CN108232165A - A kind of preparation method of carbon-silicon composite material - Google Patents
A kind of preparation method of carbon-silicon composite material Download PDFInfo
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- CN108232165A CN108232165A CN201810039074.4A CN201810039074A CN108232165A CN 108232165 A CN108232165 A CN 108232165A CN 201810039074 A CN201810039074 A CN 201810039074A CN 108232165 A CN108232165 A CN 108232165A
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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
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 invention relates to a kind of preparation methods of carbon-silicon composite material, it includes the following steps：(a) catalyst is dissolved in the first solvent and is configured to catalyst solution；The catalyst is the mixture formed selected from one or more of molysite, nickel salt, cobalt salt and mantoquita；(b) carbon source is dissolved in the second solvent and is configured to carbon source solution；(c) adding in silicon materials in the catalyst solution makes catalyst be supported on the silicon materials surface, then being added into carbon source solution makes carbon source be supported on its surface；Or add in silicon materials in the mixed solution that the catalyst solution and the carbon source solution are formed, catalyst and carbon source is made to be supported on the silicon materials surface；(d) product of step (c) in reducibility gas is calcined, then cleaned.The impurity such as metal salt, oxide and the carbide after catalyst reduction can be effectively removed, effectively keep the capacity of silicium cathode material.
Description
Technical field
The invention belongs to lithium ion battery negative material fields, are related to a kind of carbon-silicon composite material, and in particular to a kind of carbon
The preparation method of silicon composite.
Background technology
Silicon materials are due to the big 4200mAh/g of its theoretical capacity, the advantages that mature preparation process, are considered as very likely substituting
Graphite material is as next-generation lithium battery negative material；Especially every profession and trade development bottleneck is already known in current battery capacity
Stage, the large capacity of silicium cathode material is more exposed to concern.The technical issues of silicium cathode material mainly faces be lithium from
Violent expansion occurs for silicon materials volume during son disengaging, generates the consequence of material dusting；A grade piece capacity is caused to be remarkably decreased,
Pierce through the problems such as short circuit occurs for film.The silicium cathode material preparation process being widely studied is concentrated mainly on elementary silicon nanometer
Change, to provide the access way of lithium ion, improve its charge-discharge performance, while reduce dusting degree.Silicon-carbon can also be prepared to answer
Condensation material, carbon material cladding silicon materials tolerate its volume expansion etc..The preparation of silicon-carbon cathode material has ball-milling method, chemical vapor deposition
Area method, high-temperature cracking method etc., wherein chemical vapor deposition need to use such as acetylene of the gas containing carbon source, methane etc., test work
Skill is complicated, dangerous high, and vapor deposition can only be deposited on the surface of agglomerated materials, and carbon material cannot good homoepitaxial
On the surface of silicon materials.
Invention content
A kind of preparation method of carbon-silicon composite material is provided the invention aims to overcome the deficiencies in the prior art.
In order to achieve the above objectives, the technical solution adopted by the present invention is：A kind of preparation method of carbon-silicon composite material, it is wrapped
Include following steps：
(a) catalyst is dissolved in the first solvent and is configured to catalyst solution；The catalyst be selected from molysite, nickel salt,
The mixture of one or more of cobalt salt and mantoquita composition；
(b) carbon source is dissolved in the second solvent and is configured to carbon source solution；The carbon source be selected from quinolinic acid, sodium alginate,
The mixture of one or more of polyvinylpyrrolidone, starch, cellulose and polyacrylic resin composition；Described first is molten
Agent and second solvent are independently of one another one in distilled water, ethyl alcohol, methanol, isopropanol, ethylene glycol and glycerine
The mixture of kind or several compositions；
(c) adding in silicon materials in the catalyst solution makes catalyst be supported on the silicon materials surface, then is added
Entering makes carbon source be supported on its surface in carbon source solution；Or silicon materials are added in into the catalyst solution and the carbon source solution shape
Into mixed solution in, catalyst and carbon source is made to be supported on the silicon materials surface；
(d) product of step (c) in reducibility gas is calcined, then cleaned.
Another object of the present invention is to provide the preparation method of another carbon-silicon composite material, it includes the following steps：
(a) catalyst is dissolved in the first solvent and is configured to catalyst solution；The catalyst be selected from molysite, nickel salt,
The mixture of one or more of cobalt salt and mantoquita composition；
(b) adding in silicon materials in the catalyst solution makes catalyst be supported on the silicon materials surface；
(c) product of step (b) is collectively disposed at carbon source in reducibility gas and calcined, then cleaned.
Optimally, the catalyst is selected from Fe (NO3)3、FeCl3、Fe2(SO4)3、Ni(CH3COO)2、NiCO3、NiCl2、
Ni(NO3)2、NiSO4、Co(CH3COO)2、CoCO3、Co(NO3)2、CoSO4、Cu(CH3COO)2、CuCO3、CuCl2、Cu(NO3)2With
CuSO4One or more of composition mixture.
Optimally, the temperature of the calcining is 500~1200 DEG C, and calcination time is 0.1~48h.
Optimally, the ratio of the silicon materials and the catalyst is 1~1000：1.
Further, the silicon materials and the mass ratio of the carbon source are 1：0.2~100.
Optimally, the cleaning is first is cleaned, then cleaned with deionized water to neutrality using cleaning solution；It is described clear
Mixture of the dilution for one or more of hydrochloric acid, nitric acid and hydrofluoric acid composition.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：Carbon silicon of the present invention is compound
The preparation method of material by silicon materials catalyst supported on surface, carbon source, and carries out calcining cleaning, in this way can be in silicon material
Expect surface in situ growth carbon nanotube or carbon fiber, not only simple for process, suitable large-scale production can be very good in silicon material
Expect surface homoepitaxial carbon nanotube and carbon fiber, the inhomogeneities that vapour deposition process is overcome to grow；And it can effectively go
Except the oxide that metal salt, the silicon materials after catalyst reduction generate under the high temperature conditions, the impurity such as carbide effectively keep silicon
The capacity of negative material；And the carbon nanotube in silicon face generation obtains the sky that carbon fiber is capable of providing silicon volume expansion in the circulating cycle
Between, and increase the electric conductivity and mechanical property between silicon particle, effectively improve the long-term cycle performance and high rate performance of material.
Description of the drawings
Fig. 1 is Si-C composite material SEM figures obtained in embodiment 1；
Fig. 2 is Si-C composite material SEM figures obtained in embodiment 2-3；
Fig. 3 is Si-C composite material first charge-discharge curve obtained in comparative sample and embodiment 1；
Fig. 4 is the long-term cycle performance of Si-C composite material assembled battery obtained in embodiment 1；
Specific embodiment
The preparation method of carbon-silicon composite material of the present invention, it includes the following steps：(a) catalyst is dissolved in the first solvent
It is configured to catalyst solution；The catalyst is the mixing formed selected from one or more of molysite, nickel salt, cobalt salt and mantoquita
Object；(b) carbon source is dissolved in the second solvent and is configured to carbon source solution；The carbon source is selected from quinolinic acid, sodium alginate, polyethylene
The mixture of one or more of pyrrolidones, starch, cellulose and polyacrylic resin composition；First solvent and institute
It states the second solvent and is independently of one another one kind or several in distilled water, ethyl alcohol, methanol, isopropanol, ethylene glycol and glycerine
The mixture of kind composition；(c) adding in silicon materials in the catalyst solution makes catalyst be supported on the silicon materials surface, then
Being added into carbon source solution makes carbon source be supported on its surface；Or silicon materials are added in into the catalyst solution and the carbon source
In the mixed solution that solution is formed, catalyst and carbon source is made to be supported on the silicon materials surface；(d) product of step (c) is existed
It is calcined in reducibility gas, is then cleaned.Another group of preparation method of carbon-silicon composite material of the present invention, it include with
Lower step：(a) catalyst is dissolved in the first solvent and is configured to catalyst solution；The catalyst is selected from molysite, nickel salt, cobalt
The mixture of one or more of salt and mantoquita composition；(b) adding in silicon materials in the catalyst solution bears catalyst
It is loaded in the silicon materials surface；(c) it is calcined in reducibility gas after the product of step (b) is mixed with carbon source, then
Cleaning.Above two method carries out calcining cleaning by silicon materials catalyst supported on surface, carbon source, not only technique
Simply, it is suitble to large-scale production；And the impurity such as metal salt, oxide after catalyst reduction can be effectively removed, effectively
Keep the capacity of silicium cathode material.
In the above method, the catalyst is selected from Fe (NO3)3、FeCl3、Fe2(SO4)3、Ni(CH3COO)2、NiCO3、
NiCl2、Ni(NO3)2、NiSO4、Co(CH3COO)2、CoCO3、Co(NO3)2、CoSO4、Cu(CH3COO)2、CuCO3、CuCl2、Cu
(NO3)2And CuSO4One or more of composition mixture.The temperature of the calcining is 500~1200 DEG C, and calcination time is
0.1~48h.The ratio of the silicon materials and the catalyst is preferably 1~1000：1.The silicon materials and the matter of the carbon source
Amount is than preferably 1：0.2~100.The cleaning is first is cleaned, then cleaned with deionized water to neutrality using cleaning solution；
Mixture of the cleaning solution for one or more of hydrochloric acid, nitric acid and hydrofluoric acid composition.
The present invention is further described below in conjunction with embodiment.
Embodiment 1
The present invention provides a kind of preparation method of carbon-silicon composite material, it includes the following steps：
(a) Ni (CH of 0.1M are prepared using distilled water3COO)2Solution (i.e. catalyst solution)；
(b) sodium alginate soln (i.e. carbon source solution) of 3%wt is prepared using distilled water；
(c) silicon materials (100nm, Shenzhen section crystalline substance intelligence reach Science and Technology Ltd.) are added to Ni (CH3COO)2(Ni in solution
(CH3COO)2Mass ratio with silicon is 1：20, it stirs 2 hours, and in 100 DEG C of heat dryings, obtains the silicon material of catalyst load
Material；The silicon materials by catalyst load are added in carbon source solution again so that the silicon materials of catalyst load and the mass ratio of carbon source
It is 1：10, it stirs 2 hours, is dried to obtain the silicon materials of the catalyst load of carbon source cladding；
(d) product of step (c) is placed in crucible, is then charged into tube furnace, be filled with the gaseous mixture of hydrogen and argon gas
(volume ratio of hydrogen and argon gas is 5 to body：95) 700 DEG C of temperature then, are warming up to 5 DEG C/h of speed；It is raised to target temperature
Afterwards, 2 hours are kept the temperature and carries out high-temperature calcination, cooled to room temperature；The hydrochloric acid that obtained product is added to a concentration of 10wt% is molten
(being about 10 minutes) is cleaned in liquid, is then cleaned with deionized water to neutrality, products obtained therefrom is as shown in Figure 1, silicon-carbon is answered
Condensation material is prepared shown in battery first charge-discharge curve such as Fig. 3 (right part of flg), and long-term cycle and efficiency are as shown in Figure 4.
Embodiment 2
The present invention provides a kind of preparation method of carbon-silicon composite material, it includes the following steps：
(a) Ni (CH of 0.1M are prepared using distilled water3COO)2Solution (i.e. catalyst solution)；
(b) it is added to catalyst using as the silicon materials of basis material (100nm, Shenzhen section crystalline substance intelligence reach Science and Technology Ltd.)
(mass ratio of catalyst and silicon is 1 in solution：20) it, stirs 2 hours, and heat drying, obtains the silicon materials of catalyst load；
(c) product of step (b) is placed in crucible, is then charged into tube furnace and (is put into quinoline in the front end of tube furnace
Acid is mixed with preceding product), the mass ratio of quinolinic acid and the silicon materials of catalyst load is 20：1, it is filled with hydrogen and argon gas
Gaseous mixture (5/95), 700 DEG C of temperature are then warming up to 5 DEG C/h of speed；；After being raised to target temperature, 2 hours are kept the temperature
After carrying out high temperature reduction, cooled to room temperature；Obtained substance is added in the hydrochloric acid solution of a concentration of 10wt% and carries out clearly
It washes (be about 10 minutes), is then cleaned with deionized water to neutrality, shown in products obtained therefrom such as Fig. 2 (the SEM figures in left side).
Embodiment 3
The present invention provides a kind of preparation method of carbon-silicon composite material, it includes the following steps：
(a) Ni (CH of 0.1M are prepared using distilled water3COO)2Solution (i.e. catalyst solution)；
(b) sodium alginate soln (i.e. carbon source solution) of 3%wt is prepared using distilled water；
(c) catalyst solution and carbon source solution are mixed so that silicon materials and carbon source, catalyst mass ratio be 1：
10：0.05, it stirs 2 hours, and heat drying, obtains catalyst and the silicon materials of carbon source load；
(d) product of step (c) is placed in crucible, is then charged into tube furnace, be filled with the gaseous mixture of hydrogen and argon gas
Body (is same as above), is then warming up to 700 DEG C of temperature with 5 DEG C/h of speed；After being raised to target temperature, keep the temperature 2 hours and carry out high temperature
Calcining, cooled to room temperature；It (is about 10 that obtained product, which is added in the hydrochloric acid solution of a concentration of 10wt% and is cleaned,
Minute), it is then cleaned with deionized water to neutrality, shown in products obtained therefrom such as Fig. 2 (the SEM figures on right side).
Embodiment 4
The present invention provides a kind of preparation method of carbon-silicon composite material, and step is different with basically identical in embodiment 1
Be：The catalyst used in step (a) is Cu (CH3COO)2。
Embodiment 5
The present invention provides a kind of preparation method of carbon-silicon composite material, and step is different with basically identical in embodiment 1
Be：The catalyst used in step (a) is Fe (NO3)3。
Embodiment 6
The present invention provides a kind of preparation method of carbon-silicon composite material, and step is different with basically identical in embodiment 1
Be：The carbon source used in step (b) is sodium alginate.
Embodiment 7
The present invention provides a kind of preparation method of carbon-silicon composite material, and step is different with basically identical in embodiment 1
Be：The carbon source used in step (b) is polyvinylpyrrolidone.
Embodiment 8
The present invention provides a kind of preparation method of carbon-silicon composite material, and step is different with basically identical in embodiment 1
Be：The carbon source used in step (b) is starch.
Embodiment 9
The present invention provides a kind of preparation method of carbon-silicon composite material, and step is different with basically identical in embodiment 1
Be：The carbon source used in step (b) is polyacrylic resin.
By carbon-silicon composite material obtained in the various embodiments described above respectively with sodium alginate and acetylene black according to mass ratio 70:
15:15 are dispersed in water and are sufficiently stirred 30min, obtain uniformly mixed mixture paste, and be coated on copper foil of affluxion body, dry
Dry, slice.Dry pole piece is moved on in glove box, using lithium piece as to electrode, 2032 button cells of assembling (electrolyte 1M
LiPF6Volume ratio for conductive salt is 1：1：1 EC/DMC/DEC solution, and add in VC and quality point that mass fraction is 2%
The FEC that number is 10% is as additive)；By the battery seal of assembling, 10h is stood.By the battery stood in charge-discharge test
Constant current test chemical property on instrument (wherein charge-discharge magnification is 0.2C, and voltage range is in 0.01~1V).
The Si-C composite material prepared in 1 embodiment 1-5 of table is assembled into the chemical property table of battery
It can be seen that different carbon sources, decomposition temperature has very big difference, and the carbon material of formation is also different, wherein polyacrylic acid
The generation of resin high temperature is hard carbon material, has the advantages of capacity is high, and cyclicity is good, while there is also first all efficiency is low, low electricity
Position storage lithium high rate performance is poor.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention, all according to the present invention
The equivalent change or modification that Spirit Essence is made, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of carbon-silicon composite material, which is characterized in that it includes the following steps：
(a) catalyst is dissolved in the first solvent and is configured to catalyst solution；The catalyst is selected from molysite, nickel salt, cobalt salt
With the mixture of one or more of mantoquita composition；
(b) carbon source is dissolved in the second solvent and is configured to carbon source solution；The carbon source is selected from quinolinic acid, sodium alginate, poly- second
The mixture of one or more of alkene pyrrolidone, starch, cellulose and polyacrylic resin composition；First solvent and
Second solvent be independently of one another one kind in distilled water, ethyl alcohol, methanol, isopropanol, ethylene glycol and glycerine or
The mixture of several compositions；
(c) adding in silicon materials in the catalyst solution makes catalyst be supported on the silicon materials surface, then is added into carbon
Carbon source is made to be supported on its surface in the solution of source；Or silicon materials are added in what the catalyst solution and the carbon source solution were formed
In mixed solution, catalyst and carbon source is made to be supported on the silicon materials surface；
(d) product of step (c) in reducibility gas is calcined, then cleaned.
2. a kind of preparation method of carbon-silicon composite material, which is characterized in that it includes the following steps：
(a) catalyst is dissolved in the first solvent and is configured to catalyst solution；The catalyst is selected from molysite, nickel salt, cobalt salt
With the mixture of one or more of mantoquita composition；
(b) adding in silicon materials in the catalyst solution makes catalyst be supported on the silicon materials surface；
(c) product of step (b) is collectively disposed at carbon source in reducibility gas and calcined, then cleaned.
3. the preparation method of carbon-silicon composite material according to claim 1 or claim 2, it is characterised in that：The catalyst be selected from
Fe(NO3)3、FeCl3、Fe2(SO4)3、Ni(CH3COO)2、NiCO3、NiCl2、Ni(NO3)2、NiSO4、Co(CH3COO)2、CoCO3、
Co(NO3)2、CoSO4、Cu(CH3COO)2、CuCO3、CuCl2、Cu(NO3)2And CuSO4One or more of composition mixing
Object.
4. the preparation method of carbon-silicon composite material according to claim 1 or claim 2, it is characterised in that：The temperature of the calcining is
500~1200 DEG C, calcination time is 0.1~48h.
5. the preparation method of carbon-silicon composite material according to claim 1 or claim 2, it is characterised in that：The silicon materials with it is described
The ratio of catalyst is 1~1000：1.
6. the preparation method of carbon-silicon composite material according to claim 5, it is characterised in that：The silicon materials and the carbon source
Mass ratio be 1：0.2~100.
7. the preparation method of carbon-silicon composite material according to claim 1 or claim 2, it is characterised in that：The cleaning is first uses
Cleaning solution is cleaned, then is cleaned with deionized water to neutrality；The cleaning solution is one in hydrochloric acid, nitric acid and hydrofluoric acid
The mixture of kind or several compositions.
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| CN109713265A (en) * | 2018-12-21 | 2019-05-03 | 桑德集团有限公司 | A kind of silicon-carbon cathode material and preparation method thereof |
| CN111799448A (en) * | 2019-04-08 | 2020-10-20 | 江苏天奈科技股份有限公司 | Method for growing carbon nano-tube in situ by silicon or oxide thereof |
| CN110828809A (en) * | 2019-11-20 | 2020-02-21 | 厦门大学 | Silicon-carbon composite material in form of bubble coral and preparation method and application thereof |
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