CN114171728A - Three-dimensional porous silicon-carbon composite material, preparation method and application thereof - Google Patents
Three-dimensional porous silicon-carbon composite material, preparation method and application thereof Download PDFInfo
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- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000011863 silicon-based powder Substances 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 150000003926 acrylamides Chemical class 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 239000011247 coating layer Substances 0.000 claims description 6
- 239000011856 silicon-based particle Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000007773 negative electrode material Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 2
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- PLUPPIWWCYTVMF-UHFFFAOYSA-N 2-[4-(hydroxyamino)phenyl]prop-2-enamide Chemical compound C=C(C1=CC=C(C=C1)NO)C(=O)N PLUPPIWWCYTVMF-UHFFFAOYSA-N 0.000 claims 1
- XEZHXJNYSZVBPF-UHFFFAOYSA-N C=C(C(N)=O)C(C=C1)=CCC1=S(=O)=O Chemical group C=C(C(N)=O)C(C=C1)=CCC1=S(=O)=O XEZHXJNYSZVBPF-UHFFFAOYSA-N 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000010406 cathode material Substances 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000005543 nano-size silicon particle Substances 0.000 abstract 3
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910000733 Li alloy Inorganic materials 0.000 description 3
- ZVLDJSZFKQJMKD-UHFFFAOYSA-N [Li].[Si] Chemical compound [Li].[Si] ZVLDJSZFKQJMKD-UHFFFAOYSA-N 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000001989 lithium alloy Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- NNOVDYYESLNENK-UHFFFAOYSA-N N-[4-(hydroxyamino)phenyl]prop-2-enamide Chemical compound C(C=C)(=O)NC1=CC=C(C=C1)NO NNOVDYYESLNENK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000012698 colloidal precursor Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- -1 silicon ions Chemical class 0.000 description 2
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 description 1
- JYJTXYSFADPEOL-UHFFFAOYSA-N C=CC(NC(C=C1)=CCC1=S(=O)=O)=O Chemical group C=CC(NC(C=C1)=CCC1=S(=O)=O)=O JYJTXYSFADPEOL-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Images
Classifications
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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
-
- 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
-
- 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
- H01M4/62—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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 provides a three-dimensional porous silicon-carbon composite material, a preparation method and application thereof, and belongs to the field of micro-nano material synthesis. The silicon-carbon composite material prepared by the invention comprises porous nitrogen-doped carbon-coated silicon nanoparticles, and the particle size of the silicon nanoparticles in the silicon-carbon composite material is 40-80 nm. The nitrogen-doped carbon is in a unique three-dimensional network shape and has a rich pore structure, so that the agglomeration of silicon nano particles can be effectively prevented, the overall conductivity of the composite material is improved, the toughness of the composite material can be increased, and the structural damage of an electrode material caused by volume change in the charging and discharging process is prevented. In addition, the invention has the advantages of easily obtained raw materials, simple process, strong repeatability and low overall preparation cost of products, and is suitable for industrial production. The prepared silicon-carbon composite material has distinct morphology and characteristic, and has better electrochemical performance when being used as a lithium ion battery cathode material.
Description
Technical Field
The invention belongs to the field of synthesis of micro-nano materials, and particularly relates to a three-dimensional porous silicon-carbon composite material, a preparation method and application thereof.
Background
The lithium ion battery is one of the most important electrochemical energy storage devices at present, the theoretical specific capacity of the commercialized graphite cathode is low, and the rapid development of a new generation of high-energy-density lithium ion battery is limited. The silicon negative electrode has the theoretical specific capacity of 3590mAh g-1, and is one of the lithium battery negative electrode materials with the most application prospect. However, the volume change of the silicon-lithium alloy reaches 360%, and the structure is extremely unstable in the charging and discharging process, so that the capacity of the battery is rapidly attenuated. At present, one of the main solutions is to compound the silicon negative electrode with a carbon material, so as to improve the conductivity of the silicon negative electrode and alleviate the volume change of the silicon-lithium alloy.
For example, in chinese patent CN201810396791.2, silica powder is wrapped by graphitized carbon micro powder, and then spray-dried to obtain the silicon carbon microsphere. Chinese patent CN202010473716.9 uses graphene to coat silicon ions to form primary silicon-carbon particles, then uses silane coupling agent to perform secondary coating, adds carbon nanotubes to further improve the conductivity of the material, and finally forms secondary silicon-carbon particles by calcination. Chinese patent CN201710270675.1 sprays graphene coating slurry and silicon slurry into a coating chamber respectively, and makes the coating chamber carry opposite charges, and forms a silicon-carbon cathode material by adjusting air flow. Although the silicon-carbon cathode material disclosed above has certain improvements in aspects of controlling the volume change of silicon, improving the electrochemical performance of the lithium ion battery, and the like, the raw materials and equipment used are expensive, and the preparation process is complex, so that the overall cost of the product is high, and the industrial production is not facilitated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a three-dimensional porous silicon-carbon composite material, a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a three-dimensional porous silicon-carbon composite material comprises the following steps:
1) dispersing silicon powder and acrylamide in deionized water to obtain dispersion liquid A;
2) dissolving potassium persulfate and acrylamide derivatives in deionized water to obtain a mixed solution B;
3) adding the mixed solution B into the dispersion solution A, uniformly stirring, and then reacting for 1-3 hours at 50-80 ℃;
4) washing the reaction product with absolute ethyl alcohol for several times, and then drying in vacuum at 50-80 ℃ for 1-10 hours;
5) and calcining the dried product in an argon or nitrogen atmosphere at the calcining temperature of 500-900 ℃ for 1-5 hours to obtain the three-dimensional porous silicon-carbon composite material.
Furthermore, in the step 1), the mass ratio of the silicon powder to the acrylamide is 1 (1-10).
Further, in the step 1), 10-50 mL of deionized water is added for every 1.0g of silicon powder.
Further, in the step 2), the mass ratio of the potassium persulfate to the acrylamide derivative is 1 (0.1-1).
Further, in the step 2), 10-50 mL of deionized water is added for every 1.0g of potassium persulfate.
Further, in the step 2), the acrylamide derivative is 4-sulfonylphenyl acrylamide, p-hydroxyaminophenyl acrylamide, N-methylol acrylamide or N, N-methylene-bis-acrylamide.
The three-dimensional porous silicon-carbon composite material prepared by the preparation method is provided.
Furthermore, the surface of the silicon particle is coated with a three-dimensional porous carbon coating layer doped with nitrogen elements.
The three-dimensional porous silicon-carbon composite material is applied as a lithium ion battery cathode material.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the three-dimensional porous silicon-carbon composite material has the advantages of common and easily-obtained raw materials, low price, simple preparation process and strong repeatability, and all the used equipment is conventional equipment, and is favorable for industrial large-scale production. In addition, the overall cost of the preparation process is low, the product size is controllable, the service performance of the material can be obviously improved, and the industrial production is facilitated. If acrylamide is added independently in the preparation process, only one carbon coating layer can be formed on the surface of silicon powder finally, and a target product cannot be prepared yet, the invention adds acrylamide derivatives, utilizes the mutual crosslinking property of the substances and the acrylamide, can form a three-dimensional cross-linked colloidal precursor on the surface of the silicon powder, and builds a three-dimensional porous carbon coating layer on the surface of silicon particles in situ through calcination, thereby solving the following two main problems of the common silicon-carbon negative electrode material at present: 1) the carbon layer is too thick to facilitate the performance of the capacity of the silicon anode. 2) The carbon layer is too thin and the structure is easily broken during charging and discharging.
According to the three-dimensional porous silicon-carbon composite material, a colloidal precursor with cross-linking in a shape like Regulada in three dimensions is formed on the surface of silicon powder, and a three-dimensional porous carbon coating layer is constructed in situ on the surface of silicon particles through calcination; in addition, the electron transport property of the composite material can be further improved by doping a small amount of nitrogen element in the carbon layer. The coating of the three-dimensional porous carbon can prevent the agglomeration of silicon particles, improve the overall conductivity of the composite material, and the abundant pore structure can also increase the toughness of the material.
The three-dimensional porous silicon-carbon composite material is applied as a lithium ion battery cathode material, and the three-dimensional porous carbon coating layer is constructed on the surface of the silicon particles in situ, so that the space for accommodating the volume change of the silicon-lithium alloy in the lithium desorption process is increased, the structural damage of the electrode material caused by the volume change is reduced, and the battery has higher specific capacity and good cycling stability.
Drawings
FIG. 1 is the XRD pattern of the three-dimensional porous silicon carbon composite material of example 1;
FIG. 2 is a scanning electron microscope image of the three-dimensional porous Si-C composite material of example 1;
fig. 3 is a charge-discharge cycle diagram of the three-dimensional porous silicon-carbon composite material of example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
1.0g of silicon powder and acrylamide are respectively weighed and dispersed in 50mL of deionized water, a dispersion liquid is marked as A, 1.0g of potassium persulfate and N-hydroxymethyl acrylamide are respectively weighed and dissolved in 10mL of deionized water, a mixed solution is marked as B, the mixed solution B is added into the dispersion liquid A, the mixture is stirred for 0.5 hour and then placed in an oven, the mixture is pre-dried for 3 hours at 50 ℃, then absolute ethyl alcohol is used for washing for a plurality of times, the mixture is dried for 10 hours in vacuum at 50 ℃, and a dried product is calcined for 5 hours at 500 ℃ under the argon atmosphere, so that the three-dimensional porous silicon-carbon composite material is prepared.
Referring to fig. 1, fig. 1 is an XRD chart of the silicon-carbon composite material prepared in example 1, where relatively sharp peaks at 28 °, 47 °, and 56 ° 2 θ correspond to cubic phase silicon, and PDF cards are 27-1402. A broad peak around 2 θ ═ 21 ° corresponds to nitrogen-doped carbon.
Referring to fig. 2, fig. 2 is a scanning electron microscope image of the product of example 1, wherein the prepared silicon-carbon composite material has a vivid morphology and is three-dimensional porous.
Referring to fig. 3, fig. 3 is a cycle chart of the silicon-carbon composite material of example 1 as a negative electrode material of a lithium ion battery, wherein the specific discharge capacity after 100 cycles is 1014mAh/g and the coulombic efficiency is 99% at a current density of 1.0A/g.
Example 2
1.0g and 10g of silicon powder and acrylamide are respectively weighed and dispersed in 50mL of deionized water, a dispersion liquid is marked as A, 1.0g and 0.1g of potassium persulfate and 4-sulfonyl phenyl acrylamide are respectively weighed and dissolved in 10mL of deionized water, a mixed solution is marked as B, the mixed solution B is added into the dispersion liquid A, stirred for 1 hour and then placed in an oven, pre-dried for 1 hour at 80 ℃, then washed for a plurality of times by absolute ethyl alcohol, dried for 10 hours in vacuum at 80 ℃, and a dried product is calcined for 1 hour at 900 ℃ under the argon atmosphere to prepare the three-dimensional porous silicon-carbon composite material.
Example 3
1.0g of silicon powder and acrylamide are respectively weighed and dispersed in 20mL of deionized water, the dispersion liquid is marked as A, 1.0g of potassium persulfate and p-hydroxyaminophenyl acrylamide are respectively weighed and dissolved in 30mL of deionized water, the mixed solution is marked as B, the mixed solution B is added into the dispersion liquid A, the mixture is stirred for 0.5 hour and then placed in a drying oven, the pre-drying is carried out for 3 hours at 50 ℃, then absolute ethyl alcohol is used for washing for a plurality of times, the vacuum drying is carried out for 10 hours at 50 ℃, the dried product is calcined for 4 hours at 600 ℃ under the argon atmosphere, and the three-dimensional porous silicon-carbon composite material is prepared.
Example 4
1.0g of silicon powder and acrylamide are respectively weighed and dispersed in 50mL of deionized water, a dispersion liquid is marked as A, 1.0g and 0.5g of potassium persulfate and N, N-methylene bisacrylamide are respectively weighed and dissolved in 30mL of deionized water, a mixed solution is marked as B, the mixed solution B is added into the dispersion liquid A, stirred for 1 hour and then placed in an oven, pre-dried for 2 hours at 60 ℃, then washed for a plurality of times by absolute ethyl alcohol, dried for 5 hours at 60 ℃, and a dried product is calcined for 3 hours at 800 ℃ under the argon atmosphere, so that the three-dimensional porous silicon-carbon composite material is prepared.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. The preparation method of the three-dimensional porous silicon-carbon composite material is characterized by comprising the following steps of:
1) dispersing silicon powder and acrylamide in deionized water to obtain dispersion liquid A;
2) dissolving potassium persulfate and acrylamide derivatives in deionized water to obtain a mixed solution B;
3) adding the mixed solution B into the dispersion solution A, uniformly stirring, and then reacting for 1-3 hours at 50-80 ℃;
4) washing the reaction product with absolute ethyl alcohol for several times, and then drying in vacuum at 50-80 ℃ for 1-10 hours;
5) and calcining the dried product in an argon or nitrogen atmosphere at the calcining temperature of 500-900 ℃ for 1-5 hours to obtain the three-dimensional porous silicon-carbon composite material.
2. The preparation method of the three-dimensional porous silicon-carbon composite material according to claim 1, wherein in the step 1), the mass ratio of the silicon powder to the acrylamide is 1 (1-10).
3. The method for preparing the three-dimensional porous silicon-carbon composite material according to claim 2, wherein in the step 1), 10-50 mL of deionized water is added for every 1.0g of silicon powder.
4. The preparation method of the three-dimensional porous silicon-carbon composite material according to claim 1, wherein in the step 2), the mass ratio of the potassium persulfate to the acrylamide derivative is 1 (0.1-1).
5. The method for preparing the three-dimensional porous silicon-carbon composite material according to claim 4, wherein in the step 2), 10-50 mL of deionized water is added for every 1.0g of potassium persulfate.
6. The method for preparing the three-dimensional porous silicon-carbon composite material according to claim 1, wherein in the step 2), the acrylamide derivative is 4-sulfonylphenylacrylamide, p-hydroxyaminophenylacrylamide, N-methylolacrylamide or N, N-methylenebisacrylamide.
7. The three-dimensional porous silicon-carbon composite material prepared by the preparation method according to any one of claims 1 to 6.
8. The three-dimensional porous silicon-carbon composite material according to claim 7, wherein the surface of the silicon particles is coated with a nitrogen-doped three-dimensional porous carbon coating layer.
9. Use of the three-dimensional porous silicon-carbon composite material according to claim 7 or 8 as a negative electrode material for a lithium ion battery.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012126338A1 (en) * | 2011-03-18 | 2012-09-27 | 上海交通大学 | Silicon-carbon composite cathode material for lithium ion battery and preparation method thereof |
| CN104103807A (en) * | 2013-04-12 | 2014-10-15 | 华为技术有限公司 | Silicon-carbon composite anode material, preparation method thereof and lithium ion battery |
| CN106941174A (en) * | 2017-05-10 | 2017-07-11 | 中国林业科学研究院林产化学工业研究所 | A kind of nitrogen doped silicon charcoal composite negative pole material and preparation method thereof |
| CN107565109A (en) * | 2017-08-23 | 2018-01-09 | 山东精工电子科技有限公司 | A kind of lithium-ion battery silicon-carbon anode material of high stable and preparation method thereof |
| CN108550827A (en) * | 2018-05-08 | 2018-09-18 | 广东迈纳科技有限公司 | A kind of preparation method of three-dimensional porous shape silicon-carbon cathode material and application |
| CN110474034A (en) * | 2019-08-22 | 2019-11-19 | 陕西科技大学 | A kind of nitrogen mixes porous nano-sheet Si-C composite material and its preparation method and application |
| CN112289985A (en) * | 2020-09-22 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | C @ MgAl2O4Composite coating modified silicon-based negative electrode material and preparation method thereof |
-
2021
- 2021-11-30 CN CN202111450753.9A patent/CN114171728A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012126338A1 (en) * | 2011-03-18 | 2012-09-27 | 上海交通大学 | Silicon-carbon composite cathode material for lithium ion battery and preparation method thereof |
| CN104103807A (en) * | 2013-04-12 | 2014-10-15 | 华为技术有限公司 | Silicon-carbon composite anode material, preparation method thereof and lithium ion battery |
| CN106941174A (en) * | 2017-05-10 | 2017-07-11 | 中国林业科学研究院林产化学工业研究所 | A kind of nitrogen doped silicon charcoal composite negative pole material and preparation method thereof |
| CN107565109A (en) * | 2017-08-23 | 2018-01-09 | 山东精工电子科技有限公司 | A kind of lithium-ion battery silicon-carbon anode material of high stable and preparation method thereof |
| CN108550827A (en) * | 2018-05-08 | 2018-09-18 | 广东迈纳科技有限公司 | A kind of preparation method of three-dimensional porous shape silicon-carbon cathode material and application |
| CN110474034A (en) * | 2019-08-22 | 2019-11-19 | 陕西科技大学 | A kind of nitrogen mixes porous nano-sheet Si-C composite material and its preparation method and application |
| CN112289985A (en) * | 2020-09-22 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | C @ MgAl2O4Composite coating modified silicon-based negative electrode material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 潘启亮: ""锂离子电池高容量硅基负极材料的设计、制备及性能研究"", 《中国博士学位论文全文数据库（电子期刊）》 * |
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