CN109659529A - A kind of preparation process of silicon-carbon cathode material - Google Patents
A kind of preparation process of silicon-carbon cathode material Download PDFInfo
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- CN109659529A CN109659529A CN201811540091.2A CN201811540091A CN109659529A CN 109659529 A CN109659529 A CN 109659529A CN 201811540091 A CN201811540091 A CN 201811540091A CN 109659529 A CN109659529 A CN 109659529A
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- 239000010406 cathode material Substances 0.000 title claims abstract description 28
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
- 239000010439 graphite Substances 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004411 aluminium Substances 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 8
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002210 silicon-based material Substances 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000003832 thermite Substances 0.000 claims description 9
- 239000013354 porous framework Substances 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 6
- 239000007773 negative electrode material Substances 0.000 abstract description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000007770 graphite material Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000010408 sweeping Methods 0.000 description 3
- 230000009967 tasteless effect Effects 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
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
- H01M4/362—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
- 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
- H01M4/38—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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention proposes a kind of preparation process of silicon-carbon cathode material, negative electrode material obtained has higher energy density for lithium ion battery and recycles number.The technique includes following sequential steps: carrying out the silicon oxide particle of diameter 200nm and aluminium powder to be uniformly mixed to get mixture A；Obtained mixture A is put into tube furnace, under the protection of argon gas, 720 °C are roasted 5 hours, obtain product B；Responseless aluminium in product B is removed with the hydrochloric acid of concentration 1%, obtains product C；Using responseless silica in hafnium solution removal product C, the silicon materials D with 3D honeycomb multicellular frame structure is obtained；Porous silica material D and graphite are merged according to the ratio of molar ratio 1:9, so that the surface of porous silica material D coats one layer of graphite, obtain silicon-carbon cathode material.The preparation process of silicon-carbon cathode material of the invention can effectively improve the energy density of battery, have good practicability.
Description
Technical field
The present invention relates to lithium ion battery manufacture technology fields, particularly relate to a kind of preparation process of silicon-carbon cathode material.
Background technique
Negative electrode material is the important component of lithium ion battery, it directly affects the energy density of battery, circulation longevity
The key indexes such as life and security performance.As new-energy automobile is constantly mentioned to what course continuation mileage required in actual application
Height, power battery associated materials also develop towards the direction for providing high-energy-density, the graphite cathode material of conventional lithium ion battery
It can no longer meet the demand of existing market, the negative electrode material of high-energy density has become enterprise and all kinds of scientific research institutions chase
New focus.Silicon based anode material due to have the theoretical specific capacity of energy storage abundant and superelevation be increasingly becoming battery enterprise and
Lithium electric material industry improve cathode preferential selection, and at present most potential novel cathode material for lithium ion battery it
One.
Summary of the invention
The present invention proposes that a kind of preparation process of silicon-carbon cathode material, negative electrode material obtained have higher energy close
Spend and recycle number.
The technical scheme of the present invention is realized as follows: the preparation process of silicon-carbon cathode material, including following sequential steps
S1. it carries out the silicon oxide particle of diameter 200nm and aluminium powder to be uniformly mixed to get mixture A；
S2. thermite reaction is used, obtained mixture A is put into tube furnace, under the protection of argon gas, 720 DEG C
Roasting 5 hours, obtains product B；
Thermite reaction is as follows:
S3. responseless aluminium in product B is removed with the hydrochloric acid of concentration 1%, obtains product C；
It chemically reacts as follows: Al+HCl → Al Cl3+H2↑
S4. using responseless silica in hafnium solution removal product C, the silicon with 3D honeycomb multicellular frame is obtained
Carrier of the material D as graphite particle；
S5. the porous silica material D and graphite are merged according to the ratio of molar ratio 1:9, graphite particle is micro- according to 5
Rice, 9 microns of two kinds of partial size equal proportions are added, so that the surface of porous silica material D coats one layer of graphite, obtain silicon-carbon cathode material
Material.
As a preferred embodiment, in the step S3
S31. product B is persistently stirred 6-8 hours in the hydrochloric acid of concentration 1%, is removed without the aluminium of reaction, obtains product
C。
As a preferred embodiment, in the step S4
S41. product C is reacted 10-12 hours in hafnium solution, is removed without the silica of reaction, obtained with 3D bee
The silicon materials D of nido porous framework.
As a preferred embodiment, in the step S5
S51. one layer of graphite is coated on the surface of the porous silica material D using mechanofusion method.
After above-mentioned technical proposal, the beneficial effects of the present invention are: thermite reaction prepares 3D honeycomb multicellular
The specific surface area of silicon materials improves 60% or more, and aluminium is conventional metal material, at low cost, is easy to produce in enormous quantities.3D bee
The evenly distributed structure of nest cellular greatly improves the quantity of graphite particle filling, and the porous connected structure of honeycomb can be absorbed
The heat that lithium ion generates during deintercalation reduces battery to reduce the expansion rate of silicon in charge and discharge process
Thermal expansion and drum phenomenon, improve charge and discharge number and efficiency, significantly improve the cycle performance of lithium battery, test data table
Bright, the efficiency in first charge-discharge is 92%, reaches 99% by 10 charge and discharge cycles behind efficiencies, by 800 examinations
Testing rear coulombic efficiency has 91%, and coulombic efficiency still has 82% after 1500 times.
10% silica is added in graphite material, may make the specific capacity of graphite cathode material by limiting value
372mAh/g is improved to 550mAh/g, improves 48% compared to traditional graphite cathode material capacity, energy density is theoretically achievable
300Wh/kg。
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other drawings based on these drawings.
Fig. 1 is silicon-carbon cathode material atomic diagram in the present invention；
Fig. 2 is that 3D porous silica material cavernous structure of the present invention forms schematic diagram.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment one:
The preparation process of the silicon-carbon cathode material of the embodiment, including following sequential steps
S1. silica is a kind of nonmetallic amorphous material, and with high-purity, partial size is small, is evenly distributed, specific surface area
Greatly, the features such as high surface, and it is nontoxic, tasteless, the silicon oxide particle of diameter 200nm is uniformly mixed to get with aluminium powder
Mixture A；
S2. thermite reaction is used, obtained mixture A is put into tube furnace, under the protection of argon gas, 720 DEG C
Roasting 5 hours, obtains product B；
Thermite reaction is as follows:
S3. product B is persistently stirred 6 hours in the hydrochloric acid of concentration 1%, is removed without the aluminium of reaction, obtain product C；
It chemically reacts as follows: Al+HCl → Al Cl3+H2↑
S4. product C is reacted 10 hours in hafnium solution, is removed without the silica of reaction, obtained with 3D honeycomb
The silicon materials D of porous framework structure, as shown in Fig. 2, being the formation schematic diagram of the 3D honeycomb porous material；
S5. porous silica material D and graphite are merged according to the ratio of molar ratio 1:9, graphite particle is according to 5 microns, 9
Two kinds of partial size equal proportions of micron are added, and coat one layer of graphite on the surface of the porous silica material D using mechanofusion method, pass through
Electronics surface sweeping microscope SEM shows that, by above-mentioned reaction process, the graphite material of two kinds of different-grain diameters uniformly incorporates honeycomb
In porous framework structure, silicon-carbon cathode material is obtained, as shown in Figure 1, being the atomic diagram of silicon-carbon cathode material.
Embodiment two:
The preparation process of the silicon-carbon cathode material of the embodiment, including following sequential steps
S1. silica is a kind of nonmetallic amorphous material, and with high-purity, partial size is small, is evenly distributed, specific surface area
Greatly, the features such as high surface, and it is nontoxic, tasteless, the silicon oxide particle of diameter 200nm is uniformly mixed to get with aluminium powder
Mixture A；
S2. thermite reaction is used, obtained mixture A is put into tube furnace, under the protection of argon gas, 720 DEG C
Roasting 5 hours, obtains product B；
S3. product B is persistently stirred 7 hours in the hydrochloric acid of concentration 1%, is removed without the aluminium of reaction, obtain product C；
S4. product C is reacted 11 hours in hafnium solution, is removed without the silica of reaction, obtained with 3D honeycomb
The silicon materials D of porous framework structure；
S5. porous silica material D and graphite are merged according to the ratio of molar ratio 1:9, graphite particle is according to 5 microns, 9
Two kinds of partial size equal proportions of micron are added, and coat one layer of graphite on the surface of the porous silica material D using mechanofusion method, pass through
Electronics surface sweeping microscope SEM shows that, by above-mentioned reaction process, the graphite material of two kinds of different-grain diameters uniformly incorporates honeycomb
In porous framework structure, silicon-carbon cathode material is obtained,
Embodiment three:
The preparation process of the silicon-carbon cathode material of the embodiment, including following sequential steps
S1. silica is a kind of nonmetallic amorphous material, and with high-purity, partial size is small, is evenly distributed, specific surface area
Greatly, the features such as high surface, and it is nontoxic, tasteless, the silicon oxide particle of diameter 200nm is uniformly mixed to get with aluminium powder
Mixture A；
S2. thermite reaction is used, obtained mixture A is put into tube furnace, under the protection of argon gas, 720 DEG C
Roasting 5 hours, obtains product B；
S3. product B is persistently stirred 8 hours in the hydrochloric acid of concentration 1%, is removed without the aluminium of reaction, obtain product C；
S4. product C is reacted 12 hours in hafnium solution, is removed without the silica of reaction, obtained with 3D honeycomb
The silicon materials D of porous framework structure；
S5. porous silica material D and graphite are merged according to the ratio of molar ratio 1:9, graphite particle is according to 5 microns, 9
Two kinds of partial size equal proportions of micron are added, and coat one layer of graphite on the surface of the porous silica material D using mechanofusion method, pass through
Electronics surface sweeping microscope SEM shows that, by above-mentioned reaction process, the graphite material of two kinds of different-grain diameters uniformly incorporates honeycomb
In porous framework structure, silicon-carbon cathode material is obtained,
By experiments have shown that: in graphite cathode material be added 10% silica, circulation 800 times after still have
The capacity of 506mAh/g, capacity retention ratio 92%, the coulombic efficiency in cyclic process reach 98.8%.
Therefore, the preparation process of silicon-carbon cathode material of the invention can effectively improve the energy density of battery, circulation benefit
With number, shorten the charging time, improve charge efficiency, there is good practicability.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (4)
1. the preparation process of silicon-carbon cathode material, it is characterised in that: including following sequential steps
S1. it carries out the silicon oxide particle of diameter 200nm and aluminium powder to be uniformly mixed to get mixture A；
S2. thermite reaction is used, obtained mixture A is put into tube furnace, under the protection of argon gas, 720 DEG C of roastings 5
Hour, obtain product B；
Thermite reaction is as follows:
S3. responseless aluminium in product B is removed with the hydrochloric acid of concentration 1%, obtains product C；
It chemically reacts as follows: Al+HCl → AlCl3+H2↑
S4. using responseless silica in hafnium solution removal product C, the silicon materials with 3D honeycomb multicellular frame are obtained
Carrier of the D as graphite particle；
S5. the porous silica material D and graphite are merged according to the ratio of molar ratio 1:9, graphite particle is according to 5 microns, 9
Two kinds of partial size equal proportions of micron are added, so that the surface of porous silica material D coats one layer of graphite, obtain silicon-carbon cathode material.
2. the preparation process of silicon-carbon cathode material as described in claim 1, it is characterised in that: in the step S3
S31. product B is persistently stirred 6-8 hours in the hydrochloric acid of concentration 1%, is removed without the aluminium of reaction, obtain product C.
3. the preparation process of silicon-carbon cathode material as described in claim 1, it is characterised in that: in the step S4
S41. product C is reacted 10-12 hours in hafnium solution, is removed without the silica of reaction, obtained with 3D honeycomb
The silicon materials D of porous framework.
4. the preparation process of silicon-carbon cathode material as described in claim 1, it is characterised in that: in the step S5
S51. one layer of graphite is coated on the surface of the porous silica material D using mechanofusion method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811540091.2A CN109659529A (en) | 2018-12-17 | 2018-12-17 | A kind of preparation process of silicon-carbon cathode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112582593A (en) * | 2020-12-14 | 2021-03-30 | 绍兴小竹新能源有限公司 | Preparation method of porous silicon/carbon composite material and application of porous silicon/carbon composite material as negative electrode of lithium ion battery |
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Application publication date: 20190419 |