CN110429262A - Si-C composite material and preparation method thereof - Google Patents
Si-C composite material and preparation method thereof Download PDFInfo
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- CN110429262A CN110429262A CN201910736348.XA CN201910736348A CN110429262A CN 110429262 A CN110429262 A CN 110429262A CN 201910736348 A CN201910736348 A CN 201910736348A CN 110429262 A CN110429262 A CN 110429262A
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- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 79
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 50
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 33
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 27
- 239000010703 silicon Substances 0.000 claims abstract description 27
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 23
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 16
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 11
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims description 34
- 239000010453 quartz Substances 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000003708 ampul Substances 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- -1 dichloro silicon Alkane Chemical class 0.000 claims 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 230000002427 irreversible effect Effects 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 239000007772 electrode material Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 58
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 52
- 229910052786 argon Inorganic materials 0.000 description 26
- 238000000151 deposition Methods 0.000 description 22
- 230000008021 deposition Effects 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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 Si-C composite materials and preparation method thereof, are related to battery material technical field.The preparation method of Si-C composite material of the invention is using dimethyldichlorosilane, trimethyl dichlorosilane as silicon source, using benzene or toluene as carbon source, graphite nodule, graphene, carbon nanotube are selected respectively as carbon base body, and Si-C composite material is synthesized by chemical vapor deposition method.The carbon-based conductivity for improving material in composite material, and silicon and carbon base body are stably connected with by the network structure that the agraphitic carbon deposited is constituted, and are effectively alleviated expansion of the silicon electrode in charge and discharge process, be ensure that the stability of electrode material.Oxygen element is free of in silicon source and carbon source, oxygen content reduces in gained Si-C composite material, can reduce the irreversible capacity of Si-C composite material.
Description
Technical field
The present invention relates to battery material technical fields, in particular to Si-C composite material and preparation method thereof.
Background technique
Current commercialized lithium ion battery material graphite, capacity exploitation value have been approached theoretical capacity.In order to chase after
Higher capacity is sought, silicon is the maximum negative electrode material of theoretical specific capacity.One of common effective ways of silicon materials are exactly to disperse silicon
In the matrix of carbon, Si-C composite material is synthesized.But the irreversible capacity of Si-C composite material in the prior art is higher.
In consideration of it, the present invention is specifically proposed.
Summary of the invention
The purpose of the present invention is to provide a kind of Si-C composite materials and preparation method thereof, to improve silicon-carbon in the prior art
The higher problem of composite material irreversible capacity.
The present invention is implemented as follows:
In a first aspect, the embodiment of the present invention provides a kind of preparation method of Si-C composite material, by silicon source, passing through of carbon source
The method for learning vapor deposition is deposited on carbon base body, to obtain Si-C composite material；Wherein, the silicon source is dimethyldichlorosilane
Or trimethyl dichlorosilane, the carbon source are benzene or toluene, the carbon base body is graphite nodule, graphene or carbon nanotube.
In alternative embodiments, catalyst is used during the chemical vapor deposition, the catalyst is
At least one of copper, platinum, gold, silver.
In alternative embodiments, the catalyst is sheet, when carrying out the chemical vapor deposition, the carbon base body
It is placed on the catalyst of sheet.
In alternative embodiments, the catalyst is graininess, granular when carrying out the chemical vapor deposition
The catalyst is scattered on the carbon base body.
In alternative embodiments, the median particle diameter of the granular catalyst is 20~200 microns.
In alternative embodiments, the step of chemical vapor deposition carries out in quartz ampoule, the gaseous silicon
Source and the carbon source pass through gas washing, enter in the quartz ampoule after removal impurity and are deposited.
In alternative embodiments, the tail gas after the chemical vapor deposition, which is passed through in sodium hydroxide solution, absorbs.
In alternative embodiments, the temperature of the chemical vapor deposition is 900 DEG C~1100 DEG C.
In alternative embodiments, the duration of the chemical vapor deposition is 3h~7h.
Second aspect, the embodiment of the present invention provide a kind of Si-C composite material, pass through any one of aforementioned embodiments institute
The preparation method for the Si-C composite material stated is made.
The invention has the following advantages:
The embodiment of the present invention, as silicon source, is made using dimethyldichlorosilane, trimethyl dichlorosilane using benzene or toluene
For carbon source, graphite nodule, graphene, carbon nanotube are selected respectively as carbon base body, silicon-carbon is synthesized by chemical vapor deposition method
Composite material.The carbon-based conductivity for improving material in composite material, and the network structure that the agraphitic carbon deposited is constituted will
Silicon and carbon base body are stably connected with, and are effectively alleviated expansion of the silicon electrode in charge and discharge process, be ensure that the steady of electrode material
It is qualitative.Oxygen element is free of in silicon source and carbon source, oxygen content reduces in gained Si-C composite material, can reduce Si-C composite material
Irreversible capacity.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the device figure of chemical vapor deposition in the embodiment of the present invention；
Fig. 2 is the XRD spectrum of the carbon-silicon composite material of carbon nanotube and the embodiment of the present invention 1；
Fig. 3 is that the SEM of the carbon-silicon composite material of carbon nanotube and the embodiment of the present invention 1 schemes；
Fig. 4 is the XPS figure of the carbon-silicon composite material of the embodiment of the present invention 1；
Fig. 5 is the first charge-discharge curve graph of the carbon-silicon composite material of carbon nanotube and the embodiment of the present invention 1；
Fig. 6 is the circulation and efficiency curve of the carbon-silicon composite material of carbon nanotube and the embodiment of the present invention 1.
Icon: 10- quartz ampoule；12- drexel bottle；14- carbon base body；16- beaker；18- carrier.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The embodiment of the present invention provides a kind of carbon-silicon composite material and preparation method thereof.The preparation method includes:
Silicon source, carbon source are deposited on carbon base body by the method for chemical vapor deposition, to obtain Si-C composite material.
Wherein, the silicon source be dimethyldichlorosilane or trimethyl dichlorosilane, the carbon source be benzene or toluene, it is described
Carbon base body is graphite nodule, graphene or carbon nanotube.The embodiment of the present invention chooses dimethyldichlorosilane or trimethyl dichloro
Silane, as silicon source, toxicity is smaller, from a wealth of sources, cheap.Reduce cost pressure, the security risk of production.Benzene and
Toluene is used as toluene (or benzene) and DMDCS (dimethyl dichloro in carbon source, such as the embodiment of the present invention in vapor deposition synthesis
Silane) according to a certain volume example mix, the two compatibility is preferable, and toluene is under the premise of protecting DMDCS not hydrolyzed
Carbon source as deposition simultaneously, in addition, being free of oxygen element in carbon source and silicon source, oxygen content is reduced in gained carbon-silicon composite material,
The irreversible capacity of carbon-silicon composite material can be reduced.
Fig. 1 is the device figure of chemical vapor deposition in the embodiment of the present invention.As shown in Figure 1, first by carbon base body 14 and
The carrier 18 that catalyst needed for chemical vapor deposition is put into advance in quartz ampoule 10 is (for carrying target to be vapor-deposited
Object) on, it is then continually fed into inert gas (such as argon gas), the air in quartz ampoule 10 is drained, avoids occurring oxidation etc. instead
It answers.In embodiments of the present invention, catalyst can be at least one of platinum, gold, copper, silver or two or more mixtures.
The form of catalyst can be sheet, and carbon base body is placed on the catalyst of sheet；The form of catalyst is also possible to graininess,
To increase its effective active area.The median particle diameter of granular catalyst can be 20-200 microns.
During vapor deposition method nano materials, production of the component, content and distribution of catalyst to synthesis
The pattern and structure of object have vital influence, and the pattern of different catalysts particle can synthesize the nanometer of diverse microcosmic structure
Material, catalyst particle size determine the height of catalyst activity, and catalyst granules distribution has decided on whether to reunite.With
For copper catalyst, high temperature makes the copper atom on copper surface play catalytic action.When catalyst is embedded failure in precipitation process
When, copper sheet can continually provide new catalytic activity point.
It is continually fed into protective gas, and quartz ampoule 10 is heated, rises to depositing temperature.Protective gas can be argon gas, helium
Gas etc..Carbon source and silicon source are conveyed into quartz ampoule 10 at this time.In the embodiment shown in fig. 1, carbon source and silicon source are entering stone
Impurity is washed away by drexel bottle 12 before English pipe 10.In embodiments of the present invention, optionally, protective gas and carbon source, silicon source one
Conveying is played, protective gas can be used as the carrier gas of carbon source, silicon source.When conveying carbon source, silicon source, gas circuit passes through drexel bottle 12, when stopping
Blocking source, silicon source conveying when, can gas circuit (without drexel bottle) only from above to quartz ampoule 10 convey protective gas.
In chemical vapor deposition processes, depositing temperature is chosen as 900 DEG C~1100 DEG C, for example, 900 DEG C, 1000 DEG C,
The median of 1100 DEG C or any two points, sedimentation time are chosen as 3h~7h, such as the median of 3h, 5h, 7h or any two points.
Throughput can choose in 120ccm~150ccm, such as the median of 120ccm, 130ccm, 150ccm or any two points.Change
The tail gas for learning vapor deposition, which is passed through in the beaker 16 in 10 downstream of quartz ampoule, to be absorbed, and it is molten to be loaded with sodium hydroxide in beaker 16
Liquid.
After chemical vapor deposition terminates, stopping is passed through carbon source, silicon source, continues to be passed through protective gas, until being down to room
Temperature.Carbon-silicon composite material and catalyst that deposition finishes are taken out, catalyst can utilize again after cleaning.
Feature and performance of the invention are described in further detail below in conjunction with each specific embodiment.
Embodiment 1
The present embodiment provides a kind of preparation methods of Si-C composite material, comprising:
Quartz ampoule heating zone in tube furnace is lain in after carrier is cleaned, it will be as the carbon nanotube of carbon base body and as urging
The copper sheet of agent is put on the carrier, and certainly, carrier itself may be copper.Lead to first in pipe argon gas 30 minutes, row
Inner air tube to the greatest extent.It keeps argon gas to be continually fed into, according to 5 DEG C/min heating rate, rises to 1000 DEG C of depositing temperature.It opens at this time molten
Liquid gas circuit (passes through drexel bottle), is brought dimethyldichlorosilane and toluene in quartz ampoule by carrier gas argon gas, heat preservation deposition 5h,
Throughput is stablized in 120ccm.The tail gas of quartz ampoule discharge, which is passed through in sodium hydroxide solution, to be absorbed.After the completion of deposition reaction, close
Solution gas circuit persistently leads to argon gas, until being down to room temperature.It can be taken off carbon-silicon composite material at this time, and take out the copper sheet in quartz ampoule,
It is washed, is to be measured.
Embodiment 2
The present embodiment provides a kind of preparation methods of Si-C composite material, comprising:
It will be laid on clean carrier as the carbon nanotube of carbon base body and copper sheet, carrier then lain in into quartz
Pipe is placed in heating zone in tube furnace by Guan Zhong, is led to argon gas 60 minutes first in pipe, is drained inner air tube.Argon gas is kept to continue
It is passed through, according to 10 DEG C/min heating rate, rises to 900 DEG C of depositing temperature.Solution gas circuit (passing through drexel bottle) is opened at this time, is passed through
Carrier gas argon gas brings dimethyldichlorosilane and benzene in quartz ampoule into, and heat preservation deposition 6h, throughput is stablized in 150ccm.Quartz ampoule
The tail gas of discharge, which is passed through in sodium hydroxide solution, to be absorbed, and after the completion of deposition reaction, is closed solution gas circuit, is persistently led to argon gas, until
It is down to room temperature.Si-C composite material and catalyst are taken out, washing is to be measured.
Embodiment 3
The present embodiment provides a kind of preparation methods of Si-C composite material, comprising:
Quartz ampoule heating zone in tube furnace is lain in after carrier is cleaned, it will be as the carbon nanotube of carbon base body and as urging
The gold particle of agent is put on the carrier.Lead to first in pipe argon gas 30 minutes, drains inner air tube.Argon gas is kept persistently to lead to
Enter, according to 5 DEG C/min heating rate, rises to 1100 DEG C of depositing temperature.Solution gas circuit (passing through drexel bottle) is opened at this time, passes through load
Gas argon gas brings trimethyl dichlorosilane and toluene in quartz ampoule into, and heat preservation deposition 7h, throughput is stablized in 130ccm.Quartz ampoule
The tail gas of discharge, which is passed through in sodium hydroxide solution, to be absorbed.After the completion of deposition reaction, solution gas circuit is closed, persistently leads to argon gas, until
It is down to room temperature.Si-C composite material and catalyst are then taken out, is washed, it is to be measured.
Embodiment 4
The present embodiment provides a kind of preparation methods of Si-C composite material, comprising:
Quartz ampoule heating zone in tube furnace is lain in after carrier is cleaned, it will be as the graphene of carbon base body and as catalysis
The platinum grain of agent is put on the carrier.Lead to first in pipe argon gas 40 minutes, drains inner air tube.Argon gas is kept persistently to lead to
Enter, according to 8 DEG C/min heating rate, rises to 900 DEG C of depositing temperature.Solution gas circuit (passing through drexel bottle) is opened at this time, passes through load
Gas argon gas brings dimethyldichlorosilane and toluene in quartz ampoule into, and heat preservation deposition 3h, throughput is stablized in 150ccm.Quartz ampoule
The tail gas of discharge, which is passed through in sodium hydroxide solution, to be absorbed.After the completion of deposition reaction, solution gas circuit is closed, persistently leads to argon gas, until
It is down to room temperature.It can be taken off carbon-silicon composite material and catalyst granules at this time, washed, is to be measured.
Embodiment 5
The present embodiment provides a kind of preparation methods of Si-C composite material, comprising:
Quartz ampoule heating zone in tube furnace is lain in after carrier is cleaned, it will be as the graphite nodule of carbon base body and as catalysis
The Argent grain of agent is put on the carrier.Lead to first in pipe argon gas 50 minutes, drains inner air tube.Argon gas is kept persistently to lead to
Enter, according to 10 DEG C/min heating rate, rises to 1100 DEG C of depositing temperature.Solution gas circuit (passing through drexel bottle) is opened at this time, is passed through
Carrier gas argon gas brings trimethyl dichlorosilane and benzene in quartz ampoule into, and heat preservation deposition 3h, throughput is stablized in 120ccm.Quartz ampoule
The tail gas of discharge, which is passed through in sodium hydroxide solution, to be absorbed.After the completion of deposition reaction, solution gas circuit is closed, persistently leads to argon gas, until
It is down to room temperature.It can be taken off carbon-silicon composite material and catalyst granules at this time, washed, is to be measured.
Embodiment 6
The present embodiment provides a kind of preparation methods of Si-C composite material, comprising:
Quartz ampoule heating zone in tube furnace is lain in after carrier is cleaned, it will be as the graphene of carbon base body and as catalysis
The platinum grain of agent is put on the carrier.Lead to first in pipe argon gas 40 minutes, drains inner air tube.Argon gas is kept persistently to lead to
Enter, according to 10 DEG C/min heating rate, rises to 1000 DEG C of depositing temperature.Solution gas circuit (passing through drexel bottle) is opened at this time, is passed through
Carrier gas argon gas brings dimethyldichlorosilane and benzene in quartz ampoule into, and heat preservation deposition 5h, throughput is stablized in 120ccm.Quartz ampoule
The tail gas of discharge, which is passed through in sodium hydroxide solution, to be absorbed.After the completion of deposition reaction, solution gas circuit is closed, persistently leads to argon gas, until
It is down to room temperature.It can be taken off carbon-silicon composite material and catalyst granules at this time, washed, is to be measured.
Carbon-silicon composite material to embodiment 1 and the carbon nanotube used are tested.Fig. 2 is carbon nanotube and this hair
XRD (X-ray diffraction) map of the carbon-silicon composite material of bright embodiment 1；(a)~(d) is that carbon is received under different amplification in Fig. 3
SEM (scanning electron microscope) figure of mitron and the carbon-silicon composite material of the embodiment of the present invention 1；Fig. 4 is that the carbon silicon of the embodiment of the present invention 1 is multiple
XPS (X-ray photoelectron spectroscopic analysis) figure of condensation material；Fig. 5 is the carbon-silicon composite material of carbon nanotube and the embodiment of the present invention 1
First charge-discharge curve graph；Fig. 6 is the circulation and efficiency song of the carbon-silicon composite material of carbon nanotube and the embodiment of the present invention 1
Line.It can be seen that 1 obtained Si-C composite material through the embodiment of the present invention from above-mentioned test result and reducing preparation cost
It can also guarantee preferable performance simultaneously.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of Si-C composite material, which is characterized in that the method that silicon source, carbon source are passed through chemical vapor deposition
It is deposited on carbon base body, to obtain Si-C composite material；Wherein, the silicon source is dimethyldichlorosilane or trimethyl dichloro silicon
Alkane, the carbon source are benzene or toluene, and the carbon base body is graphite nodule, graphene or carbon nanotube.
2. the preparation method of Si-C composite material according to claim 1, which is characterized in that in the chemical vapor deposition
During use catalyst, the catalyst be at least one of copper, platinum, gold, silver.
3. the preparation method of Si-C composite material according to claim 2, which is characterized in that the catalyst is sheet,
When carrying out the chemical vapor deposition, the carbon base body is placed on the catalyst of sheet.
4. the preparation method of Si-C composite material according to claim 2, which is characterized in that the catalyst is particle
Shape, when carrying out the chemical vapor deposition, the granular catalyst is scattered on the carbon base body.
5. the preparation method of Si-C composite material according to claim 4, which is characterized in that the granular catalyst
Median particle diameter be 20~200 microns.
6. the preparation method of Si-C composite material according to claim 1, which is characterized in that the chemical vapor deposition
Step carries out in quartz ampoule, and the gaseous silicon source and the carbon source pass through gas washing, enters the quartz after removal impurity
It is deposited in pipe.
7. the preparation method of Si-C composite material according to claim 6, which is characterized in that the chemical vapor deposition it
Tail gas afterwards, which is passed through in sodium hydroxide solution, to be absorbed.
8. the preparation method of Si-C composite material according to claim 1, which is characterized in that the chemical vapor deposition
Temperature is 900 DEG C~1100 DEG C.
9. the preparation method of Si-C composite material according to claim 1, which is characterized in that the chemical vapor deposition
Duration is 3h~7h.
10. a kind of Si-C composite material, which is characterized in that pass through Si-C composite material of any of claims 1-9
Preparation method be made.
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