CN109659548A - A kind of core-shell structure Co-SiO2The preparation method of/C negative electrode material - Google Patents
A kind of core-shell structure Co-SiO2The preparation method of/C negative electrode material Download PDFInfo
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- CN109659548A CN109659548A CN201811647606.9A CN201811647606A CN109659548A CN 109659548 A CN109659548 A CN 109659548A CN 201811647606 A CN201811647606 A CN 201811647606A CN 109659548 A CN109659548 A CN 109659548A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The present invention provides a kind of core-shell structure Co-SiO2The preparation method of/C negative electrode material, cobalt salt and surfactant are dissolved in dilute hydrochloric acid, and silicate, agitating and heating, standing, cooling, washing, suction filtration is then added, and cobalt Nano-meter SiO_2 is mixed in preparation2Colloidal sol, then calcining, washing and drying, obtain cobalt doped Nano-meter SiO_22Powder, then cobalt doped Nano-meter SiO_22Powder is added in organic solvent, and silylating reagent is then added, and reflux filters, washing, dry, carbonization, obtains Co-SiO2/ C composite.The present invention solves the problems, such as that the huge volume change generated during removal lithium embedded causes poor circulation caused by cracking and dusting.
Description
Technical field
The invention belongs to technical field of lithium ion battery negative, it is related to a kind of lithium ion battery negative material and its system
The hud typed silicon-carbon cathode material of Preparation Method, especially lithium ion battery.
Background technique
The demand for being constantly progressive and developing to the energy of society is increasing, at present world's main energy sources fossil class A fuel A
(coal, petroleum, natural gas) resource is increasingly depleted.And lithium ion battery is because of its higher energy conversion efficiency, cleanliness without any pollution
As a kind of ideal energy storage and reforming unit, and it is widely used in people's daily life.However, commercialized at present
Lithium ion battery has been unable to meet demand of the people to high-energy density and high power electrical source of power.In negative electrode of lithium ion battery material
Material aspect, current widely applied graphite type material theoretical specific capacity is 372mAh/g, limits lithium ion battery specific capacity
It further increases, therefore the negative electrode material of developmental research Novel high-specific capacity flexible, high security is extremely urgent.
Because of high theoretical storage lithium specific capacity (4200mAh/g) and moderate embedding de- lithium potential, silicon is considered as lithium of new generation
The ideal negative electrode material of ion battery.However, silicon volume expansion reaches 300% during removal lithium embedded, electrode has been seriously affected
Cyclical stability.Compared with elemental silicon, Li that silicon oxide compound material is formed in discharge process for the first time2O and a series of silicon
Sour lithium salts (Li2SiO3, Li2SiO4And Li2Si2O5) there is certain buffering work to the volume expansion of silicon in subsequent cyclic process
With, therefore silicon oxide compound electrode has relatively better cyclical stability.For the silica of good crystal form, due to its Si-O
Key is highly stable, hardly performance electro-chemical activity, has patent (CN201610130175.3) report amorphous silica negative
Pole materials theory specific capacity reaches 1965mAh g-1, significantly larger than existing graphite cathode material, and silica is in nature
In content it is higher, charge and discharge platform is lower, but the silica storage lithium activity difficult to realize of micrometer structure, can not be in lithium ion
It is actually used in battery.It is silicon source that Inst. of Physics, CAS Wang Zhaoxiang, which teaches research group using TEOS, passes through hydro-thermal
Method prepares silica/hard carbon composite material.With electrode prepared by the material, reversible specific capacity is up to 630 mAh/ for the first time
G(B.K. Guo, J. Shu, et al. Electrochemistry Communications 10 (2008): 1876-
1878), but cycle performance is general.Should be due to silicon oxide compound during removal lithium embedded along with huge volume change,
Cause cracking and dusting, to influence cycle performance.
Summary of the invention
In view of the problems of the existing technology, the object of the present invention is to provide a kind of core-shell type nano SiO2Negative electrode material and
Preparation method.It is characterized by: core is the Nano-meter SiO_2 of cobalt doped2(the SiO that silicate and hydrochloric acid generate2And its silanization examination
The SiO that agent generates when hydrolyzing2), shell is that silylating reagent is carbonized the organic carbon-coating to be formed.The negative electrode active material is conductive
The advantages that good, cycle performance, high first effect.
In order to achieve the above object, the present invention is achieved by the following scheme.
A kind of core-shell structure Co-SiO2The preparation method of/C negative electrode material, which comprises the following steps:
B1, cobalt salt and surfactant are dissolved in dilute hydrochloric acid, are uniformly mixed and form mixed liquor, silicon is then added into mixed liquor
Hydrochlorate, agitating and heating 6-8 hours at a temperature of 150 DEG C -200 DEG C, then stand, cool down, wash, filter, cobalt nanometer is mixed in preparation
SiO2Colloidal sol, then at temperature lower calcination 3-5 hours of 550-700 DEG C, washing and drying obtains cobalt doped Nano-meter SiO_22Powder, letter
Claim Co-SiO2。
B2, the cobalt doped Nano-meter SiO_2 for preparing step B 12Powder is added in the three-necked flask equipped with organic solvent, then
Silylating reagent is added, flow back 8-12h, and reflux temperature is set in the boiling point of organic solvent or more, and it then filters, wash, is dry,
It is carbonized in retort again, obtains Co-SiO2/ C composite.
Preferably, the mass ratio of cobalt salt, surfactant and dilute hydrochloric acid is (1-2.5): (5-12.5): 24, dilute hydrochloric acid
Concentration is 0.01-0.5mol/L.
Preferably, in the step B1, silicate is according to 1:(6-9) mass ratio be added in mixed liquor.
Preferably, in step B1, the surfactant is ionic surfactant or nonionic surface active agent.
Preferably, in step B1, the surfactant be polyvinylpyrrolidone (PVP), neopelex,
One of cetyl sodium bromide.
Preferably, in step B2, cobalt doped Nano-meter SiO_22Powder is added according to the volume of organic solvent by 0.8-0.4g/ml
Into the three-necked flask of organic solvent.
Preferably, in step B2, the additional amount of silylating reagent is according to cobalt doped Nano-meter SiO_22The amount of powder determines, excellent
Choosing, the additional amount and cobalt doped Nano-meter SiO_2 of the silylating reagent2The mass ratio of powder is 1:(2-4).
Preferably, in step B2, the carbonization carries out under an inert atmosphere, and the temperature of carbonization is 800-1100 DEG C,
Carbonization time is 4-8h.
Preferably, in step B2, the organic solvent is one of ethyl alcohol, benzene, toluene；The silylating reagent includes
Molecular formula is CnH(2n+1)Si(OCH3)3 、CnH(2n-1)Si(OCH3)3Long chain silane reagent.
A kind of core-shell structure Co-SiO2The preparation method of/C negative electrode material, which comprises the following steps:
B1: cobalt doped Nano-meter SiO_2 is prepared2Powder: weighing 2-5g cobalt salt respectively and 10-25g surfactant is dissolved in 120g concentration
It in the dilute hydrochloric acid of 0.01-0.5mol/L, is uniformly mixed and forms mixed liquor, 15-24g silicate is then added into mixed liquor,
Agitating and heating 6-8 hours at a temperature of 150 DEG C -200 DEG C, then stand, cool down, wash, filter, it prepares and mixes cobalt Nano-meter SiO_22It is molten
Glue, then at temperature lower calcination 3-5 hours of 550-700 DEG C, washing and drying prepares cobalt doped Nano-meter SiO_22Powder, referred to as
Co-SiO2；
B2: preparation Co-SiO2/ C composite: the cobalt doped Nano-meter SiO_2 for taking 100g step B1 to prepare2Powder, which is added to, to be equipped with
In the three-necked flask of 120-300ml organic solvent, 25-35g silylating reagent is then added, flow back 8-12h, reflux temperature setting
More than the boiling point of organic solvent, filters, washing, drying, be then placed in retort and be carbonized under an inert atmosphere, carburizing temperature
It is 800-1100 DEG C, be carbonized 4-8h, prepares Co-SiO2/ C composite.
Compared with prior art, the present invention is had the advantages that
(1) present invention prepares weak acid principle using strong acid and prepares persursor material, and simple process is easily operated, no organic volatile
Divide, is environmental-friendly.
(2) present invention is to Nano-meter SiO_22Cobalt doped is carried out, using cobalt in SiO2Coordinate bond is formed in skeleton (mainly with cobalt
Oxide Co3O4Etc. forms exist, and Co3O4It is a kind of important transition metal oxide semiconductor), improve leading for material
Electrically.
(3) present invention is organic by, in presoma surface grafting, forming one layer in the form of chemical bond using silane reagent
Compound forms clad after carbonization.The inducing action for recycling cobalt element makes to be carbonized the clad formed more evenly, orderly,
The degree of graphitization for not only contributing to improve subsequent carbon coating layer, improves the electric conductivity of material, and also improves negative electrode material
Head effect, improves the reversible capacity of negative electrode material.
(4) Co-SiO of the method for the present invention preparation2There is/C negative electrode material good cycle performance and higher coulomb to imitate
Rate, the capacity of composite material is the 85% of initial capacity after 100 circulations, and coulombic efficiency is 73 % or so for the first time.Solves deintercalation
The huge volume change generated during lithium causes the problem of poor circulation caused by cracking and dusting, realizes micron
The storage lithium activity of grade silicon dioxide and the practical application in lithium ion battery.
Detailed description of the invention
Fig. 1 is Co-SiO prepared by the present invention2The scanning electron microscope (SEM) photograph of/C composite.
Fig. 2 is Co-SiO prepared by the present invention2The XRD diagram of/C composite.
Fig. 3 is material SiO2(a) and composite material Co-SiO2The ultraviolet spectrogram of/C (b).
Fig. 4 is Co-SiO prepared by the present invention2The Raman spectrogram of/C composite.
Fig. 5 is Co-SiO prepared by the present invention2The cycle performance curve graph of/C composite.
Specific embodiment
The present invention is described in further details combined with specific embodiments below, but the present invention is not limited to these implementations
Example.
Embodiment 1
A kind of core-shell structure Co-SiO2The preparation method and applications of/C negative electrode material, specifically includes the following steps:
(1) 5gCoCl is weighed respectively2•6(H2O) and 25g cetyl sodium bromide is dissolved in 120g dilute hydrochloric acid (concentration 0.01mol/
L it in), is uniformly mixed, then the addition 24g sodium metasilicate into mixed liquor, water-bath heating stirring 6 hours at 150 DEG C, stand, is cooling,
Washing filters, and cobalt Nano-meter SiO_2 is mixed in preparation2Colloidal sol, then calcines 3h, washing and drying at 550 DEG C, and cobalt Nano-meter SiO_2 is mixed in preparation2Powder
End, abbreviation Co-SiO2。
(2) preparation process of composite material is as follows: the Co-SiO for taking 100g step 1 to prepare2It is added equipped with 300ml toluene
In three-necked flask, 35g hexadecyl trimethoxy silane is then added, under the conditions of 120 DEG C, flow back 12h, filters, washing, does
Dry, taking-up is put into crucible, then in retort, N2Atmosphere, under the conditions of 800 DEG C, be carbonized 4h, prepares Co-SiO2/ C composite wood
Material.In research, the chemical property of electrode material is tested using the button cell of working electrode and metal lithium electrode composition.System
When making electrode plates, negative electrode active material, SBR, CMC, SP(example 80:6:4:10 in mass ratio are mixed), appropriate methyl is added dropwise
Pyrrolidones is evenly dispersed as solvent, is coated on copper foil, is dried in vacuo 24 hours, is finally punched from pole piece obtained
The disk that diameter is out is used for material, assembles button cell in the glove box of argon atmosphere, carries out constant current charge-discharge to battery
Test.
Embodiment 2
A kind of core-shell structure Co-SiO2The preparation method and applications of/C negative electrode material, specifically includes the following steps:
(1) 2gCoAc is weighed respectively2It is dissolved in 120g dilute hydrochloric acid (concentration 0.5mol/L) with 10g neopelex,
It is uniformly mixed, 15g sodium metasilicate is then added into mixed liquor, water-bath agitating and heating 8 hours at 200 DEG C are stood, cooling, water
It washes, filter, cobalt Nano-meter SiO_2 is mixed in preparation2Colloidal sol, then calcines 5h, washing and drying at 700 DEG C, and cobalt Nano-meter SiO_2 is mixed in preparation2Powder
End, abbreviation Co-SiO2。
(2) preparation process of composite material is as follows: the Co-SiO for taking 100g step 1 to prepare2It is added equipped with 120ml toluene
In three-necked flask, 25g dodecyl trimethyl silane is then added, under the conditions of 120 DEG C, flow back 8h, filters, washing, does
Dry, taking-up is put into crucible, then in retort, N2Atmosphere, under the conditions of 1100 DEG C, be carbonized 8h, prepares Co-SiO2/ C composite wood
Material.Then button cell is assembled, constant current charge-discharge test is carried out to battery.
Under the current density of 0.1A/g, the chemical property that embodiment 1 and embodiment 2 prepare material is as shown in the table:
Co-SiO prepared by embodiment 12/ C composite carries out electron-microscope scanning, spectrum analysis, performance survey mode, as a result characterizes
It is analyzed as follows:
Core-shell structure Co-SiO prepared by the embodiment of the present invention 12The scanning electron microscope (SEM) photograph of/C composite is as shown in Figure 1, electron microscope
It has been shown that, composite material have pore structure.
Core-shell structure Co-SiO prepared by the embodiment of the present invention 12The XRD diagram of/C composite is as shown in Fig. 2, can from figure
Know: in 20 ° or so appearance, one wide diffraction maximum, illustrating composite material in amorphous state.
Material SiO in the embodiment of the present invention 12(a) and composite material Co-SiO2The ultraviolet spectrogram of/C (b) such as Fig. 3 institute
Show, it is seen that occur three absorption peaks in wavelength 449nm-694nm, respectively at 518nm, 581nm and 661nm,
Cobalt ions coordinate bond characteristic absorption peak is belonged to, illustrates that Co is successfully adulterated.
Core-shell structure Co-SiO prepared by the embodiment of the present invention 12The Raman spectrogram of/C composite as shown in figure 4, from
It can be seen that in figure, composite material is in 1360cm-1And 1590cm-1There are two peaks in place, respectively corresponds agraphitic carbon and graphitization
Carbon finds out from peak area ratio, the cladding carbon-coating degree of graphitization with higher on presoma surface.
Core-shell structure Co-SiO prepared by the embodiment of the present invention 12Cycle performance curve graph such as Fig. 5 institute of/C composite
Show, it was found from figure: material has preferable cycle performance and higher coulombic efficiency, the capacity of composite material after 100 circulations
It is the 85% of initial capacity, coulombic efficiency is 73 % or so for the first time.
Claims (10)
1. a kind of core-shell structure Co-SiO2The preparation method of/C negative electrode material, which comprises the following steps:
B1, cobalt salt and surfactant are dissolved in dilute hydrochloric acid, are uniformly mixed and form mixed liquor, silicon is then added into mixed liquor
Hydrochlorate, agitating and heating 6-8 hours at a temperature of 150 DEG C -200 DEG C, then stand, cool down, wash, filter, cobalt nanometer is mixed in preparation
SiO2Colloidal sol, then at temperature lower calcination 3-5 hours of 550-700 DEG C, washing and drying obtains cobalt doped Nano-meter SiO_22Powder, letter
Claim Co-SiO2；
B2, the cobalt doped Nano-meter SiO_2 for preparing step B12Powder is added in the three-necked flask equipped with organic solvent, and silicon is then added
Alkylators, flow back 8-12h, and reflux temperature is set in the boiling point of organic solvent or more, then filters, washes, is dry, then in charcoal
Change and be carbonized in furnace, obtains Co-SiO2/ C composite.
2. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: institute
It states in step B1, the mass ratio of cobalt salt, surfactant and dilute hydrochloric acid is (1-2.5): (5-12.5): 24, the concentration of dilute hydrochloric acid
For 0.01-0.5mol/L.
3. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: institute
State in step B1, silicate is according to 1:(6-9) mass ratio be added in mixed liquor.
4. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: step
In rapid B1, the surfactant is ionic surfactant or nonionic surface active agent.
5. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: step
In rapid B1, the surfactant is polyvinylpyrrolidone (PVP), in neopelex, cetyl sodium bromide
One kind.
6. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: step
In rapid B2, cobalt doped Nano-meter SiO_22Powder is added to three mouthfuls of organic solvent according to the volume of organic solvent by 0.8-0.4g/ml
In flask.
7. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: step
In rapid B2, the additional amount of silylating reagent is according to cobalt doped Nano-meter SiO_22The amount of powder determines, it is preferred that the silanization examination
The additional amount and cobalt doped Nano-meter SiO_2 of agent2The mass ratio of powder is 1:(2-4).
8. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: step
In rapid B2, the carbonization carries out under an inert atmosphere, and the temperature of carbonization is 800-1100 DEG C, carbonization time 4-8h.
9. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, it is characterised in that: step
In rapid B2, the organic solvent is one of ethyl alcohol, benzene, toluene；The silylating reagent includes that molecular formula is CnH(2n+1)
Si(OCH3)3 、CnH(2n-1)Si(OCH3)3Long chain silane reagent.
10. a kind of core-shell structure Co-SiO according to claim 12The preparation method of/C negative electrode material, which is characterized in that
The following steps are included:
B1: cobalt doped Nano-meter SiO_2 is prepared2Powder: weighing 2-5g cobalt salt respectively and 10-25g surfactant is dissolved in 120g concentration and is
It in the dilute hydrochloric acid of 0.01-0.5mol/L, is uniformly mixed and forms mixed liquor, 15-24g silicate is then added into mixed liquor,
It agitating and heating 6-8 hours at a temperature of 150 DEG C -200 DEG C, then stands, cool down, wash, filter, prepare and mix cobalt Nano-meter SiO_22It is molten
Glue, then at temperature lower calcination 3-5 hours of 550-700 DEG C, washing and drying prepares cobalt doped Nano-meter SiO_22Powder, referred to as
Co-SiO2；
B2: preparation Co-SiO2/ C composite: the cobalt doped Nano-meter SiO_2 for taking 100g step B1 to prepare2Powder, which is added to, to be equipped with
In the three-necked flask of 120-300ml organic solvent, 25-35g silylating reagent is then added, flow back 8-12h, reflux temperature setting
More than the boiling point of organic solvent, filters, washing, drying, be then placed in retort and be carbonized under an inert atmosphere, carburizing temperature
It is 800-1100 DEG C, be carbonized 4-8h, prepares Co-SiO2/ C composite.
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