CN109638270A - A kind of silicon-graphene-porous carbon composite electrode material and its preparation method and application - Google Patents
A kind of silicon-graphene-porous carbon composite electrode material and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of silicon-graphene-porous carbon composite electrode materials and its preparation method and application.In electrode material, graphene and silicon nanoparticle are in close contact, and silicon nanoparticle high degree of dispersion, carbon is at unformed netted, coated Si graphene complex.The preparation method includes: that 3 SiC 2/graphite alkene compound will be obtained after nano-silicon and graphene mixing and ball milling；It disperses 3 SiC 2/graphite alkene compound and alkaline earth oxide in Dopamine hydrochloride solution, is heat-treated after filtration drying, is post-processed after heat treatment, silicon-graphene-porous carbon composite electrode material is made.The present invention also provides the silicon-graphene-porous carbon composite electrode materials to prepare the application in negative electrode of lithium ion battery.The porous carbon composite electrode material of silicon-graphene-of the present invention has many advantages, such as reversible capacity height, good cycling stability, is produced on a large scale.
Description
Technical field
The invention belongs to lithium ion battery negative material field, in particular to a kind of high capacity, long-life, low cost
Silicon-graphene-porous carbon composite electrode material and its preparation method and application.
Background technique
As the emerging markets such as electric car (EV), mixed power electric car (HEV) occur, to lithium ion battery
(LIB) great demand is generated.
Commercial negative electrode material is mainly the carbon material of carbon element of graphite class at present, and theoretical maximum specific capacity is only
372mAh/g constrains further increasing for lithium battery capacity.Silicon is due to its high theoretical capacity, about 4200mAh/g
(Li4.4Si alloy), it is resourceful, it is the most promising electrode material of a new generation.The lithiumation platform voltage of silicon electrode is than graphite electricity
The platform voltage of pole is high, can effectively avoid the formation of Li dendrite, promote the safety of lithium ion battery.But silicon based electrode is embedding
During lithium takes off lithium, the expansion of silicon based electrode volume, about 300% will lead to, so as to cause electrode material structural damage
The decline of peeling, dusting, conductivity with electrode, and then battery capacity decays rapidly.
Summary of the invention
Goal of the invention: for the electric conductivity for promoting silicon electrode, delay the generation of silicon electrode dusting, cracking, the present invention is prepared for
A kind of porous carbon net is coated on silicon-graphene-porous carbon electrode material of 3 SiC 2/graphite alkene compound；Another object of the present invention
It is to provide the silicon-graphene-porous carbon electrode material preparation method and application.
Technical solution:
A kind of silicon-graphene-porous carbon composite electrode material, have the following structure: graphene is tight with silicon nanoparticle
Contiguity touching, silicon nanoparticle high degree of dispersion, carbon are covered in 3 SiC 2/graphite alkene compound at unformed netted.
The present invention also provides the silicon-graphene-porous carbon composite electrode material preparation methods, comprising: will
3 SiC 2/graphite alkene compound is obtained after nano-silicon and graphene mixing and ball milling；3 SiC 2/graphite alkene compound and alkaline earth oxide are dispersed
It in Dopamine hydrochloride solution, is heat-treated after filtration drying, is post-processed after heat treatment, silicon-graphene-is made
Porous carbon composite electrode material.
The mass ratio of the nano-silicon and graphene is 3~6:1, and nano-silicon quality is too low, can make electrode material capacity
Not high, the excessively high meeting of nano-silicon quality is so that the reduction of electrode material stability, the preferred mass ratio of the nano silica fume and graphene
For 4~5:1, further preferably 4.5:1.
The time of the ball milling is 2~15 hours.Ball-milling Time is too short to be unfavorable for the uniform mixed of nano silica fume and graphene
It closes, too long in irregular shapeization that will lead to silicon particle of Ball-milling Time, the ball milling preferred time is 3~10 hours, further
Preferably 6h.
The mass ratio of the 3 SiC 2/graphite alkene compound and alkaline earth oxide is 1:0.1~3.5.Alkaline earth oxide
If magnesia powder is pore-creating template, when content is too low, the Kong Rong of composite material is smaller, and it is empty that enough expansions cannot be provided for silicon
Between；When too high levels, the composite material specific surface area prepared is excessive, and coulombic efficiency reduces for the first time；It is preferred that the 3 SiC 2/graphite alkene
The mass ratio of compound and alkaline earth oxide is 1:1~3, further preferably 1:1.
The magnesia powder partial size is 10~500nm, is further 30~200nm, but it is not limited to this.
The concentration of the Dopamine hydrochloride solution is 1~20mM.When Dopamine hydrochloride solution concentration is excessively high, combination electrode
Material phosphorus content will increase, and discharge capacity can reduce.But bar amine aqueous solution concentration is too low, the carbon content mistake in combination electrode material
It is low, it is not easy to form the reticular structure of contact, stable charge/discharge is not high.It is preferred that the concentration of the Dopamine hydrochloride solution is 5
~15mM, further preferably 10mM.
The solvent of the Dopamine hydrochloride solution is standard tris buffer, and PH is 7~9.It is preferred that the tris that PH is 8.5 is slow
Fliud flushing is best for the covering property of Dopamine hydrochloride, and compared to other carbon materials for, the cladding of dopamine is more equal
It is even controllable, there is excellent performance.
When dispersion, stir process, the mixing time is 3~48 hours, and but it is not limited to this.Vacuum can be used after drying
Dry, the vacuum drying temperature is 80~105 DEG C, and soaking time is 8~10h.
When the heat treatment, 350~400 DEG C are warming up to 1~5 DEG C/min, 1~2 hour is kept the temperature, to guarantee hydrochloric acid DOPA
The stabilization of the interface of amine and composite particles, preventing from being rapidly heated leads to falling off for Dopamine hydrochloride and compound, Zhi Houzai
700~800 DEG C are warming up to 5~10 DEG C/min, Dopamine hydrochloride starts high temperature cabonization, 2~3 hours is kept the temperature, so that hydrochloric acid is more
Bar amine is sufficiently carbonized.It is further preferred that being warming up to 400 DEG C with 1 DEG C/min, 2 hours are kept the temperature, then 5 DEG C/min is warming up to 800
DEG C, heat preservation cools to room temperature with the furnace after 3 hours, inventor has found the program effect of above-mentioned heat treatment most by a large amount of research
It is good.
It needs to post-process product after high temperature cabonization, the post-processing is that product acid such as hydrochloric acid solution is clear
It washes, to remove removing template alkaline earth oxide, then filtration drying.
The present invention also provides the silicon-graphene-porous carbon composite electrode materials to prepare lithium ion battery negative
Application in extremely.
The present invention also provides the silicon-graphene-porous carbon electrode materials in preparing negative electrode of lithium ion battery
Using.
Compared with prior art, the invention has the benefit that
Silicon-graphene-porous carbon electrode material good cycling stability provided by the invention, electric conductivity is excellent, is prepared into
This is low and environmental-friendly.
For the present invention by ball-milling treatment, silicon-graphene-of alkali or alkaline earth metal oxide template pore-creating, acquisition is more
Hole carbon electrode material.Porous carbon net provides expansion space of the silicon in charge and discharge process, and to nano-silicon and graphene into
It has gone nanometer confinement, has substantially improved the stable circulation performance of silicon electrode.The addition of graphene significantly improves the ion of electrode
Conduction, improves the electric conductivity of electrode material, and can reduce the reunion of silicon particle, is that the reserved buffering of expansion of silicon is empty
Between.The doping of graphene provides more stable channel to the transmission of lithium ion, accelerates the transmission of lithium ion.Therefore, silicon-graphite
Alkene-porous carbon electrode material has higher electric conductivity, and first circulation coulombic efficiency than simple silicon porous carbon.
Detailed description of the invention
Fig. 1 is silicon-graphene-porous carbon materials scanning electron microscopic picture；
Fig. 2 is silicon-graphene-porous carbon materials transmission electron microscope picture；
Fig. 3 is silicon-graphene-porous carbon materials XRD test chart；
Fig. 4 is the electrochemical cycle stability comparison of silicon-graphene-porous carbon materials and commodity nano silicon material；
Fig. 5 is the AC impedance comparison of silicon-graphene-porous carbon materials and commodity nano silicon material.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention
The modification of form falls within the application range as defined in the appended claims.
The partial size for the commodity nano-silicon that following embodiment uses is 20-60nm, and nano magnesia powder diameter is 50nm, graphite
Alkene is commercial graphene, commercial Dopamine hydrochloride, trishydroxymethylaminomethane (CAS:77-86-1).
Embodiment 1
1, silicon-graphene-porous carbon materials preparation
Commercial trishydroxymethylaminomethane 0.0969g is weighed, 80ml deionized water is added, stirring to solution is clarified, configuration
Standard tris buffer (PH is about 8.5).
It is in mass ratio that 4.5:1 carries out ball-milling treatment, ball mill model by commodity silicon nanoparticle and commercial graphene
QM-3SP2, Ball-milling Time 6h, ratio of grinding media to material 40:1, revolving speed 450r/min, the 3 SiC 2/graphite alkene compound that ball milling is obtained and
Nano magnesia is put into the standard tris buffer (Dopamine hydrochloride solution concentration is 10mM) that 37.5ml contains Dopamine hydrochloride,
3 SiC 2/graphite alkene compound (0.075g) and nano magnesia mass ratio are 1:1.Beaker equipped with sample is put in magnetic stirring apparatus
On, stirring for 24 hours, is put into vacuum oven after being filtered with alcohol washes, 100 DEG C drying 10 hours.
Gained drying sample, which is put into tube calciner, carries out high-temperature heat treatment, is warming up to 400 DEG C with 1 DEG C/min, heat preservation 2
Hour, then 5 DEG C/min is warming up to 800 DEG C, and heat preservation cooled to room temperature with the furnace after 3 hours.In high-temperature heat treatment process, whole process is logical
The Ar gas for entering 40-60sccm makees protective gas；Sample after carbonization is put into 3 hours of magnetic agitation in 1M HCl solution, with
The MgO particle in sample is removed, pore structure is obtained, after deionized water cleaning for several times, is filtered, gained powder is silicon-graphite
Alkene-porous carbon materials.
2, structure and performance detection
Electronic Speculum and transmission electron microscope observing are scanned to the silicon-graphene-porous carbon materials being prepared, as a result respectively such as
Shown in Fig. 1, Fig. 2.Scanning electron microscope can see electrode material surface in cellular, and be evenly distributed.Transmission electron microscope can be seen
Silicon particle and graphene are covered to porous carbon net, graphene and silicon nanoparticle are in close contact, and silicon particle is in inner part cloth
Uniformly.
XRD (X-ray diffraction) test is carried out to the silicon-graphene being prepared-porous carbon materials, test result is shown in Fig. 3.
What XRD was measured is simple silicon phase as the result is shown, since porous carbon is at unformed netted, is not displayed in XRD spectrum.
Usual graphene is also unformed state.
Take out silicon-graphene-porous carbon composite powder, conductive black super P and binder alginic acid obtained
Sodium 8:1:1 in mass ratio mixing is added appropriate amount of deionized water and is tuned into uniform slurry, coats (about 5 μm of thickness) in collector copper
On foil.The copper foil for being coated with sample is put into vacuum oven, 100 DEG C drying 10 hours.Sample after taking out drying, punching electricity
Pole piece, electrode slice diameter are 12mm.
Electro-chemical test carries out in 2032 type button cell systems, and electrolyte is 1M LiPF6It is dissolved in addition 2%VC
EC/DEC (ethylene carbonate/diethyl carbonate, the volume ratio 1:1) solution of (vinylene carbonate), is metal lithium sheet to electrode.
Stopping potential 0.01V (vs.Li/Li is first discharged to the current density of 200mA/g+), after standing 2min, then with 200mA/g
Current density charge to stopping potential 2V (vs.Li/Li+), obtain circulation volume figure (Fig. 4).
Silicon-graphene-porous carbon sample prepared by the present embodiment, 40 times circulation after specific discharge capacity be
1330.3mAh/g, simple nano-silicon only 560.78mAh/g after 40 circulations has compared to simple commodity nano-silicon significantly to be mentioned
It rises.
The electrochemical impedance spectroscopy of sample is tested by the CHI604E type Electrochemical Comprehensive Tester of Shanghai Chen Hua instrument company
It arrives, test frequency obtains ac impedance spectroscopy from 100kHz to 1Hz (see Fig. 5).Silicon-graphene-porous carbon materials electric charge transfer
Impedance value is 309.2 Ω, and the Charge-transfer resistance value of nano-silicon is 352.1 Ω, and silicon-graphene-porous carbon materials have lower
Charge-transfer resistance, therefore chemical property is more excellent.
The above-mentioned performance of the present invention first cycle efficieny compared with silicon-porous carbon materials gets a promotion, promotion nearly 20%, and
It is still able to maintain the high discharge capacity of 1330.3mAh/g after 40 circulations, is improved compared with silicon-porous carbon materials, is promoted close
14%.
Claims (8)
1. a kind of silicon-graphene-porous carbon composite electrode material, which is characterized in that have the following structure: graphene and nanometer
Silicon particle is in close contact, and silicon nanoparticle high degree of dispersion, carbon is at unformed netted, coated Si graphene complex.
2. silicon-graphene according to claim 1-porous carbon composite electrode material preparation method, which is characterized in that
It include: that 3 SiC 2/graphite alkene compound will be obtained after nano-silicon and graphene mixing and ball milling；By 3 SiC 2/graphite alkene compound and alkaline-earth metal oxygen
Compound is scattered in Dopamine hydrochloride solution, is heat-treated after filtration drying, is post-processed after heat treatment, is made
Silicon-graphene-porous carbon composite electrode material.
3. silicon-graphene according to claim 2-porous carbon composite electrode material preparation method, which is characterized in that
The mass ratio of the nano-silicon and graphene is 3~6:1；Ball-milling Time is 2~15 hours.
4. silicon-graphene according to claim 2-porous carbon composite electrode material preparation method, which is characterized in that
The mass ratio of the 3 SiC 2/graphite alkene compound and alkaline earth oxide is 1:0.1~3.5.
5. silicon-graphene according to claim 2-porous carbon composite electrode material preparation method, which is characterized in that
The concentration of the Dopamine hydrochloride solution is 1~20mM.
6. silicon-graphene according to claim 2-porous carbon composite electrode material preparation method, which is characterized in that
When heat treatment, 350~400 DEG C are warming up to 1~5 DEG C/min, keeps the temperature 1~2 hour, then 700 are warming up to 5~10 DEG C/min~
800 DEG C, keep the temperature 2~3 hours.
7. silicon-graphene according to claim 2-porous carbon composite electrode material preparation method, which is characterized in that
Alkaline earth oxide is magnesia；Acid is hydrochloric acid；The solvent of Dopamine hydrochloride solution is tris buffer.
8. silicon-graphene according to claim 1-porous carbon composite electrode material is in preparing negative electrode of lithium ion battery
Application.
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| CN110828814A (en) * | 2019-11-07 | 2020-02-21 | 东南大学 | Silicon-carbon-graphene electrode material with interlayer hollow double-shell structure, and preparation method and application thereof |
| CN111261864A (en) * | 2020-02-10 | 2020-06-09 | 马鞍山科达普锐能源科技有限公司 | Silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
| CN114122372A (en) * | 2021-11-10 | 2022-03-01 | 云南中晟新材料有限责任公司 | Low-expansion silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
| CN115836027A (en) * | 2021-04-16 | 2023-03-21 | 瓦克化学股份公司 | Silicon carbon composite particles |
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| CN114122372A (en) * | 2021-11-10 | 2022-03-01 | 云南中晟新材料有限责任公司 | Low-expansion silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
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Application publication date: 20190416 |