CN109428062A - A kind of graphene-silicon composite cathode material and preparation method thereof - Google Patents
A kind of graphene-silicon composite cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene-silicon composite cathode materials and preparation method thereof.Its preparation process are as follows: disperse 3- amino-4-hydroxy benzene sulfonic acid for carboxyl silicon nitride material first and prepare uniform solution, it is added drop-wise in graphene oxide solution later, after mixing evenly, hydrogen peroxide, nitrogen source are added again, after mixing evenly, it is then transferred in autoclave, the composite material of high-density graphite alkene cladding silicon materials is prepared by hydro-thermal reaction, low temperature drying, thermal reduction.Its composite material prepared prepares graphene with characteristics such as density height, capacity height using hydro-thermal reaction, and it is coated on silicon materials surface, reduce its expansion rate, and the high graphene oxide-silicon precursor material of consistency is formed by low temperature drying technology, and have many advantages, such as that conductivity is high by the graphene after thermal reduction, and graphene and silicon materials are keyed by chemistry, have many advantages, such as that structural stability is strong, suitable nano aperture.
Description
Technical field
The invention belongs to field of lithium ion battery material preparation, specifically a kind of graphene-silicon composite cathode material
And preparation method thereof.
Background technique
With the rapid development of electric vehicles, it is desirable that lithium ion battery has higher energy density and security performance, and
Negative electrode material is the critical material for forming lithium ion battery, the negative electrode material of existing market mainly based on graphite type material,
And with its good cycle, stability it is strong, cheap and its become negative electrode material the advantages that high with compatibility of electrolyte
Primary selection, but with the raising that market requires negative electrode material energy density, current graphite negative electrodes material without
Method meets the requirement of the marketization, therefore the negative electrode material for developing high capacity seems very urgent, and current high capacity cathode
Material mainly has silicon-carbon cathode, tin cathode, alloy anode etc., and with silicon-carbon cathode material technology relative maturity, current silicon
Carbon anode due in charge and discharge process volume expansion it is larger, conductivity is low, product is difficult to industrial application.For silicon-carbon cathode
There are the shortcomings that, studies in China person, which mainly passes through the measures such as silicon materials surface cladding, reduces the expansion of silicon materials, such as patent
(CN105118974 A) provides a kind of silicon based anode material and preparation method thereof, reduces due to introducing carbon nano-fiber system
The volume expansion of nano silicon particles avoids the phenomenon that silicon particle is broken and SEI film repeatedly generates, improves the machine of negative electrode material
Tool intensity, but it is since carbon nanotube density is smaller, reduces the tap density of its silicon carbon material, and carbon nanotube and silicon materials
It is to be combined by adsorption capacity, there are covering materials in charge and discharge process to remove, and causes its cycle performance deviation.And hydro-thermal reaction method
The material prepared, the material prepared are keyed by chemistry, the material of formation have that consistency is high, conductivity is strong and
The advantages that its stable structure, and adopt this method and prepare the Si-C composite material country and be rarely reported.
Summary of the invention
For current silicon-carbon cathode material existing for that there are expansion rates is big, conductivity is poor and its tap density is relatively low etc.
Defect, the purpose of the present invention is preparing the Si-C composite material of dopen Nano silicon between graphene layer by hydro-thermal reaction method, with
Improve the conductivity, tap density and its cycle performance for reducing material of silicon carbon material.
To achieve the above object, the invention provides the following technical scheme: a kind of graphene-silicon composite cathode material and its system
Preparation Method, silicon materials of the composite negative pole material by nitrogen-doped graphene and its between being entrained in form, and wherein the content of silicon is
(1~10) %.Its preparation process the following steps are included:
1) configuration of silicon solution:
(1~10) g carboxylated nano silica fume is added in the secondary distilled water of 100ml, after mixing evenly, then add (5~
15) the 3- amino-4-hydroxy benzene sulfonic acid of g filters after mixing evenly, is dried to obtain functionalized nano silicon materials A；
2) hydro-thermal reaction
The graphene oxide solution 500ml that concentration is (1~10) mg/ml is weighed, (0.01~0.1) g functionalization is added later and receives
Rice silicon materials A after mixing evenly, then adds the nitrogen source of (1~4) ml, the hydrogen peroxide that (10~30) ml concentration is 0.3%, and stirring is equal
It is even to obtain mixed liquid B, it is transferred in autoclave later, and in 150~200 DEG C of 1~6h of reaction, filter later, and pass through
Low temperature drying technology obtains the high composite material B of consistency；
3) sintering is modified
Composite material B is subjected to tabletting and is transferred in tube furnace, and in argon gas/hydrogen mixed gas (volume ratio 1:1) atmosphere
It is warming up to (800~900) DEG C, keeps the temperature (2~6) h, Temperature fall to room temperature, obtains composite negative pole material later.
Preferably, nitrogen source is one of urea, melamine, ammonium hydroxide, pyrroles in the step 2.
Preferably, in the step 2 low temperature drying technology the following steps are included:
First in a vacuum drying oven, (40~60) DEG C are warming up to, are repeated 1~10 time using nitrogen displacement method, later using true
Sky pump persistently takes out 6-24h, makes its vacuum degree≤- 0.098mpa, is finally warming up to vacuum oven (80~100) DEG C, and
Dry (24~72) h at a temperature of this.
Compared with prior art, the beneficial effects of the present invention are:
1) by coating one layer of 3- amino-4-hydroxy benzene sulfonic acid on nano silicon material surface, the group of silicon materials in a solvent is avoided
It is poly-, between making it that nano silicon material part is doped into graphene layer, allow its silicon materials sufficiently with passing through of graphene oxide
It learns bond to close, improves the binding force between material；
2) special dry technology is used, is replaced by nitrogen remove the most of moisture in material first, while to graphite
The contraction of alkene gel does not impact, and later using technology is persistently taken out, Nano/micron hydrone is taken away, and material continues later
It shrinks, forms micron hole, finally by heating by the moisture evaporative removal of micron hole, and shunk, obtain storeroom
With nano aperture structure.
3) graphene oxide/silicone-hydrogel material is prepared with uniformly mixed, binding force is strong, consistency is high using hydro-thermal method
The advantages that, and nitrogen is adulterated at it, the specific capacity and conductivity of graphene on the one hand can be improved, and carboxylated can be promoted to receive
The consistency for coming into full contact with, improving its material between rice silicon powder and nitrogen source, graphene oxide.
Detailed description of the invention
Fig. 1 is the SEM figure for the Si-C composite material that the embodiment of the present invention 1 is prepared.
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 1
Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of graphene-silicon composite cathode material and preparation method thereof, it is multiple
It closes silicon materials of the negative electrode material by nitrogen-doped graphene and its between being entrained in form, wherein the content of silicon is (1~10) %.
Its preparation process the following steps are included:
1) configuration of silicon solution:
5g carboxylated nano silica fume is added in the secondary distilled water of 100ml, after mixing evenly, then adds the 3- amino-of 10g
4- hydroxy benzene sulfonic acid filters after mixing evenly, is dried to obtain functionalized nano silicon materials A；
2) hydro-thermal reaction
The graphene oxide solution 500ml that concentration is 5mg/ml is weighed, adds 0.05g functionalized nano silicon materials A, stirring later
It after uniformly, then adds the pyrroles of 3ml, the hydrogen peroxide that 20ml concentration is 0.3%, is uniformly mixing to obtain mixed liquid B, is transferred to later
In autoclave, and in 180 DEG C of reaction 3h, filters later, obtain hydrogel graphene composite material, it is dry by low temperature later
Dry technology (first in a vacuum drying oven, is warming up to 50 DEG C, is repeated 5 times using nitrogen displacement method, continued later using vacuum pump
12h is taken out, makes its vacuum degree≤- 0.098mpa, vacuum oven is finally warming up to 90 DEG C, and dries 36h at this temperature)
The composite negative pole material high to consistency；
3) sintering is modified
Composite material B is subjected to tabletting and is transferred in tube furnace, and in argon gas/hydrogen mixed gas (volume ratio 1:1) atmosphere
850 DEG C are warming up to, keeps the temperature 3h, Temperature fall to room temperature, obtains composite material C later.
Embodiment 2
A kind of graphene-silicon composite cathode material and preparation method thereof, composite negative pole material is by nitrogen-doped graphene and its to mix
The miscellaneous silicon materials composition between, wherein the content of silicon is (1~10) %.Its preparation process the following steps are included:
1) configuration of silicon solution:
1g carboxylated nano silica fume is added in the secondary distilled water of 100ml, after mixing evenly, then adds the 3- amino-of 5g
4- hydroxy benzene sulfonic acid filters after mixing evenly, is dried to obtain functionalized nano silicon materials A；
2) hydro-thermal reaction
The graphene oxide solution 500ml that concentration is 1mg/ml is weighed, adds 0.01g functionalized nano silicon materials A, stirring later
It after uniformly, then adds the ammonium hydroxide of 1ml, the hydrogen peroxide that 10ml concentration is 0.3%, is uniformly mixing to obtain mixed liquid B, is transferred to later
It in autoclave, and in 150 DEG C of reaction 6h, filters later, and (first in a vacuum drying oven, by low temperature drying technology
Be warming up to 40 DEG C, be repeated 10 times using nitrogen displacement method, 6h is persistently taken out using vacuum pump later, make its vacuum degree≤-
Vacuum oven is finally warming up to 80 DEG C by 0.098mpa, and dries 72h at this temperature), obtain the high composite wood of consistency
Expect B；
3) sintering is modified
Composite material B is subjected to tabletting later and is transferred in tube furnace, and in argon gas/hydrogen mixed gas (volume ratio 1:1) gas
It is warming up to 800 DEG C in atmosphere, keeps the temperature 6h, Temperature fall to room temperature, obtains composite negative pole material later.
Embodiment 3
A kind of graphene-silicon composite cathode material and preparation method thereof, composite negative pole material is by nitrogen-doped graphene and its to mix
The miscellaneous silicon materials composition between, wherein the content of silicon is (1~10) %.Its preparation process the following steps are included:
1) configuration of silicon solution:
10g carboxylated nano silica fume is added in the secondary distilled water of 100ml, after mixing evenly, then adds the 3- ammonia of 15g
Base -4- hydroxy benzene sulfonic acid filters after mixing evenly, is dried to obtain functionalized nano silicon materials A；
2) hydro-thermal reaction
The graphene oxide solution 500ml that concentration is 10mg/ml is weighed, adds 0.1g functionalized nano silicon materials A, stirring later
It after uniformly, then adds the urea of 4ml, the hydrogen peroxide that 30ml concentration is 0.3%, is uniformly mixing to obtain mixed liquid B, is transferred to later
It in autoclave, and in 200 DEG C of reaction 1h, filters later, and (first in a vacuum drying oven, by low temperature drying technology
Be warming up to 60 DEG C, be repeated 5 times using nitrogen displacement method, 6h is persistently taken out using vacuum pump later, make its vacuum degree≤-
Vacuum oven is finally warming up to 100 DEG C by 0.098mpa, and is dried for 24 hours at this temperature) obtain the high composite wood of consistency
Expect B；
3) sintering is modified
Composite material B is subjected to tabletting and is transferred in tube furnace, and in argon gas/hydrogen mixed gas (volume ratio 1:1) atmosphere
900 DEG C are warming up to, keeps the temperature 2h, Temperature fall to room temperature, obtains composite negative pole material later.
Comparative example
By nano silica fume directly with graphene is compound prepares graphene/nanometer silicon composite.Its preparation process is as follows:
5 carboxylated nano silica fumes and 2.5g graphene powder are added to after mixing in 500ml secondary distilled water, and are turned
It moves on in ball mill, silicon/graphene composite material is obtained after high speed dispersion is uniform.
The following test of design
SEM test
The silicon prepared to embodiment 1/graphene composite material carries out surface sweeping Electronic Speculum (SEM) test, as can be seen from Figure, silicon
Material by graphene completely/part coats, while having part nano-silicon is to adsorb on the surface of graphene.
Electrochemical property test:
1) button cell is tested
Lithium ion battery negative material obtained in Examples 1 to 3 and comparative example is assembled into button cell A1, A2, A3 respectively；
Preparation method are as follows: binder, conductive agent and solvent are added in negative electrode material, is stirred slurrying, are coated on copper foil, warp
Cross dry, roll it is obtained.Binder used is LA132 binder, and conductive agent SP, negative electrode material is what Examples 1 to 3 was prepared
Negative electrode material, solvent are secondary distilled water, its ratio be: negative electrode material: SP:LA132: secondary distilled water=95g:1g:4g:
220mL；Electrolyte is LiPF6/ EC+DEC (1:1), metal lithium sheet are to electrode, and diaphragm uses polyethylene (PE), polypropylene
(PP) or poly- second propylene (PEP) composite membrane, simulated battery are assemblied in the glove box for be flushed with hydrogen gas and carry out, and chemical property is in Wuhan
It is carried out on the blue new prestige 5v/10mA type cell tester of electricity, charging/discharging voltage range is 0.005V to 2.0V, and charge-discharge velocity is
0.1C。
Claims (4)
1. a kind of graphene-silicon composite cathode material and preparation method thereof, it is characterised in that: composite negative pole material is by N doping
Graphene and its silicon materials composition between being entrained in, wherein the content of silicon is (1~10) %.
2. its preparation process the following steps are included:
1) configuration of silicon solution:
(1~10) g carboxylated nano silica fume is added in the secondary distilled water of 100ml, after mixing evenly, then add (5~
15) the 3- amino-4-hydroxy benzene sulfonic acid of g filters after mixing evenly, is dried to obtain functionalized nano silicon materials A；
2) hydro-thermal reaction
The graphene oxide solution 500ml that concentration is (1~10) mg/ml is weighed, (0.01~0.1) g functionalization is added later and receives
Rice silicon materials A after mixing evenly, then adds the nitrogen source of (1~4) ml, the hydrogen peroxide that (10~30) ml concentration is 0.3%, and stirring is equal
It is even to obtain mixed liquid B, it is transferred in autoclave later, and in 150~200 DEG C of 1~6h of reaction, filter later, and pass through
Low temperature drying technology obtains the high composite material B of consistency；
3) sintering is modified
Composite material B is subjected to tabletting and is transferred in tube furnace, and in argon gas/hydrogen mixed gas (volume ratio 1:1) atmosphere
It is warming up to (800~900) DEG C, keeps the temperature (2~6) h, Temperature fall to room temperature, obtains composite negative pole material later.
3. a kind of graphene-silicon composite cathode material according to claim 1 and preparation method thereof, which is characterized in that institute
Stating nitrogen source in step 2 is one of urea, melamine, ammonium hydroxide, pyrroles.
4. a kind of graphene-silicon composite cathode material according to claim 1 and preparation method thereof, which is characterized in that institute
State low temperature drying technology in step 2 the following steps are included:
First in a vacuum drying oven, (40~60) DEG C are warming up to, are repeated 1~10 time using nitrogen displacement method, later using true
Sky pump persistently takes out 6-24h, makes its vacuum degree≤- 0.098mpa, is finally warming up to vacuum oven (80~100) DEG C, and
Dry (24~72) h at a temperature of this.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111628156A (en) * | 2020-06-29 | 2020-09-04 | 蜂巢能源科技有限公司 | Molybdenum-doped porous silicon-carbon composite material, preparation method thereof and lithium ion battery |
| CN111697219A (en) * | 2020-06-30 | 2020-09-22 | 深圳市金牌新能源科技有限责任公司 | Silicon-carbon composite material, preparation method thereof, negative electrode and application thereof |
| CN111933916A (en) * | 2020-10-12 | 2020-11-13 | 长沙矿冶研究院有限责任公司 | Negative electrode active material and preparation method thereof |
| CN113380997A (en) * | 2021-05-25 | 2021-09-10 | 万向一二三股份公司 | High-first-efficiency silicon-based negative electrode material of lithium ion battery and preparation method thereof |
| WO2024031867A1 (en) * | 2022-08-10 | 2024-02-15 | 胜华新能源科技(东营)有限公司 | Nitrogen-doped graphene-coated silicon-carbon composite material, and preparation method therefor and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111628156A (en) * | 2020-06-29 | 2020-09-04 | 蜂巢能源科技有限公司 | Molybdenum-doped porous silicon-carbon composite material, preparation method thereof and lithium ion battery |
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| CN113380997A (en) * | 2021-05-25 | 2021-09-10 | 万向一二三股份公司 | High-first-efficiency silicon-based negative electrode material of lithium ion battery and preparation method thereof |
| CN113380997B (en) * | 2021-05-25 | 2022-07-29 | 万向一二三股份公司 | Silicon-based negative electrode material of lithium ion battery and preparation method thereof |
| WO2024031867A1 (en) * | 2022-08-10 | 2024-02-15 | 胜华新能源科技(东营)有限公司 | Nitrogen-doped graphene-coated silicon-carbon composite material, and preparation method therefor and use thereof |
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Application publication date: 20190305 |