CN108807927A - A kind of silicon-carbon composite cathode material and preparation method thereof - Google Patents
A kind of silicon-carbon composite cathode material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of silicon-carbon composite cathode material and preparation method thereof, the silicon-carbon composite cathode material is nano-silicon/C/M/ organic carbon source composite materials, wherein C is carbon material, and M is metal chloride；The silicon-carbon composite cathode material is added metal chloride, is dispersed in organic carbon source using nano-silicon and carbon material as raw material, through high temperature cabonization, broken obtains.The advantage of the invention is that：Silicon-carbon composite cathode material of the present invention, being used as lithium ion battery negative material, there is high power capacity, high magnification, high circulation stability greatly to improve the chemical property of pure silicon；And preparation method of the present invention is simple, production procedure is shorter, and no harsh conditions, cost is relatively low, is easy to industrialize.
Description
Technical field
The invention belongs to lithium ion battery negative material field, more particularly to a kind of lithium ion power and energy-storage battery silicon
Carbon compound cathode materials and preparation method thereof.
Background technology
With the fast development in power train in vehicle application lithium ion battery market, people want the performance of lithium ion battery negative material
Seek the higher standard that also proposed, high power capacity, high magnification, long circulation life lithium ion battery negative material become industry development
Direction, traditional commercial lithium-ion batteries mainly use graphite-like carbon material as negative material.However, carbons cathode material
Material is relatively low because of its specific capacity（372mAh/g）The safety issue come with the lithium string of deposits prevents it from meeting power type and high power capacity
Lithium ion battery is high-power, high power capacity requirement, thus need to research and develop the high-energy density of alternative carbon material, high safety performance,
The novel cathode material for lithium ion battery of long circulation life.Silicon is as a kind of novel cathode material for lithium ion battery, because of its theory
Specific capacity is high（4200mAh/g）And it attracts attention.But its volume expansion present in charge and discharge process（400%）
And cause active particle dusting that negative pole structure irreversibility is caused to destroy, and then cause capacity quickly to decline because losing electrical contact
Subtract.
Therefore, researching and developing a kind of high power capacity, high magnification, long circulation life lithium ion battery negative material and preparation method thereof is
Industry is had to go to the toilet technical barrier to be solved.
Invention content
The technical problem to be solved in the present invention is to provide a kind of high power capacity, high magnification, long circulation life lithium ion battery silicons
Carbon compound cathode materials and preparation method thereof and preparation method thereof.
In order to solve the above technical problems, the technical scheme is that：A kind of silicon-carbon composite cathode material, innovative point exist
In：The silicon-carbon composite cathode material is nano-silicon/C/M/ organic carbon source composite materials, wherein C is carbon material, and M is metal chlorine
Compound.
Further, the carbon material is carbon nanotube, graphene, carbon fiber, natural graphite, artificial graphite, interphase
One or more of carbosphere and fullerene.
Further, the metal chloride is ZnCl2、FeCl3、CoCl2、NiCl2、CuCl2、MnCl2, NaCl and KCl
One or more of.
Further, the organic carbon source is epoxy resin, phenolic resin, carboxymethyl cellulose, pitch, ethyl-methyl carbon
Acid esters, polyvinyl alcohol, polystyrene, polymethyl methacrylate, polytetrafluoroethylene (PTFE), Kynoar, polyacrylonitrile, butylbenzene rubber
Glue, polyvinyl chloride, polyethylene, polyethylene oxide, polypropylene oxide, polyethylene glycol succinate, poly- decanedioic acid ethylene glycol, poly- second
Glycol imines, polyacetylene gather to benzene, polyaniline, polypyrrole, polyacene, poly m-phenylene diamine, poly-phenylene vinylene (ppv), polythiophene, gather
One or more of acrylonitrile, polyimides and polyphenylene sulfide.
A kind of preparation method of above-mentioned silicon-carbon composite cathode material, innovative point are：The silicon-carbon composite cathode material
Material is added metal chloride, is dispersed in organic carbon source using nano-silicon and carbon material as raw material, through high temperature cabonization, is crushed
It arrives；It is as follows：
（1）Nano-silicon and carbon material are mixed in metal chloride solutions, and heated, slurry is uniformly mixing to obtain；
（2）By step（1）Obtained slurry continues heating and is concentrated, obtains solid phase intermediate, then cool to room temperature；
（3）By step（2）It is added in organic carbon source liquid phase, stirs evenly among obtained solid, obtain slurry；
（4）By step（3）Obtained slurry heating is cured, and gel phase is obtained；
（5）By step（4）Obtained gel mutually leads to protection gas and is sintered in the high temperature environment, obtains sintering phase, will finally burn
Knot is mutually crushed, and obtains silicon-carbon composite cathode material.
Further, the step（1）The mass ratio of metal chloride and water is 1 in middle metal chloride solutions：:500
~5000, the mass ratio of nano-silicon and carbon material is 1:1~9, the mass ratio of nano-silicon and metal chloride is 450:1~9:1,
Step（1）In heating temperature be 35 DEG C~230 DEG C, mixing speed be the r/min of 100r/min~2200.
Further, the step（2）In heating temperature be 35 DEG C~230 DEG C.
Further, the step（3）The dosage of middle organic carbon source is step（1）0.6~2 times of middle nano-silicon, step
（3）In mixing speed be the r/min of 100r/min~2200.
Further, the step（4）In heating temperature be 35 DEG C~230 DEG C.
Further, the step（5）Middle protection gas is one kind in nitrogen, helium, neon, argon gas, Krypton and xenon,
It is 0.1 m to protect the flow of gas3The m of/h~6.53/ h, step（5）In hot environment be with the liter of 1 DEG C/min~20 DEG C/min
Warm rate rises to 200 DEG C~1200 DEG C, and keeps the temperature 0.5h~for 24 hours, step（5）In particle size after cracking be 1.5 μm~66.5 μm.
The advantage of the invention is that：
（1）Silicon-carbon composite cathode material of the present invention, using nano-silicon as capacity provider, chloride is buffered as volume to be situated between
Matter, carbon material play capacity auxiliary, conductive network and reduce the stress that silicon substrate generates in charge and discharge process and broken to material structure
Bad effect, and then silicon-carbon composite cathode material of the present invention is used as lithium ion battery negative material with high power capacity, high magnification, Gao Xun
Ring stability greatly improves the chemical property of pure silicon；
（2）The preparation method of silicon-carbon composite cathode material of the present invention, preparation method is simple, and production procedure is shorter, no harsh conditions,
Cost is relatively low, is easy to industrialize；And the silicon-carbon composite cathode material prepared by the preparation method, particle size are equal
It is even, good dispersion.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is 1 silicon-carbon composite cathode material electromicroscopic photograph of the embodiment of the present invention.
Fig. 2 is 1 silicon-carbon composite cathode material high power stereoscan photograph of the embodiment of the present invention.
Fig. 3 is the X- x ray diffraction collection of illustrative plates of 1 silicon-carbon composite cathode material of the embodiment of the present invention.
Fig. 4 is the charge-discharge performance curve of 1 silicon-carbon composite cathode material of the embodiment of the present invention.
Specific implementation mode
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment 1
0.01gZncl2 is configured to the aqueous solution of 50ml, then 1.09g nano-silicons are added with 8.91g carbon nanotubes above-mentioned molten
Liquid stirs 1h at 45 DEG C with 150r/min, and after stirring evenly, then heating is concentrated into solid phase at 60 DEG C, and 2g is added in solid phase
Liquid-state epoxy resin, and 1h is stirred with the mixing speed of 450r/min, then cure to obtain gel phase at 95 DEG C again, gel is communicated
Nitrogen, flow 1.2m3/ min rises to 500 DEG C with the heating rate of 10 DEG C/min, and keeps the temperature 8h, and being finally down to room temperature will be sintered
Object is crushed to 3.5 μm of silicon-carbon composite cathode material.
Embodiment 2
0.03gFecl2 is configured to the aqueous solution of 50ml, then 1.87g nano-silicons are added with 8.13g graphenes above-mentioned molten
Liquid stirs 1h at 60 DEG C with 300r/min, and after stirring evenly, then heating is concentrated into solid phase at 120 DEG C, and 1g is added in solid phase
Liquid phenolic resin, and 1h is stirred with the mixing speed of 600r/min, then cure to obtain gel phase at 100 DEG C again, by gel phase
Helium injection gas, flow 1.6m3/ min rises to 650 DEG C with the heating rate of 12 DEG C/min, and keeps the temperature 10.5h, and being finally down to room temperature will
Sinter is crushed to 9.5 μm of silicon-carbon composite cathode material.
Embodiment 3
0.05gCocl2 is configured to the aqueous solution of 50ml, then by 2.75g nano-silicons and 3.15g natural graphites, 4.1g carbon fibers
Above-mentioned solution is added in dimension, and 1h is stirred with 550r/min at 75 DEG C, and after stirring evenly, then heating is concentrated into solid phase at 95 DEG C,
2.3g liquid carboxymethyl celluloses are added in solid phase, and 1h is stirred with the mixing speed of 750r/min, are then cured again at 145 DEG C
Gel phase is obtained, gel is communicated into neon, flow 2.4m3/ min rises to 950 DEG C with the heating rate of 14 DEG C/min, and keeps the temperature
12.5h is finally down to the silicon-carbon composite cathode material that sinter is crushed to 27.5 μm by room temperature.
Embodiment 4
0.07gNicl2 is configured to the aqueous solution of 50ml, then by 3.38g nano-silicons and 2.32g artificial graphites, 4.1g graphite
Above-mentioned solution is added in alkene, and 1h is stirred with 450r/min at 100 DEG C, and after stirring evenly, then heating is concentrated into admittedly at 115 DEG C
Solid phase is added 3.5g liquid pvas, and stirs 1h with the mixing speed of 800r/min by phase, is then cured again at 120 DEG C
Gel phase is obtained, gel is communicated into argon gas, flow 0.8m3/ min rises to 1050 DEG C with the heating rate of 16 DEG C/min, and keeps the temperature
16.5h is finally down to the silicon-carbon composite cathode material that sinter is crushed to 35.5 μm by room temperature.
Embodiment 5
0.09gCucl2 is configured to the aqueous solution of 50ml, then by 3.97g nano-silicons and 3.01g carbonaceous mesophase spherules, 3.02
Above-mentioned solution is added in carbon nanotube, and 1h is stirred with 800r/min at 140 DEG C, after stirring evenly, then concentration is heated at 130 DEG C
To solid phase, 2.97g liquid polypropylene nitriles are added in solid phase, and 1h is stirred with the mixing speed of 900r/min, then again at 155 DEG C
Cure to obtain gel phase, gel is communicated into Krypton, flow 3.2m3/ min rises to 850 DEG C with the heating rate of 15 DEG C/min, and protects
Warm 16h is finally down to the silicon-carbon composite cathode material that sinter is crushed to 37.5 μm by room temperature.
Embodiment 6
0. 1gNacl is configured to the aqueous solution of 50ml, then by 4.63g nano-silicons and 3.06g carbon nanotubes, 2.31g graphite
Above-mentioned solution is added in alkene, and 1h is stirred with 800r/min at 160 DEG C, and after stirring evenly, then heating is concentrated into admittedly at 205 DEG C
Solid phase is added 2.81g liquid Kynoar, and stirs 1h with the mixing speed of 1450r/min by phase, then again at 190 DEG C
Cure to obtain gel phase, gel is communicated into xenon, flow 6m3/ min rises to 1200 DEG C with the heating rate of 20 DEG C/min, and keeps the temperature
20h is finally down to the silicon-carbon composite cathode material that sinter is crushed to 45.5 μm by room temperature.
The silicon-carbon composite cathode material of embodiment 1 is observed, the result is shown in Figure 1.The silicon-carbon composite cathode material of the present invention
Material is near-spherical particle and random shape, and even particle size, particle size range concentrates on 18um or so in 5-48um, grain size.
High power scanning electron microscope observation is carried out to the silicon-carbon composite cathode material of embodiment 1, as a result sees Fig. 2, silicon of the invention
Carbon compound cathode materials surface topography is smooth, and the processing performance of electrode slurry can be improved as negative material.
XRD detections are carried out to the silicon-carbon composite cathode material of embodiment 1, as a result see that Fig. 3, Fig. 3 show Si-C composite material
The diffraction maximum feature for showing apparent carbon material shows that material clad structure is more complete, and this complete structure can be effective
The side reaction between material and electrolyte is avoided, charge efficiency is improved.
Use the silicon-carbon composite cathode material of embodiment 1 as electrode, lithium foil is used as to electrode fabrication button cell.Its charge and discharge
Electric cycle performance curve is shown in Fig. 4, from fig. 4, it can be seen that synthesized silicon-carbon composite cathode material initial discharge capacity is 710mAh/g,
Primary charging capacity is 605mAh/g, and charging capacity is 642mAh/g after recycling 50 times, shows that the material of synthesis has preferably appearance
Measure performance and cycle performance.
The basic principles and main features and advantages of the present invention of the present invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (10)
1. a kind of silicon-carbon composite cathode material, it is characterised in that：The silicon-carbon composite cathode material is nano-silicon/C/M/ organic carbons
Source composite material, wherein C is carbon material, and M is metal chloride.
2. silicon-carbon composite cathode material according to claim 1, it is characterised in that：The carbon material is carbon nanotube, stone
One or more of black alkene, carbon fiber, natural graphite, artificial graphite, carbonaceous mesophase spherules and fullerene.
3. silicon-carbon composite cathode material according to claim 1, it is characterised in that：The metal chloride is ZnCl2、
FeCl3、CoCl2、NiCl2、CuCl2、MnCl2, one or more of NaCl and KCl.
4. silicon-carbon composite cathode material according to claim 1, it is characterised in that：The organic carbon source be epoxy resin,
Phenolic resin, carboxymethyl cellulose, pitch, ethyl methyl carbonate, polyvinyl alcohol, polystyrene, polymethyl methacrylate,
Polytetrafluoroethylene (PTFE), Kynoar, polyacrylonitrile, butadiene-styrene rubber, polyvinyl chloride, polyethylene, polyethylene oxide, polycyclic oxygen third
Alkane, polyethylene glycol succinate, poly- decanedioic acid ethylene glycol, polyethylene glycol imines, polyacetylene, it is poly- to benzene, polyaniline, polypyrrole,
Polyacene, poly m-phenylene diamine, poly-phenylene vinylene (ppv), polythiophene, polypropylene be fine, polyimides and one kind or several in polyphenylene sulfide
Kind.
5. a kind of preparation method of silicon-carbon composite cathode material described in claim 1, it is characterised in that：The silicon-carbon Compound Negative
Pole material is added metal chloride, is dispersed in organic carbon source using nano-silicon and carbon material as raw material, through high temperature cabonization, breaks
It is broken to obtain；It is as follows：
（1）Nano-silicon and carbon material are mixed in metal chloride solutions, and heated, slurry is uniformly mixing to obtain；
（2）By step（1）Obtained slurry continues heating and is concentrated, obtains solid phase intermediate, then cool to room temperature；
（3）By step（2）It is added in organic carbon source liquid phase, stirs evenly among obtained solid, obtain slurry；
（4）By step（3）Obtained slurry heating is cured, and gel phase is obtained；
（5）By step（4）Obtained gel mutually leads to protection gas and is sintered in the high temperature environment, obtains sintering phase, will finally burn
Knot is mutually crushed, and obtains silicon-carbon composite cathode material.
6. the preparation method of silicon-carbon composite cathode material according to claim 5, it is characterised in that：The step（1）In
The mass ratio of metal chloride and water is 1 in metal chloride solutions：:500~5000, the mass ratio of nano-silicon and carbon material is
1:1~9, the mass ratio of nano-silicon and metal chloride is 450:1~9:1, step（1）In heating temperature be 35 DEG C~230
DEG C, mixing speed is the r/min of 100r/min~2200.
7. the preparation method of silicon-carbon composite cathode material according to claim 5, it is characterised in that：The step（2）In
Heating temperature be 35 DEG C~230 DEG C.
8. the preparation method of silicon-carbon composite cathode material according to claim 5, it is characterised in that：The step（3）In
The dosage of organic carbon source is step（1）0.6~2 times of middle nano-silicon, step（3）In mixing speed be 100r/min~2200
r/min。
9. the preparation method of silicon-carbon composite cathode material according to claim 5, it is characterised in that：The step（4）In
Heating temperature be 35 DEG C~230 DEG C.
10. the preparation method of silicon-carbon composite cathode material according to claim 5, it is characterised in that：The step（5）In
Protection gas is one kind in nitrogen, helium, neon, argon gas, Krypton and xenon, and it is 0.1 m to protect the flow of gas3The m of/h~6.53/
H, step（5）In hot environment be with the heating rate of 1 DEG C/min~20 DEG C/min to rise to 200 DEG C~1200 DEG C, and keep the temperature
0.5h~for 24 hours, step（5）In particle size after cracking be 1.5 μm~66.5 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110615997A (en) * | 2019-08-26 | 2019-12-27 | 深圳市华星光电技术有限公司 | Composite material, preparation method thereof and display panel |
| CN110854371A (en) * | 2019-11-26 | 2020-02-28 | 宁夏百川新材料有限公司 | Carbon composite negative electrode material and preparation method thereof |
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| CN103367727A (en) * | 2013-07-12 | 2013-10-23 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium ion battery silicon-carbon anode material and preparation method thereof |
| CN105742599A (en) * | 2016-03-18 | 2016-07-06 | 苏州协鑫集成科技工业应用研究院有限公司 | Silicon carbon composite material, fabrication method thereof, anode material and battery |
| CN107634208A (en) * | 2017-09-20 | 2018-01-26 | 赣州市瑞富特科技有限公司 | A kind of preparation method of lithium ion battery silicon-carbon cathode material |
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| CN103346305A (en) * | 2013-07-01 | 2013-10-09 | 华南师范大学 | Preparation and application of lithium battery silicon-carbon composite material taking synthetic graphite as carrier |
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| CN110615997A (en) * | 2019-08-26 | 2019-12-27 | 深圳市华星光电技术有限公司 | Composite material, preparation method thereof and display panel |
| CN110615997B (en) * | 2019-08-26 | 2021-11-23 | Tcl华星光电技术有限公司 | Composite material, preparation method thereof and display panel |
| CN110854371A (en) * | 2019-11-26 | 2020-02-28 | 宁夏百川新材料有限公司 | Carbon composite negative electrode material and preparation method thereof |
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