CN107195884B - A kind of lithium metasilicate doped graphene lithium ion battery negative material and preparation method thereof - Google Patents
A kind of lithium metasilicate doped graphene lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN107195884B CN107195884B CN201710402299.7A CN201710402299A CN107195884B CN 107195884 B CN107195884 B CN 107195884B CN 201710402299 A CN201710402299 A CN 201710402299A CN 107195884 B CN107195884 B CN 107195884B
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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Abstract
The invention belongs to technical field of lithium ion, more particularly to a kind of lithium ion battery negative material.The invention particularly discloses a kind of lithium metasilicate doped graphene lithium ion battery negative materials, are made by following steps: silicon powder and graphite oxide mixture being added in the ethanol water containing lithium hydroxide, synthesize Li using hydro-thermal method2SiO3/ GE presoma；Li2SiO3/ GE presoma obtains lithium metasilicate doped graphene lithium ion battery negative material through sintering under protection of argon gas.Lithium metasilicate doped graphene lithium ion battery negative material provided by the invention, tests prove that, battery specific capacity and cycle performance can be improved.
Description
Technical field
The present invention relates to technical field of lithium ion, more particularly to a kind of lithium ion battery negative material.
Background technique
With the development of electric car and aero-space electronic equipment, to lithium ion battery specific capacity and cycle performance
It is required that it is higher and higher, and the performance of lithium ion battery depends on the performance of critical material, to push new type lithium ion battery
The exploitation and development of electrode material.
The negative electrode material of lithium ion battery plays a key effect for the performance of entire battery, thus negative electrode material become grind
The hot spot studied carefully.Graphene has many advantages, such as excellent electric conductivity, the specific surface area of superelevation and good mechanical strength, it is considered to be
Most potential lithium ion battery negative material.But since van der Waals interaction is easy to happen between graphene nano lamella
The problems such as accumulation or reunion, it will affect cycle performance and high rate performance of the graphene as negative electrode material.It therefore, can be by right
The structure of grapheme material is improved, surface functional group is modified and improves graphene as lithium with the means such as doping, compound
The research of ion battery cathode material, this respect is of great significance.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of lithium metasilicate doped graphene (Li2SiO3/ GE) lithium ion
Battery specific capacity and cycle performance can be improved in cell negative electrode material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of lithium metasilicate doped graphene lithium from
Sub- cell negative electrode material is made by following steps: the ethyl alcohol containing lithium hydroxide is added in silicon powder and graphite oxide mixture
In aqueous solution, Li is synthesized using hydro-thermal method2SiO3/ GE presoma；The Li2SiO3/ GE presoma is under protection of argon gas through being sintered
Obtain lithium metasilicate doped graphene (Li2SiO3/ GE) lithium ion battery negative material.
Specifically, the preparation method of lithium metasilicate doped graphene lithium ion battery negative material, comprising the following steps:
S1: silicon powder and graphite oxide are mixed, and silicon powder and graphite oxide mixture is made, and the silicon powder and graphite oxide are mixed
The mass percentage content for closing graphite oxide in object is 0.5%~40%；
S2: silicon powder and graphite oxide mixture are added in the ethanol water of lithium hydroxide, lithium hydroxide and silicon powder
Molar ratio are as follows: lithium hydroxide: silicon powder=2:1, be made reaction mixture；
S3: the reaction mixture is placed in the stainless steel cauldron of polytetrafluoroethyllining lining, carries out hydro-thermal reaction, hydro-thermal
The temperature of reaction is 160 DEG C~200 DEG C, and the reaction time is 16h~for 24 hours；
S4: filtering after reaction, obtains in an oven in 50 DEG C~80 DEG C dryings after obtained solid is washed
Li2SiO3/ GE presoma；
S5: the Li2SiO3/ GE presoma is sintered 3h~4h in 500 DEG C~600 DEG C argon atmospheres, obtains lithium metasilicate
Doped graphene (Li2SiO3/ GE) lithium ion battery negative material.
In an embodiment of the invention, in ethanol water dehydrated alcohol and water volume ratio are as follows: VDehydrated alcohol:VWater=3:
1。
Preferably, in step S1, the mass percentage content of graphite oxide is in the silicon powder and graphite oxide mixture
33%.
Preferably, in step S2, the concentration of silicon powder is 7.5g/L in reaction mixture obtained.
Preferably, in step S3, the temperature of hydro-thermal reaction is 180 DEG C, reaction time 18h.
Preferably, in step S4, drying temperature is 60 DEG C in an oven.
Preferably, in step S5, Li2SiO3/ GE presoma is sintered 3h in 600 DEG C of argon atmospheres.
The study found that the performance of graphene composite material is not only related with the performance of independent component, also and between them
Complex method has very big relationship.It is very crucial to control the proportion of component, space structure in graphene complex, to graphite obtained
The performance of alkene composite material has a significant impact.
Lithium metasilicate doped graphene (Li provided by the invention2SiO3/ GE) lithium ion battery negative material, it can by SEM figure
Know, pattern is by countless Li2SiO3Little particle is dispersed on the graphene film full of gauffer.It is produced by the present invention uniformly and
Stable lithium metasilicate doped graphene (Li2SiO3/ GE) material, pass through Li2SiO3(GE is graphene by (lithium metasilicate) and GE
English abbreviation) doped and compounded, and by control its pattern, not only ensure that the convenience of the carrier in charge and discharge process
Transmission, ensure that the channel of electrolyte solution exchange, and shorten the ion distance of charge and discharge process, therefore can be used as lithium
The negative electrode material of ion battery, with certain capacity and good cycle performance.Lithium metasilicate doping produced by the present invention
Graphene (Li2SiO3/ GE) material, combine sintering directly to synthesize using hydro-thermal method, preparation method is simple, easy to operate.
Detailed description of the invention
Fig. 1 is the XRD spectra of product made from the embodiment of the present invention 1；
Fig. 2 is the SEM spectrogram of product made from the embodiment of the present invention 1；
Fig. 3 is preceding 2 charge and discharges that test example 2 of the present invention obtains under the conditions of current density 150mA/g (0.01-3.0V)
Electric curve graph；
Fig. 4 is the cycle performance figure that test example 2 of the present invention obtains under the conditions of current density 150mA/g (0.01-3.0V).
Specific embodiment
Technical solution of the present invention is described in detail below by embodiment.
Embodiment 1
Silicon powder and graphite oxide mixture are added in the ethanol water of lithium hydroxide, wherein the concentration of silicon powder is
The mass ratio of graphite oxide is 33% in 7.5g/L, silicon powder and graphite oxide mixture, the molar ratio of lithium hydroxide and silicon powder
Are as follows: lithium hydroxide: silicon powder=2:1, the volume ratio of dehydrated alcohol and water in ethanol water are as follows: VDehydrated alcohol:VWater=3:1；It stirs later
It mixes uniformly, reaction mixture is made, is subsequently placed in the stainless steel cauldron of polytetrafluoroethyllining lining, in 180 DEG C of hydro-thermal temperature
Degree is lower to react 18h, in an oven in 60 DEG C of dryings, will obtain Li after products therefrom filtration washing2SiO3/ GE presoma, then in
3 hours are sintered in 600 DEG C of argon atmospheres to get product.
XRD and the SEM figure of product are as depicted in figs. 1 and 2 respectively.As shown in Figure 1, the main diffraction peak and Li of product2SiO3
The standard card (JCPDS 29-0829) of crystal is almost the same, illustrates that product is Li2SiO3, graphene is unformed knot in product
Structure is not shown in XRD.As shown in Figure 2, countless Li2SiO3Little particle is dispersed on the graphene film full of gauffer, thus
Illustrate that the product that the embodiment of the present invention 1 obtains is uniform and stable lithium metasilicate doped graphene (Li2SiO3/ GE) material.
Embodiment 2
Silicon powder and graphite oxide mixture are added in the ethanol water of lithium hydroxide, wherein the concentration of silicon powder is
The mass ratio of graphite oxide is 0.5% in 7.5g/L, silicon powder and graphite oxide mixture, the molar ratio of lithium hydroxide and silicon powder
Are as follows: lithium hydroxide: silicon powder=2:1, the volume ratio of dehydrated alcohol and water in ethanol water are as follows: VDehydrated alcohol:VWater=3:1；It stirs later
It mixes uniformly, reaction mixture is made, is subsequently placed in the stainless steel cauldron of polytetrafluoroethyllining lining, in 160 DEG C of hydro-thermal temperature
The lower reaction of degree for 24 hours, in an oven in 50 DEG C of dryings, will obtain Li after product filtration washing2SiO3/ GE presoma, then in 500
4 hours are sintered in DEG C argon atmosphere to get product lithium metasilicate doped graphene (Li2SiO3/ GE) material.
Embodiment 3
Silicon powder and graphite oxide mixture are added in the ethanol water of lithium hydroxide, wherein the concentration of silicon powder is
The mass ratio of graphite oxide is 40% in 7.5g/L, silicon powder and graphite oxide mixture, the molar ratio of lithium hydroxide and silicon powder
Are as follows: lithium hydroxide: silicon powder=2:1, the volume ratio of dehydrated alcohol and water in ethanol water are as follows: VDehydrated alcohol:VWater=3:1；It stirs later
It mixes uniformly, reaction mixture is made, is subsequently placed in the stainless steel cauldron of polytetrafluoroethyllining lining, in 200 DEG C of hydro-thermal temperature
Degree is lower to react 16h, in an oven in 80 DEG C of dryings, will obtain Li after product filtration washing2SiO3/ GE presoma, then in 600
4 hours are sintered in DEG C argon atmosphere to get product lithium metasilicate doped graphene (Li2SiO3/ GE) material.
Embodiment 4
Silicon powder and graphite oxide mixture are added in the ethanol water of lithium hydroxide, wherein the concentration of silicon powder is
The mass ratio of graphite oxide is 10% in 7.5g/L, silicon powder and graphite oxide mixture, the molar ratio of lithium hydroxide and silicon powder
Are as follows: lithium hydroxide: silicon powder=2:1, the volume ratio of dehydrated alcohol and water in ethanol water are as follows: VDehydrated alcohol:VWater=3:1；It stirs later
It mixes uniformly, reaction mixture is made, is subsequently placed in the stainless steel cauldron of polytetrafluoroethyllining lining, in 180 DEG C of hydro-thermal temperature
Degree is lower to react 18h, in an oven in 70 DEG C of dryings, will obtain Li after product filtration washing2SiO3/ GE presoma, then in 600
3 hours are sintered in DEG C argon atmosphere to get product lithium metasilicate doped graphene (Li2SiO3/ GE) material.
Comparative example
Silicon powder is added in the ethanol water of lithium hydroxide, wherein the concentration of silicon powder be 7.5g/L, lithium hydroxide with
The molar ratio of silicon powder are as follows: lithium hydroxide: silicon powder=2:1, the volume ratio of dehydrated alcohol and water in ethanol water are as follows: VDehydrated alcohol:VWater
=3:1；It stirs evenly later, reaction mixture is made, is subsequently placed in the stainless steel cauldron of polytetrafluoroethyllining lining, In
18h is reacted under 180 DEG C of hydrothermal temperature, in an oven in 60 DEG C of dryings, presoma will be obtained after products therefrom filtration washing, and
3 hours are sintered in 600 DEG C of argon atmospheres afterwards to get product lithium metasilicate (Li2SiO3) material.
Effect test
Test example 1
By product lithium metasilicate (Li made from comparative example2SiO3) material is assembled into CR2032 button cell, with lithium piece (Φ
=16, purity > 99.9%) it is to electrode, with polypropylene porous film (Φ=18) for diaphragm, with LiPF6Ethylene carbonate
(EC) and dimethyl carbonate (DMC) (VEC:VDMC=1:1) mixed solution as electrolyte, CR2032 battery is full of argon gas
Glove box in complete.Electrode is formed with the tape casting membrane, slurry used be 80% (mass percent) active material,
10% PVDF solution, 10% conductive black and 1-Methyl-2-Pyrrolidone (NMP) mix, and the substrate of electrode film is
Metal copper foil.
Under the conditions of current density 750mA/g, charge-discharge performance test is carried out, charging/discharging voltage range is 0.01-3.0V.
Measuring first discharge specific capacity is 400.9mAh/g, initial charge specific capacity 116.1mAh/g, and discharge ratio after 200 circulations
Capacity keeps 202.1mAh/g, coulombic efficiency 99.7%.
Test example 2
By product lithium metasilicate doped graphene (Li made from embodiment 12SiO3/ GE) material is assembled into CR2032 button
Battery is to electrode, with polypropylene porous film (Φ=18) for diaphragm, with LiPF with lithium piece (Φ=16, purity > 99.9%)6
Ethylene carbonate (EC) and dimethyl carbonate (DMC) (VEC:VDMC=1:1) mixed solution as electrolyte, CR2032 battery
It is to be completed in the glove box full of argon gas.Electrode is formed with the tape casting membrane, and slurry used is 80% (quality percentage
Than) active material, 10% PVDF solution, 10% conductive black and 1-Methyl-2-Pyrrolidone (NMP) mix,
The substrate of electrode film is metal copper foil.
Under the conditions of current density 150mA/g, charge-discharge performance test is carried out, charging/discharging voltage range is 0.01-3.0V.
Obtained preceding 2 charging and discharging curves are as shown in figure 3, cycle performance is as shown in Figure 4.
As can be seen from figs. 3 and 4 product made from embodiment 1 is under the conditions of current density 150mA/g (0.01-3.0V), it is first
Secondary specific discharge capacity can reach 872.5mAh/g, initial charge specific capacity 372.9mAh/g, and discharge specific volume after 200 circulations
Amount keeps 255.5mAh/g, and coulombic efficiency is up to 99.7%.
Then under the conditions of current density 300mA/g, charge-discharge performance test is carried out, charging/discharging voltage range is 0.01-
3.0V.The first discharge specific capacity for measuring product can reach 782.2mAh/g, initial charge specific capacity 277.3mAh/g, pass through
Specific discharge capacity keeps 271.1mAh/g after 200 circulations, and coulombic efficiency is up to 100%.
Later again under the conditions of current density 750mA/g, charge-discharge performance test is carried out, charging/discharging voltage range is
0.01-3.0V.The first discharge specific capacity for measuring product can reach 576.0mAh/g, initial charge specific capacity 197.4mAh/g,
Specific discharge capacity keeps 189.2mAh/g after 200 circulations, and coulombic efficiency is up to 99.7%.
By the test result of test example 1 and test example 2 it is found that under conditions of same current density, lithium metasilicate doping
Graphene increases compared to single lithium metasilicate material, first discharge specific capacity, and cycle performance is good.By test example 2
Test result under conditions of charging/discharging voltage range is 0.01-3.0V, is adopted it is found that in 150,300 and 750mA/g of current density
Battery made of the product made from the embodiment of the present invention 1, first discharge specific capacity are above the theoretical of commercialized carbon and hold
Amount keeps capacity also higher after 200 circulations.Therefore lithium metasilicate doped graphene compound can be used as lithium-ion electric
Pond negative electrode material uses.
Claims (7)
1. a kind of lithium metasilicate doped graphene lithium ion battery negative material, which is characterized in that be made by following steps: will
Silicon powder and graphite oxide mixture are added in the ethanol water containing lithium hydroxide, synthesize Li using hydro-thermal method2SiO3Before/GE
Drive body；The Li2SiO3It is negative that/GE presoma obtains lithium metasilicate doped graphene lithium ion battery through sintering under protection of argon gas
Pole material；
Preparation method the following steps are included:
S1: silicon powder and graphite oxide are mixed, and silicon powder and graphite oxide mixture, the silicon powder and graphite oxide mixture is made
The mass percentage content of middle graphite oxide is 0.5%~40%；
S2: silicon powder and graphite oxide mixture are added in the ethanol water of lithium hydroxide, and lithium hydroxide and silicon powder rub
That ratio are as follows: lithium hydroxide: reaction mixture is made in silicon powder=2:1；
S3: the reaction mixture is placed in the stainless steel cauldron of polytetrafluoroethyllining lining, carries out hydro-thermal reaction, hydro-thermal reaction
Temperature be 160 DEG C~200 DEG C, the reaction time is 16h~for 24 hours；
S4: filtering after reaction, obtains Li in 50 DEG C~80 DEG C dryings in an oven after obtained solid is washed2SiO3/GE
Presoma；
S5: the Li2SiO3/ GE presoma is sintered 3h~4h in 500 DEG C~600 DEG C argon atmospheres, obtains lithium metasilicate doping
Graphene lithium ion battery negative electrode material.
2. lithium metasilicate doped graphene lithium ion battery negative material according to claim 1, which is characterized in that ethyl alcohol
The volume ratio of dehydrated alcohol and water in aqueous solution are as follows: VDehydrated alcohol:VWater=3:1.
3. lithium metasilicate doped graphene lithium ion battery negative material according to claim 2, which is characterized in that step
In S1, the mass percentage content of graphite oxide is 33% in the silicon powder and graphite oxide mixture.
4. lithium metasilicate doped graphene lithium ion battery negative material according to claim 3, which is characterized in that step
In S2, the concentration of silicon powder is 7.5g/L in the reaction mixture obtained.
5. lithium metasilicate doped graphene lithium ion battery negative material according to claim 4, which is characterized in that step
In S3, the temperature of hydro-thermal reaction is 180 DEG C, reaction time 18h.
6. lithium metasilicate doped graphene lithium ion battery negative material according to claim 5, which is characterized in that step
In S4, drying temperature is 60 DEG C in an oven.
7. lithium metasilicate doped graphene lithium ion battery negative material according to claim 6, which is characterized in that step
In S5, Li2SiO3/ GE presoma is sintered 3h in 600 DEG C of argon atmospheres.
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| CN109524651B (en) * | 2018-11-15 | 2022-01-28 | 合肥国轩电池材料有限公司 | Battery negative electrode material and preparation method and application thereof |
| CN111099599A (en) * | 2020-01-20 | 2020-05-05 | 西安通鑫半导体辅料有限公司 | Lithium silicate solution and preparation method thereof |
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| CN105762351A (en) * | 2016-05-04 | 2016-07-13 | 合肥工业大学 | Lithium titanate/M-graphene composite cathode material for lithium ion battery and preparation method of lithium titanate/M-graphene composite cathode material |
| CN106410199A (en) * | 2016-09-20 | 2017-02-15 | 江苏大学 | Preparation method of graphene/ferro-tin alloy composite anode material for lithium ion battery |
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