CN106340630B - A kind of SiO2The preparation method of/C composite nano materials and its application in lithium cell cathode material - Google Patents
A kind of SiO2The preparation method of/C composite nano materials and its application in lithium cell cathode material Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M10/058—Construction or manufacture
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention discloses a kind of SiO2The preparation method of/C composite nano materials and its application in lithium cell cathode material, SiO2The preparation method of/C composite nano materials：Room temperature under nitrogen protection, sequentially adds carbon source, stabilizer and Si O organic matters, stirs evenly in deionized water, be placed in 150~180 DEG C of sealing stainless steel cauldrons and heat 6~9h, wash, dry, obtains predecessor；Above-mentioned predecessor is placed in the tube furnace of nitrogen protection, 7~9h is calcined at 600~800 DEG C, natural cooling obtains the SiO2/ C composite nano materials；By above-mentioned SiO2/ C composite nano materials are used for cathode of lithium battery active material；And the test battery as lithium cell cathode material.Compared with prior art, advantage of the present invention：Preparation process is simple, the period is short, can be used in cathode of lithium battery active material, applies in fast charging and discharging field, has good market prospects and economic value.
Description
Technical field
The present invention relates to lithium battery material fields, and in particular to a kind of SiO2The preparation method of/C composite nano materials and its
In the application of lithium cell cathode material.
Background technology
Since lithium battery has the characteristics that higher energy density and power density, it is therefore widely used in electric vehicle
With the mobile energy storage device of electronic product.Although current graphite commercial applications in lithium ion battery negative material,
Its lower theoretical specific capacity (372 mAh/g) is difficult to the requirement for meeting market to cathode material for high capacity lithium ion battery.Cause
This, people constantly probe into the negative material of the lithium ion battery with high specific capacity.It is 2014, German《Advanced material》It is miscellaneous
Will (Adv Mater, volume 2014,26, page 6750), which reports elemental silicon, has higher storage lithium specific capacity, but it is being filled
It is easy to happen Volumetric expansion in discharge process, leads to charge 3 times or more of the volume that the volume after electricity reaches before charging, from
And seriously hinder its commercial applications.However, 2014, it is Dutch《The energy》(J Power Sources, the 2014, the 246th
Volume, page 168) magazine ran SiO2Cheap and rich reserves on earth, and with similar relatively low of elemental silicon
Charge and discharge platform therefore can replace negative material of the elemental silicon as lithium ion battery.But SiO2In charge and discharge
It is also easy to happen Volumetric expansion in the process.It is 2015, Dutch《Electrochemistry journal》(Electrochimica Acta,
Volume 2015,176, page 1002) report SiO2It is compound with carbon material, SiO can be effectively prevented from2Body in charge and discharge process
Product bulking effect, and carbon material can improve SiO2Electric conductivity.
Currently, people prepare SiO frequently with two-step method2/ C composite nano materials are coated with carbon material and prepare SiO in advance2
Nano material, the process complexity, period length and cost that such method prepares composite material are higher, are unfavorable for commercialization and promote.
Invention content
In view of the above-mentioned problems, the present invention proposes a kind of SiO2The preparation method of/C composite nano materials and its be used as lithium battery
Negative material tests battery, and as the negative material of lithium battery, preparation method is simple, and the period is short, and electric conductivity is high.
The present invention adopts the following technical solutions solves the above problems：
A kind of SiO2The preparation method of/C composite nano materials, includes the following steps：Room temperature environment under nitrogen protection, is gone
Carbon source, stabilizer and-Si-O- organic matters are sequentially added in ionized water, is stirred evenly, and are placed in 150~180 DEG C of reaction kettles and are heated
6~9h is washed, dry, obtains SiO2/ C composite nano materials predecessors；
Above-mentioned predecessor is placed in the tube furnace of nitrogen protection, 7~9h is calcined at 600~800 DEG C, natural cooling obtains
The SiO2/ C composite nano materials.
Further, carbon source is one kind in glucose, sucrose, phenolic resin；- Si-O- organic matters are 3- aminopropyls three
One kind in Ethoxysilane, vinyl silane triisopropoxide, γ-methacryloxypropyl trimethoxy silane；Surely
It is sodium citrate to determine agent.
Further, the dosage of deionized water is 30~45mL, and the mass ratio of stabilizer and carbon source is 1:1 ,-Si-O- are organic
The addition of object is 0.3~0.8mL.
Further, in order to which solvent is uniformly mixed, 1~3h of magnetic agitation to solution is uniformly mixed.
Further, pure predecessor in order to obtain, washs dried product exhibited 3~5 times with water and ethyl alcohol respectively, is placed in
Dry 5~7h in 40~70 DEG C of baking ovens.
A kind of SiO2The preparation method of/C composite nano materials, under room temperature environment, by 1g trisodium citrates and 1g grapes
Sugar is added in the deionized water of 30ml under nitrogen protection, then three ethoxy of 0.5ml 3- aminopropyls is added into above-mentioned solution
After magnetic agitation 1h, above-mentioned solution is transferred in 50ml stainless steel cauldrons for base silane, is sealed.Aforesaid reaction vessel is set again
In being heated 8 hours in 180 DEG C of baking ovens；After washing above-mentioned sample respectively three times with water and ethyl alcohol, dry 6 are placed in 60 DEG C of baking ovens
Hour, obtain brown predecessor；
Above-mentioned predecessor is placed in the tube furnace for being passed through nitrogen, is calcined 8 hours at 800 DEG C, after cooled to room temperature,
Obtain SiO2/ C composite nano materials.
A kind of lithium cell cathode material, including anode active material layer, contained negative electrode active material is in negative electrode material layer
SiO made from the above method2/ C composite nano materials.
It is a kind of by above-mentioned SiO2Preparation method of/C the composite nano materials for the test battery of lithium cell cathode material, with
Metal lithium sheet is cathode；SiO2/ C composite nano materials, acetylene black and Kynoar are with mass ratio (60%~80%)：
(10%~20%)：(10%~20%) it is uniformly mixed, said mixture painting is uniformly overlying on copper foil, anode electrode is made
Piece；Using polypropylene film as diaphragm, button cell is assembled into the glove box of argon atmosphere protection to get test electricity
Pond.
Further, the electrolyte for testing battery is the mixed liquor of ethylene carbonate, diethyl carbonate, lithium hexafluoro phosphate.
Further, the mass ratio of ethylene carbonate and diethyl carbonate is 1:1, lithium hexafluoro phosphate a concentration of 0.5~
1.5mol/L。
Compared with prior art, the beneficial effects of the present invention are：
1, preparation process is simple, and the period is short；Before being prepared under hydrothermal conditions by stabilizer, carbon source and-Si-O- organic matters
Object is driven, then calcines predecessor in nitrogen and obtains SiO2/ C composite nano materials effectively simplify and prepare SiO2/ C composite Nanos
The technique of material, is expected to be promoted and industrialization production.
2, SiO obtained2/ C composite nano materials have loose porous structure, specific surface area larger；It drives before calcination
During object, has a large amount of carbon dioxide and hydrone overflows, lead to finally obtained SiO2/ C composite nano materials have
There is loose porous composite construction.
3、SiO2The loose porous composite construction of/C composite nano materials can be applied to lithium ion battery negative material；It is loose
Porous structure is conducive to lithium ion and electrolyte disengaging active material；Larger specific surface area and porous structure can increase
SiO2With the contact area of electrolyte, shorten the diffusion length of lithium ion and electrolyte；Carbon substrate can improve entire electrode material
The electric conductivity of material.
4、SiO2The loose porous composite structure anode material of/C composite nano materials is with very high capacity and well
Cyclical stability；In the charge and discharge process of high current 2A/g, after recycling 800 times, 525mAh/g can be kept, can be applied
Fast charging and discharging field.
Description of the drawings
Fig. 1 is SiO in embodiment 12The X-ray diffractogram of/C composite nano materials；
Fig. 2 is SiO in embodiment 12The Raman spectrogram of/C composite nano materials；
Fig. 3 is SiO in embodiment 12The infrared spectrum of/C composite nano materials；
Fig. 4 is SiO in embodiment 12The stereoscan photograph (Fig. 4 (a)) and transmission electron microscope photo of/C composite nano materials
(Fig. 4 (b, c))；
Fig. 5 is SiO in embodiment 12The aerial hot weight curve of/C composite nano materials；
Fig. 6 is SiO in embodiment 12The nitrogen adsorption of/C composite nano materials-desorption curve figure；
Fig. 7 is gained test discharge capacity of the cell and cycle-index curve (discharge current density 100mA/ in embodiment 2
g)；
Fig. 8 is gained half-cell discharge capacity and cycle-index curve (discharge current density 2A/g) in embodiment 2；
Fig. 9 is capacity and cycle-index curve of the gained half-cell under different discharge current densities in embodiment 2.
Specific implementation mode
Embodiment 1
SiO2The preparation of/C composite nano materials：Room temperature environment, under nitrogen protection, in the deionized water of 30ml successively
1g trisodium citrates and 1g glucose is added, 0.5ml 3- aminopropyltriethoxywerene werenes are added, are mixed after magnetic agitation 1h
Uniformly, above-mentioned mixed solution is transferred in 50ml stainless steel cauldrons, is sealed；Reaction kettle is placed in 180 DEG C of baking ovens and heats 8
Hour, natural cooling；Above-mentioned desciccate is washed respectively 3 times, product is placed in 60 DEG C of baking ovens dry 6 after washing with water and ethyl alcohol
Hour, obtain brown predecessor.
Above-mentioned predecessor is placed in the tube furnace for being passed through nitrogen, is calcined 8 hours at 800 DEG C, after cooled to room temperature,
Obtain SiO2/ C composite nano materials.
It is as shown in Figure 1 the SiO in the present embodiment2The X-ray diffraction of/C composite nano materialsFigure.
From figure 1 it appears that 23 ° or so of broad peak is carbon substrate and the superposition peak of unformed SiO2,43 ° or so of broad peak is carbon-based
The diffraction maximum at bottom.
The SiO being illustrated in figure 2 in the present embodiment2The Raman spectrogram of/C composite nano materials, 1350cm-1With
1580cm-1The peak at place corresponds to the D bands and G bands of carbon material respectively；Raman spectrogram may be used to determine the graphitization of composite material
Degree, it can be seen from the figure that the intensity of G bands is more than the intensity of D bands, illustrate the degree of graphitization of carbon substrate in composite material compared with
It is high.
The SiO being illustrated in figure 3 in the present embodiment2The infrared spectrogram of/C composite nano materials, sees from figure,
1100cm-1And 800cm-1Two peaks at place are by SiO2What the stretching vibration of middle Si-O-Si generated, 970cm-1The peak at place be by
What the stretching vibration of Si-OH generated.
It is illustrated in figure 4 the SiO of gained in the present embodiment2The scanning electron microscope sem (a) and transmission electricity of/C composite nano materials
Mirror TEM (b-c) figure, it can be seen that SiO from figure a2/ C composite nano materials are smooth by exhibiting high surface, the particle group of random shape
At it can be seen that SiO from figure b-c2/ C composite nano materials are solid construction, SiO2It is distributed in the composite with C more
Even, grain size is about 50nm.
It is illustrated in figure 5 the aerial hot weight curve of products therefrom in this example example, it can be seen from the figure that compound
Material thermal degradation at 580 DEG C is complete, and remaining mass loss 60% or so illustrates SiO in composite material2Quality be about
40%.
It is illustrated in figure 6 nitrogen adsorption-desorption curve figure of products therefrom in the present embodiment, it can be seen from the figure that
SiO2It is 186.7 m that/C composite nano materials, which have porous structure, specific surface area,2/ g, average pore size 4nm.
Embodiment 2
SiO2/ C composite nano materials are used as the preparation of the test battery of ion cathode material lithium：Made from embodiment 1
SiO2/ C composite nano materials and acetylene black and Kynoar PVDF in mass ratio 80%：10%：10% is mixed and made into mud
Slurry like material is evenly coated on copper foil, and after being dried in 80 DEG C of baking oven, copper foil is cut into the circular electrode of a diameter of 14mm
Piece；There is SiO with load2The electrode slice of/C composite nano materials is anode, using the circular metal lithium piece of a diameter of 14mm as cathode,
With by ethylene carbonate EC and diethyl carbonate DEC in mass ratio 1:Hexafluoro phosphorus that 1 mixing is constituted, containing a concentration of 1mol/L
The mixed solution of sour lithium LiPF6 is electrolyte, using the round polypropylene film of a diameter of 16mm as diaphragm, is protected in argon atmosphere
Glove box in be assembled into button half-cell, as test battery.
It is tested using battery test system Neware BTS-610.
Influence for test battery charging and discharging cycle-index to specific capacity as shown in FIG. 7 and 8；It is illustrated in figure 7 test electricity
Pond current density is under 100mA/g, and after recycling 100 times, discharge capacity is maintained at 888mAh/g；It is illustrated in figure 8 test battery
In the case where current density is 2A/g, after recycling 800 times, discharge capacity is maintained at 525mAh/g；
Multiplying power test is also to weigh a battery to stablize an important parameter.It is illustrated in figure 9 and prepares in the present embodiment
Half-cell is tested under conditions of current density is 100mA/g, 200mA/g, 400 mA/g, 800mA/g and 1600mA/g respectively,
Its charge and discharge cycles curve as shown in figure 9, it can be seen from the figure that when current density be respectively 100mA/g, 200mA/g,
When being tested under conditions of 400mA/g, 800mA/g and 1600mA/g, corresponding average size be 785mAh/g, 632mAh/g,
547mAh/g, 441mAh/g and 338mAh/g.This is the results show that the half-cell in the present embodiment has preferable stability
Energy.
Embodiment 3
SiO2The preparation of/C composite nano materials：Room temperature environment, under nitrogen protection, in the deionized water of 40ml successively
2g trisodium citrates and 2g glucose is added, 0.3ml 3- aminopropyltriethoxywerene werenes are added, are mixed after magnetic agitation 2h
Uniformly, above-mentioned mixed solution is transferred in 50ml stainless steel cauldrons, is sealed；It is small that reaction kettle is placed in heating 9 in 150 DEG C of baking ovens
When, natural cooling；Above-mentioned desciccate is washed respectively 4 times, it is small to be placed in 40 DEG C of baking ovens dry 7 for product after washing with water and ethyl alcohol
When, obtain brown predecessor；
Above-mentioned predecessor is placed in the tube furnace for being passed through nitrogen, is calcined 9 hours at 600 DEG C, after cooled to room temperature,
Obtain SiO2/ C composite nano materials.
SiO2/ C composite nano materials are used as the preparation of the test battery of ion cathode material lithium：It will be obtained above
SiO2/C composite nano materials and acetylene black and Kynoar PVDF in mass ratio 60%：20%：20% is mixed and made into mud
Slurry like material is evenly coated on copper foil, and after being dried in 90 DEG C of baking oven, copper foil is cut into the circular electrode of a diameter of 14mm
Piece；There is SiO with load2The electrode slice of/C composite nano materials is anode, is negative with the circular metal lithium piece of a diameter of 14mm
Pole, with by ethylene carbonate EC and diethyl carbonate DEC in mass ratio 1:1 mixes constituting, containing a concentration of 0.5mol/L six
The mixed solution of lithium fluophosphate LiPF6 is electrolyte, using the round polypropylene film of a diameter of 16mm as diaphragm, in argon atmosphere
Button half-cell is assembled into the glove box of protection, as test battery.
Embodiment 4
SiO2The preparation of/C composite nano materials：Room temperature environment, under nitrogen protection, in the deionized water of 45ml successively
2.5g trisodium citrates and 2.5g glucose is added, is added 0.8ml 3-aminopropyltriethoxysilane, after magnetic agitation 3h
It is uniformly mixed, above-mentioned mixed solution is transferred in 50ml stainless steel cauldrons, seal；Reaction kettle, which is placed in 160 DEG C of baking ovens, to be added
Heat 7 hours, natural cooling；Above-mentioned desciccate is washed respectively 5 times, product is placed in 70 DEG C of baking ovens and does after washing with water and ethyl alcohol
Dry 5 hours, obtain brown predecessor；
Above-mentioned predecessor is placed in the tube furnace for being passed through nitrogen, is calcined 7 hours at 700 DEG C, after cooled to room temperature,
Obtain SiO2/ C composite nano materials.
SiO2/ C composite nano materials are used as the preparation of the test battery of ion cathode material lithium：By SiO obtained above2/
C composite nano materials and acetylene black and Kynoar PVDF in mass ratio 70%：15%：15% is mixed and made into slurry
Matter is evenly coated on copper foil, and after being dried in 80 DEG C of baking oven, copper foil is cut into the circular electric pole piece of a diameter of 14mm；With negative
It is loaded with SiO2The electrode slice of/C composite nano materials is anode, using the circular metal lithium piece of a diameter of 14mm as cathode, with by carbon
Sour ethyl EC and diethyl carbonate DEC in mass ratio 1:Lithium hexafluoro phosphate that 1 mixing is constituted, containing a concentration of 0.5mol/L
The mixed solution of LiPF6 is electrolyte, using the round polypropylene film of a diameter of 16mm as diaphragm, in the hand of argon atmosphere protection
Button half-cell is assembled into casing, as test battery.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (9)
1. a kind of SiO2The preparation method of/C composite nano materials, which is characterized in that include the following steps：Room temperature environment, nitrogen are protected
Stabilizer, carbon source and-Si-O- organic matters are sequentially added under shield, in deionized water, is stirred evenly, and 150~180 DEG C of sealings are placed in
6~9h is heated in stainless steel cauldron, is washed, it is dry, obtain SiO2/ C composite nano materials predecessors；
Above-mentioned predecessor is placed in the tube furnace of nitrogen protection, 7~9h is calcined at 600~800 DEG C, natural cooling obtains described
SiO2/ C composite nano materials；
The carbon source is one or more in glucose, sucrose, phenolic resin；- Si-O- the organic matters are 3- aminopropyls
One kind in triethoxysilane, vinyl silane triisopropoxide, γ-methacryloxypropyl trimethoxy silane；
The stabilizer is sodium citrate.
2. a kind of SiO according to claim 12The preparation method of/C composite nano materials, which is characterized in that the deionization
The dosage of water is 30~45mL, and the mass ratio of the stabilizer and carbon source is 1:1, the addition of-Si-O- organic matters is
0.3~0.8mL.
3. a kind of SiO according to claim 12The preparation method of/C composite nano materials, which is characterized in that the stirring is
1~3h of magnetic agitation.
4. a kind of SiO according to claim 12The preparation method of/C composite nano materials, which is characterized in that the washing is
It is washed respectively 3~5 times with water and ethyl alcohol, the drying is dry 5~7h in 40~70 DEG C of baking ovens.
5. a kind of SiO2The preparation method of/C composite nano materials, which is characterized in that under room temperature environment, by 1g trisodium citrates
It is added in the deionized water of 30ml under nitrogen protection with 1g glucose, adds 0.5ml 3- aminopropyl triethoxysilicanes
After magnetic agitation 1h, acquired solution is transferred in 50ml stainless steel cauldrons for alkane, is sealed；Aforesaid reaction vessel is placed in 180 again
It is heated 8 hours in DEG C baking oven；After washing gained sample respectively with water and ethyl alcohol three times, drying 6 hours in 60 DEG C of baking ovens are placed in, are obtained
To brown predecessor；
Above-mentioned predecessor is placed in the tube furnace for being passed through nitrogen, is calcined 8 hours at 800 DEG C, cooled to room temperature, is obtained described
SiO2/ C composite nano materials.
6. a kind of lithium cell cathode material being used to prepare anode active material layer, which is characterized in that the negative electrode active material
Contained negative electrode active material is the SiO described in claim 5 in layer2SiO prepared by the preparation method of/C composite nano materials2/C
Composite nano materials.
7. the SiO being prepared using 5 any the method for Claims 1 to 52/ C composite nano materials are used for lithium ion battery anode material
The preparation method of the test battery of material, using metal lithium sheet as cathode, which is characterized in that the SiO2/ C composite nano materials, second
Acetylene black and Kynoar are with mass ratio (60%~80%)：(10%~20%)：(10%~20%) it is uniformly mixed, by gained
Mixture is evenly applied on copper foil, and anode electrode piece is made；Using polypropylene film as diaphragm, in the gloves of argon atmosphere protection
Button cell is assembled into case to get the test battery.
8. SiO according to claim 72The preparation side of/C composite nano materials for the test battery of lithium cell cathode material
Method, which is characterized in that the electrolyte of the test battery is the mixing of ethylene carbonate, diethyl carbonate and lithium hexafluoro phosphate
Liquid.
9. SiO according to claim 82The preparation side of/C composite nano materials for the test battery of lithium cell cathode material
Method, which is characterized in that the mass ratio of the ethylene carbonate and diethyl carbonate is 1:1, the lithium hexafluoro phosphate it is a concentration of
0.5~1.5mol/L.
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| CN110620224A (en) * | 2019-09-27 | 2019-12-27 | 广东省稀有金属研究所 | Negative electrode material for lithium battery, preparation method of negative electrode material and lithium battery |
| CN111403744A (en) * | 2020-03-25 | 2020-07-10 | 广东凯金新能源科技股份有限公司 | Nitrogen-containing silicon oxygen carbon compound composite negative electrode material of lithium ion secondary battery and preparation method |
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