CN108807892A - A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material - Google Patents
A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material Download PDFInfo
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- CN108807892A CN108807892A CN201810572978.3A CN201810572978A CN108807892A CN 108807892 A CN108807892 A CN 108807892A CN 201810572978 A CN201810572978 A CN 201810572978A CN 108807892 A CN108807892 A CN 108807892A
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- silicon
- sodium chloride
- negative pole
- nanometer sheet
- lithium cell
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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
- H01M4/364—Composites as mixtures
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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
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation methods of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, specifically comprise the steps of：By certain mass than nano-silicon and sodium chloride carry out ball milling, obtain sodium chloride and silica flour is sufficiently mixed object；Certain pitch carbon source is added later, continues ball milling certain time；Pitch, nano-silicon, sodium chloride are sufficiently mixed object, at 780 ~ 850 DEG C and argon gas protection 1 ~ 3 h of lower charing, obtain the mixture of silicon-carbon nanosheet composite material and sodium chloride；Suitable water is added in said mixture to be washed, filter, silicon-carbon nanosheet composite material is obtained after vacuum dried.The invention has the advantages of low raw material cost, abundance, and preparation process is simple, and template is easily recycled and green non-pollution, and silicon-carbon nanometer sheet has good multiplying power and cycle performance for lithium cell negative pole material, while also meeting requirement of the high-capacity battery to electrode material.
Description
Technical field
The present invention relates to lithium cell negative pole material technical fields, and in particular to arrives a kind of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole
The preparation method of material.
Background technology
Lithium ion battery is because it is high with operating voltage, have extended cycle life, memory-less effect, self discharge effect are small and environment
The advantages that friendly, is widely used in the mobile electronic devices such as mobile phone, laptop, digital camera, in Medical Devices, electricity
The related fields such as electrical automobile also play an important role.And important composition one of of the negative material as lithium ion battery, it is right
Its electrology characteristic has irreplaceable role.
Currently, graphite is most ripe lithium cell negative pole material, however due to its theoretical specific capacity（372 mAh/g）Exploitation is
Close to theoretical value, it has been difficult to meet the needs of market is to large capacity, high power and inexpensive battery.Silicon naturally enrich, environment
It is friendly and with very high theoretical lithium storage content（3587 mAh/g, 25 DEG C）, become most promising instead of conventional graphite
Material.But silicon（Si）When as negative material, because conductive（<10-3S/cm, 25 DEG C）Poor and big bulk effect（>
270%）And it is difficult to be widely applied.Therefore, Many researchers are proposed silicon nanosizing or Composite, to improve silicon as bearing
The defect of pole material.Wherein, it is considered as a kind of more effective path for solving silicon volume expansion by silicon Composite.Currently, having
Many materials can be compound with silicon, such as Carbon materials（Such as carbon nanotube, mesocarbon microspheres, unformed charcoal）And non-carbon material
（Such as magnesium, silver）.What wherein application was most is carbon material.
Patent CN107346820A reports a kind of composite negative pole material and preparation method thereof of three-dimensional porous carbon package silicon.
The mixture of starch, sodium hydroxide and water is coated on carbon cloth by the invention first, through drying, is calcined, after salt acid elution to obtain the final product
To the carbon cloth with three-dimensional porous carbon-coating, the carbon cloth of three-dimensional porous carbon-coating and the alcoholic solvent containing nano-silicon are subjected to hydro-thermal later
The composite negative pole material that three-dimensional porous carbon wraps up silicon is obtained after reaction, then washed, drying.Patent CN107785560A is a kind of high
The preparation method of performance silicon-carbon cathode material uses what liquid phase ball-milling method obtained nano-silicon and graphite to be sufficiently mixed object first,
Pitch is added after drying-granulating, is granulated through the broken Composite for realizing graphite/nano-silicon/pitch of kneading-compacting-, finally again
Through mechanical fusion, be carbonized, break up, sieve after to get to a kind of high performance silicon-carbon cathode material.Patent CN107749474A mono-
The preparation method and the silicon-carbon cathode material of kind of silicon-carbon cathode material, using ionic liquid or with other organic matters（Such as pitch, Portugal
Grape sugar, starch, sucrose etc.）It coats to obtain Si-C composite material in conjunction with high temperature pyrolysis is carried out to silicon.Although these above-mentioned method energy
Enough performances for improving silicium cathode material to a certain extent, but preparation process is relatively complicated, high expensive, equipment requirement
Harshness, batch production is difficult, is difficult to scale volume production.
For the present invention using sodium chloride as template, pitch is carbon source, prepares a kind of silicon-carbon nanosheet composite material.In material
In preparation process, template is easily recycled and cheap, used carbon source abundance and at low cost.
Invention content
The present invention proposes a kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, to be easily recycled, green
The sodium chloride of color is template, pitch is carbon source, is prepared a kind of with height ratio capacity, good high rate performance and Gao Shouxiao
Silicon-carbon nanosheet composite material, with this, to solve, volume change of the single silicon for generating during lithium cell negative pole be big and cyclicity
Can be poor the problems such as.
Realize the technical scheme is that：A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, packet
Include following steps：
（1）Nano-silicon and sodium chloride are subjected to ball milling, at 100 ~ 300 r/min of rotating speed, 2 ~ 4 h of ball milling, obtain sodium chloride with
Silicon is sufficiently mixed object, and pitch is added later, and what 2 ~ 4 h of ball milling obtained pitch, silicon and sodium chloride three again is sufficiently mixed object；
（2）Under gas shield, to step（1）The object that is sufficiently mixed for obtaining pitch, silicon and sodium chloride carries out charing process,
Obtain the mixture of silicon-carbon nanosheet composite material and sodium chloride；
（3）To step（2）In the mixture of obtained silicon-carbon nanosheet composite material and sodium chloride be added water washed, mistake
Filter, it is vacuum dried after obtain silicon-carbon nanosheet composite material.
The step（1）Middle pitch is asphalt, and 85 ~ 120 DEG C of softening point, toluene and quinoline insolubles are respectively less than 1 %.
The step（1）The particle size range of middle nano-silicon is 10 ~ 100 nm.
The step（1）Middle sodium chloride purity is more than 99%.
The step（1）The mass ratio of middle nano-silicon, pitch and sodium chloride is 1:（5-20）：（100-300）.
The step（2）In carbonization temperature be 780 ~ 850 DEG C, heating rate be 4 ~ 7 DEG C/min, carbonization time be 1 ~
3 h, protective gas are argon gas or nitrogen, 20 ~ 100 mL/min of flow velocity.
The step（3）Middle vacuum drying time is 12 ~ 24 h, and absolute pressure is 133 ~ 500 Pa, and temperature is 60 ~ 90
℃。
The step（4）Middle filtrate is evaporated under the conditions of 100 ~ 150 DEG C of heating temperature, and obtained sodium chloride continues to use
In step（1）In.
By step（3）The silicon-carbon nanometer sheet of acquisition is 8 in mass ratio with Kynoar, conductive agent acetylene black:1:1 is added
Into ball grinder, suitable N-Methyl pyrrolidone is added, 2 h are mixed with the ball milling speed of 150 r/min；It uniformly applies later
It applies on copper foil, 24 h is dried in vacuo at 80 DEG C, experimental cell pole piece is prepared after taking-up.
The beneficial effects of the invention are as follows：
（1）Template sodium chloride derives from a wealth of sources, cheap and be easily recycled, and not can cause environmental pollution.
（2）Asphalt source is abundant, cheap.
（3）Silicon-carbon nanometer sheet preparation process is simple, is easy to industrialized production.
（4）Silicon-carbon nanometer sheet has preferably high rate performance and good cycle performance as lithium cell negative pole material.
Description of the drawings
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 technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Obtain other attached drawings according to these attached drawings.
Fig. 1 is the stereoscan photograph of silicon charcoal nanometer sheet prepared by the embodiment of the present invention 1.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
The every other embodiment that those of ordinary skill in the art are obtained under the premise of not making the creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, is mainly made of following steps：
50 mg grain sizes are taken to be added in ball grinder for the silica flour of 50 nm and 5 g sodium chloride, under conditions of 100 r/min of rotating speed
4 h of ball milling；The asphalt of 1.0 g is added later, continues 4 h of ball milling to get filling to nano-silicon, sodium chloride and pitch three
Divide mixture；By in the mixture merging retort after ball milling, 850 DEG C are warming up to the rate of 7 DEG C/min, is protected in argon gas
1 h of the lower constant temperature of shield；After natural cooling, the deionized water of the product after charing is fully washed 3 times, through filtering, being dried in vacuo
Later to get to silicon-carbon nanometer sheet negative material.
The electromicroscopic photograph of silicon-carbon nanometer sheet negative material prepared by the present embodiment is as shown in Figure 1, it can be seen that nano-silicon
The uniform inside for being embedded into nanometer sheet.Silicon-carbon nanometer sheet in the embodiment is pressed with Kynoar, conductive agent acetylene black
Mass ratio is 8:1:1 is added in ball grinder, adds suitable N-Methyl pyrrolidone, 150 r/min's of ball milling speed
Under the conditions of mix 2 h and reach uniform state, even application is dried in vacuo 24 h at 80 DEG C, is made after taking-up on copper foil later
Standby experimental cell pole piece.
In the glove box full of argon gas, the electrode slice with above-mentioned preparation is working electrode, and lithium piece is used as to electrode, assembling
At lithium ion button shape cell.The battery first discharge specific capacity 1132 mAh/g, 807 mAh/g of initial charge specific capacity, for the first time
71.2 % of coulombic efficiency, its capacity retention ratio is 87 % after 50 circles are recycled under conditions of 300 mA/g of current density.Battery has
There is good multiplying power property curve.
Embodiment 2
A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, is mainly made of following steps：
40 mg grain sizes are taken to be added in ball grinder for the silica flour of 15 nm and 12 g sodium chloride, in the condition of 100 r/min of rotating speed
Lower 3 h of ball milling；The asphalt of 0.2 g is added later, continues 3 h of ball milling；It will obtain nano-silicon, sodium chloride and pitch three
The object that is sufficiently mixed move in retort, be warming up to 780 DEG C with the rate of 6 DEG C/min, 2 h of the lower constant temperature of argon gas protection；It waits for certainly
After so cooling, the deionized water of the product after charing fully wash 3 times, through filtering, being dried in vacuo 24 h later to get to silicon
Carbon nanosheet negative material.
The assembling process of battery pole piece and battery is same as Example 1.1140 mAh/ of first discharge specific capacity of the battery
G, 677 mAh/g of initial charge specific capacity, 59.3 % of coulombic efficiency, recycles under conditions of 300 mA/g of current density for the first time
Its capacity hardly happens variation after 120 circles.
Embodiment 3
A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, is mainly made of following steps：
25 mg grain sizes are taken to be added in ball grinder for the silica flour of 50 nm and 6 g sodium chloride, under conditions of 200 r/min of rotating speed
2 h of ball milling；The asphalt of 0.5 g is added later, continues 3 h of ball milling；It will obtain nano-silicon, sodium chloride and pitch three
It is sufficiently mixed object to move in retort, is warming up to 820 DEG C with the rate of 5 DEG C/min, 3 h of the lower constant temperature of argon gas protection；Wait for nature
After cooling, the deionized water of the product after charing is fully washed 3 times, through filtering, being dried in vacuo after 24 h to get to silicon-carbon
Nanometer sheet negative material.
The assembling process of battery pole piece and battery is the same as embodiment 1.932 mAh/g of first discharge specific capacity of the battery, it is first
701 mAh/g of secondary charge specific capacity, for the first time 75.2 % of coulombic efficiency, after 50 circles are recycled under conditions of 300 mA/g of current density
Its capacity retention ratio is 90 %.
Embodiment 4
A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, is mainly made of following steps：
75 mg grain sizes are taken to be added in ball grinder for the silica flour of 50 nm and 10 g sodium chloride, in the condition of 150 r/min of rotating speed
Lower 2 h of ball milling；The asphalt of 0.6 g is added later, continues 4 h of ball milling；It will obtain nano-silicon, sodium chloride and pitch three
The object that is sufficiently mixed move in retort, be warming up to 800 DEG C with the rate of 4 DEG C/min, 3 h of the lower constant temperature of argon gas protection；It waits for certainly
After so cooling, the deionized water of the product after charing fully wash 3 times, through filtering, being dried in vacuo 24 h later to get to silicon
Carbon nanosheet negative material.
The assembling process of battery pole piece and battery is same as Example 1.1490 mAh/ of first discharge specific capacity of the battery
G, 1032 mAh/g of initial charge specific capacity, 69.3 % of coulombic efficiency, recycles under conditions of 300 mA/g of current density for the first time
Its capacity retention ratio is 83% after 50 circles.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (8)
1. a kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material, it is characterised in that include the following steps：
Nano-silicon and sodium chloride are subjected to ball milling, obtain sodium chloride and silicon is sufficiently mixed object, pitch is added later, again ball milling
Obtain pitch, silicon and sodium chloride three is sufficiently mixed object；
Under gas shield, to step（1）The object that is sufficiently mixed for obtaining pitch, silicon and sodium chloride carries out charing process, obtains
To the mixture of silicon-carbon nanosheet composite material and sodium chloride；
To step（2）Water is added in the mixture of obtained silicon-carbon nanosheet composite material and sodium chloride to be washed, filtered, passed through
Silicon-carbon nanosheet composite material is obtained after vacuum drying.
2. the preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material according to claim 1, it is characterised in that：Institute
State step（1）Middle pitch is asphalt, and 85 ~ 120 DEG C of softening point, toluene and quinoline insolubles are respectively less than 1 %.
3. the preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material according to claim 1, it is characterised in that：Institute
State step（1）The particle size range of middle nano-silicon is 10 ~ 100 nm.
4. the preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material according to claim 1, it is characterised in that：Institute
State step（1）Middle sodium chloride purity is more than 99%.
5. the preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material according to claim 1, it is characterised in that：Institute
State step（1）The mass ratio of middle nano-silicon, pitch and sodium chloride is 1:（5-20）：（100-300）.
6. the preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material according to claim 1, it is characterised in that：Institute
State step（2）In carbonization temperature be 780 ~ 850 DEG C, carbonization time be 1 ~ 3 h, protective gas be argon gas or nitrogen, flow velocity 20
~100 mL/min。
7. the preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material according to claim 1, it is characterised in that：Institute
State step（3）Middle vacuum drying time is 12 ~ 24 h, and absolute pressure is 133 ~ 500 Pa, and temperature is 60 ~ 90 DEG C.
8. the preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material according to claim 1, it is characterised in that：Institute
State step（4）Middle filtrate is evaporated under the conditions of 100 ~ 150 DEG C of heating temperature, and obtained sodium chloride continues on for step（1）
In.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111320161A (en) * | 2020-03-08 | 2020-06-23 | 大连理工大学 | Preparation method and application of asphalt-based carbon nanosheet |
| CN111646472A (en) * | 2020-05-22 | 2020-09-11 | 兰州理工大学 | Method for in-situ preparation of porous silicon-carbon composite negative electrode material |
| CN111900348A (en) * | 2020-07-14 | 2020-11-06 | 中国科学院山西煤炭化学研究所 | Method for preparing silicon-carbon composite material based on ball milling method and application thereof |
| CN112054165A (en) * | 2019-06-05 | 2020-12-08 | 上海杉杉科技有限公司 | Mesocarbon microbeads, graphite negative electrode material, preparation method of mesocarbon microbeads and graphite negative electrode material, and lithium ion battery |
| CN114122371A (en) * | 2021-11-02 | 2022-03-01 | 北京科技大学 | Preparation method of porous silicon-carbon negative electrode material of lithium ion battery |
| CN115676804A (en) * | 2022-12-23 | 2023-02-03 | 郑州中科新兴产业技术研究院 | Asphalt-based porous hard carbon negative electrode material and preparation method and application thereof |
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| CN106784736A (en) * | 2017-02-08 | 2017-05-31 | 大连理工大学 | A kind of sodium-ion battery negative pole coats the preparation method and application of tin particles nanometer sheet with coal tar pitch resin base amorphous carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112054165A (en) * | 2019-06-05 | 2020-12-08 | 上海杉杉科技有限公司 | Mesocarbon microbeads, graphite negative electrode material, preparation method of mesocarbon microbeads and graphite negative electrode material, and lithium ion battery |
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| CN114122371A (en) * | 2021-11-02 | 2022-03-01 | 北京科技大学 | Preparation method of porous silicon-carbon negative electrode material of lithium ion battery |
| CN115676804A (en) * | 2022-12-23 | 2023-02-03 | 郑州中科新兴产业技术研究院 | Asphalt-based porous hard carbon negative electrode material and preparation method and application thereof |
| CN115676804B (en) * | 2022-12-23 | 2024-01-30 | 郑州中科新兴产业技术研究院 | Porous hard carbon anode material based on asphalt, and preparation method and application thereof |
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