CN108565410A - Lithium ion battery stannic oxide/graphene composite negative pole and preparation method thereof - Google Patents
Lithium ion battery stannic oxide/graphene composite negative pole and preparation method thereof Download PDFInfo
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Abstract
Lithium ion battery stannic oxide/graphene composite negative pole and preparation method thereof, the composite negative pole material is made of following methods:(1)Graphene oxide is dispersed in low alcohol, graphene oxide dispersion is obtained;(2)Organic tin source is dissolved in graphene oxide dispersion, is heated, constant temperature is stirred to solvent and is evaporated;(3)It calcines in air, it is cooling,.Composite negative pole material electron conduction of the present invention and ionic conductivity are high, and ion diffusion admittance is short, and bulk effect is small, it is assembled into battery, at 0.01~2.00V, 50mA/g, the gram volume that discharges for the first time is up to 1846.8mAh/g, after cycle 10 times, specific capacity is up to 800mAh/g or more, and under 1A/g, specific capacity can be stablized in 500mAh/g or more, under 2.5A/g, specific capacity is still up to 400mAh/g;The present invention is simple, and the period is short, and reaction temperature is low, at low cost, can largely synthesize.
Description
Technical field
The present invention relates to a kind of composite cathode material for lithium ion cell and preparation method thereof, and in particular to a kind of lithium-ion electric
Pond stannic oxide/graphene composite negative pole and preparation method thereof.
Background technology
With the progress of science and technology, new-energy automobile, portable electronic device it is universal, to the battery as its energy
More stringent requirements are proposed.Wherein, lithium ion battery is high, environmental-friendly by its energy density, steady performance is de- clever
And go out.Currently, the cathode of lithium ion battery mainly uses graphite material, theoretical capacity is relatively low, only 372 mAh/g, restricts
The development of lithium ion battery.
Since stannic oxide has theoretical capacity high(782mAh/g), it is cheap, it is pollution-free the features such as, therefore, become
One of negative electrode of lithium ion battery optional material.But stannic oxide, in electrochemistry cyclic process, bulk effect is larger, leads
It is electrically poor, as a result, it is often necessary to be modified to it.
CN103078095 A disclose a kind of preparation of the compound lithium ion battery negative material of stannic oxide/graphene
Choline chloride, ethylene glycol and graphene oxide are uniformly mixed by method, obtain mixed liquor, and protochloride then is added to mixed liquor
Tin carries out ultrasonic vibration reaction, then post-treated obtains product.But the compound lithium of stannic oxide/graphene obtained by the technique
The capacity of ion battery cathode material is relatively low.
CN104600275A discloses a kind of preparation side of graphene-based hollow tin dioxide lithium ion battery negative pole material
Method is after reacting graphene dispersing solution in autoclave with presoma, then uses hydrazine hydrate reduction.But due to this
Method is prepared using autoclave, and preparation time is long, it is difficult to mass production.
CN 104953101A disclose a kind of preparation method of graphene aerogel load tin dioxide electrode material, are
Graphene aqueous solution, stannic oxide ethanol solution, L-AA are uniformly mixed in proportion, after heating reaction, freeze-drying,
Calcining,.But this method needs the stannic oxide prepared using hydro-thermal method, then it is compound with graphene progress, and graphene
It needs to restore, preparation time is longer.
CN102255072A discloses a kind of preparation method of stannic oxide and graphene sheet layer composite material, and being will be organic
After solvent, the graphene oxide layer hydrosol are mixed with pink salt, calcined again after back flow reaction.But this method needs two
Step reaction, obtained product particle about 50nm, grain size is larger, and needs the flows such as centrifugation, dry, relatively complicated.
Invention content
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide a kind of electric conductivity
Well, bulk effect is small, and electric discharge gram volume is high, and good cycle, preparation flow is simple, and the period is short, and reaction temperature is low, environmentally protective
Lithium ion battery stannic oxide/graphene composite negative pole and preparation method thereof.
The technical solution adopted by the present invention to solve the technical problems is as follows:Lithium ion battery stannic oxide/graphene is multiple
Negative material is closed, is made of following methods:
(1)Graphene oxide is dispersed in low alcohol, graphene oxide dispersion is obtained;
(2)Organic tin source is dissolved in step(1)In gained graphene oxide dispersion, heating, constant temperature is stirred to solvent and is evaporated, obtains
Brown viscous shape substance;
(3)By step(2)Gained brown viscous shape substance is calcined in air, is cooled to room temperature with the furnace, is obtained lithium ion battery two
Tin oxide/graphene composite negative pole.
Preferably, step(1)In, dispersion amount of the graphene oxide in low alcohol is 0.3~0.7mg/mL.If oxygen
The excessive concentration of graphite alkene, then graphene oxide free settling, if the concentration of graphene oxide is too low, graphene oxide content
It is very few.
Preferably, step(1)In, the low alcohol is one or more of methanol, ethyl alcohol or propyl alcohol etc..The low member
Alcohol is absolute alcohol.
Preferably, step(2)In, organic tin source in graphene oxide dispersion a concentration of 0.01~0.03
mmol/mL.Graphene oxide is in the preparation process of composite negative pole material of the present invention, as hard template, while providing carbon source,
Organic tin source is more advantageous under the concentration to be adsorbed on graphene oxide.
Preferably, step(2)In, organic tin source is dibutyl tin laurate and/or tin dilaurate dioctyl tin
Deng.When carrying out pyrolysis using organic tin source, tin oxide nano particles can be directly generated, and can remain with
Part carbon in machine tin source forms in-stiu coating.
Preferably, step(2)In, the temperature of the heating is 30~55 DEG C.The purpose of the heating is that low alcohol is made to steam
Hair.
Preferably, step(3)In, the temperature of the calcining is 300~500 DEG C, and the time is 0.4~2.0h(More preferable 0.5
~1.5h).Calcining makes organic tin source directly decompose generation nano-stannic oxide, and generates some carbon in decomposable process and wrap in situ
Cover, if temperature is too low, decomposition reaction is difficult to happen, if temperature is excessively high, can make in composite material from organic tin source and
The carbon residual quantity of graphene is less, or all ablated idle most.
Preferably, step(3)In, by room temperature with 1~5 DEG C/min(More preferable 2~4 DEG C/min)Rate be warming up to calcining
Temperature.If heating rate is excessively high, it is easy to happen reunion.
Lithium ion battery stannic oxide/graphene composite negative pole of the present invention, first passes through dissolving, organic tin source is adsorbed
On graphene alkene, in calcination process, the directly pyrolysis of organic tin source forms Nanoparticulate stannic oxide, and remains organic
Part carbon in tin source, while negative material is formed by compound remaining graphene, improve the electrochemistry of stannic oxide
Can, to improve the electric conductivity of composite material.
Beneficial effects of the present invention are as follows:
(1)In lithium ion battery stannic oxide/graphene composite negative pole of the present invention, nano-stannic oxide is evenly distributed on stone
Black alkene on piece, the particle of nano-stannic oxide is uniform, and primary particle is less than 10nm;
(2)Lithium ion battery stannic oxide/graphene composite negative pole of the present invention has electron conduction and ionic conductivity
The advantages that height, ion diffusion admittance is short, and bulk effect is small during deintercalate lithium ions;By lithium ion battery titanium dioxide of the present invention
Tin/graphene composite negative pole is assembled into battery, in the voltage range of 0.01~2.00V, under the current density of 50mA/g,
Electric discharge gram volume may be up to 1846.8mAh/g for the first time, and after recycling 10 times, specific capacity can be stablized in 800mAh/g or more, 1A/g electricity
Under current density, specific capacity can be stablized at 500mAh/g or more, 2.5A/g current densities, and specific capacity is still up to 400mAh/g;
(3)Preparation flow of the present invention is simple, and the period is short, and reaction temperature is low, at low cost, environmentally protective, can largely synthesize and product
Yield is high.
Description of the drawings
Fig. 1 is the SEM figures of 1 gained lithium ion battery stannic oxide of the embodiment of the present invention/graphene composite negative pole;
Fig. 2 is the TEM figures of 1 gained lithium ion battery stannic oxide of the embodiment of the present invention/graphene composite negative pole;
Fig. 3 is the XRD diagram of 1 gained lithium ion battery stannic oxide of the embodiment of the present invention/graphene composite negative pole;
Fig. 4 is 1 gained lithium ion battery stannic oxide of the embodiment of the present invention/graphene composite negative pole under different multiplying
Cycle charge-discharge curve graph;
Fig. 5 is 1 gained stannic oxide of comparative example of the present invention and cycle charge discharge of the graphene sheet layer composite material under different multiplying
Electric curve graph.
Specific implementation mode
With reference to embodiment and attached drawing, the invention will be further described.
Chemical reagent used in the embodiment of the present invention is obtained by routine business approach unless otherwise specified.
Embodiment 1
(1)50mg graphene oxides are dispersed in 100mL absolute ethyl alcohols, 100mL graphene oxide dispersions are obtained;
(2)2mmol dibutyl tin laurates are dissolved in step(1)In gained 100mL graphene oxide dispersions, it is heated to 45
DEG C, constant temperature is stirred to alcohol solvent and is evaporated, and obtains brown viscous shape substance;
(3)By step(2)Gained brown viscous shape substance is warming up to 400 DEG C with the rate of 3 DEG C/min in air, by room temperature,
1h is calcined, room temperature is cooled to the furnace, obtains lithium ion battery stannic oxide/graphene composite negative pole.
As shown in Figure 1, in lithium ion battery stannic oxide/graphene composite negative pole obtained by the embodiment of the present invention, receive
Rice stannic oxide is evenly distributed on graphene film.
As shown in Fig. 2, in lithium ion battery stannic oxide/graphene composite negative pole obtained by the embodiment of the present invention, receive
The primary particle of rice stannic oxide is uniform, and grain size is less than 10nm.
As shown in figure 3, the dioxy in lithium ion battery stannic oxide/graphene composite negative pole obtained by present example
Change tin is pure phase, and no other impurity generate.
The assembling of battery:Weigh lithium ion battery stannic oxide/graphene Compound Negative obtained by the 0.16 g embodiment of the present invention
Pole material, addition 0.02g acetylene blacks make conductive agent and 0.02g Kynoar makees binder, and N-Methyl pyrrolidone, which is used as, to be divided
Powder is applied on copper foil and negative plate is made after mixing, is anode with metal lithium sheet, with pe, pp in vacuum glove box
Composite membrane be diaphragm, 1mol/L lithium hexafluoro phosphates/DMC:EC(Volume ratio 1:1)For electrolyte, it is assembled into the button of CR2025
Battery.
As shown in figure 4, by the battery assembled in 0.01~2.00V voltage ranges, under 50mA/g current densities, for the first time
Electric discharge gram volume is 1846.8mAh/g, and after recycling 10 times, specific capacity is stablized at 800mAh/g or more, 1A/g current densities, than
Capacity is still stablized at 500mAh/g or more, 2.5A/g current densities, and specific capacity is still up to 400mAh/g.
Embodiment 2
(1)30mg graphene oxides are dispersed in 100mL anhydrous propyl alcohols, 100mL graphene oxide dispersions are obtained;
(2)3mmol tin dilaurate dioctyl tins are dissolved in step(1)In gained 100mL graphene oxide dispersions, it is heated to 55
DEG C, constant temperature is stirred to propanol solvent and is evaporated, and obtains brown viscous shape substance;
(3)By step(2)Gained brown viscous shape substance is warming up to 300 DEG C with the rate of 2 DEG C/min in air, by room temperature,
1h is calcined, room temperature is cooled to the furnace, obtains lithium ion battery stannic oxide/graphene composite negative pole.
After testing, in lithium ion battery stannic oxide/graphene composite negative pole obtained by the embodiment of the present invention, nanometer two
Tin oxide is evenly distributed on graphene film.
After testing, in lithium ion battery stannic oxide/graphene composite negative pole obtained by the embodiment of the present invention, nanometer two
The primary particle of tin oxide is uniform, and grain size is less than 10nm.
After testing, the titanium dioxide in lithium ion battery stannic oxide/graphene composite negative pole obtained by present example
Tin is pure phase, and no other impurity generate.
The assembling of battery:Weigh lithium ion battery stannic oxide/graphene Compound Negative obtained by the 0.16 g embodiment of the present invention
Pole material, addition 0.02g acetylene blacks make conductive agent and 0.02g Kynoar makees binder, and N-Methyl pyrrolidone, which is used as, to be divided
Powder is applied on copper foil and negative plate is made after mixing, is anode with metal lithium sheet, with pe, pp in vacuum glove box
Composite membrane be diaphragm, 1mol/L lithium hexafluoro phosphates/DMC:EC(Volume ratio 1:1)For electrolyte, it is assembled into the button of CR2025
Battery.
After testing, it by the battery assembled in 0.01~2.00V voltage ranges, under 50mA/g current densities, puts for the first time
Electric gram volume is 1798.2mAh/g, and after recycling 10 times, specific capacity is stablized at 800mAh/g or more, 1A/g current densities, specific volume
Amount is still stablized at 495mAh/g or more, 2.5A/g current densities, and specific capacity is still up to 390mAh/g.
Embodiment 3
(1)70mg graphene oxides are dispersed in 100mL absolute ethyl alcohols, 100mL graphene oxide dispersions are obtained;
(2)1.5mmol dibutyl tin laurates and 1.5mmol tin dilaurate dioctyl tins are dissolved in step(1)Gained 100mL
In graphene oxide dispersion, 50 DEG C are heated to, constant temperature is stirred to alcohol solvent and is evaporated, and obtains brown viscous shape substance;
(3)By step(2)Gained brown viscous shape substance is warming up to 500 DEG C with the rate of 4 DEG C/min in air, by room temperature,
0.5h is calcined, room temperature is cooled to the furnace, obtains lithium ion battery stannic oxide/graphene composite negative pole.
After testing, in lithium ion battery stannic oxide/graphene composite negative pole obtained by the embodiment of the present invention, nanometer two
Tin oxide is evenly distributed on graphene film.
After testing, in lithium ion battery stannic oxide/graphene composite negative pole obtained by the embodiment of the present invention, nanometer two
The primary particle of tin oxide is uniform, and grain size is less than 10nm.
After testing, the titanium dioxide in lithium ion battery stannic oxide/graphene composite negative pole obtained by present example
Tin is pure phase, and no other impurity generate.
The assembling of battery:Weigh lithium ion battery stannic oxide/graphene Compound Negative obtained by the 0.16 g embodiment of the present invention
Pole material, addition 0.02g acetylene blacks make conductive agent and 0.02g Kynoar makees binder, and N-Methyl pyrrolidone, which is used as, to be divided
Powder is applied on copper foil and negative plate is made after mixing, is anode with metal lithium sheet, with pe, pp in vacuum glove box
Composite membrane be diaphragm, 1mol/L lithium hexafluoro phosphates/DMC:EC(Volume ratio 1:1)For electrolyte, it is assembled into the button of CR2025
Battery.
After testing, it by the battery assembled in 0.01~2.00V voltage ranges, under 50mA/g current densities, puts for the first time
Electric gram volume is 1741.4mAh/g, and after recycling 10 times, specific capacity is stablized at 750mAh/g or more, 1A/g current densities, specific volume
Amount is still stablized at 485mAh/g or more, 2.5A/g current densities, and specific capacity is still up to 380mAh/g.
Comparative example 1
By the graphene oxide layer hydrosol and ethylene glycol of 10g 10wt%(Beijing Chemical Plant, analysis are pure)According to 1:40 body
After ultrasonic disperse is uniform under the power of 200W, two hydrated stannous chlorides of 3.0g are added into obtained colloidal sol for product mixing(State
Yao Ji chemical reagent Co., Ltd)With the NaHB of 0.2g4(Sinopharm Chemical Reagent Co., Ltd.)In the rotating speed of 5000r/min
Lower centrifugation removes unreacted pink salt, by the obtained black precipitate water washing 3~5 times of 500mL, then at 80 DEG C
Under, it is dried in vacuo 8h, obtains the stannic oxide and graphene oxide layer compound substance of the black of 1.5g.
In N2Under gas shield, the stannic oxide of black obtained above and graphene oxide layer compound substance are placed in
0.5h is heated in 700 DEG C of tube furnace, taking-up is cooled to room temperature, and the stannic oxide and graphene sheet layer composite wood of 1.3g can be obtained
Material.
As shown in figure 5, stannic oxide and graphene sheet layer composite material of the comparative example 1 using art methods preparation,
In 1C(About 0.8A/g)Lower reversible capacity is only 310mAh/g, well below 500mAh/g under 1A/g in the embodiment of the present invention 1
Specific capacity.By Fig. 4,5 comparison it is found that 1 gained lithium ion battery stannic oxide of the embodiment of the present invention/graphene composite negative material
The chemical property of material is substantially better than stannic oxide and graphene sheet layer composite wood obtained by method of the comparative example 1 using the prior art
Material, and preparation process of the present invention, without the processes such as washing, dry, preparation method is simple, and flow is shorter.
Claims (8)
1. lithium ion battery stannic oxide/graphene composite negative pole, which is characterized in that be made of following methods:
(1)Graphene oxide is dispersed in low alcohol, graphene oxide dispersion is obtained;
(2)Organic tin source is dissolved in step(1)In gained graphene oxide dispersion, heating, constant temperature is stirred to solvent and is evaporated, obtains
Brown viscous shape substance;
(3)By step(2)Gained brown viscous shape substance is calcined in air, is cooled to room temperature with the furnace, is obtained lithium ion battery two
Tin oxide/graphene composite negative pole.
2. lithium ion battery stannic oxide/graphene composite negative pole according to claim 1, it is characterised in that:Step
(1)In, dispersion amount of the graphene oxide in low alcohol is 0.3~0.7mg/mL.
3. lithium ion battery stannic oxide/graphene composite negative pole according to claim 1 or claim 2, it is characterised in that:Step
Suddenly(1)In, the low alcohol is one or more of methanol, ethyl alcohol or propyl alcohol.
4. according to one of claims 1 to 3 lithium ion battery stannic oxide/graphene composite negative pole, feature exists
In:Step(2)In, a concentration of 0.01~0.03 mmol/mL of the organic tin source in graphene oxide dispersion.
5. according to one of Claims 1 to 4 lithium ion battery stannic oxide/graphene composite negative pole, feature exists
In:Step(2)In, organic tin source is dibutyl tin laurate and/or tin dilaurate dioctyl tin.
6. according to one of Claims 1 to 5 lithium ion battery stannic oxide/graphene composite negative pole, feature exists
In:Step(2)In, the temperature of the heating is 30~55 DEG C.
7. according to one of claim 1~6 lithium ion battery stannic oxide/graphene composite negative pole, feature exists
In:Step(3)In, the temperature of the calcining is 300~500 DEG C, and the time is 0.4~2.0h.
8. according to one of claim 1~7 lithium ion battery stannic oxide/graphene composite negative pole, feature exists
In:Step(3)In, calcination temperature is warming up to the rate of 1~5 DEG C/min by room temperature.
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