CN109950507A - A kind of preparation method of the water-soluble plastic structure for lithium cobalt battery anode material - Google Patents
A kind of preparation method of the water-soluble plastic structure for lithium cobalt battery anode material Download PDFInfo
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- CN109950507A CN109950507A CN201910265830.XA CN201910265830A CN109950507A CN 109950507 A CN109950507 A CN 109950507A CN 201910265830 A CN201910265830 A CN 201910265830A CN 109950507 A CN109950507 A CN 109950507A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to a kind of preparation methods of water-soluble plastic structure for lithium cobalt battery anode material, the following steps are included: taking sheet graphene oxide, PBS solvent is added, obtain finely dispersed GO solution, weigh lithium carbonate powder, it is added in dilute sulfuric acid, then cobaltous sulfate crystal powder is slowly added to mixing liquid, ultrasonic agitation is until powder all dissolves, obtain lithium-cobalt mixed solution, lithium-cobalt mixed solution is taken to be added in reaction kettle, microwave reaction 15h~20h, obtain ultra-fine cobalt acid lithium powder, ultra-fine cobalt acid lithium powder is added to GO solution, ultrasound is broken up, hydro-thermal reaction 10~for 24 hours is carried out under protective gas, lithium/cobalt-graphene hydrosol is obtained after the reaction was completed.The utility model has the advantages that lithium/water-soluble glue material of cobalt-graphene shows super good chemical property；Unique profile and cross structure with graphene shorten the distance of lithium ion diffusion, avoid common problem caused by volume expansion during lithiation/go lithiation.
Description
Technical field
The present invention relates to electrode material of lithium battery preparation fields, and in particular to a kind of water for lithium cobalt battery anode material
The preparation method of collosol structure.
Background technique
Since the 21th century, energy crisis and environmental problem have become the whole mankind must face two big severe challenges.
In terms of the energy, its supply relies primarily on fossil fuel for a long time, excessive consumption to we shut out can ecological environment and and
Economic development all produces many problems, such as haze problem and greenhouse effects.Therefore, countries in the world change this tight in effort
High situation, global scientific worker are also actively developing new energy research and development.On the one hand, development of renewable energy is used
Electricity substituted traditional fuel power generation function, such as wind energy, solar energy, but these reproducible new energy have it is apparent intermittent, because
This, which will develop renewable energy and provides lasting electric energy, just needs to be equipped with suitable energy reserve device, and secondary cell comes into being
And rapidly developed, secondary cell mainly has lead-acid battery, nickel-metal hydride battery, nickel-cadmium cell and lithium ion battery at present.
Lithium ion battery has many advantages, such as that voltage is high, capacity is big, memory-less effect and service life are long, can be widely applied to move
The power tools such as the digital products such as phone, digital camera, laptop and electric vehicle, hybrid electric vehicle.However, current lithium
Ion battery positive electrode can't meet the high request to lithium ion battery well, and volumetric properties and cycle performance are evaluations
The key index of cell positive material quality, in current research, the two indexs are often difficult to meet simultaneously, therefore find
Meet main target of the anode material for lithium-ion batteries of high capacity and good cycle performance as each researcher simultaneously.It finds and closes
Suitable anode material for lithium-ion batteries, it is necessary to from the following aspects go: (1) material has stratiform or tunnel knot
Structure, convenient for the deintercalation of lithium ion, and main structure is able to maintain stabilization during deintercalation, guarantees the cyclical stability of battery；
(2) more lithium ion deintercalation can be allowed, to obtain biggish capacity；(3) lithium ion has preferable in its structure deintercalation
Diffusion coefficient and conductivity so that have preferable high rate performance；(4) material has relatively high voltage to lithium,
Thus obtain big cell output voltage；(5) in the entire voltage range of battery charging and discharging, which has chemistry well
Stability, and can have good compatibility with electrolyte；(6) cost of raw material of the material requires relatively low, from a wealth of sources,
It is readily synthesized, it is pollution-free.Traditional material is all difficult to meet the requirement of the above positive electrode simultaneously, it is therefore necessary to carry out to them
Modification appropriate improves its chemical property.
Summary of the invention
To overcome the deficiency, the purpose of the present invention is to provide a kind of for the water-soluble cementing of lithium cobalt battery anode material
The preparation method of structure.Using this method obtain anode material shorten lithium ion diffusion distance, also avoid lithiation/
Remove common problem caused by volume expansion during lithiation.
The technical solution adopted by the present invention to solve the technical problems is: a kind of for the water-soluble of lithium cobalt battery anode material
The preparation method of plastic structure, comprising the following steps:
Step 1: taking 2mg~10mg sheet graphene oxide, and the PBS solvent (phosphate-buffered salt of 100mL~200mL is added
Solution), 60 DEG C~80 DEG C heating water baths carry out ultrasonic disperse 1h~5h, obtain finely dispersed GO solution.
Specifically, the sheet graphene oxide is prepared using modified Hummer method.
Step 2: weighing 4mg~10mg lithium carbonate powder, and the dilute sulfuric acid that 100mL~200mL mass fraction is 2% is added
In, then ultrasonic disperse is slowly added to 4mg~10mg cobaltous sulfate crystal powder until powder all dissolves into mixing liquid
(CoSO4·7H2O), ultrasonic agitation is until powder all dissolutions, i.e. acquisition lithium-cobalt mixed solution.
Step 3: lithium obtained in step 2-cobalt mixed solution 100mL~200mL is taken, the reaction of polytetrafluoroethylene (PTFE) is added
In kettle, in the pressure of 2MPa~3MPa, the protective atmosphere of 150 DEG C~200 DEG C of argon gas, microwave reaction 15h~20h is collected
The particulate matter of precipitating obtains ultra-fine cobalt acid lithium powder.
Step 4: the ultra-fine cobalt acid lithium powder of the 5mg~10mg obtained in step 3 is added to the step of 200mL~300mL
The GO solution obtained in rapid one, ultrasound break up 1h~2h, are then adjusted to mixed solution alkalescent (pH value 7-8), are added
EDA reducing agent, by after the container sealing for containing solution, mechanical oscillation 3-5min avoids viscosity after EDA is added from increasing, avoids mixing
Solution wadding is heavy, then carries out magnetic agitation 0.5h~1h again, i.e. acquisition lithium/cobalt-GO solution.
Step 5: lithium/cobalt-GO solution that step 4 obtains is put into the reaction kettle of polytetrafluoroethylene (PTFE), under protective gas
Carry out hydro-thermal reaction, reaction temperature be 120~240 DEG C, the time be 10~for 24 hours, protection gas use argon gas, obtain after the reaction was completed
Lithium/cobalt-graphene the hydrosol.
The invention has the following advantages: LiCoO can be improved2Structural stability and avoid electrolyte decomposition, from
And obtain better stable circulation performance；This lithium/water-soluble glue material of cobalt-graphene shows super good chemical property；
The cross structure of unique profile and they and redox graphene shortens the distance of lithium ion diffusion, also avoids
Lithiation/remove some common problems as caused by volume expansion during lithiation.
Specific embodiment
It is described in detail to various aspects of the present invention below, unless specific instructions, various raw materials of the invention can pass through
It is prepared or is commercially available according to the conventional method of this field.
Embodiment 1
A kind of preparation method of the water-soluble plastic structure for lithium cobalt battery anode material, comprising the following steps:
Step 1: taking 2mg sheet graphene oxide, and the PBS solvent (phosphate buffered saline solution) of 100mL, 60 DEG C of water are added
Bath heating, carries out ultrasonic disperse 1h, obtains finely dispersed GO solution.
Specifically, the sheet graphene oxide is prepared using modified Hummer method.
Step 2: weighing 4mg lithium carbonate powder, is added in the dilute sulfuric acid that 100mL mass fraction is 2%, ultrasonic disperse, directly
It is all dissolved to powder, 4mg cobaltous sulfate crystal powder (CoSO is then slowly added into mixing liquid4·7H2O), it is stirred by ultrasonic
Until powder all dissolves, that is, obtain lithium-cobalt mixed solution.
Step 3: taking lithium obtained in step 2-cobalt mixed solution 100mL, be added in the reaction kettle of polytetrafluoroethylene (PTFE),
The pressure of 2MPa, in the protective atmosphere of 150 DEG C of argon gas, microwave reaction 15h collects the particulate matter of precipitating, that is, obtains ultra-fine cobalt
Sour powder for lithium.
Step 4: the GO obtained in the step of ultra-fine cobalt acid lithium powder of the 5mg obtained in step 3 is added to 200mL one
Solution, ultrasound break up 1h, are then adjusted to mixed solution alkalescent (pH value 7-8), and EDA reducing agent is added, will contain solution
Container sealing after, mechanical oscillation 3min avoids viscosity after EDA is added from increasing, avoids mixed solution wadding heavy, then carry out magnetic again
Power stirs 0.5h, i.e. acquisition lithium/cobalt-GO solution.
Step 5: lithium/cobalt-GO solution that step 4 obtains is put into the reaction kettle of polytetrafluoroethylene (PTFE), under protective gas
Hydro-thermal reaction is carried out, reaction temperature is 120 DEG C, time 10h, and protection gas uses argon gas, obtains lithium/cobalt-stone after the reaction was completed
The black alkene hydrosol.
Embodiment two
A kind of preparation method of the water-soluble plastic structure for lithium cobalt battery anode material, comprising the following steps:
Step 1: taking 2mg sheet graphene oxide, and the PBS solvent (phosphate buffered saline solution) of 200mL, 60 DEG C of water are added
Bath heating, carries out ultrasonic disperse 1h, obtains finely dispersed GO solution.
Specifically, the sheet graphene oxide is prepared using modified Hummer method.
Step 2: weighing 4mg lithium carbonate powder, is added in the dilute sulfuric acid that 200mL mass fraction is 2%, ultrasonic disperse, directly
It is all dissolved to powder, 4mg cobaltous sulfate crystal powder (CoSO is then slowly added into mixing liquid4·7H2O), it is stirred by ultrasonic
Until powder all dissolves, that is, obtain lithium-cobalt mixed solution.
Step 3: taking lithium obtained in step 2-cobalt mixed solution 100mL, be added in the reaction kettle of polytetrafluoroethylene (PTFE),
The pressure of 3MPa, in the protective atmosphere of 200 DEG C of argon gas, microwave reaction 20h collects the particulate matter of precipitating, that is, obtains ultra-fine cobalt
Sour powder for lithium.
Step 4: the GO obtained in the step of ultra-fine cobalt acid lithium powder of the 5mg obtained in step 3 is added to 300mL one
Solution, ultrasound break up 1h, are then adjusted to mixed solution alkalescent (pH value 7-8), and EDA reducing agent is added, will contain solution
Container sealing after, mechanical oscillation 5min avoids viscosity after EDA is added from increasing, avoids mixed solution wadding heavy, then carry out magnetic again
Power stirs 1h, i.e. acquisition lithium/cobalt-GO solution.
Step 5: lithium/cobalt-GO solution that step 4 obtains is put into the reaction kettle of polytetrafluoroethylene (PTFE), under protective gas
Hydro-thermal reaction is carried out, reaction temperature is 240 DEG C, and the time is that for 24 hours, protection gas uses argon gas, obtains lithium/cobalt-stone after the reaction was completed
The black alkene hydrosol.
Embodiment three
A kind of preparation method of the water-soluble plastic structure for lithium cobalt battery anode material, comprising the following steps:
Step 1: taking 10mg sheet graphene oxide, and the PBS solvent (phosphate buffered saline solution) of 100mL, 60 DEG C of water are added
Bath heating, carries out ultrasonic disperse 1h, obtains finely dispersed GO solution.
Specifically, the sheet graphene oxide is prepared using modified Hummer method.
Step 2: weighing 10mg lithium carbonate powder, is added in the dilute sulfuric acid that 100mL mass fraction is 2%, ultrasonic disperse,
Until powder all dissolves, 10mg cobaltous sulfate crystal powder (CoSO is then slowly added into mixing liquid4·7H2O), ultrasonic
Stirring is until powder all dissolutions, i.e. acquisition lithium-cobalt mixed solution.
Step 3: taking lithium obtained in step 2-cobalt mixed solution 100mL, be added in the reaction kettle of polytetrafluoroethylene (PTFE),
The pressure of 2MPa, in the protective atmosphere of 150 DEG C of argon gas, microwave reaction 15h collects the particulate matter of precipitating, that is, obtains ultra-fine cobalt
Sour powder for lithium.
Step 4: it is obtained in the step of ultra-fine cobalt acid lithium powder of the 10mg obtained in step 3 is added to 200mL one
GO solution, ultrasound break up 1h, are then adjusted to mixed solution alkalescent (pH value 7-8), EDA reducing agent are added, by Sheng Rong
After the container sealing of liquid, mechanical oscillation 3min avoids viscosity after EDA is added from increasing, avoids mixed solution wadding heavy, then carry out again
Magnetic agitation 0.5h, i.e. acquisition lithium/cobalt-GO solution.
Step 5: lithium/cobalt-GO solution that step 4 obtains is put into the reaction kettle of polytetrafluoroethylene (PTFE), under protective gas
Hydro-thermal reaction is carried out, reaction temperature is 120 DEG C, time 10h, and protection gas uses argon gas, obtains lithium/cobalt-stone after the reaction was completed
The black alkene hydrosol.
Example IV
A kind of preparation method of the water-soluble plastic structure for lithium cobalt battery anode material, comprising the following steps:
Step 1: taking 10mg sheet graphene oxide, and the PBS solvent (phosphate buffered saline solution) of 200mL, 80 DEG C of water are added
Bath heating, carries out ultrasonic disperse 5h, obtains finely dispersed GO solution.
Specifically, the sheet graphene oxide is prepared using modified Hummer method.
Step 2: weighing 10mg lithium carbonate powder, is added in the dilute sulfuric acid that 200mL mass fraction is 2%, ultrasonic disperse,
Until powder all dissolves, 10mg cobaltous sulfate crystal powder (CoSO is then slowly added into mixing liquid4·7H2O), ultrasonic
Stirring is until powder all dissolutions, i.e. acquisition lithium-cobalt mixed solution.
Step 3: taking lithium obtained in step 2-cobalt mixed solution 200mL, be added in the reaction kettle of polytetrafluoroethylene (PTFE),
The pressure of 3MPa, in the protective atmosphere of 200 DEG C of argon gas, microwave reaction 20h collects the particulate matter of precipitating, that is, obtains ultra-fine cobalt
Sour powder for lithium.
Step 4: it is obtained in the step of ultra-fine cobalt acid lithium powder of the 10mg obtained in step 3 is added to 300mL one
GO solution, ultrasound break up 2h, are then adjusted to mixed solution alkalescent (pH value 7-8), EDA reducing agent are added, by Sheng Rong
After the container sealing of liquid, mechanical oscillation 5min avoids viscosity after EDA is added from increasing, avoids mixed solution wadding heavy, then carry out again
Magnetic agitation 1h, i.e. acquisition lithium/cobalt-GO solution.
Step 5: lithium/cobalt-GO solution that step 4 obtains is put into the reaction kettle of polytetrafluoroethylene (PTFE), under protective gas
Hydro-thermal reaction is carried out, reaction temperature is 240 DEG C, and the time is that for 24 hours, protection gas uses argon gas, obtains lithium/cobalt-stone after the reaction was completed
The black alkene hydrosol.
The present invention is not limited to the embodiment, anyone should learn that the structure made under the inspiration of the present invention becomes
Change, the technical schemes that are same or similar to the present invention are fallen within the scope of protection of the present invention.
Technology not described in detail in the present invention, shape, construction portion are well-known technique.
Claims (3)
1. a kind of preparation method of the water-soluble plastic structure for lithium cobalt battery anode material, it is characterised in that: the following steps are included:
Step 1: 2mg~10mg sheet graphene oxide is taken, (phosphate-buffered salt is molten for the PBS solvent of addition 100mL~200mL
Liquid), 60 DEG C~80 DEG C heating water baths carry out ultrasonic disperse 1h~5h, obtain finely dispersed GO solution.
Step 2: weighing 4mg~10mg lithium carbonate powder, is added in the dilute sulfuric acid that 100mL~200mL mass fraction is 2%, surpasses
Then sound dispersion is slowly added to 4mg~10mg cobaltous sulfate crystal powder until powder all dissolves into mixing liquid
(CoSO4·7H2O), ultrasonic agitation is until powder all dissolutions, i.e. acquisition lithium-cobalt mixed solution.
Step 3: taking lithium obtained in step 2-cobalt mixed solution 100mL~200mL, is added in reaction kettle, 2MPa~
The pressure of 3MPa, in 150 DEG C~200 DEG C of protective atmosphere, microwave reaction 15h~20h collects the particulate matter of precipitating, that is, obtains
Ultra-fine cobalt acid lithium powder.
Step 4: the step of ultra-fine cobalt acid lithium powder of the 5mg~10mg obtained in step 3 is added to 200mL~300mL one
The GO solution of middle acquisition, ultrasound break up 1h~2h, are then adjusted to mixed solution alkalescent (pH value 7-8), and EDA is added also
Former agent, by after the container sealing for containing solution, mechanical oscillation 3-5min avoids viscosity after EDA is added from increasing, mixed solution is avoided to wad a quilt with cotton
It is heavy, magnetic agitation 0.5h~1h is then carried out again, i.e. acquisition lithium/cobalt-GO solution.
Step 5: lithium/cobalt-GO solution that step 4 obtains being put into reaction kettle, carries out hydro-thermal reaction under protective gas, reaction
Temperature be 120~240 DEG C, the time be 10~for 24 hours, obtain lithium/cobalt-graphene hydrosol after the reaction was completed.
2. a kind of preparation method of water-soluble plastic structure for lithium cobalt battery anode material according to claim 1, special
Sign is: the reaction kettle uses ptfe autoclave, and the protective atmosphere uses argon atmosphere.
3. a kind of preparation method of water-soluble plastic structure for lithium cobalt battery anode material according to claim 1, special
Sign is: the sheet graphene oxide is prepared using modified Hummer method.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112266026A (en) * | 2020-10-30 | 2021-01-26 | 常州大学 | Method for preparing cobaltate perovskite material |
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Application publication date: 20190628 |