CN110176601A - A kind of carbon coating oxidation Asia silicium cathode material and its preparation method and application - Google Patents
A kind of carbon coating oxidation Asia silicium cathode material and its preparation method and application Download PDFInfo
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- CN110176601A CN110176601A CN201910418235.5A CN201910418235A CN110176601A CN 110176601 A CN110176601 A CN 110176601A CN 201910418235 A CN201910418235 A CN 201910418235A CN 110176601 A CN110176601 A CN 110176601A
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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
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Abstract
The invention discloses a kind of carbon coatings to aoxidize sub- silicium cathode material and its preparation method and application, and carbon coating, which aoxidizes sub- silicium cathode material, has core-shell structure, including the nucleome, buffer layer and outer layer being sequentially distributed from the inside to the outside；Nucleome is that hypoxemia value aoxidizes sub- silicon, and buffer layer is carbon nanotube, and outer layer is carbon coating layer.Wherein, hypoxemia value, which aoxidizes sub- silicon, can effectively improve the specific capacity of material, electrochemical contact caused by the sub- silicon of oxidation ruptures during removal lithium embedded because of volume expansion can be effectively relieved as textured buffer layers in carbon nanotube, while carbon coating can effectively improve its electric conductivity and stablize and aoxidize sub- silicon structure change during electrode cycle.Using battery made of this negative electrode material, there is high specific discharge capacity, high coulombic efficiency for the first time and more stable cycle performance, have broad application prospects in high specific energy batteries field.And preparation method is simple, at low cost, environmental-friendly, is suitble to industrialization large-scale production.
Description
Technical field
The invention belongs to electrochemical energy storage field of new generation, specifically a kind of carbon coating aoxidizes sub- silicium cathode material and its system
Preparation Method and application.
Background technique
With the fast development of electric car, energy-accumulating power station and portable electronic device etc..High specific energy lithium ion battery is received
To more and more concerns.However, graphite cathode is still firmly in occupation of dominant position, theoretical specific capacity 372mAh/g at present
It can no longer meet the requirement of high specific energy batteries negative electrode material, seriously constrain the raising of lithium battery energy density.Next life many years
The scientist of boundary various regions attempts to develop the negative electrode material that can substitute graphite, such as silicon based anode material, tin-based material and titanium
Sour lithium material.And silicium cathode material is the currently the only novel high-capacity negative electrode material for realizing commercial applications,
The commercialized silicon monoxide composite cathode material of mainstream has generally all carried out carbon coating at present, and this aspect improves
The electric conductivity of material, while also avoiding aoxidizing sub- silicon materials directly and electrolyte contacts, improve the cycle performance of material.
Silicon based anode material large-scale application still suffers from numerous tests, further improves the cycle performance of material, and reduce and be produced into
This, vast researcher and manufacturer still shoulder heavy responsibilities.
Summary of the invention
The object of the present invention is to provide a kind of carbon coatings to aoxidize sub- silicium cathode material and its preparation method and application, to solve
The problem of silicon based anode material cycle performance is undesirable in the prior art, high production cost.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of sub- silicium cathode material of carbon coating oxidation, it is characterised in that: it is core that the carbon coating, which aoxidizes sub- silicium cathode material,
The material of shell structure, including the nucleome, buffer layer and outer layer being sequentially distributed from the inside to the outside；The nucleome is that the oxidation of hypoxemia value is sub-
Silicon, chemical formula SiOx, wherein x is 0.95~0.99；The buffer layer is carbon nanotube；The outer layer is carbon coating layer.
Further scheme, the quality of the carbon coating layer are the 2%~3% of the sub- siliceous amount of hypoxemia value oxidation.
The present invention also provides the preparation methods that above-mentioned carbon coating aoxidizes sub- silicium cathode material, include the following steps:
(1) it after the sub- silicon of oxidation is crushed, removes magnetic, mixes with carbon nano tube paste, is dried to obtain at a temperature of 80~100 DEG C
Mixed material；Sub- silicon is wherein aoxidized except the content < 10ppm, magnetic magazine content < 2ppm of Fe, Co, Ni after magnetic.
(2) mixed material is placed in rotary furnace, is passed through nitrogen hydrogen gas mixture, in 600~650 DEG C of 2~3h of calcining
Afterwards, stop being passed through nitrogen hydrogen gas mixture, this stage restores partial oxidation Asia silicon using the reproducibility of hydrogen, and it is sub- to reduce oxidation
Oxygen content in silicon obtains the oxidation Asia silicon of hypoxemia value, can effectively improve the specific capacity of material；Then pass to the mixing of nitrogen acetylene
Gas, and 850~950 DEG C are warming up to, continue 2~3h of calcining, carries out chemical vapor deposition reaction by the cracking of acetylene in material
Expect that surface forms carbon coating layer, natural cooling after calcining obtains carbon coating and aoxidizes sub- silicium cathode material.
Further scheme, the sub- smashed median particle diameter of silicon (D50) of the oxidation are 4~5um, and D10 > 1.5.It is described
D50 is more preferably 4um.
Further scheme, the absolute dry mass of the carbon nano tube paste are the 0.5%~1.5% of the sub- siliceous amount of oxidation, into
One step is preferably 1%.The carbon nano tube paste is multi-walled carbon nanotube slurry.
Further scheme, the revolving speed of the rotary furnace are 0.3-1 revs/min.
Further scheme, the volume fraction of hydrogen is 5%~10% in the nitrogen hydrogen gas mixture, further preferably
It is 10%.
Further scheme, the volume fraction of acetylene is 40%~50% in the nitrogen acetylene gas mixture, further excellent
It is selected as 50%.
It is a further object to provide above-mentioned carbon coatings to aoxidize the application of sub- silicium cathode material in the battery.
Compared with the prior art, the advantages of the present invention are as follows:
(1) preparation process of the present invention is simple, crush except magnetic, with conductive agent by the way that the raw material being easy to get are aoxidized sub- silicon
After carbon nanotube is stirred, drying to obtain mixed material；Then mixed material can be obtained carbon through one kettle way solid phase calcination
Cladding aoxidizes sub- silicium cathode material；Preparation method is simple, at low cost, no pollution to the environment, is suitble to industrialization large-scale production.
(2) present invention is using hydrogen as reducing gas, and as cladding carbon source, calcine in mixed gas is had acetylene
The carbon coating of core-shell structure aoxidizes sub- silicium cathode material.Wherein, the oxygen aoxidized in sub- silicon is reduced by the reduction of hydrogen to contain
Amount, obtains the oxidation Asia silicon of hypoxemia value, can effectively improve the specific capacity of material；Carbon nanotube can effectively be delayed as textured buffer layers
Solution aoxidizes electrochemical contact caused by sub- silicon ruptures during removal lithium embedded because of volume expansion；Carbon coating layer can be mentioned effectively simultaneously
Its high electric conductivity simultaneously stablizes the sub- silicium cathode of carbon coating oxidation for aoxidizing sub- silicon structure change during electrode cycle, being prepared
Excellent material performance.
(3) carbon coating that the present invention is prepared aoxidizes battery made of sub- silicium cathode material, has high electric discharge specific volume
Amount, high coulombic efficiency for the first time and more stable cycle performance, before there is wide application in high specific energy batteries field
Scape.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that carbon coating prepared by embodiment 1 aoxidizes sub- silicium cathode material；
Fig. 2 is the Raman map that carbon coating prepared by embodiment 1 aoxidizes sub- silicium cathode material and raw material aoxidize sub- silicon；
Fig. 3 is that carbon coating prepared by embodiment 1 aoxidizes sub- silicium cathode material and raw material aoxidize button electricity made of sub- silicon
Pond first charge-discharge curve graph.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention will be further explained.Obviously, described embodiment is this
Invention a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art exist
Every other embodiment obtained under the premise of creative work is not made, shall fall within the protection scope of the present invention.
Embodiment 1
30Kg business pure zirconia Asia silicon is crushed using airslide disintegrating mill, crushes unit frequency 30Hz, the oxidation of crushing
Sub- silicon powder material mixes after removing magnetic with multi-walled carbon nanotube slurry, and the absolute dry mass of multi-walled carbon nanotube slurry is the sub- siliceous amount of oxidation
1%, mixed material is stirred in 95 DEG C of temperature to drying, mixed material is obtained.Mixed material is placed in rotary furnace
In under nitrogen hydrogen gas mixture 600 DEG C of heat preservations calcine 2 hours, the revolving speed of rotary furnace is 0.3 rev/min, the nitrogen hydrogen
The volume fraction of hydrogen is 10% in oxygen mixture；This stage restores partial oxidation Asia silicon using the reproducibility of hydrogen, reduces
The oxygen content in sub- silicon is aoxidized, the oxidation Asia silicon of hypoxemia value is obtained, the specific capacity of material can be effectively improved.600 DEG C keep the temperature 2 hours
Afterwards, stop being passed through nitrogen hydrogen gas mixture, be passed through nitrogen acetylene gas mixture, and be continuously heating to 900 DEG C with 5 DEG C/min,
3 hours are kept the temperature, the volume fraction of acetylene is 50% in the nitrogen acetylene gas mixture, and it is anti-that this stage carries out chemical vapor deposition
Carbon coating layer should be formed on the surface of the material by the cracking of acetylene.After soaking time reaches, cooled to room temperature is finally obtained
Carbon coating with core-shell structure aoxidizes sub- silicium cathode material, wherein the quality of carbon coating layer is the sub- siliceous amount of hypoxemia value oxidation
2%.
The structure that the carbon coating that the present invention is prepared aoxidizes sub- silicium cathode material is core-shell structure, and structural schematic diagram is such as
Shown in Fig. 1, including the nucleome, buffer layer and outer layer being sequentially distributed from the inside to the outside；Wherein, nucleome is that hypoxemia value aoxidizes sub- silicon, is changed
Formula is SiOx, wherein x is 0.95~0.99；Buffer layer is carbon nanotube；Outer layer is carbon coating layer.
Sub- silicium cathode material is aoxidized to carbon coating prepared by embodiment 1 and untreated business SiO material has carried out Raman
Atlas analysis and electrochemical property test.From the Raman detection profiling results of Fig. 2 it is found that compared to business SiO material, example
1 carbon coating aoxidizes sub- silicium cathode material without the characteristic peak of apparent oxide, illustrates there is apparent covered effect.Together
When, the carbon coating that example 1 is prepared aoxidizes sub- silicium cathode material ID/IGIt improves compared to the 1.04 of business SiO to 1.10,
Further demonstrate that material has apparent carbon coating.
Carbon coating obtained is aoxidized into sub- silicium cathode material, superconduction carbon black and bonding agent LA133 80:10:10 in mass ratio
Proportion mixing, adds suitable quantity of water and is made into slurry, be applied on copper foil after mixing, obtain pole piece after 70 DEG C of dry 12h.With
Lithium metal is cathode, and Celgard2400 is diaphragm, contains 1M LiPF6EC:DMC:DEC (volume ratio 1:1:1) solution be electricity
Liquid is solved, 2032 type button cells are assembled in argon atmosphere glove box, then carry out electrochemical property test.
Fig. 3 is that carbon coating aoxidizes button cell that sub- silicium cathode material and business SiO are respectively prepared in 0.05C multiplying power (1C
=1300mA/g), voltage range is the first charge-discharge curve under the conditions of 0.05-1.5V.Wherein, it is detained made of business SiO
Formula battery first discharge specific capacity be 1769.3mAh/g, charge specific capacity 720.5mAh/g, for the first time coulombic efficiency be only
40.69%.And aoxidizing button cell first discharge specific capacity made of sub- silicium cathode material carbon coating is 2019.4mAh/g,
Charge specific capacity is 1503.5mAh/g, for the first time coulombic efficiency 74.45%, shows higher coulombic efficiency for the first time and fills for the first time
Electric specific capacity, this is for improving the capacity of full battery and for the first time coulombic efficiency has a very big significance.Meanwhile carbon coating oxidation is sub-
The discharge platform of button cell made of silicium cathode material is shown lesser significantly lower than button cell made of business SiO
Polarization.Therefore, untreated business SiO material is compared, carbon coating aoxidizes button cell made of sub- silicium cathode material and shows
Higher specific capacity and for the first time coulombic efficiency, and material polarization is small, has preferable chemical property.
Embodiment 2
30Kg business pure zirconia Asia silicon is crushed using airslide disintegrating mill, crushes unit frequency 30Hz, the oxidation of crushing
Sub- silicon powder material mixes after removing magnetic with multi-walled carbon nanotube slurry, and the absolute dry mass of multi-walled carbon nanotube slurry is the sub- siliceous amount of oxidation
0.5%, mixed material is stirred in 80 DEG C of temperature to drying, mixed material is obtained.Mixed material is placed in revolution
650 DEG C of heat preservations are calcined 3 hours under nitrogen hydrogen gas mixture in furnace, and the revolving speed of rotary furnace is 1 rev/min, the nitrogen hydrogen
The volume fraction of hydrogen is 5% in oxygen mixture.After 650 DEG C keep the temperature 3 hours, stopping is passed through nitrogen hydrogen gas mixture, leads to
Enter nitrogen acetylene gas mixture, and be continuously heating to 850 DEG C with 5 DEG C/min, keeps the temperature 3 hours, the nitrogen acetylene gas mixture
The volume fraction of middle acetylene is 40%.After soaking time reaches, cooled to room temperature finally obtains the carbon with core-shell structure
Cladding aoxidizes sub- silicium cathode material.
Embodiment 3
30Kg business pure zirconia Asia silicon is crushed using airslide disintegrating mill, crushes unit frequency 30Hz, the oxidation of crushing
Sub- silicon powder material mixes after removing magnetic with multi-walled carbon nanotube slurry, and the absolute dry mass of multi-walled carbon nanotube slurry is the sub- siliceous amount of oxidation
1.5%, mixed material is stirred in 100 DEG C of temperature to drying, mixed material is obtained.Mixed material is placed in revolution
650 DEG C of heat preservations are calcined 2.5 hours under nitrogen hydrogen gas mixture in furnace, and the revolving speed of rotary furnace is 0.6 rev/min, the nitrogen
The volume fraction of hydrogen is 8% in gas hydrogen gas mixture.After 650 DEG C keep the temperature 2.5 hours, stopping is passed through nitrogen hydrogen mixed gas
Body is passed through nitrogen acetylene gas mixture, and is continuously heating to 950 DEG C with 5 DEG C/min, keeps the temperature 2.5 hours, the nitrogen acetylene is mixed
The volume fraction for closing acetylene in gas is 45%.After soaking time reaches, cooled to room temperature is finally obtained with nucleocapsid knot
The carbon coating of structure aoxidizes sub- silicium cathode material.
Claims (9)
1. a kind of carbon coating aoxidizes sub- silicium cathode material, it is characterised in that: it is nucleocapsid that the carbon coating, which aoxidizes sub- silicium cathode material,
The material of structure, including the nucleome, buffer layer and outer layer being sequentially distributed from the inside to the outside；The nucleome is that hypoxemia value aoxidizes sub- silicon,
Its chemical formula is SiOx, wherein x is 0.95~0.99；The buffer layer is carbon nanotube；The outer layer is carbon coating layer.
2. carbon coating according to claim 1 aoxidizes sub- silicium cathode material, it is characterised in that: the quality of the carbon coating layer
It is the 2~3% of the sub- siliceous amount of hypoxemia value oxidation.
3. the preparation method that carbon coating as described in claim 1 aoxidizes sub- silicium cathode material, it is characterised in that: including walking as follows
It is rapid:
(1) it after the sub- silicon of oxidation is crushed, removes magnetic, is mixed with carbon nano tube paste, is dried to obtain mixing at a temperature of 80~100 DEG C
Material；
(2) mixed material is placed in rotary furnace, is passed through nitrogen hydrogen gas mixture, after 600~650 DEG C of 2~3h of calcining, stopped
Only it is passed through nitrogen hydrogen gas mixture；It is passed through nitrogen acetylene gas mixture, and is warming up to 850~950 DEG C, continues 2~3h of calcining,
Natural cooling after calcining obtains carbon coating and aoxidizes sub- silicium cathode material.
4. preparation method according to claim 3, it is characterised in that: the sub- smashed median particle diameter of silicon of the oxidation is 4
~5um.
5. preparation method according to claim 3, it is characterised in that: the absolute dry mass of the carbon nano tube paste is oxidation
The 0.5%~1.5% of sub- siliceous amount, the carbon nano tube paste are multi-walled carbon nanotube slurry.
6. preparation method according to claim 3, it is characterised in that: the revolving speed of the rotary furnace is 0.3-1 revs/min.
7. preparation method according to claim 3, it is characterised in that: the volume of hydrogen in the nitrogen hydrogen gas mixture
Score is 5%~10%.
8. preparation method according to claim 3, it is characterised in that: the volume of acetylene in the nitrogen acetylene gas mixture
Score is 40%~50%.
9. carbon coating as claimed in claim 1 or 2 aoxidizes the application of sub- silicium cathode material in the battery.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111342031A (en) * | 2020-03-28 | 2020-06-26 | 兰溪致德新能源材料有限公司 | Multi-element gradient composite high-first-efficiency lithium battery negative electrode material and preparation method thereof |
| CN112186145A (en) * | 2020-09-08 | 2021-01-05 | 合肥国轩高科动力能源有限公司 | Magnesium reduced carbon coated silica material and preparation method and application thereof |
| CN113161531A (en) * | 2021-03-31 | 2021-07-23 | 溧阳紫宸新材料科技有限公司 | Carbon-coated silicon oxide cathode material of lithium ion battery and preparation method and application thereof |
| CN113363432A (en) * | 2021-04-21 | 2021-09-07 | 万向一二三股份公司 | Negative plate containing silicon-based negative electrode material with high initial coulombic efficiency and lithium ion battery |
| CN113839027A (en) * | 2021-08-31 | 2021-12-24 | 湖南宸宇富基新能源科技有限公司 | Carbon-coated oxygen-hole double-gradient silicon protoxide material and preparation and application thereof |
| CN114039038A (en) * | 2021-12-01 | 2022-02-11 | 安徽科达新材料有限公司 | Preparation method of coated modified silicon monoxide long-cycle negative electrode |
| CN114388770A (en) * | 2022-01-24 | 2022-04-22 | 浙江锂宸新材料科技有限公司 | High-capacity high-first-efficiency silica anode material and preparation method thereof |
| CN114464785A (en) * | 2021-12-31 | 2022-05-10 | 长沙矿冶研究院有限责任公司 | Carbon-coated silicon monoxide negative electrode material, preparation method thereof and lithium ion battery |
| CN114864887A (en) * | 2022-04-07 | 2022-08-05 | 湖南金硅科技有限公司 | Modification method for fluidity of silicon monoxide |
| CN115775885A (en) * | 2022-11-14 | 2023-03-10 | 佛山市格瑞芬新能源有限公司 | Silica anode material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111342031A (en) * | 2020-03-28 | 2020-06-26 | 兰溪致德新能源材料有限公司 | Multi-element gradient composite high-first-efficiency lithium battery negative electrode material and preparation method thereof |
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| CN112186145B (en) * | 2020-09-08 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | Magnesium reduced carbon coated silica material and preparation method and application thereof |
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| CN113161531A (en) * | 2021-03-31 | 2021-07-23 | 溧阳紫宸新材料科技有限公司 | Carbon-coated silicon oxide cathode material of lithium ion battery and preparation method and application thereof |
| CN113363432A (en) * | 2021-04-21 | 2021-09-07 | 万向一二三股份公司 | Negative plate containing silicon-based negative electrode material with high initial coulombic efficiency and lithium ion battery |
| CN113839027A (en) * | 2021-08-31 | 2021-12-24 | 湖南宸宇富基新能源科技有限公司 | Carbon-coated oxygen-hole double-gradient silicon protoxide material and preparation and application thereof |
| CN113839027B (en) * | 2021-08-31 | 2023-10-13 | 湖南宸宇富基新能源科技有限公司 | Carbon-coated oxygen-pore double-gradual-change silicon oxide material and preparation and application thereof |
| CN114039038A (en) * | 2021-12-01 | 2022-02-11 | 安徽科达新材料有限公司 | Preparation method of coated modified silicon monoxide long-cycle negative electrode |
| CN114464785A (en) * | 2021-12-31 | 2022-05-10 | 长沙矿冶研究院有限责任公司 | Carbon-coated silicon monoxide negative electrode material, preparation method thereof and lithium ion battery |
| CN114464785B (en) * | 2021-12-31 | 2024-03-22 | 长沙矿冶研究院有限责任公司 | Carbon-coated silicon oxide negative electrode material, preparation method thereof and lithium ion battery |
| CN114388770A (en) * | 2022-01-24 | 2022-04-22 | 浙江锂宸新材料科技有限公司 | High-capacity high-first-efficiency silica anode material and preparation method thereof |
| CN114864887A (en) * | 2022-04-07 | 2022-08-05 | 湖南金硅科技有限公司 | Modification method for fluidity of silicon monoxide |
| CN114864887B (en) * | 2022-04-07 | 2023-09-22 | 湖南金硅科技有限公司 | Modification method for fluidity of silicon oxide |
| CN115775885A (en) * | 2022-11-14 | 2023-03-10 | 佛山市格瑞芬新能源有限公司 | Silica anode material and preparation method and application thereof |
| CN115775885B (en) * | 2022-11-14 | 2024-02-06 | 佛山市格瑞芬新能源有限公司 | Silicon-oxygen anode material and preparation method and application thereof |
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Application publication date: 20190827 |