CN109873151A - A kind of three-dimensional porous silicon-carbon composite cathode material and preparation method thereof - Google Patents
A kind of three-dimensional porous silicon-carbon composite cathode material and preparation method thereof Download PDFInfo
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- CN109873151A CN109873151A CN201910220756.XA CN201910220756A CN109873151A CN 109873151 A CN109873151 A CN 109873151A CN 201910220756 A CN201910220756 A CN 201910220756A CN 109873151 A CN109873151 A CN 109873151A
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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 present invention relates to lithium ion battery material technical fields, and a kind of three-dimensional porous silicon-carbon composite cathode material is disclosed, the raw material including following number: calomel 100-120 parts of 50-100 parts of ethyl alcohol, 50-100 parts of deionized water, 10-20 parts of amino silane organic compound, 20-30 parts of acetic acid, 20-30 parts of sodium acetate, 70-90 parts of foamy carbon, 100-120 parts of platinized platinum and saturation.The three-dimensional porous silicon-carbon composite cathode material and preparation method thereof, by configuring amino silane solution, foam carbon surface is deposited on by electrochemical deposition method later, it is deposited on its silane compound between the hole of foamy carbon and surface, 400 degrees Celsius of carbonizations later form silicon oxide compound after making the cracking carbonization of its silane compound, and in the coated porous carbon material in its surface, use oxidation foamy carbon for matrix, and amide group can be formed with amino silane and improves fastness between its material, avoid the separation in charge and discharge process between foamed carbon material and silicon oxide compound, improve its cycle performance.
Description
Technical field
The present invention relates to lithium ion battery material technical field, specially a kind of three-dimensional porous silicon-carbon composite cathode material and
Preparation method.
Background technique
Commercial negative electrode material is mainly graphite carbon material at present, however the theoretical specific capacity of graphite is only 372m Ah/
G, is unable to satisfy the demand of increasingly developed high-energy-density densitybattery, and silicon is a kind of to store up lithium and forming alloy with lithium
Negative electrode material, theoretical capacity are up to 4200m Ah/g, meanwhile, the discharge platform of silicon is slightly above carbon material, and the peace of battery can be improved
Full performance, and material source is extensive, still, in charge and discharge cycles, the repeatedly embedding of lithium ion de- will cause the huge body of material
Product variation (volume expansion > 300%), resulting mechanical stress will lead to the avalanche, dusting, peeling of material lattice structure,
So as to cause between silicon particle, lose electrical contact between particle and collector, internal resistance increases, ultimately cause reversible capacity it is quick under
Drop, it is difficult to industrialization, and be one of the expanding method for reducing its material by nanosizing to silicon materials and its pore-creating, and nanometer
Porous silica material also has both duct abundant, while its continuous structure can form the huge network of electronics and ionic conduction,
The storage lithium performance better than traditional silicon materials is shown, still, it is not good enough that nanoporousization not can be well solved silicon materials electric conductivity
The shortcomings that, it is a good developing direction by silicon and the good porous carbon materials Material cladding of electric conductivity, on the one hand can serves as " slow
Rush skeleton " structure of carrying out stable silicon, tiny silicon particle can also be dispersed, inhibit the reunion of silicon in charge and discharge process, another party
The electric conductivity of composite material is improved in face, and therefore, the cycle performance of this silicon based anode material has greatly improved compared with elemental silicon,
It has broad application prospects.
The preparation method of nanoporous silica-base material mainly includes thermal reduction, template, chemical vapour deposition technique at present
Deng, these methods generally require the corrosion or higher temperature of violent in toxicity HF, and complicated for operation, expensive, be not suitable for scale
Metaplasia produces, and process is difficult to control accurately, and which prevent the practicalizations of silicium cathode material, and electrochemical deposition method has preparation
The advantages that process control, consistency are high and its environmentally friendly, such as by silicon compound deposited in the kernel and table of porous carbon materials
Face, can significantly improve the structural stability and cycle performance of material, so propose a kind of three-dimensional porous silicon-carbon composite cathode material
Material and preparation method thereof.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of three-dimensional porous silicon-carbon composite cathode material and its preparation sides
Method solves conventional method method and generally requires severe toxicity the advantages that having that preparation process is controllable, consistency is high and is environmentally friendly
The corrosion of object HF or higher temperature, and it is complicated for operation, expensive, be not suitable for large-scale production, process is difficult to control accurately
The problem of.
(2) technical solution
To realize that above-mentioned preparation process is controllable, consistency is high and environmentally friendly purpose, the present invention provides following technical side
Case: a kind of three-dimensional porous silicon-carbon composite cathode material, the raw material including following number: 50-100 parts of ethyl alcohol, deionized water 50-
100 parts, 10-20 parts of amino silane organic compound, 20-30 parts of acetic acid, 20-30 parts of sodium acetate, 70-90 parts of foamy carbon, platinized platinum
100-120 parts and calomel 100-120 parts of saturation.
Preferably, 10-20 parts of the amino silane organic compound are aminopropyltriethoxy diethoxy silane, γ-diethyl
Alkene triamine hydroxypropyl methyl dimethoxysilane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, N- aminoethyl -3- ammonia third
One of ylmethyl dimethoxysilane and 3-aminopropyltriethoxysilane.
A kind of preparation method of three-dimensional porous silicon-carbon composite cathode material, comprising the following steps:
1) 50-100 parts of ethyl alcohol, 50-100 parts of deionized water and 10-20 parts of amino silane organic compound are uniformly mixed
Afterwards, it is adjusted using 20-30 parts and sodium acetate 20-30 parts of acetic acid and arrives pH value PH=6.5-7, be hydrolyzed to obtain silane later
Mixed liquor A；
2) oxidation foamy carbon is obtained by the way that oxygen treatments applied is modified by 70-90 parts of foamy carbon, as working electrode, platinized platinum 100-
120 parts is, to electrode, calomel 100-120 parts of saturation is, to electrode, silane mixture liquid A are electrolyte；
3) by electrochemical deposition method, foam carbon surface deposit silicon compounds is aoxidized at it, pass through cleaning and drying later,
And be transferred in tube furnace, it carries out carbonization 3h hours for 400 degrees Celsius under an inert atmosphere, obtains three-dimensional porous silicon-carbon composite wood
Material.
Preferably, the electrochemical deposition method is one of cyclic voltammetry, constant flow method and constant-voltage method.
(3) beneficial effect
Compared with prior art, the present invention provides a kind of three-dimensional porous silicon-carbon composite cathode material and preparation method thereof,
Have it is following the utility model has the advantages that
1, three-dimensional porous silicon-carbon composite cathode material and preparation method thereof, by configuring amino silane solution, Zhi Houtong
It crosses electrochemical deposition method and is deposited on foam carbon surface, be deposited on its silane compound between the hole of foamy carbon and surface, it
400 degrees Celsius of carbonizations form silicon oxide compound after making the cracking carbonization of its silane compound afterwards, and in the coated porous carbon materials in its surface
On the one hand material reduces the expansion in charge and discharge process, on the other hand improves its electric conductivity, use oxidation foamy carbon for matrix, and
Amide group can be formed with amino silane and improve fastness between its material, avoid in charge and discharge process foamed carbon material with
Separation between silicon oxide compound improves its cycle performance.
2, three-dimensional porous silicon-carbon composite cathode material and preparation method thereof, by by ethyl alcohol, deionized water and amino silicone
Alkane organic compound after mixing, is adjusted to pH value PH=6.5-7 using acetic acid and sodium acetate, is hydrolyzed to obtain later
Oxidation foamy carbon is obtained by the way that oxygen treatments applied is modified to silane mixture liquid A and by foamy carbon, as working electrode, platinized platinum is to electricity
Pole, saturation calomel are to electrode, and silane mixture liquid A is electrolyte, and preparation process is controllable, and consistency is high and environmentally friendly.
Detailed description of the invention
Fig. 1 is the three-dimensional porous silicon that a kind of three-dimensional porous silicon-carbon composite cathode material of the present invention and preparation method thereof is prepared
The SEM of carbon composite schemes.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment one: a kind of three-dimensional porous silicon-carbon composite cathode material, the raw material including following number: 50 parts of ethyl alcohol is gone
50 parts of ionized water, γ -10 parts of diethylenetriamine hydroxypropyl methyl dimethoxysilane, 20 parts of acetic acid, 20 parts of sodium acetate, foamy carbon
100 parts of calomel of 70 parts, 100 parts of platinized platinum and saturation.
A kind of preparation method of three-dimensional porous silicon-carbon composite cathode material, comprising the following steps:
1) 50 parts of ethyl alcohol, 50 parts of deionized water and γ -10 parts of diethylenetriamine hydroxypropyl methyl dimethoxysilane are mixed
It after uniformly, is adjusted using 20 parts of acetic acid and 20 parts of sodium acetate and arrives pH value PH=6.5-7, be hydrolyzed to obtain silane later mixed
Close liquid A；
2) oxidation foamy carbon is obtained by oxygen treatments applied modified (flow 10ml/min, time 60min) by 70 parts of foamy carbon,
As working electrode, 100 parts of platinized platinum is, to electrode, 100 parts of calomel of saturation is, to electrode, silane mixture liquid A are electrolyte；
3) by constant-voltage method (voltage 2V, time 60min), in its oxidation foam carbon surface deposit silicon compounds, Zhi Houtong
Cross deionized water cleaning, 80 degrees Celsius of vacuum drying and are transferred in tube furnace, under argon inert atmosphere 400 degrees Celsius into
Row carbonization 3h hours, obtains three-dimensional porous Si-C composite material.
SEM test:
Cellular network pore structure is presented in material near-spherical structure it can be seen from Fig. 1, surface, and material size distribution is equal
Even, reasonable, partial size is between (5~15) μm.
2) physicochemical property and its button cell test:
Respectively by Examples 1 to 3 and comparative example gained lithium ion battery negative material be assembled into button cell A1, A2,
A3,B1；Preparation method are as follows: add binder, conductive agent and solvent in negative electrode material, be stirred slurrying, be coated in copper
Obtained by drying, rolling on foil, binder used is LA132 binder, and conductive agent SP, negative electrode material is respectively embodiment 1
~3 and the negative electrode material prepared of comparative example, solvent NMP, its ratio be: negative electrode material: SP:PVDF:NMP=95g:1g:
4g:220mL；Electrolyte is LiPF6/EC+DEC (1:1), and metal lithium sheet is 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 blue electricity CT2001A type cell tester, charging/discharging voltage range is 0.005V to 2.0V, charge-discharge velocity 0.1C.
See Table 1 for details -2:
Wherein: GBT_245332009 " silicon/carbon/graphite in lithium ion batteries class negative electrode material " tests its material according to national standards
Specific surface area and tap density.
Table 1, embodiment and comparative example buckle electrical testing compared with
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Tap density (g/cm3) | 0.78 | 0.76 | 0.75 | 1.12 |
| Specific capacity (mAh/g) | 958.6 | 955.4 | 954.5 | 547.6 |
| First charge discharge efficiency (%) | 89.5 | 89.2 | 88.1 | 87.4 |
| Specific surface area (g/m2) | 20.4 | 19.8 | 18.3 | 10.3 |
| Multiplying power (5C/1C, %) | 93.1 | 92.1 | 91.2 | 85.1 |
As can be seen from Table 1, the tap density for the material that embodiment is prepared is significantly lower than comparative example, the reason for this is that
Three-dimensional porous carbon material has tap density small, and hole is more, to reduce the tap density of its material, while porous structure has
High specific surface area, while it is that abundance is provided in its charge and discharge process that porous structure carbon material, which can store more electrolyte,
Lithium ion, to improve its high rate performance.
Compared with table 2, embodiment are held with the specific surface of comparative example and its hole
As can be seen from Table 2, the specific surface area and Kong Rong for the three-dimensional porous Si-C composite material that embodiment is prepared are greater than
Comparative example improves the specific surface area of its material the reason for this is that having high Nano/micron hole using three-dimensional porous carbon material,
And therefore improve the Kong Rong of its material.
3) soft-package battery is tested:
Respectively using embodiment 1, embodiment 2, embodiment 3 and comparative example resulting materials as negative electrode material, with LiFePO4
It is electrolyte using LiPF6/EC+DEC (volume ratio 1:1, concentration 1.3mol/L) for positive electrode, 2400 film of Celgard is
Diaphragm prepares 5Ah soft-package battery C1, C2, C3 and D1 and its corresponding cathode pole piece, and tests the imbibition of its cathode pole piece
Liquid-keeping property, pole piece be least, cycle performance and its surface resistance.
The imbibition liquid-keeping property contrast table of 3 different materials pole piece of table
From table 3 it can be seen that the imbibition liquid-keeping property of negative electrode material obtained by Examples 1 to 3 is apparently higher than comparative example, test
The result shows that negative electrode material of the invention imbibition liquid-keeping property with higher, reason are: three-dimensional porous Si-C composite material
With high specific surface area and its hole configurations, more electrolyte can be stored.
The circulation of 4 different materials of table compares figure
| Battery | Negative electrode material | Recycle 500 capacity retention ratios (%) |
| C1 | Embodiment 1 | 92.62 |
| C2 | Embodiment 2 | 91.78 |
| C3 | Embodiment 3 | 90.39 |
| D1 | Comparative example | 85.55 |
The cycle performance curve graph of the soft-package battery of 4 gained negative electrode material of table preparation, as can be seen that embodiment is electric in table
The cycle performance in pond is obviously due to comparative example, the reason for this is that embodiment material has high specific surface area, in charge and discharge process
Storage and release electrolyte, improve its cycle performance.
Embodiment two: a kind of three-dimensional porous silicon-carbon composite cathode material, the raw material including following number: 75 parts of ethyl alcohol is gone
75 parts of ionized water, γ -15 parts of diethylenetriamine hydroxypropyl methyl dimethoxysilane, 25 parts of acetic acid, 25 parts of sodium acetate, foamy carbon
110 parts of calomel of 80 parts, 110 parts of platinized platinum and saturation.
A kind of preparation method of three-dimensional porous silicon-carbon composite cathode material, comprising the following steps:
1) 75 parts of ethyl alcohol, 75 parts of deionized water and γ -15 parts of diethylenetriamine hydroxypropyl methyl dimethoxysilane are mixed
It after uniformly, is adjusted using 25 parts of acetic acid and 25 parts of sodium acetate and arrives pH value PH=6.5-7, be hydrolyzed to obtain silane later mixed
Close liquid A；
2) oxidation foamy carbon is obtained by oxygen treatments applied modified (flow 10ml/min, time 60min) by 80 parts of foamy carbon,
As working electrode, 110 parts of platinized platinum is, to electrode, 110 parts of calomel of saturation is, to electrode, silane mixture liquid A are electrolyte；
3) by constant-voltage method (voltage 2V, time 60min), in its oxidation foam carbon surface deposit silicon compounds, Zhi Houtong
Cross deionized water cleaning, 80 degrees Celsius of vacuum drying and are transferred in tube furnace, under argon inert atmosphere 400 degrees Celsius into
Row carbonization 3h hours, obtains three-dimensional porous Si-C composite material.
Embodiment three: a kind of three-dimensional porous silicon-carbon composite cathode material, the raw material including following number: 100 parts of ethyl alcohol is gone
100 parts of ionized water, γ -20 parts of diethylenetriamine hydroxypropyl methyl dimethoxysilane, 30 parts of acetic acid, 30 parts of sodium acetate, foamy carbon
120 parts of calomel of 90 parts, 120 parts of platinized platinum and saturation.
A kind of preparation method of three-dimensional porous silicon-carbon composite cathode material, comprising the following steps:
1) 100 parts of ethyl alcohol, 100 parts of deionized water and γ -20 parts of diethylenetriamine hydroxypropyl methyl dimethoxysilane is mixed
After closing uniformly, is adjusted using 30 parts and 30 parts of sodium acetate of acetic acid and arrive pH value PH=6.5-7, be hydrolyzed to obtain silane later
Mixed liquor A；
2) oxidation foamy carbon is obtained by oxygen treatments applied modified (flow 10ml/min, time 60min) by 90 parts of foamy carbon,
As working electrode, 120 parts of platinized platinum is, to electrode, 120 parts of calomel of saturation is, to electrode, silane mixture liquid A are electrolyte；
3) by constant-voltage method (voltage 2V, time 60min), in its oxidation foam carbon surface deposit silicon compounds, Zhi Houtong
Cross deionized water cleaning, 80 degrees Celsius of vacuum drying and are transferred in tube furnace, under argon inert atmosphere 400 degrees Celsius into
Row carbonization 3h hours, obtains three-dimensional porous Si-C composite material.
The beneficial effects of the present invention are: the three-dimensional porous silicon-carbon composite cathode material and preparation method thereof, by configuring ammonia
Base silane solution is deposited on foam carbon surface by electrochemical deposition method later, its silane compound is made to be deposited on foamy carbon
Between hole and surface, 400 degrees Celsius of carbonizations later form silicon oxide compound after making the cracking carbonization of its silane compound, and at it
On the one hand the coated porous carbon material in surface reduces the expansion in charge and discharge process, its electric conductivity is on the other hand improved, using oxidation
Foamy carbon is matrix, and can form amide group with amino silane and improve fastness between its material, avoids charge and discharge
Separation in journey between foamed carbon material and silicon oxide compound improves its cycle performance, by by ethyl alcohol, deionized water and amino
Silane organic compound after mixing, is adjusted to pH value PH=6.5-7 using acetic acid and sodium acetate, is hydrolyzed to obtain later
It obtains silane mixture liquid A and foamy carbon is obtained into oxidation foamy carbon by the way that oxygen treatments applied is modified, as working electrode, platinized platinum is pair
Electrode, saturation calomel are to electrode, and silane mixture liquid A is electrolyte, and preparation process is controllable, and consistency is high and environmentally friendly.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of three-dimensional porous silicon-carbon composite cathode material, which is characterized in that the raw material including following number: ethyl alcohol 50-100
Part, 50-100 parts of deionized water, 10-20 parts of amino silane organic compound, 20-30 parts of acetic acid, 20-30 parts of sodium acetate, foam
Calomel 100-120 parts of 70-90 parts of carbon, 100-120 parts of platinized platinum and saturation.
2. a kind of three-dimensional porous silicon-carbon composite cathode material according to claim 1, which is characterized in that the amino silane
10-20 parts of organic compound for aminopropyltriethoxy diethoxy silane, γ-diethylenetriamine hydroxypropyl methyl dimethoxysilane,
N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, N- aminoethyl -3- aminopropyltriethoxy dimethoxysilane and 3- amino
One of propyl-triethoxysilicane.
3. a kind of preparation method of three-dimensional porous silicon-carbon composite cathode material, which comprises the following steps:
1) after mixing by 10-20 parts of 50-100 parts of ethyl alcohol, 50-100 parts of deionized water and amino silane organic compound, make
It is adjusted with 20-30 parts and sodium acetate 20-30 parts of acetic acid and arrives pH value PH=6.5-7, be hydrolyzed to obtain silane mixture later
Liquid A；
2) oxidation foamy carbon is obtained by the way that oxygen treatments applied is modified by 70-90 parts of foamy carbon, as working electrode, platinized platinum 100-120
Part is, to electrode, calomel 100-120 parts of saturation is, to electrode, silane mixture liquid A is electrolyte；
3) by electrochemical deposition method, foam carbon surface deposit silicon compounds is aoxidized at it, later by cleaning and drying, and are turned
It moves on in tube furnace, carries out carbonization 3h hours for 400 degrees Celsius under an inert atmosphere, obtain three-dimensional porous Si-C composite material.
4. a kind of preparation method of three-dimensional porous silicon-carbon composite cathode material according to claim 3, which is characterized in that institute
The electrochemical deposition method stated is one of cyclic voltammetry, constant flow method and constant-voltage method.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110176598A (en) * | 2019-06-27 | 2019-08-27 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery and preparation method thereof |
| CN113353911A (en) * | 2021-03-26 | 2021-09-07 | 万向一二三股份公司 | Porous carbon material added into silicon-based negative electrode, silicon-based negative electrode and lithium ion battery |
| CN114709390A (en) * | 2022-04-01 | 2022-07-05 | 蔚来汽车科技(安徽)有限公司 | Silicon anode material, secondary battery and device |
-
2019
- 2019-03-22 CN CN201910220756.XA patent/CN109873151A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110176598A (en) * | 2019-06-27 | 2019-08-27 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery and preparation method thereof |
| CN110176598B (en) * | 2019-06-27 | 2022-03-22 | 蜂巢能源科技有限公司 | Negative electrode material of lithium ion battery and preparation method thereof |
| CN113353911A (en) * | 2021-03-26 | 2021-09-07 | 万向一二三股份公司 | Porous carbon material added into silicon-based negative electrode, silicon-based negative electrode and lithium ion battery |
| CN113353911B (en) * | 2021-03-26 | 2022-12-13 | 万向一二三股份公司 | Porous carbon material added into silicon-based negative electrode, silicon-based negative electrode and lithium ion battery |
| CN114709390A (en) * | 2022-04-01 | 2022-07-05 | 蔚来汽车科技(安徽)有限公司 | Silicon anode material, secondary battery and device |
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Application publication date: 20190611 |