/CNT/SiNPs) precursor solution of nano silicon particles are prepared；
(2) using the method for suction filtration be prepared " conchoidal " structure silicon-carbon composite electrode material (suction filtration effect under oxygen
Together, the place that there is CNT in centre is supported out graphite alkene lamella Close stack, forms " conchoidal " hole), by filter membrane and
The filter cake of its side is removed together；
(3) high temperature cabonization is carried out to material under 850-950 DEG C, gas shield environment, graphene oxide is reduced into also
Former graphene oxide, and the filter membrane after carbonization is removed；
(4) resulting materials are immersed in the etching solution containing hydrogen fluoride, by the SiO of silicon grain top layer autoxidation2Layer is carved
Ablation is gone.
Scheme according to the present invention, the redox graphene layer being prepared using vacuum filtration are constituted " conchoidal "
Structure, and carbon nanotubes provides support in redox graphene interlayer, provides space interval for nano silicon particles, the sky
Between be charging, discharging electric batteries during, silicon volumetric expansion provides headspace, be conducive to keep negative active core-shell material structure it is complete
It is whole, so that, the capacity of battery is high and is not easy to decay, and cyclicity is good, service life length.Meanwhile the conductive mesh that carbon nanotubes is formed
Network is connected to redox graphene lamella, and during which is charging, discharging electric batteries, the transmission of electronics provides logical
Road, is conducive to shorten the transmission path of electronics, so that, the charge-discharge velocity of battery is fast, and power-performance is good.
Preferably, step (1) is：Nano silicon particles, carbon nanotubes and graphene oxide are separately added into aqueous solution, added
The ratio entered is independently of each other 1-6mg/mL, is disperseed, and obtains the aqueous dispersion liquid of three；By three kinds of aqueous dispersions
Liquid carries out ultrasonic mixing, obtains mixed liquor.
Wherein, step (2) is：Using equipment is filtered by vacuum, the mixed liquor is filtered onto filter membrane, to form conchoidal
Composite construction, the filter cake of filter membrane and its side is removed together.The optional cellulose mixture filter membrane of filter membrane used.Suction filtration should have enough
Time, typically filters to filter membrane supernatant liquid and drains completely, and no liquid continues to flow out below suction funnel.
In order to make the stress of composite particles preferably be discharged, 3 segmentation temperature-raising methods are taken：From 0~300 DEG C, heating speed
Rate is slow, and in 3 DEG C/min or so, this process slowly heats up gradually to discharge stress in filter membrane carbonisation；From 300~600 DEG C,
Heating rate is fast slightly, and in 5 DEG C/min or so, its speed of this process control is made with gradually causing filter membrane carbonized structure to stablize
Surface of graphene oxide functional group dehydrating condensation；From 600~950 DEG C, then accelerate heating rate, in 7.5 DEG C/min or so, this mistake
Micro-structure is substantially stationary in journey, and by filter membrane carbonization, and GO is converted into the higher rGO of reducing degree.
Specifically, three-stage is taken to heat up in step (3)：From -300 DEG C of room temperature, heating rate is 3 ± 0.5 DEG C/min,
300 DEG C of holding 0.5h；From 300-600 DEG C, heating rate is 5 ± 0.5 DEG C/min, and 0.5h is kept at 600 DEG C；From 600-950 DEG C,
Heating rate is 7.5 ± 0.5 DEG C/min, and 1h is kept at 850-950 DEG C.
Wherein, in step 4), the etching solution is HF, 35-55wt% water of 2-6wt%, the ethanol group of 40-60wt%
Into.
The lithium ion battery prepared using the shelly texture silicon-carbon composite electrode material is weighed, the carbon-silicon composite material
Negative active core-shell material as battery.
The beneficial effects of the present invention are：
Cell negative electrode material proposed by the present invention, redox graphene layer constitutes " conchoidal " structure, and carbon is received
Mitron provides support in redox graphene interlayer, and space interval is provided for nano silicon particles, which fills, puts for battery
In electric process, silicon volumetric expansion provides headspace, is conducive to keep the structural integrity of negative active core-shell material, so that, battery
Capacity it is high and be not easy to decay, cyclicity is good, service life length.Meanwhile the conductive network that carbon nanotubes is formed is connected to reduction
Graphene oxide layer, the conductive network is during charging, discharging electric batteries, the transmission of electronics provides passage, is conducive to shorten
The transmission path of electronics, so that, the charge-discharge velocity of battery is fast, and power-performance is good.
The battery of anode using the present invention, battery capacity is high and is not easy to decay, and cyclicity is good, and service life length, has
Good high rate performance and fast charging and discharging ability.According to an embodiment of the invention, battery initial specific capacities of the invention reach
2372.77mAh/g, it is 1438.21mAh/g to have reversible specific capacity after 100 charge and discharge cycles, and capacity retention ratio is reachable
60.62% (there is high specific capacity and good cycle performance).Under high magnification (5C) discharge and recharge, still have
1112.64mAh/g, (has good high rate performance and quick far above the specific capacity 372mAh/g of general commercial graphite cathode
Charging and discharging capabilities).
Brief description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become in the description from combination accompanying drawings below to embodiment
Substantially and it is readily appreciated that, wherein：
The process flow chart of " conchoidal " structure silicon-carbon composite electrode material anode is filtered by vacuum in Fig. 1；
Fig. 2 " conchoidal " structure silicon-carbon composite electrode material SEM schemes；
The cycle performance curve map of " conchoidal " structure silicon-carbon composite electrode material of Fig. 3 difference silicon ratios；
The high rate performance curve map of " conchoidal " structure silicon-carbon composite electrode material of Fig. 4 .65wt%.
Embodiment
Now illustrate the present invention with following embodiments, but be not limited to the scope of the present invention.The hand used in embodiment
Section, unless otherwise instructed, using the means of this area routine.
Embodiment 1：
The present embodiment prepares the material that silicone content accounts for quality of materials 28wt%.
Fig. 1 illustrates the processing and fabricating flow that " conchoidal " structure silicon-carbon composite electrode material is prepared with vacuum filtration method,
Wherein SiNPs is silicon nanoparticle (particle diameter 30-50nm), and GO is graphene oxide, and rGO is redox graphene, and CNT is carbon
Nanotube (diameter 8-10nm, 8-15 μm of length), SiO2For the silicon dioxide layer of silicon nanoparticle top layer autoxidation.Specific side
Method is as follows：
(1) GO/CNT/SiNPs precursor solutions are prepared：Take 50mg silicon nanoparticles, carbon nanotubes, graphene oxide point
It is not dispersed in 10mL aqueous solutions, obtains the aqueous dispersion liquid of 5mg/mL concentration；Three kinds of aqueous dispersion liquid press 5：3：10 into
Row ultrasonic mixing, it is water-soluble with 55 mass parts of graphene oxide to obtain 28 mass parts of nano silicon particles, 17 mass parts of carbon nanotubes
Liquid mixed liquor.(2) " conchoidal " structure silicon-carbon composite electrode material is prepared using the method for suction filtration：Set using vacuum filtration
It is standby, mixed liquor obtained by step (2) is filtered onto filter membrane, is then removed together the filter cake of filter membrane and its side.Filter membrane used
It is cellulose mixture filter membrane (CA-CN), its aperture is at 0.45 micron.
(3) high temperature cabonization is carried out to material under Ar environmental protections, GO is reduced into rGO, and the filter membrane after carbonization is gone
Remove.High temperature cabonization takes three-stage to heat up：From -300 DEG C of room temperature, heating rate is 3 DEG C/min, and 0.5h is kept at 300 DEG C；From
300-600 DEG C, heating rate is 5 DEG C/min, and 0.5h is kept at 600 DEG C；From 600-950 DEG C, heating rate is 7.5 DEG C/min,
1h is kept at 900 DEG C.
(4) resulting materials are immersed in 4wt%HF, 46wt% water, 50wt% ethanol systems, silicon grain top layer autoxidation
SiO2Layer is etched；
(5) described " conchoidal " structure silicon-carbon composite electrode material is obtained.
Fig. 2 show the SEM figures of " conchoidal " structure silicon-carbon composite electrode material of gained after above-mentioned technological process.Fig. 2
Its (a) is the pattern of edge of materials, it is seen that graphene is closed in edge, encased silicon grain.Fig. 2 its (b) and (c) are Fig. 1
The material at Section A-A shown, it can be seen that the reduction-oxidation graphite of " conchoidal " structure among silicon grain is dispersed in
Alkene interlayer, carbon nano tube network play good supporting role, provide space for the expansion of silicon grain and (are in high temperature cabonization
Convenience, material is cut, but shine Electronic Speculum when can choose edge and center Fig. 2 (a) according to Electronic Speculum
It is edge).
Embodiment 2：
The present embodiment prepares the material that silicone content accounts for quality of materials 35wt%.Step (1) is：
Prepare GO/CNT/SiNPs precursor solutions：50mg silicon nanoparticles, carbon nanotubes, graphene oxide is taken to divide respectively
It is dissipated in 10mL aqueous solutions, obtains the aqueous dispersion liquid of 5mg/mL concentration；Three kinds of aqueous dispersion liquid ultrasonic mixing in proportion,
Obtain 35 mass parts of nano silicon particles, the aqueous solution mixed liquor of 15 mass parts of carbon nanotubes and 50 mass parts of graphene oxide.Its
He is operated with embodiment 1.
Embodiment 3：
The present embodiment prepares the material that silicone content accounts for quality of materials 50wt%.Step (1) is：
Prepare GO/CNT/SiNPs precursor solutions：50mg silicon nanoparticles, carbon nanotubes, graphene oxide is taken to divide respectively
It is dissipated in 10mL aqueous solutions, obtains the aqueous dispersion liquid of 5mg/mL concentration；Three kinds of aqueous dispersion liquid ultrasonic mixing in proportion,
Obtain 50 mass parts of nano silicon particles, the aqueous solution mixed liquor of 12 mass parts of carbon nanotubes and 38 mass parts of graphene oxide.Its
He is operated with embodiment 1.
Embodiment 4：
The present embodiment prepares the material that silicone content accounts for quality of materials 65%.Step (1) is：
Prepare GO/CNT/SiNPs precursor solutions：50mg silicon nanoparticles, carbon nanotubes, graphene oxide is taken to divide respectively
It is dissipated in 10mL aqueous solutions, obtains the aqueous dispersion liquid of 1mg/mL concentration；Three kinds of aqueous dispersion liquid carry out ultrasound in proportion
Mixing, obtains 65 mass parts of nano silicon particles, 8 mass parts of carbon nanotubes are mixed with the aqueous solution of 27 mass parts of graphene oxide
Liquid.
Other operations are the same as embodiment 1.
Electro-chemical test
Button-shaped half-cell is made with the material of embodiment 1-4, with conventional method, test result is as follows：
Fig. 3 show " conchoidal " the structure silicon-carbon composite electrode material of above-mentioned different silicon mass ratio as anode lithium from
The cycle performance curve of sub- half-cell, is that silicone content 28wt%, 35wt%, 50wt% and 65wt% can be seen that initially respectively
Specific capacity with silicone content increase and lift, once but silicone content is excessive, the decay of capacity can be caused to accelerate, integrate two in terms of
Consider, the sample of 50wt% silicone contents has best cycle performance, i.e., 1438.31mAh/g after 100 times circulations.In addition, silicon contains
After amount increase to a certain extent, cycle performance can be caused to decline, therefore exist between lifting specific capacity and lifting cycle performance
Compromise considers, it is preferable that the composite material of 50wt% silicone contents illustrates more preferably comprehensive performance.
Fig. 4 show the high rate performance curve of above-mentioned 65wt% " conchoidal " structure silicon-carbon composite electrode material.It can see
Go out, under 5C multiplying powers, the specific discharge capacity of " conchoidal " structure silicon-carbon composite electrode material still has 1112.64mAh/
G, far above the specific capacity 372mAh/g of general commercial graphite cathode, illustrates good high rate performance and fast charging and discharging energy
Power.
More than embodiment be only the preferred embodiment of the present invention is described, not to the scope of the present invention into
Row limits, on the premise of design spirit of the present invention is not departed from, technical side of this area ordinary skill technical staff to the present invention
The all variations and modifications that case is made, should all fall into the protection domain that claims of the present invention determines.
Claims (10)
- A kind of 1. shelly texture silicon-carbon composite electrode material, it is characterised in that by redox graphene, nano silicon particles and Carbon nanotubes is formed, and nano silicon particles are scattered in the redox graphene interlayer of multilayer, and nano silicon particles and reduction-oxidation There is gap between graphene, the carbon nanotubes supports the redox graphene, makes redox graphene piece as shellfish Shell equally includes nano silicon particles.
- 2. shelly texture silicon-carbon composite electrode material according to claim 1, it is characterised in that the nano silicon particles Particle diameter be 30-50nm, the diameter 8-10nm of the carbon nanotubes, 8-15 μm of length, two layers of reduction comprising nano silicon particles The spacing of graphene oxide is 100nm-1000nm.
- 3. shelly texture silicon-carbon composite electrode material according to claim 1 or 2, it is characterised in that by 56-20 mass Part redox graphene, 28-66 mass parts nano silicon particles and 6-18 mass parts carbon nanotubes are formed.
- 4. shelly texture silicon-carbon composite electrode material according to claim 3, it is characterised in that by 30-20 mass parts Redox graphene, 62-66 mass parts nano silicon particles and 6-10 mass parts carbon nanotubes are formed.
- 5. the preparation method of claim 1-4 any one of them shelly texture silicon-carbon composite electrode materials, it is characterised in that Including step：(1) graphene oxide, carbon nanotubes, the GO/CNT/SiNPs precursor solutions of nano silicon particles are prepared；(2) " conchoidal " structure silicon-carbon composite electrode material is prepared using the method for suction filtration, by the filter of filter membrane and its side Cake is removed together；(3) high temperature cabonization is carried out to material under 850-950 DEG C, gas shield environment, graphene oxide is reduced into oxygen reduction Graphite alkene, and the filter membrane after carbonization is removed；(4) resulting materials are immersed in the etching solution containing hydrogen fluoride, by the SiO of silicon grain top layer autoxidation2Layer etching is removed Go.
- 6. preparation method according to claim 5, it is characterised in that step (1) is：By nano silicon particles, carbon nanotubes It is separately added into graphene oxide in aqueous solution, the ratio of addition is independently of each other 1-6mg/mL, obtains the aqueous solution of three Dispersion liquid；Three kinds of aqueous dispersion liquid are subjected to ultrasonic mixing, obtain mixed liquor.
- 7. preparation method according to claim 5, it is characterised in that step (2) is：Using equipment is filtered by vacuum, by institute State mixed liquor to filter onto filter membrane, to form conchoidal composite construction, the filter cake of filter membrane and its side is removed together；Filter used Film is cellulose mixture filter membrane.
- 8. according to claim 5-7 any one of them preparation methods, it is characterised in that the high temperature cabonization process of step (3) is adopted Three-stage is taken to heat up：From -300 DEG C of room temperature, heating rate is 3 ± 0.5 DEG C/min, and 0.5h is kept at 300 DEG C；From 300-600 DEG C, Heating rate is 5 ± 0.5 DEG C/min, and 0.5h is kept at 600 DEG C；From 600-950 DEG C, heating rate is 7.5 ± 0.5 DEG C/min, 1h is kept at 850-950 DEG C.
- 9. according to claim 5-7 any one of them preparation methods, it is characterised in that in step 4), the etching solution is HF, 35-55wt% water of 2-6wt%, the ethanol composition of 40-60wt%.
- 10. lithium ion battery prepared by any one of the application claim 1-4 shelly texture silicon-carbon composite electrode material, its It is characterized in that, negative active core-shell material of the carbon-silicon composite material as battery.
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| CN109761239A (en) * | 2019-01-18 | 2019-05-17 | 齐鲁工业大学 | It is a kind of sensing, photoelectricity or lithium ion battery composite material and preparation method |
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