CN109888194A - The preparation method of graphene/silicon/carbon composite sandwich electrode - Google Patents
The preparation method of graphene/silicon/carbon composite sandwich electrode Download PDFInfo
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- CN109888194A CN109888194A CN201910265848.XA CN201910265848A CN109888194A CN 109888194 A CN109888194 A CN 109888194A CN 201910265848 A CN201910265848 A CN 201910265848A CN 109888194 A CN109888194 A CN 109888194A
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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
- 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 a kind of preparation methods of the sandwich electrode of graphene/silicon/carbon composite, comprising the following steps: prepares carbon-coating substrate；Prepare silicon source, by mass concentration be 50% benzene and mass concentration be 50% trim,ethylchlorosilane solution, with (10-15): 100 ratio mixes；Graphene presoma is prepared, graphene oxide is put into dispersion liquid, the graphene oxide dispersion of 1-10mg/mL is formed, dispersing agent is added in dispersion liquid；Prepare nanometer silicon layer；Prepare graphene layer.The present invention reduces the size of silicon particle to Nano grade, silicon particle is distributed on graphene and carbon, inhibit volume expansion, using hard carbon material have unordered graphite-like structure microcrystalline coating) and a large amount of pore structure, interlamellar spacing be typically larger than graphite 0.34-0.4, can be silicon layer adjacent thereto, expansion space is provided, it prevents silicon layer from falling off, inhibits electrode to crush, maintain the integrity degree of electrode.
Description
Technical field
The present invention relates to the preparation fields of electrode, and in particular to a kind of sandwich electricity of graphene/silicon/carbon composite
The preparation method of pole.
Background technique
Lithium ion battery has capacity high, has extended cycle life, pollution-free, the characteristics such as has a safety feature, is applied to portable electricity
Sub- product and power battery field need higher energy storage and energy conversion in the research of electrochmical power source, while also to have
There are high-energy-density, high-specific-power, long-life.And there is also many deficiencies, lithium ion batteries for the lithium ion battery being commercialized now
Negative electrode material be to influence the key factor of battery performance, current commodity lithium ion battery mostly uses the carbonaceous cathode such as graphite,
Its theoretical capacity is 372mAh/g, it is difficult to meet the needs of high capacity.And silicon materials rich reserves, and there is very high specific volume
It measures (4200mAh/g), but silicon materials do electrode in use, in lithium ion insertion crystalline silicon, are with the presence of a variety of alloy morphologies
, such as a variety of alloys such as Li12Si7, Li14Si6, Li13Si4, Li22Si5, their unit cell volume be all larger than crystalline silicon
Unit cell volume for the first time in discharge process, will cause huge volume expansion, lead to the dusting of active material, and active material is from collection
It falls off on fluid, battery capacity is caused to decay rapidly, as the carry out material volume variation of reaction (about can reach substance significantly
Long-pending 4 times), this makes silicon electrode silicon particle fall off chipping and dusting, and due to this bulk effect, silicon is always difficult in electrolyte
To form stable surface solid dielectric film (Solid ElectrolyteInterface, SEI), electrode structure is destroyed,
The silicon face newly exposed can constantly form new SEI film, cause efficiency for charge-discharge low, accelerate capacity attenuation, can not practical application.
Summary of the invention
In order to solve the deficiencies in the prior art, the present invention provides a kind of sandwiches of graphene/silicon/carbon composite
The preparation method of electrode.
The technical solution adopted by the present invention to solve the technical problems is: a kind of interlayer of graphene/silicon/carbon composite
The preparation method of structure electrode, comprising the following steps:
D1 prepares carbon-coating substrate
NMP is added according to the mass ratio of (8-10): 1:1 with conductive agent and binder in hard carbon after grinding to mix
It is even, it is coated uniformly on copper foil, then obtains carbon-coating substrate in a vacuum drying oven with 120 DEG C of vacuum drying 12h；
D2 prepares silicon source
By mass concentration be 50% benzene and mass concentration be 50% trim,ethylchlorosilane solution, with (10-15): 100
Ratio mix, be put into silicon source container, be placed on ultrasonic atomizer, ultrasonic atomizatio is carried out with the frequency of 20000Hz,
Form atomized liquid；
D3 prepares graphene presoma
Graphene oxide is put into dispersion liquid, the graphene oxide dispersion of 1-10mg/mL is formed, is added in dispersion liquid
Then dispersing agent carries out ultrasonic disperse processing, form suspension, be added in carbon source container, carbon source container is placed in ultrasonic atomizatio
Ultrasonic atomizatio, frequency 20000Hz, time 30min are carried out on device；
D4 prepares nanometer silicon layer
Using CVD chemical precipitation method on carbon-coating deposited silicon layer, will be covered with the copper foil of carbon-coating substrate, be transferred in tube furnace
Quartz ampoule heating zone keeps argon gas to be continually fed into, according to 5 firstly, draining the air in pipe for argon gas 30min is passed through in pipe
DEG C/heating rate of min, 800 DEG C of depositing temperature are risen to, silicon source pipeline is opened, is brought silicon source in quartz ampoule by carrier gas, is protected
Temperature deposition 6h, throughput are stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction
After, close silicon source pipe pipeline；
D5 prepares graphene layer
Graphene layer is deposited on silicon layer in step D4 after silicon-containing layer deposition using CVD chemical precipitation method to be continually fed into
Argon gas is down to 400 DEG C to temperature, opens silicon source pipeline, brought graphene oxide in quartz ampoule by carrier gas, heat preservation precipitating,
Throughput is stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction 1h, and deposition is anti-
After answering, carbon source pipeline is closed, continues to be passed through argon gas being cooled to room temperature, obtains graphene/silicon/carbon composite interlayer knot
Structure electrode.
Specifically, the conductive agent uses carbon black.
Specifically, the binder uses PVDF, PVDF Kynoar.
Specifically, the hard carbon uses biomass carbon, selected from pyrolytic carbons such as banana skin, seaweed, eggshell, orange peel, rice husks.
Specifically, the dispersing agent is in propylene glycol, polyacrylamide, polyethylene glycol oxide, polyvinyl alcohol, polyethylene glycol
At least one.
Specifically, the silicon layer control is in 15-30nm.
The invention has the following advantages: the size for reducing silicon particle can shorten lithium ion to Nano grade in this way
With the transmission path of electronics, reduce stress problem；Using graphene/silicon/carbon three-ply sandwich structure, silicon particle is distributed to graphite
On alkene and carbon, inhibit volume expansion, while the specific capacity of composite material and the structural stability of material, graphene can be improved
There is bigger specific surface area and more surface defects relative to graphite, therefore more multiposition can be provided for the presence of Li,
The chemical property of silicon can be improved, graphene is with the mechanical performance out of other any carbon materials, in addition its lamella fold knot
Structure preferably accommodates the volume change of silicon face, maintains the stability of electrode structure, the fabulous electronics of graphene, ionic conduction
Property and biggish surface area energy reinforcing material itself electric conductivity and electrochemical reaction activity, graphene is capable of forming well
Conductive network, increase silicon active particle between and the electrical contact with collector；And graphene layer to silicon layer it is effective package or
Double team can also hinder contact of the silicon particle with electrolyte, prevent the further generation of SEI film, silicon layer is effectively protected, reduction declines
Subtract degree；In addition carbon-coating uses hard carbon, and hard carbon refers to difficult graphitized carbon from definition, usually obtained by pyrolysis high molecular polymer
It arrives, this kind of carbon is also difficult to be graphitized at a high temperature of 2500 DEG C or more, drives what the carbon atom in object was cross-linked with each other before carbonization
Structure hinders the growth that in-plane occurs for the carbon-coating in pyrolytic process, therefore has unordered class graphite using hard carbon material
Structure microcrystalline coating and a large amount of pore structure, interlamellar spacing are typically larger than graphite 0.34-0.4, can be silicon layer adjacent thereto, provide
Expansion space prevents silicon layer from falling off, and inhibits electrode to crush, maintains the integrity degree of electrode.
Specific embodiment
It is described in detail to various aspects of the present invention below, unless specific instructions, various raw materials of the invention can pass through
It is prepared or is commercially available according to the conventional method of this field.
Embodiment 1
A kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite, comprising the following steps:
D1 prepares carbon-coating substrate
NMP (N-Methyl pyrrolidone) is added according to the mass ratio of 8:1:1 with carbon black, binder in hard carbon after grinding
It is uniformly mixed, is coated uniformly on copper foil, then obtains carbon-coating base in a vacuum drying oven with 120 DEG C of vacuum drying 12h
Bottom；
D2 prepares silicon source
By mass concentration be 50% benzene and mass concentration be 50% trim,ethylchlorosilane solution, with the ratio of 10:100
It mixes, is put into silicon source container, is placed on ultrasonic atomizer, ultrasonic atomizatio is carried out with the frequency of 20000Hz, forms mist
Change liquid；
D3 prepares graphene presoma
Graphene oxide is put into dispersion liquid, the graphene oxide dispersion of 1-10mg/mL is formed, is added in dispersion liquid
Then dispersing agent carries out ultrasonic disperse processing, form suspension, be added in carbon source container, carbon source container is placed in ultrasonic atomizatio
Ultrasonic atomizatio, frequency 20000Hz, time 30min are carried out on device；
D4 prepares nanometer silicon layer
Using CVD chemical precipitation method on carbon-coating deposited silicon layer, will be covered with the copper foil of carbon-coating substrate, be transferred in tube furnace
Quartz ampoule heating zone keeps argon gas to be continually fed into, according to 5 firstly, draining the air in pipe for argon gas 30min is passed through in pipe
DEG C/heating rate of min, 800 DEG C of depositing temperature are risen to, silicon source pipeline is opened, is brought silicon source in quartz ampoule by carrier gas, is protected
Temperature deposition 6h, throughput are stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction
After, close silicon source pipe pipeline；
D5 prepares graphene layer
Graphene layer is deposited on silicon layer in step D4 after silicon-containing layer deposition using CVD chemical precipitation method to be continually fed into
Argon gas is down to 400 DEG C to temperature, opens silicon source pipeline, brought graphene oxide in quartz ampoule by carrier gas, heat preservation precipitating,
Throughput is stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction 1h, and deposition is anti-
After answering, carbon source pipeline is closed, continues to be passed through argon gas being cooled to room temperature, obtains graphene/silicon/carbon composite interlayer knot
Structure electrode.
Specifically, the binder uses PVDF, PVDF Kynoar.
Specifically, the hard carbon uses biomass carbon, selected from pyrolytic carbons such as banana skin, seaweed, eggshell, orange peel, rice husks.
Specifically, the dispersing agent is in propylene glycol, polyacrylamide, polyethylene glycol oxide, polyvinyl alcohol, polyethylene glycol
At least one.
Specifically, the silicon layer control is in 15-30nm.
Embodiment 2
A kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite, comprising the following steps:
D1 prepares carbon-coating substrate
NMP is added according to the mass ratio of 9:1:1 with conductive agent and binder in hard carbon after grinding to be uniformly mixed, by it
It is coated uniformly on copper foil, then obtains carbon-coating substrate in a vacuum drying oven with 120 DEG C of vacuum drying 12h；
D2 prepares silicon source
By mass concentration be 50% benzene and mass concentration be 50% trim,ethylchlorosilane solution, with the ratio of 13:100
It mixes, is put into silicon source container, is placed on ultrasonic atomizer, ultrasonic atomizatio is carried out with the frequency of 20000Hz, forms mist
Change liquid；
D3 prepares graphene presoma
Graphene oxide is put into dispersion liquid, the graphene oxide dispersion of 1-10mg/mL is formed, is added in dispersion liquid
Then dispersing agent carries out ultrasonic disperse processing, form suspension, be added in carbon source container, carbon source container is placed in ultrasonic atomizatio
Ultrasonic atomizatio, frequency 20000Hz, time 30min are carried out on device；
D4 prepares nanometer silicon layer
Using CVD chemical precipitation method on carbon-coating deposited silicon layer, will be covered with the copper foil of carbon-coating substrate, be transferred in tube furnace
Quartz ampoule heating zone keeps argon gas to be continually fed into, according to 5 firstly, draining the air in pipe for argon gas 30min is passed through in pipe
DEG C/heating rate of min, 800 DEG C of depositing temperature are risen to, silicon source pipeline is opened, is brought silicon source in quartz ampoule by carrier gas, is protected
Temperature deposition 6h, throughput are stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction
After, close silicon source pipe pipeline；
D5 prepares graphene layer
Graphene layer is deposited on silicon layer in step D4 after silicon-containing layer deposition using CVD chemical precipitation method to be continually fed into
Argon gas is down to 400 DEG C to temperature, opens silicon source pipeline, brought graphene oxide in quartz ampoule by carrier gas, heat preservation precipitating,
Throughput is stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction 1h, and deposition is anti-
After answering, carbon source pipeline is closed, continues to be passed through argon gas being cooled to room temperature, obtains graphene/silicon/carbon composite interlayer knot
Structure electrode.
Specifically, the binder uses PVDF, PVDF Kynoar.
Specifically, the hard carbon uses biomass carbon, selected from pyrolytic carbons such as banana skin, seaweed, eggshell, orange peel, rice husks.
Specifically, the dispersing agent is in propylene glycol, polyacrylamide, polyethylene glycol oxide, polyvinyl alcohol, polyethylene glycol
At least one.
Embodiment 3
A kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite, comprising the following steps:
D1 prepares carbon-coating substrate
NMP is added according to the mass ratio of 10:1:1 with conductive agent and binder in hard carbon after grinding to be uniformly mixed, it will
It is coated uniformly on copper foil, then obtains carbon-coating substrate in a vacuum drying oven with 120 DEG C of vacuum drying 12h；
D2 prepares silicon source
By mass concentration be 50% benzene and mass concentration be 50% trim,ethylchlorosilane solution, with the ratio of 15:100
It mixes, is put into silicon source container, is placed on ultrasonic atomizer, ultrasonic atomizatio is carried out with the frequency of 20000Hz, forms mist
Change liquid；
D3 prepares graphene presoma
Graphene oxide is put into dispersion liquid, the graphene oxide dispersion of 1-10mg/mL is formed, is added in dispersion liquid
Then dispersing agent carries out ultrasonic disperse processing, form suspension, be added in carbon source container, carbon source container is placed in ultrasonic atomizatio
Ultrasonic atomizatio, frequency 20000Hz, time 30min are carried out on device；
D4 prepares nanometer silicon layer
Using CVD chemical precipitation method on carbon-coating deposited silicon layer, will be covered with the copper foil of carbon-coating substrate, be transferred in tube furnace
Quartz ampoule heating zone keeps argon gas to be continually fed into, according to 5 firstly, draining the air in pipe for argon gas 30min is passed through in pipe
DEG C/heating rate of min, 800 DEG C of depositing temperature are risen to, silicon source pipeline is opened, is brought silicon source in quartz ampoule by carrier gas, is protected
Temperature deposition 6h, throughput are stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction
After, close silicon source pipe pipeline；
D5 prepares graphene layer
Graphene layer is deposited on silicon layer in step D4 after silicon-containing layer deposition using CVD chemical precipitation method to be continually fed into
Argon gas is down to 400 DEG C to temperature, opens silicon source pipeline, brought graphene oxide in quartz ampoule by carrier gas, heat preservation precipitating,
Throughput is stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, deposition reaction 1h, and deposition is anti-
After answering, carbon source pipeline is closed, continues to be passed through argon gas being cooled to room temperature, obtains graphene/silicon/carbon composite interlayer knot
Structure electrode.
Specifically, the binder uses PVDF, PVDF Kynoar.
Specifically, the hard carbon uses biomass carbon, selected from pyrolytic carbons such as banana skin, seaweed, eggshell, orange peel, rice husks.
Specifically, the dispersing agent is in propylene glycol, polyacrylamide, polyethylene glycol oxide, polyvinyl alcohol, polyethylene glycol
At least one.
Specifically, the silicon layer control is in 15-30nm.
The present invention is not limited to the embodiment, anyone should learn that the structure made under the inspiration of the present invention becomes
Change, the technical schemes that are same or similar to the present invention are fallen within the scope of protection of the present invention.
Technology not described in detail in the present invention, shape, construction portion are well-known technique.
Claims (8)
1. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite, it is characterised in that: including following step
It is rapid:
D1 prepares carbon-coating substrate
NMP is added according to the mass ratio of (8-10): 1:1 with conductive agent and binder in hard carbon after grinding to be uniformly mixed, it will
It is coated uniformly on copper foil, then obtains carbon-coating substrate in a vacuum drying oven with 120 DEG C of vacuum drying 12h；
D2 prepares silicon source
By mass concentration be 50% benzene and mass concentration be 50% trim,ethylchlorosilane solution, with (10-15): 100 ratio
Example mixes, and is put into silicon source container, is placed on ultrasonic atomizer, carries out ultrasonic atomizatio with the frequency of 20000Hz, is formed
Atomized liquid；
D3 prepares graphene presoma
Graphene oxide is put into dispersion liquid, the graphene oxide dispersion of 1-10mg/mL is formed, dispersion is added in dispersion liquid
Then agent carries out ultrasonic disperse processing, form suspension, be added in carbon source container, carbon source container is placed on ultrasonic atomizer
Carry out ultrasonic atomizatio, frequency 20000Hz, time 30min；
D4 prepares nanometer silicon layer
Using CVD chemical precipitation method on carbon-coating deposited silicon layer；
D5 prepares graphene layer
Graphene layer is deposited on silicon layer using CVD chemical precipitation method.
2. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite according to claim 1,
It is characterized in that: the method for deposited silicon layer in the step D4 are as follows: the copper foil that will be covered with carbon-coating substrate is transferred in tube furnace quartzy
Pipe heating zone keeps argon gas to be continually fed into, according to 5 DEG C/min firstly, draining the air in pipe for argon gas 30min is passed through in pipe
Heating rate, rise to 800 DEG C of depositing temperature, open silicon source pipeline, brought silicon source in quartz ampoule by carrier gas, heat preservation deposition
6h, throughput are stablized in 120ccm, and the tail gas of quartz ampoule discharge is passed through in NaOH solution, is recycled, after deposition reaction,
Close silicon source pipe pipeline.
3. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite according to claim 1,
It is characterized in that: depositing the method for graphene layer in the step D5 are as follows: in step D4 after silicon-containing layer deposition, be continually fed into argon
Gas is down to 400 DEG C to temperature, opens silicon source pipeline, brought graphene oxide in quartz ampoule by carrier gas, heat preservation precipitating, gas
Stability of flow is passed through in NaOH solution, is recycled, deposition reaction 1h, deposition reaction in 120ccm, the tail gas of quartz ampoule discharge
After, carbon source pipeline is closed, continues to be passed through argon gas being cooled to room temperature, obtains graphene/silicon/carbon composite sandwich
Electrode.
4. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite according to claim 1,
Be characterized in that: the conductive agent uses carbon black or conducting polymer.
5. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite according to claim 1,
Be characterized in that: the binder uses PVDF, PVDF Kynoar.
6. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite according to claim 1,
Be characterized in that: the hard carbon uses biomass carbon, selected from pyrolytic carbons such as banana skin, seaweed, eggshell, orange peel, rice husks.
7. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite according to claim 1,
Be characterized in that: the dispersing agent in propylene glycol, polyacrylamide, polyethylene glycol oxide, polyvinyl alcohol, polyethylene glycol at least
It is a kind of.
8. a kind of preparation method of the sandwich electrode of graphene/silicon/carbon composite according to claim 1,
Be characterized in that: the silicon layer control is in 15-30nm.
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