CN107611406A - A kind of preparation method of silicon/graphene/carbon composite negative pole material - Google Patents
A kind of preparation method of silicon/graphene/carbon composite negative pole material Download PDFInfo
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Abstract
A kind of preparation method of silicon/graphene/carbon composite negative pole material, comprises the following steps：（1）Nano silicon particles are evenly spread in absolute ethyl alcohol under supersound process；（2）By stirring the surface modification processing for adding TSL 8330 and carrying out silicon；（3）The nano silicon particles that dispersion liquid is modified by obtaining APS after centrifugation and drying, the APS nano silicon particles modified are scattered in absolute ethyl alcohol and form dispersion liquid, graphene solution are added dropwise under agitation, through centrifuge washing, freeze-drying process；（4）Composite coated in formation consistency of thickness on copper current collector together with after well mixed with polyvinyladine floride, and dried in vacuum drying chamber；（5）High-temperature heat treatment is carried out in an inert atmosphere.Gained negative material specific discharge capacity of the invention is high, and charge-discharge characteristic is good, and cyclical stability is higher；Technological process is simple, and silicon accounting is big in material, easily implements and is adapted to large-scale production.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of system of silicon/graphene/carbon composite negative pole material
Preparation Method.
Background technology
Lithium ion battery turns into just due to having the characteristics that high voltage, high-energy-density, long circulation life and environmentally friendly
Take the preferable supporting power supply of formula electronics, mobile product, electric automobile.Due to miniaturization of electronic products, high-energy-density, portable
The development of the growth requirement of change, especially smart mobile phone and new energy battery, more next is required to the energy density of lithium ion battery
Higher, the improvement to performance of lithium ion battery depends primarily on the raising of intercalation materials of li ions energy density and cycle life, and current
Theoretical capacity using materials such as graphite as the lithium ion battery of negative pole only has 372 mAh/g, far can not meet the daily life of people
To the demand of energy storage device in work, exploitation novel high-performance negative material is into the task of top priority.Research is found, silica-base material is answered
There is high specific capacity for negative electrode of lithium ion battery, wherein theoretical capacity can reach 3579 mAh/g, therefore, by silicon substrate
Material receives more and more attention as lithium ion battery negative material.
But using negative pole of the silicon materials as lithium ion battery, in the cyclic process of battery charging and discharging, Li-Si
The reversible generation of alloy will be along with huge Volume Changes, so as to cause the differentiation of silicium cathode material and split with decomposing
Seam, causes the avalanche of material structure and coming off for electrode material, and then causes electrode material to depart from conductive network, and internal resistance increases
Add, cause reversible capacity to be decayed rapidly, cause the drastically decline of the cycle performance of silicon cathode lithium ion battery.It is simultaneously because secondary anti-
The generation answered, substantial amounts of gas can be produced in charge and discharge process, easily cause the inside flatulence of battery.In view of the above-mentioned problems, grind
The persons of studying carefully try to explore the method for improving silicium cathode material circulation performance, such as reduce silicon materials grain diameters, formed porous material,
Silicon thin film material, silicon nanowires, silicon composite etc..Wherein relatively effective method is to be prepared into silicon based composite material to alleviate
Volumetric expansion in charge and discharge process, the method are had been widely used in the study on the modification of lithium ion battery negative material.
CN180094A discloses a kind of graphene coated silicium cathode material and preparation method, using the side of electrostatic self-assembled
Method by graphene coated in silicium cathode material surface, improve graphene coated silicon cathode lithium ion battery storage lithium specific capacity and
Cycle performance of battery.But graphene can not protect the efflorescence of silicon nanoparticle well.
CN105024076A discloses a kind of lithium ion battery negative material and its preparation method and application, and material is divided into two
Layer：Carbon core layer and silicon clad, it can effectively alleviate the expansion of silicon materials, so as to improve the cyclicity of battery material
Can, but simple carbon coating is to improving the ability of conductivity of composite material or limited.
The process described above can not fundamentally solve silicon materials negative electrode lithium ion battery body in charge and discharge process
Long-pending drastically expansion issues.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of preparation side of silicon/graphene/carbon composite negative pole material
Method, silicon/graphene/carbon composite negative pole material prepared by this method, can fundamentally solve silicon materials negative electrode lithium ion battery and exist
The drastically expansion issues of volume in charge and discharge process, so as to improve the efficiency for charge-discharge of silicon cathode lithium ion battery, extend and use
Life-span.
The technical solution adopted for the present invention to solve the technical problems is：A kind of silicon/graphene/carbon composite negative pole material
Preparation method, comprise the following steps：
（1）Nano silicon particles are evenly spread in absolute ethyl alcohol under supersound process, form nano silicon particles dispersion liquid；
（2）To step（1）In the nano silicon particles dispersion liquid of gained TSL 8330 is added by stirring（APS）
Carry out the surface modification processing of silicon；
（3）By step（2）In obtained dispersion liquid by obtaining the nano silicon particles of APS modifications after centrifugation and drying, APS is repaiied
The nano silicon particles of decorations are scattered in absolute ethyl alcohol and form dispersion liquid, are added dropwise to graphene solution under agitation, through centrifuge washing, cold
Nano silicon particles/graphene composite material is obtained after freezing drying process；
（4）By step（3）Nano silicon particles/the graphene composite material and polyvinyladine floride of gained（PVDF）It is well mixed latter
The composite coated in formation consistency of thickness on copper current collector is played, and is dried in vacuum drying chamber；
（5）By step（4）Composite after drying carries out high-temperature heat treatment in an inert atmosphere, and it is multiple to obtain silicon/graphene/carbon
Close negative material.
Preferably, step（1）In, the particle size ranges of described nano silicon particles is the nm of 30 nm~70.
Preferably, step（1）In, the concentration of described nano silicon particles dispersion liquid is the mg/mL of 0.5 mg/mL~2.
Preferably, step（2）In, the APS of addition percent by volume（APS volume and nano silicon particles dispersion liquid
The ratio between volume）For 0.5%~2%.
Preferably, step（3）In, the concentration of the dispersion liquid of the nano silicon particles of APS modifications is the mg/ of 0.5 mg/mL~2
mL。
Preferably, step（3）In, the graphene solution concentration of the addition is the mg/mL of 1 mg/mL~2.5.
Preferably, step（3）In, when adding graphene solution, control the matter of nano silicon particles and graphene in dispersion liquid
Amount is than being 9~11:1.
Preferably, step（4）In, the mass ratio of described nano silicon particles/graphene composite material and polyvinyladine floride
For 1~3:1.
Preferably, step（4）In, described vacuum drying temperature is 60 DEG C~120 DEG C.
Preferably, step（5）In, described inert atmosphere is the one or more in argon hydrogen gaseous mixture, argon gas, nitrogen.
Preferably, step（5）In, described high-temperature heat treatment temperature is 500 DEG C~850 DEG C.
Silicon/graphene/carbon composite negative pole material specific discharge capacity prepared by the present invention is high（0.5 A g-1Circulating current
Under, discharge capacity 3932.5mAh/g first）, charge-discharge characteristic it is good（0.5 A g-1Circulating current under, coulombic efficiency is first
81.47%）, cyclical stability it is higher（0.5 A g-1Circulating current under, discharge and recharge 30 times, there remains 2010 mAh/g's
Specific capacity）.
The silicon cathode lithium ion battery prepared using the present invention, compared with prior art, on the one hand, including directly using viscous
Tie agent polyvinyladine floride（PVDF）Surface coating is carried out to silicon particle as carbon source, one layer of formation encapsulates entirely on silicon particle surface
Carbon coating layer so that in battery charge and discharge process, electrode material lithiumation speed improves 3-4.5 times, improves efficiency for charge-discharge；
And this is flexible, amorphousness carbon structure clad changes " multiple crackses efflorescence " process of silicon particle in charge and discharge process
For " efflorescence of simple check line " process, battery is added.On the other hand, including graphene coated silicon particle can increase material
The electric conductivity of material, so as to further increase the efficiency for charge-discharge of silicon cathode lithium ion battery.The silicon cathode lithium ion battery is 0.5
A g-1Circulating current under, discharge and recharge 30 times, there remains 2010 mAh/g specific capacity；In 4 A g-1Circulating current
Under, discharge and recharge 100 times, it there remains 750 mAh/g specific capacity.
Brief description of the drawings
Fig. 1 is the SEM electron microscopes of silicium cathode electrode slice prepared by the embodiment of the present invention 1；
Fig. 2 is silicon/graphene/carbon composite negative pole material of the preparation of the embodiment of the present invention 1 in 0.5 A g-1Before under current density
3 charge-discharge performances；
Fig. 3 is silicon/graphene/carbon composite negative pole material of the preparation of the embodiment of the present invention 1 in 0.5 A g-1Following under current density
Ring performance curve.
Embodiment
As described below is the preferred embodiment of the embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, on the premise of principle of the embodiment of the present invention is not departed from, some improvements and modifications can also be made, these improvement
The protection domain of the embodiment of the present invention is also considered as with retouching.
Embodiment 1
（1）By 80 mg nano silicon particles（40 nm~60 nm）Evenly spread under supersound process in 100 ml absolute ethyl alcohols,
Form the nano silicon particles dispersion liquid that concentration is 0.8mg/mL；
（2）To step（1）0.8 mL aminopropyl trimethoxies are added by magnetic agitation in the nano silicon particles dispersion liquid of gained
Base silane（APS）Carry out the surface modification processing of silicon；
（3）By step（2）In obtained dispersion liquid by obtaining the nano silicon particles of APS modifications after centrifugation and drying, APS is repaiied
The nano silicon particles of decorations are scattered in absolute ethyl alcohol and form the dispersion liquid that concentration is 0.8 mg/mL, are added dropwise to stone under magnetic stirring
Black alkene solution（1.26mg/mL）, it is 10 to make the mass ratio of nano silicon particles and graphene:1, at centrifuge washing, freeze-drying
Nano silicon particles/graphene composite material is obtained after reason；
（4）By nano silicon particles/graphene composite material and polyvinyladine floride（PVDF）In mass ratio 6:4 are well mixed for ratio
Composite together coated in formation consistency of thickness on copper current collector afterwards, and 120 DEG C of drying in vacuum drying chamber；
（5）Composite after drying is heat-treated for 550 DEG C in argon gas atmosphere, obtains silicon/graphene/carbon composite negative pole
Material.
The SEM electron microscopes of silicium cathode electrode slice prepared by silicon/graphene/carbon composite negative pole material obtained by the present embodiment,
As shown in Figure 1.It is observed that graphene and nano Si uniform particle mix in figure, and graphene has very to nano Si particle
Good cladding.
Battery assembles：Composite after calcination processing is dried in vacuum drying chamber, in the closed gloves of applying argon gas
Using lithium metal as to pole, using microporous polypropylene membrane as barrier film, 1.0 M LiPF in case6 Be dissolved in volume ratio for 1:1 carbonic acid
Vinyl acetate（EC）And dimethyl carbonate（DMC）Mixed solvent is used as to electrode as electrolyte, lithium metal, is assembled into CR2025's
Button cell.By battery in 0.02~1 V voltage ranges, its charge-discharge performance is tested.
In 0.5 A g-13 times charge-discharge performance under current density, as shown in Fig. 2 as shown in Figure 2, silicon/graphene
Carbon/composite negative pole material specific capacity is high（0.5 A g-1Circulating current under, first discharge specific capacity up to 3932.5 mAh/g,
Coulombic efficiency is 81.47% first.）
In 0.5 A g-1Cycle performance curve under current density, as shown in figure 3,0.5 A g-1Circulating current under, discharge and recharge
30 times, it there remains 2010 mAh/g specific capacity.
Embodiment 2
（1）By 80 mg nano silicon particles（40 nm~55 nm）Evenly spread under supersound process in 100 ml absolute ethyl alcohols,
Form the nano silicon particles dispersion liquid that concentration is 0.8 mg/mL；
（2）0.8 mL TSL 8330s are added by magnetic agitation into nano silicon particles dispersion liquid（APS）Enter
The surface modification processing of row silicon；
（3）By step（2）In obtained dispersion liquid by obtaining the nano silicon particles of APS modifications after centrifugation and drying, APS is repaiied
The nano silicon particles of decorations are scattered in absolute ethyl alcohol and form the dispersion liquid that concentration is 0.8 mg/mL, are added dropwise to stone under magnetic stirring
Black alkene solution（1.26mg/mL）, it is 10 to make the mass ratio of nano silicon particles and graphene:1, at centrifuge washing, freeze-drying
Nano silicon particles/graphene composite material is obtained after reason；
（4）By nano silicon particles/graphene composite material and polyvinyladine floride（PVDF）It is 6 in mass ratio:4 ratios are well mixed
Composite together coated in formation consistency of thickness on copper current collector afterwards, and 120 DEG C of drying in vacuum drying chamber；
（5）Composite is heat-treated for 800 DEG C in argon nitrogen atmosphere, obtains silicon/graphene/carbon composite negative pole material.
Battery assembles：Composite after calcination processing is dried in vacuum drying chamber, in the closed gloves of applying argon gas
Using lithium metal as to pole, using microporous polypropylene membrane as barrier film, 1.0 M LiPF in case6 Be dissolved in volume ratio for 1:1 carbonic acid
Vinyl acetate（EC）And dimethyl carbonate（DMC）Mixed solvent is used as to electrode as electrolyte, lithium metal, is assembled into CR2025's
Button cell.By battery in 0.02~1 V voltage ranges, its charge-discharge performance is tested.
Silicon/graphene carbon/composite negative pole material specific capacity obtained by the present embodiment is high（0.5 A g-1Circulating current under,
First discharge specific capacity is 80.47% up to 3234.5 mAh/g, first coulombic efficiency）；0.5 A g-1Circulating current under, fill
Electric discharge 30 times, there remains 1845 mAh/g specific capacity.
Embodiment 3
（1）By 80 mg nano silicon particles（45 nm~60 nm）Evenly spread under supersound process in 100 ml absolute ethyl alcohols,
Form the nano silicon particles dispersion liquid that concentration is 0.8 mg/mL；
（2）0.8 mL TSL 8330s are added by magnetic agitation into nano silicon particles dispersion liquid（APS）Enter
The surface modification processing of row silicon；
（3）By step（2）In obtained dispersion liquid by obtaining the nano silicon particles of APS modifications after centrifugation and drying, APS is repaiied
The nano silicon particles of decorations are scattered in absolute ethyl alcohol and form the dispersion liquid that concentration is 0.8 mg/mL, are added dropwise to stone under magnetic stirring
Black alkene solution（1.26 mg/mL）, it is 10 to make the mass ratio of nano silicon particles and graphene:1, at centrifuge washing, freeze-drying
Nano silicon particles/graphene composite material is obtained after reason；
（4）By nano silicon particles/graphene composite material and polyvinyladine floride（PVDF）It is 6 in mass ratio:4 ratio mixing is equal
Composite after even together coated in formation consistency of thickness on copper current collector, and 120 DEG C of drying in vacuum drying chamber；
（5）Composite is subjected to high-temperature heat treatment for 850 DEG C in nitrogen atmosphere, obtains silicon/graphene/carbon composite negative pole material
Material.
Battery assembles：Composite after calcination processing is dried in vacuum drying chamber, in the closed gloves of applying argon gas
Using lithium metal as to pole, using microporous polypropylene membrane as barrier film, 1.0 M LiPF in case6 Be dissolved in volume ratio for 1:1 carbonic acid
Vinyl acetate（EC）And dimethyl carbonate（DMC）Mixed solvent is used as to electrode as electrolyte, lithium metal, is assembled into CR2025's
Button cell.By battery in 0.02~1 V voltage ranges, its charge-discharge performance is tested.
The high negative material specific capacity of silicon/graphene/carbon composite negative pole material specific capacity obtained by the present embodiment is high（0.5 A
g-1Circulating current under, first discharge specific capacity is up to 3136.5mAh/g, and coulombic efficiency is 79.7% first）；0.5 A g-1's
Under circulating current, discharge and recharge 30 times, 1789 mAh/g specific capacity there remains.
Claims (10)
1. the preparation method of a kind of silicon/graphene/carbon composite negative pole material, it is characterised in that comprise the following steps：
（1）Nano silicon particles are evenly spread in absolute ethyl alcohol under supersound process, form nano silicon particles dispersion liquid；
（2）To step（1）In the nano silicon particles dispersion liquid of gained TSL 8330 progress is added by stirring
The surface modification processing of silicon；
（3）By step（2）In obtained dispersion liquid by obtaining the nano silicon particles of APS modifications after centrifugation and drying, APS is repaiied
The nano silicon particles of decorations are scattered in absolute ethyl alcohol and form dispersion liquid, are added dropwise to graphene solution under agitation, through centrifuge washing, cold
Nano silicon particles/graphene composite material is obtained after freezing drying process；
（4）By step（3）Coated together with after nano silicon particles/graphene composite material of gained is well mixed with polyvinyladine floride
The composite of consistency of thickness is formed on copper current collector, and is dried in vacuum drying chamber；
（5）By step（4）Composite after drying carries out high-temperature heat treatment in an inert atmosphere, and it is multiple to obtain silicon/graphene/carbon
Close negative material.
2. the preparation method of silicon according to claim 1/graphene/carbon composite negative pole material, it is characterised in that：Step
（1）In, the particle size ranges of described nano silicon particles is the nm of 30 nm~70.
3. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（1）In, the concentration of described nano silicon particles dispersion liquid is the mg/mL of 0.5mg/mL~2.
4. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（2）In, the APS of addition percent by volume 0.5%~2%.
5. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（3）In, the concentration of the nano silicon particles dispersion liquid of APS modifications is the mg/mL of 0.5mg/mL~2.
6. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（3）In, the graphene concentration of the addition is the mg/mL of 1mg/mL~2.5.
7. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（3）In, when adding graphene solution, it is 9~11 to control the mass ratio of nano silicon particles and graphene in dispersion liquid:1.
8. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（4）In, described nano silicon particles/graphene composite material and PVDF mass ratio are 0.25~4.5.
9. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（4）In, described vacuum drying temperature is 60 DEG C~120 DEG C.
10. the preparation method of silicon according to claim 1 or 2/graphene/carbon composite negative pole material, it is characterised in that：Step
Suddenly（5）In, described high-temperature heat treatment temperature is 500 DEG C~850 DEG C.
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