CN109860579A - A kind of negative electrode material and preparation method thereof with core-shell structure - Google Patents
A kind of negative electrode material and preparation method thereof with core-shell structure Download PDFInfo
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- CN109860579A CN109860579A CN201910260817.5A CN201910260817A CN109860579A CN 109860579 A CN109860579 A CN 109860579A CN 201910260817 A CN201910260817 A CN 201910260817A CN 109860579 A CN109860579 A CN 109860579A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The negative electrode material and preparation method thereof with core-shell structure that the present invention provides a kind of.The negative electrode material has core-shell structure, using SiO and/or Si as center core, using carbon material as buffer layer, using alumina material as shell.The present invention also provides the preparation methods of above-mentioned negative electrode material.The capacity retention ratio of negative electrode material of the invention is high, good cycle.
Description
Technical field
The negative electrode material of lithium ion battery and preparation method thereof with core-shell structure that the present invention relates to a kind of, belong to lithium from
Sub- battery technology field.
Background technique
Lithium ion battery is big with its specific energy, operating voltage is high, self-discharge rate is small, the advantages such as small in size, light-weight, from it
Since birth, revolutionary variation just has been brought to energy storage field, is widely used in various portable electronic devices and electronic
In automobile.However as the improvement of people's living standards, more stringent requirements are proposed to lithium ion battery for higher user experience:
Quality is lighter, longer etc. using the time；More excellent performance of electrode material is had to look for solve the above-mentioned problems.
Current commercialized ion cathode material lithium is mainly graphite, but its theoretical capacity is only 372mAh/g, cannot
Meet the urgent need of user, therefore, the exploitation of the negative electrode material of more height ratio capacity is extremely urgent.
As lithium ion battery negative material, silicon materials are had been a concern.Its theoretical capacity is 4200mAh/g, has been
10 times or more of commercialized graphite capacity, and there is low intercalation potential, low atomic wts, high-energy density, price more just
Preferably, the advantages such as environmental-friendly, therefore be one of the optimal selection of high-capacity cathode material of new generation.However, silicon is in de-, embedding lithium
There are huge volume change and surface that cannot form stable solid electrolyte film in the process, capacity is caused to decline rapidly with circulation
Subtract, the problem that coulombic efficiency is not high, seriously hinders its large-scale commercial application.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide one kind to inhibit silicon materials to expand, circulation
The negative electrode material of the lithium ion battery of better performances.
In order to achieve the above technical purposes, present invention firstly provides a kind of negative electrode material, which has nucleocapsid
Structure, wherein using SiO and/or Si as center core, using carbon material as buffer layer, using alumina material as shell.
Negative electrode material of the invention is acted synergistically by carbon material buffer layer and alumina case, is led improving negative electrode material
While electrical, for negative electrode material, the variation of structure and volume also functions to certain buffer function in charge and discharge, makes to have
The negative electrode material of core-shell structure has excellent high rate performance and cyclical stability.
In order to achieve the above technical purposes, invention further provides a kind of preparation sides of negative electrode material with core-shell structure
Method, the preparation method the following steps are included:
Prepare chitosan-acetic acid-aqueous solution, wherein the mass ratio of chitosan and water be 0.5:100-5:100, acetic acid with
The mass ratio of water is 0.5:100-5:100；
Chitosan-acetic acid-aqueous solution is mixed with silicon materials, the surface of silicon materials is made to coat one layer of chitosan-acetic acid-water
Solution；Wherein, silicon materials and chitosan-acetic acid-aqueous solution mass ratio are 0.5:1-2:1；
It is coated with chitosan-acetic acid-aqueous solution silicon materials and alumina powder carries out mixing and ball milling, obtain core-shell structure copolymer
Silicon materials；Wherein, the mass ratio of silicon materials and alumina powder is 1:5-1:10；
Core-shell structure copolymer silicon materials are subjected to high temperature cabonization under protective atmosphere, pulverization process is carried out after natural cooling, is had
The negative electrode material of core-shell structure.
Preparation method of the invention on the surface of matrix silicon materials uniformly wraps a layer binder, and (chitosan-acetic acid-is water-soluble
Liquid)；It is then placed in alumina powder and is uniformly mixed, centrifugal force when being rotated using ball milling makes silicon materials be squeezed and glue
The collective effect for tying the viscous force of agent promotes silicon materials surface to form one layer of close alumina layer；In being made again by high-temperature calcination
Between adhesive layer formed conductive carbon material buffer layer.Conductive carbon material buffer layer while improving negative electrode material electric conductivity,
For negative electrode material, the variation of structure and volume also functions to certain buffer function in charge and discharge, at the same with the height that closely coats
The shell structure aluminium oxide collective effect of stability, the negative electrode material with core-shell structure made have excellent electrochemistry
Energy and cyclical stability.
Preparation method of the invention includes the steps that preparing chitosan-acetic acid-aqueous solution.Wherein, chitosan-second is prepared
When acid-aqueous solution, the mass ratio of chitosan and water is 0.5:100-5:100, and the mass ratio of acetic acid and water is 0.5:100-5:
100。
In the preparation process in accordance with the present invention, using chitosan-acetic acid-aqueous solution as raw material, on the one hand, it is as carbon source
It is added, after high temperature cabonization, carbon buffer layer can be formed；On the other hand, chitosan-acetic acid-aqueous solution has distinctive
Viscosity can prepare close alumina case structure.
In a specific embodiment of the invention, chitosan, acetic acid, water are directly mixed, chitosan-second can be obtained
Acid-aqueous solution.
Preparation method of the invention includes uniformly coating one layer of chitosan-acetic acid-aqueous solution step on the surface of silicon materials
Suddenly.
In a specific embodiment of the invention, the silicon materials used can be SiO and/or Si.
Preparation method of the invention include be coated with chitosan-acetic acid-aqueous solution silicon materials and alumina powder into
Row mixing and ball milling, the step of obtaining core-shell structure copolymer silicon materials.Centrifugal force when being rotated using ball milling is squeezed silicon materials and shell
The collective effect of glycan-acetic acid-aqueous solution viscous force promotes material surface to form one layer of aluminium oxide completely coating, close
Layer.
Using the synergistic effect of high stable, corrosion resistant alumina powder and carbon buffer layer, mentioning conductive carbon material
While high negative electrode material electric conductivity, to negative electrode material, the variation of structure and volume also functions to certain delay in charge and discharge process
Punching effect, in conjunction with aluminium oxide shell structure, can control the structure change of silicon materials, volume expansion in charge and discharge process, improve
The chemical property and cyclical stability of negative electrode material.
In a specific embodiment of the invention, the revolving speed of ball milling is 5r/s-30r/s.For example, the revolving speed of ball milling can be with
For 10r/s, 15r/s, 20r/s, 25r/s etc..
In a specific embodiment of the invention, the time of ball milling is 1h-10h.For example, the time of ball milling can be
2h、3h、4h、5h、6h、7h、8h、9h。
In a specific embodiment of the invention, nanometer alpha-that the alumina powder used is 99.99% for purity
Alumina powder.
Preparation method of the invention includes that core-shell structure copolymer silicon materials are carried out to high temperature cabonization under protective atmosphere, is prepared after cooling
The step of obtaining the negative electrode material with core-shell structure.Intermediate carbon material buffer layer can be directly obtained by high temperature cabonization.
In the preparation process in accordance with the present invention, carbon materials be can control by adjusting the temperature of high temperature cabonization, heating rate and time
Thickness, structure and residual quantity of material etc..
In a specific embodiment of the invention, high temperature cabonization is warming up to the rate of 2 DEG C/min-10 DEG C/min
300 DEG C of -900 DEG C of carbonization 1h-6h.
In a specific embodiment of the invention, the flow velocity of protective atmosphere is 0.2L/min-1L/min.For example, protection
The flow velocity of atmosphere is 0.3L/min, 0.4L/min, 0.5L/min, 0.6L/min, 0.7L/min, 0.8L/min, 0.9L/min.
It, can be using one or more of nitrogen, argon gas and helium in a specific embodiment of the invention
Gas of the combination as protective atmosphere.
Preparation method of the invention is by carbon buffer layer and the synergistic effect of aluminium oxide shell structure, the silicon-based anode made
Material has more stable surface texture in de-, process of intercalation, and capacity retention ratio is high, good cycle.
The simple process of preparation method of the invention, it is easy to operate, it is easy to automation control, it is at low cost, it is suitble to industrialization
Production.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
A kind of aluminium oxide/silicon-carbon composite cathode material with core-shell structure is present embodiments provided, is by following
What step was prepared:
(1) ingredient
By chitosan: water is the mass ratio of 0.5:100, acetic acid: water is the mass ratio of 0.5:100, take chitosan, acetic acid,
Water is hybridly prepared into chitosan-acetic acid-aqueous solution；
(2) core-shell structure copolymer silicon structure is prepared
According to silicon materials: chitosan-acetic acid-aqueous solution is the mass ratio of 0.5:1, and silicon materials: alumina powder is 1:5's
Mass ratio takes silicon materials and alumina powder；Wherein silicon materials are to aoxidize sub- silicon, and alumina powder is that purity is 99.99%
Nanoscale alpha-alumina powder；Silicon materials, chitosan-acetic acid-aqueous solution are mixed evenly, apply silicon materials surface uniformly
Cover one layer of chitosan-acetic acid-aqueous solution；It is coated with chitosan-acetic acid-aqueous solution silicon materials again and alumina powder is put into
Ball milling is carried out in ball-milling device, with the revolving speed rotation cladding 6h of 10r/s, surface is made after drying and is completely coated with alumina powder
Core-shell structure copolymer silicon materials；
(3) high temperature cabonization
Above-mentioned core-shell structure copolymer silicon materials are placed in tube furnace, in the case where flow velocity is 0.2L/min nitrogen protection with the liter of 5 DEG C/min
Warm rate rises to 900 DEG C, keeps the temperature 1h；Pulverization process is carried out after natural cooling, obtains having aluminium oxide/silicon-carbon of core-shell structure multiple
Close negative electrode material.
It can be carried out following test to the electrochemistry of the present embodiment:
The chemical property of negative electrode material is studied using button cell, cathode is using deionized water as solvent, pole piece
Raw material are as follows:
Active material: SP:CMC:SBR=85:5:5:5 mixture is modulated into the slurry that solid content is 45%
Then slurry even application is put into baking oven on copper foil, 80 DEG C of vacuum drying 12h, taking-up carries out slice roller
Pressure, then 80 DEG C of vacuum drying 12h, obtained experimental cell pole piece.
Using metal lithium sheet as to electrode, electrolyte 1.0mol/LLiPF6EC and DMC (volume ratio 1:1) it is molten
Liquid, diaphragm are celgard2000 film, are assembled into CR2016 type button cell in the glove box full of argon atmosphere.
Carry out charge and discharge cycles test to the button cell: charge and discharge blanking voltage is 0.005-1.5V, charge-discharge magnification
For 0.1C.Finally, coulombic efficiency is 95.1% for the first time, taking off lithium specific capacity for the first time is 452mAh/g.Capacity is kept after circulation 100 times
Rate is 95.8%.
Embodiment 2
A kind of aluminium oxide/silicon-carbon composite cathode material with core-shell structure is present embodiments provided, is by following
What step was prepared:
(1) ingredient
By chitosan: water is the mass ratio of 2:100, acetic acid: water is the mass ratio of 5:100, takes chitosan, acetic acid, water mixed
Conjunction is configured to chitosan-acetic acid-aqueous solution；
(2) core-shell structure copolymer silicon structure is prepared
According to silicon materials: chitosan-acetic acid-aqueous solution is the mass ratio of 1:1, and silicon materials: alumina powder is 1:10's
Mass ratio takes silicon materials and alumina powder；Wherein silicon materials are nano silica fume；By silicon materials, chitosan-acetic acid-aqueous solution
It is mixed evenly, silicon materials surface is made uniformly to coat one layer of chitosan-acetic acid-aqueous solution；It is coated with chitosan-second again
Ball milling in acid-aqueous solution silicon materials and alumina powder investment ball-milling device, with the revolving speed rotation cladding 1h of 20r/s, drying
The core-shell structure copolymer silicon materials that surface is completely coated with alumina powder are made afterwards；
(3) high temperature cabonization
Above-mentioned core-shell structure copolymer silicon materials are placed in tube furnace, in the case where flow velocity is 0.5L/min nitrogen protection with the liter of 8 DEG C/min
Warm rate rises to 700 DEG C, keeps the temperature 3h；Pulverization process is carried out after natural cooling, obtains having aluminium oxide/silicon-carbon of core-shell structure multiple
Close negative electrode material.
Lithium ion battery such as embodiment 1 is prepared for using the negative electrode material of the present embodiment, and has been carried out such as embodiment 1
Performance test.Wherein, coulombic efficiency is 86.2% for the first time, and taking off lithium specific capacity for the first time is 425mAh/g.Capacity is protected after circulation 100 times
Holdup is 85.6%.
Embodiment 3
A kind of aluminium oxide/silicon-carbon composite cathode material with core-shell structure is present embodiments provided, is by following
What step was prepared:
(1) ingredient
By chitosan: water is the mass ratio of 5:100, acetic acid: water is the mass ratio of 2:100, takes chitosan, acetic acid, water mixed
Conjunction is configured to chitosan-acetic acid-aqueous solution；
(2) core-shell structure copolymer silicon structure is prepared
According to silicon materials: chitosan-acetic acid-aqueous solution is the mass ratio of 2:1, and silicon materials: alumina powder is 1:10's
Mass ratio takes silicon materials and alumina powder；Wherein silicon materials are the mixture for aoxidizing sub- silicon and nano silica fume, aoxidize sub- silicon:
The mass ratio of nano silica fume is that silicon materials, chitosan-acetic acid-aqueous solution are mixed evenly 0.5:1, keeps silicon materials surface equal
One layer of chitosan-acetic acid-aqueous solution of even coating；It is coated with chitosan-acetic acid-aqueous solution silicon materials and alumina powder again
Ball milling in ball-milling device is put into, with the revolving speed rotation cladding 2h of 30r/s, surface is made after drying and is completely coated with alumina powder
Core-shell structure copolymer silicon materials；
(3) high temperature cabonization
Above-mentioned core-shell structure copolymer silicon materials are placed in tube furnace, in the case where flow velocity is the protection of 1L/min argon gas with the heating of 5 DEG C/min
Rate rises to 300 DEG C, keeps the temperature 6h；Pulverization process is carried out after natural cooling, obtains having aluminium oxide/silicon-carbon of core-shell structure compound
Negative electrode material.
Lithium ion battery such as embodiment 1 is prepared for using the negative electrode material of the present embodiment, and has been carried out such as embodiment 1
Performance test.Wherein, coulombic efficiency is 91.5% for the first time, and taking off lithium specific capacity for the first time is 411mAh/g.Capacity is protected after circulation 100 times
Holdup is 90.1%.
Embodiment 4
A kind of aluminium oxide/silicon-carbon composite cathode material with core-shell structure is present embodiments provided, is by following
What step was prepared:
(1) ingredient
By chitosan: water is the mass ratio of 0.5:100, acetic acid: water is the mass ratio of 0.5:100, take chitosan, acetic acid,
Water is hybridly prepared into chitosan-acetic acid-aqueous solution；
(2) core-shell structure copolymer silicon structure is prepared
According to silicon materials: chitosan-acetic acid-aqueous solution is the mass ratio of 0.5:1, and silicon materials: alumina powder is 1:5's
Mass ratio takes silicon materials and alumina powder；Wherein silicon materials are to aoxidize sub- silicon, and the mixture of nano silica fume aoxidizes sub- silicon: receiving
The mass ratio of rice silicon powder is 1:1, and silicon materials, chitosan-acetic acid-aqueous solution are mixed evenly, keep silicon materials surface uniform
Coat one layer of chitosan-acetic acid-aqueous solution；It is coated with chitosan-acetic acid-aqueous solution silicon materials again and alumina powder is thrown
Enter ball milling in ball-milling device, with the revolving speed rotation cladding 10h of 5r/s, surface is made after drying and is completely coated with alumina powder
Core-shell structure copolymer silicon materials；
(3) high temperature cabonization
Above-mentioned core-shell structure copolymer silicon materials are placed in tube furnace, in the case where flow velocity is the protection of 0.5L/min helium with the liter of 2 DEG C/min
Warm rate rises to 500 DEG C, keeps the temperature 2h；Pulverization process is carried out after natural cooling, obtains having aluminium oxide/silicon-carbon of core-shell structure multiple
Close negative electrode material.
Lithium ion battery such as embodiment 1 is prepared for using the negative electrode material of the present embodiment, and has been carried out such as embodiment 1
Performance test.Wherein, coulombic efficiency is 93.0% for the first time, and taking off lithium specific capacity for the first time is 655mAh/g.Capacity is protected after circulation 100 times
Holdup is 94.5%.
Claims (10)
1. a kind of negative electrode material, which is characterized in that the negative electrode material has core-shell structure, wherein centered on SiO and/or Si
Core, using carbon material as buffer layer, using alumina material as shell.
2. a kind of preparation method of negative electrode material described in claim 1, which is characterized in that the preparation method includes following step
It is rapid:
Prepare chitosan-acetic acid-aqueous solution, wherein the mass ratio of chitosan and water is 0.5:100-5:100, acetic acid and water
Mass ratio is 0.5:100-5:100；
Chitosan-the acetic acid-aqueous solution is mixed with silicon materials, the surface of silicon materials is made to coat one layer of chitosan-acetic acid-water
Solution；Wherein, the mass ratio of the silicon materials and the chitosan-acetic acid-aqueous solution is 0.5:1-2:1；
It is coated with chitosan-acetic acid-aqueous solution silicon materials and alumina powder carries out mixing and ball milling, obtain core-shell structure copolymer silicon material
Material；Wherein, the mass ratio of the silicon materials and the alumina powder is 1:5-1:10；
Under protective atmosphere, high temperature cabonization is carried out to the core-shell structure copolymer silicon materials, natural cooling obtains having the negative of core-shell structure
Pole material.
3. preparation method according to claim 2, which is characterized in that the high temperature cabonization is with 2 DEG C/min-10 DEG C/min
Rate be warming up to 300 DEG C of -900 DEG C of carbonization 1h-6h.
4. preparation method according to claim 2, which is characterized in that the revolving speed of the ball milling is 5r/s-30r/s.
5. preparation method according to claim 2, which is characterized in that the time of the ball milling is 1h-10h.
6. preparation method according to claim 2, which is characterized in that the silicon materials are SiO and/or Si.
7. preparation method according to claim 2, which is characterized in that the alumina powder is that purity is 99.99%
Alpha-alumina powder.
8. preparation method according to claim 7, which is characterized in that the alpha-alumina powder is nanoscale alpha-oxidation
Aluminium powder body.
9. preparation method according to claim 2, which is characterized in that the flow velocity of the protective atmosphere is 0.2L/min-1L/
min。
10. preparation method according to claim 2, which is characterized in that the protective atmosphere is in nitrogen, argon gas and helium
A combination of one or more.
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| CN110265640A (en) * | 2019-06-11 | 2019-09-20 | 上海大学 | A method of preparing electrode of lithium cell carbon coating porous silica material |
| CN111900368A (en) * | 2020-07-24 | 2020-11-06 | 陕西煤业化工技术研究院有限责任公司 | Lithium ion battery-grade silicon monoxide negative electrode material, and preparation method and application thereof |
| WO2022205667A1 (en) * | 2021-03-30 | 2022-10-06 | 万向一二三股份公司 | Silicon-based negative electrode material, and preparation method therefor and application thereof |
| CN117712359A (en) * | 2024-02-06 | 2024-03-15 | 深圳索理德新材料科技有限公司 | Double-shell silicon-carbon composite anode material and preparation method and application thereof |
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