CN108448078A - A kind of preparation method of tinbase/carbon lithium ion cell negative electrode material - Google Patents
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- CN108448078A CN108448078A CN201810141412.5A CN201810141412A CN108448078A CN 108448078 A CN108448078 A CN 108448078A CN 201810141412 A CN201810141412 A CN 201810141412A CN 108448078 A CN108448078 A CN 108448078A
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- 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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Abstract
The invention discloses a kind of preparation methods of tinbase/carbon lithium ion cell negative electrode material, include the following steps：A, in deionized water by graphene oxide dissolving, ultrasonic disperse forms graphene oxide solution；B, butter of tin and thiocarbamide are dissolved in respectively in above-mentioned graphene oxide solution, and continual ultrasonic stirs evenly under room temperature state；C, the step b solution obtained is freezed, and carries out vacuum freeze drying and obtains presoma；D, presoma is ground, and is calcined under protective atmosphere.The problems such as preparation process caused by hydro-thermal method and solvent-thermal method is complicated can be solved, synthesizing mean is simple, is easy to be prepared on a large scale, and tinbase obtained/carbon lithium ion cell negative electrode material particle is uniformly tiny, circulation volume and excellent electrochemical performance.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, more particularly, to a kind of tinbase/carbon lithium from
The preparation method of sub- cell negative electrode material, belongs to lithium ion battery material and electrochemical field.
Background technology
Lithium ion battery becomes and works as since energy density is high, have extended cycle life, high security, pollutes the excellent characteristics such as few
Preceding most potential power battery and energy storage device.The electrode material of lithium-ion-power cell is the key that influence its performance
Place, and the negative material for the lithium ion battery being commercialized at present is mostly graphite type material, theoretical capacity is only 372mAh g-1,
And there are serious safety problems during high rate charge-discharge, cannot be satisfied demand of the people to battery performance.Therefore
It is most important to research and develop novel anode material.
Tin-based material is due to higher theoretical capacity (994mAh/g) and preferable security performance, and its resource is rich
The advantages that rich, at low cost, it has also become one of the research hotspot of novel cathode material for lithium ion battery in recent years.Wherein, artificial gold
(SnS2) due to resourceful, the features such as specific capacity height and stable structure is considered as most wishing to become next-generation power battery
Negative material.Zhai et al. (J.Phys.Chem.C, 2012,116,12475-12481) prepares SnS using hydro-thermal method2It is ultra-thin
Nanometer sheet is 100mA g in current density-1513mAh g are shown after 50 circle of cycle-1.Jiao et al. (RSC Advances,
2013,3,699-703) go out flower-shaped SnS using solvent structure2Material recycles 100 circles at current density 100mA g-1,
Specific discharge capacity can reach 549.5mAh g-1.Tang et al. (Appl.Surf.Sci., 2015,355,7-13) utilizes hydro-thermal method
Synthesize SnS2Nanometer sheet is embedded in the composite material in three-dimensional grapheme structure, is 2000mA g in current density-1When, electric discharge
Specific capacity reaches 670mAh g-1。
Currently, hydro-thermal method, solvent-thermal method and solid phase method can synthesize the SnS of different-shape2, but hydro-thermal method and solvent
Heat is suitable for laboratory and prepares, and mailing reagent is needed to cannot be satisfied the demand that business is produced in enormous quantities；Although solid phase method is suitble to quotient
Industry metaplasia is produced, but active material pattern is uncontrollable, it is easy to be reunited, be caused its cycle life short, significantly limit it
Commercial applications.Therefore ensureing the circulation volume of material and commercially producing, needing to carry out the preparation process of the material excellent
Change and improves.
Invention content
In view of the drawbacks of the prior art, the present invention provides a kind of preparation sides of tinbase/carbon lithium ion cell negative electrode material
Method can not only keep considerable high rate performance and cyclical stability, but also commercial applications may be implemented.
Technical solution of the present invention is as follows：A kind of preparation method of tinbase/carbon lithium ion cell negative electrode material, including following step
Suddenly：
A, in deionized water by graphene oxide dissolving, ultrasonic disperse forms graphene oxide solution；
B, butter of tin and thiocarbamide are dissolved in respectively in above-mentioned graphene oxide solution, and persistently surpassed under room temperature state
Sound stirs evenly；
C, the step b solution obtained is freezed, and carries out vacuum freeze drying and obtains presoma；
D, presoma is ground, and is calcined under protective atmosphere.
Preferably, in step a, a concentration of 1.0~2.0mg/ml of graphene oxide solution.
Preferably, in step b, the molar ratio of butter of tin and thiocarbamide is 1:2~1:3, in oxidation stone based on butter of tin
Addition is 0.05~0.1mol/L in black alkene solution.
Preferably, in step c, when solution is freezed, freezing environment temperature is less than -4 DEG C, the vacuum freeze drying time
20h or more.
Preferably, in step d, protective atmosphere is argon gas atmosphere.
Preferably, in step d, 350~500 DEG C of calcination temperature, calcination time 2h or more.
The advantages of technical solution provided by the present invention, is：It is multiple with three-dimensional grapheme that artificial gold is prepared using pyrolysismethod
Composite electrode material can solve the problems such as preparation process caused by hydro-thermal method and solvent-thermal method is complicated, and synthesizing mean is simple, hold
Easily it is prepared on a large scale.The nano particle synthesized using the method for the present invention is dispersed in graphene, and excellent electrification is shown
Learn performance.At current density 60mA/g, 0.001~3.0V voltage ranges, SnS2The initial discharge capacity of/G can reach
1280mAh g-1, in high current 3000mA g-1Under, specific discharge capacity can reach 590mAh g-1.It is 300mA in current density
When g-1, capacity may remain in 678mAh g after 200 circles-1。
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of lithium ion battery negative material artificial gold/carbon made from embodiment 1.
Fig. 2 is the XRD diagram of lithium ion battery negative material artificial gold/carbon made from embodiment 1.
Fig. 3 is the initial charge/discharge curve graph of lithium ion battery negative material artificial gold/carbon made from embodiment 1.
Fig. 4 is the high rate performance figure of lithium ion battery negative material artificial gold/carbon made from embodiment 1.
Fig. 5 is the cycle performance figure of lithium ion battery negative material artificial gold/carbon made from embodiment 1.
Specific implementation mode
With reference to embodiment, the invention will be further described, but not as a limitation of the invention.
Embodiment 1
It takes 0.050g graphene oxides to be dissolved into the deionized water of 40ml, then ultrasonic disperse 2 hours, is formed light yellow
Graphene oxide solution.Then the SnCl of 0.71g is taken4·5H2The thiocarbamide of O and 0.305g is added in graphene oxide solution, after
Continuous ultrasonic agitation 30 minutes.Above-mentioned solution is transferred in refrigerator and is freezed 24 hours, refrigerator temperature is less than -4 DEG C, carries out vacuum afterwards
It is freeze-dried 48h, obtains presoma.
It takes being placed in tube furnace for the presoma grinding being dried to obtain to calcine 2h in 400 DEG C of argon gas atmospheres, is ground after taking-up
It is target product to grind obtained powder sample.Scanning electron microscope (SEM) photograph, XRD diagram, the initial charge/discharge curve of obtained target product
Figure, high rate performance figure and cycle performance figure difference are as shown in Figures 1 to 5.
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF (binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, be placed in vacuum drying chamber 100 DEG C of dryings 10 hours.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative plate, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF of 1mol/L6/ EC+DMC (volume ratios 1:1), full of argon gas
CR2016 type button cells are assembled in the glove box of protection.Using LAND CT2001A types (the blue electricity in Wuhan) multi-channel battery test
System testing, temperature are 25 DEG C of room temperature.
The material synthesized under this condition in voltage range between 0.001~3.0V, current density be 60mA/g test when,
SnS2The initial discharge capacity of/G can reach 1280mAh g-1, in high current 3000mA g-1Under, specific discharge capacity can reach
590mAh g-1.It is 300mAg in current density-1When, capacity may remain in 678mAh g after charge and discharge cycles 200 are enclosed-1。
Embodiment 2
It takes 0.040g graphene oxides to be dissolved into the deionized water of 40ml, then ultrasonic disperse 2 hours, is formed light yellow
Graphene oxide solution.Then the SnCl of 1.42g is taken4·5H2The thiocarbamide of O and 0.61g is added in graphene oxide solution, after
Continuous ultrasonic agitation 30 minutes.Above-mentioned solution is transferred in refrigerator and is freezed 24 hours, refrigerator temperature be less than -4 DEG C, after freezed
Dry 36h, obtains presoma.
Take the presoma grinding being dried to obtain is placed on 350 DEG C of argon gas atmosphere calcining 2.5h in tube furnace, is ground after taking-up
It is target product to grind obtained powder sample.
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF (binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, be placed in vacuum drying chamber 100 DEG C of dryings 10 hours.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative plate, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF6/EC+DMC (volume ratios 1 of 1mol/L:1), full of argon gas
CR2016 type button cells are assembled in the glove box of protection.Using LAND CT2001A types (the blue electricity in Wuhan) multi-channel battery test
System testing, temperature are 25 DEG C of room temperature.
The material synthesized under this condition in voltage range between 0.001~3.0V, current density be 60mA/g test when,
SnS2The initial discharge capacity of/G can reach 1190mAh g-1, in high current 3000mA g-1Under, specific discharge capacity can reach
558mAh g-1.It is 300mAg in current density-1When, capacity may remain in 610mAh g after charge and discharge cycles 200 are enclosed-1。
Embodiment 3
It takes 0.060g graphene oxides to be dissolved into the deionized water of 40ml, then ultrasonic disperse 2 hours, is formed light yellow
Graphene oxide solution.Then the SnCl of 0.71g is taken4·5H2The thiocarbamide of O and 0.457g is added in graphene oxide solution, after
Continuous ultrasonic agitation 30 minutes.Above-mentioned solution is transferred in refrigerator and is freezed 24 hours, refrigerator temperature be less than -4 DEG C, after freezed
At dry two nights, obtain presoma.
Take the presoma grinding being dried to obtain is placed on 500 DEG C of argon gas atmosphere calcining 2h in tube furnace, is ground after taking-up
Obtained powder sample is target product.
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF (binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, be placed in vacuum drying chamber 100 DEG C of dryings 10 hours.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative plate, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF6/EC+DMC+DEC (volume ratios 1 of 1mol/L:1:1) it, is filling
CR2016 type button cells are assembled in the glove box of full argon gas protection.Using LAND CT2001A types (the blue electricity in Wuhan) multichannel electricity
Pond test system and test, temperature are 25 DEG C of room temperature.
The material synthesized under this condition in voltage range between 0.001~3.0V, current density be 60mA/g test when,
SnS2The initial discharge capacity of/G can reach 1203mAh g-1, in high current 3000mA g-1Under, specific discharge capacity can reach
570mAh g-1.It is 300mA g in current density-1When, capacity may remain in 662mAh g after charge and discharge cycles 200 are enclosed-1。
Embodiment 4
It takes 0.080g graphene oxides to be dissolved into the deionized water of 40ml, then ultrasonic disperse 2 hours, is formed light yellow
Graphene oxide solution.Then the SnCl of 1.42g is taken4·5H2The thiocarbamide of O and 0.914g is added in graphene oxide solution, after
Continuous ultrasonic agitation 30 minutes.Above-mentioned solution is transferred in refrigerator and is freezed 24 hours, refrigerator temperature be less than -4 DEG C, after freezed
At dry two nights, obtain presoma.
Take the presoma grinding being dried to obtain is placed on 450 DEG C of argon gas atmosphere calcining 2.5h in tube furnace, is ground after taking-up
It is target product to grind obtained powder sample.
By the sample (active material) of synthesis, acetylene black (conductive agent) and PVDF (binder) according to mass ratio 7:2:1,
It is uniformly mixed in NMP, is then coated on copper foil, be placed in vacuum drying chamber 100 DEG C of dryings 10 hours.It is cut into after taking out straight
Diameter is the electrode disk of 12mm.In this, as negative plate, using metal lithium sheet as to electrode, microporous polypropylene membrane Celgard
2400 be diaphragm, and nickel foam is filler, and electrolyte is the LiPF6/EC+DMC (volume ratios 1 of 1mol/L:1), full of argon gas
CR2016 type button cells are assembled in the glove box of protection.Using LAND CT2001A types (the blue electricity in Wuhan) multi-channel battery test
System testing, temperature are 25 DEG C of room temperature.
The material synthesized under this condition in voltage range between 0.001~3.0V, current density be 60mA/g test when,
SnS2The initial discharge capacity of/G can reach 1203mAh g-1, in high current 3000mA g-1Under, specific discharge capacity can reach
565mAh g-1.It is 300mA g in current density-1When, capacity may remain in 630mAh g after charge and discharge cycles 200 are enclosed-1。
Claims (6)
1. a kind of preparation method of tinbase/carbon lithium ion cell negative electrode material, which is characterized in that include the following steps：
A, in deionized water by graphene oxide dissolving, ultrasonic disperse forms graphene oxide solution；
B, butter of tin and thiocarbamide are dissolved in respectively in above-mentioned graphene oxide solution, and continual ultrasonic stirs under room temperature state
It mixes uniformly；
C, the step b solution obtained is freezed, and carries out vacuum freeze drying and obtains presoma；
D, presoma is ground, and is calcined under protective atmosphere.
2. the preparation method of tinbase according to claim 1/carbon lithium ion cell negative electrode material, which is characterized in that described
In step a, graphene oxide solution density is 1.0~2.0mg/ml.
3. the preparation method of tinbase according to claim 1/carbon lithium ion cell negative electrode material, which is characterized in that step b
In, the molar ratio of butter of tin and thiocarbamide is 1:2~1:3, addition is in graphene oxide solution based on butter of tin
0.05~0.1mol/L.
4. the preparation method of tinbase according to claim 1/carbon lithium ion cell negative electrode material, which is characterized in that described
In step c, when solution is freezed, freezing environment temperature is less than -4 DEG C, vacuum freeze drying time 20h or more.
5. the preparation method of tinbase according to claim 1/carbon lithium ion cell negative electrode material, which is characterized in that described
In step d, protective atmosphere is argon gas atmosphere.
6. the preparation method of tinbase according to claim 1/carbon lithium ion cell negative electrode material, which is characterized in that described
In step d, 350~500 DEG C of calcination temperature, calcination time 2h or more.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113903912A (en) * | 2021-09-30 | 2022-01-07 | 常熟理工学院 | Preparation method of carbon-loaded titanium carbide material, product obtained by preparation method and application of product |
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| WO2015074006A1 (en) * | 2013-11-15 | 2015-05-21 | The Regents Of The University Of California | Electrochemical devices comprising compressed gas solvent electrolytes |
| CN105869893A (en) * | 2016-04-11 | 2016-08-17 | 河南师范大学 | Method for one-step hydro-thermal synthesis of graphene-SnS2 composite counter electrode material |
| CN106654192A (en) * | 2016-08-13 | 2017-05-10 | 华南理工大学 | Tin sulfide/graphene sodium ion battery composite cathode material and preparation method thereof |
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2018
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Patent Citations (4)
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| US20140113200A1 (en) * | 2011-07-25 | 2014-04-24 | Fraser Seymour | Functionalized Carbon Electrode, Related Material, Process for Production, and Use Thereof |
| WO2015074006A1 (en) * | 2013-11-15 | 2015-05-21 | The Regents Of The University Of California | Electrochemical devices comprising compressed gas solvent electrolytes |
| CN105869893A (en) * | 2016-04-11 | 2016-08-17 | 河南师范大学 | Method for one-step hydro-thermal synthesis of graphene-SnS2 composite counter electrode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113903912A (en) * | 2021-09-30 | 2022-01-07 | 常熟理工学院 | Preparation method of carbon-loaded titanium carbide material, product obtained by preparation method and application of product |
| CN113903912B (en) * | 2021-09-30 | 2023-06-23 | 常熟理工学院 | Preparation method of carbon-loaded titanium carbide material, and product and application obtained by preparation method |
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