CN107799750A - A kind of tin ash/N doping exfoliated-graphite composite and preparation method thereof - Google Patents
A kind of tin ash/N doping exfoliated-graphite composite and preparation method thereof Download PDFInfo
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- CN107799750A CN107799750A CN201711021635.XA CN201711021635A CN107799750A CN 107799750 A CN107799750 A CN 107799750A CN 201711021635 A CN201711021635 A CN 201711021635A CN 107799750 A CN107799750 A CN 107799750A
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- H—ELECTRICITY
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- 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
- H01M4/364—Composites as mixtures
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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Abstract
The invention provides a kind of preparation method of tin ash/N doping exfoliated-graphite composite, comprise the following steps：A) Expandable graphite sheet, urea and stanniferous presoma are dispersed in absolute ethyl alcohol, stirring to absolute ethyl alcohol whole is volatilized at 60~80 DEG C, obtains persursor material；B) under protective gas atmosphere, the persursor material is carbonized, obtains tin ash/N doping exfoliated-graphite composite.Nanoscale tin ash is uniformly embedded into N doping expanded graphite sheet matrix, and N doping expanded graphite not only possesses good electric conductivity, and can suppress volumetric expansion of the stannic oxide particle in charge and discharge process, so as to the structure of stabilized electrodes.The N doping expanded graphite of laminated structure can not only provide more storage lithium sites, and be advantageous to alleviate bulk effect, and provide more passages for the infiltration of electrolyte.Present invention also offers a kind of tin ash/N doping exfoliated-graphite composite.
Description
Technical field
The invention belongs to electrochemical technology field, more particularly to a kind of tin ash/N doping exfoliated-graphite composite
And preparation method thereof.
Background technology
With the development of society, energy problem increasingly becomes an important factor for restricting social development, in addition, a large amount of fossils
The utilization of the energy causes serious pollution to environment.Finding the energy substitution fossil energy of sustainable use and cleaning turns into generation
The target of various countries of boundary.The clean energy resourcies such as wind energy, solar energy arouse great concern, but due to the shakiness of these energy
It is qualitative so that directly utilizing it as energy supply turns into problem.It is a kind of that it, which is first laid in and then recycled, using energy storage device
Effective method.Lithium ion battery lithium ion battery is as a kind of wide variety of energy storage device, because having energy
The good characteristics such as density is big, self discharge is small, operating voltage is high, have extended cycle life, memory-less effect and non-environmental-pollution, in recent years
It is rapidly developed, has been considered to one of current maximally effective energy storage mode.
But the further raising of commercialized performance of lithium ion battery still has that many problem letters are to be solved, such as extensively
The graphite-like carbon negative pole material used, although excellent with cheap, environment-friendly, high structural stability and intrinsic conductivity height etc.
Point, but its theoretical specific capacity is low, only 372mA h g-1, which limits it in electric automobile, hybrid vehicle, military affairs etc.
Need the application in the field of high-energy-density and power density output.And the application in large-scale energy storage is also by certain
Limitation.Therefore, high power capacity, the negative material replacement graphite material of good cycling stability are that current lithium ion battery negative material is ground
Study carefully one of the hot issue in field.
Tin ash as lithium ion battery negative material possess specific capacity height, it is cheap and nontoxic the advantages of.But
Tin ash is serious Volumetric expansion in charge and discharge process be present as greatest problem existing for negative material, so as to
So that capacity exhaustion is too fast and cyclical stability is poor.Therefore, tin ash can not expire directly as lithium ion battery negative material
Requirement of the sufficient people to performance of lithium ion battery, therefore, the modification to tin ash negative material is tin ash is made
For a kind of effective method of commercial Li-ion battery negative material.
The content of the invention
It is an object of the invention to provide a kind of tin ash/N doping exfoliated-graphite composite and preparation method thereof,
Tin ash/N doping exfoliated-graphite composite in the present invention can effectively alleviate bulk effect, and specific capacity is high, circulation
Stability is good.
The present invention provides a kind of preparation method of tin ash/N doping exfoliated-graphite composite, comprises the following steps：
A) Expandable graphite sheet, urea and stanniferous presoma are dispersed in absolute ethyl alcohol, stirred at 60~80 DEG C to nothing
Water-ethanol all volatilizees, and obtains persursor material；
B) under protective gas atmosphere, the persursor material is carbonized, obtains tin ash/N doping expansion
Graphite composite material.
Preferably, the stanniferous presoma stannous chloride and/or stannic chloride.
Preferably, the mass ratio of the Expandable graphite sheet, urea and stanniferous presoma is (0.1~1)：(1~10)：(5~
40)。
Preferably, the temperature of the carbonization is 500~600 DEG C；
The time of the carbonization is 1~4 hour.
Preferably, the carburizing temperature is realized by heating, the speed of the heating is 1~10 DEG C/min.
The present invention provides a kind of tin ash/N doping exfoliated-graphite composite, is made according to above-mentioned preparation method.
Preferably, in the tin ash/N doping exfoliated-graphite composite the mass fraction of tin ash for 30~
80%.
Preferably, the particle diameter of tin ash is 5~50nm in the tin ash/N doping exfoliated-graphite composite.
The invention provides a kind of preparation method of tin ash/N doping exfoliated-graphite composite, including following step
Suddenly：A) Expandable graphite sheet, urea and stanniferous presoma are dispersed in absolute ethyl alcohol, stirred at 60~80 DEG C to absolute ethyl alcohol
All volatilizations, obtain persursor material；B) under protective gas atmosphere, the persursor material is carbonized, obtains two
Tin oxide/N doping exfoliated-graphite composite.Composite in the present invention includes N doping expanded graphite matrix and uniformly
The nano-stannic oxide particle being distributed in N doping expanded graphite sheet matrix.Nanoscale tin ash is uniformly embedded into nitrogen and mixed
In miscellaneous expanded graphite sheet matrix, N doping expanded graphite not only possesses good electric conductivity, and can suppress tin ash
Volumetric expansion of the grain in charge and discharge process, so as to the structure of stabilized electrodes.The N doping expanded graphite of laminated structure not only may be used
To provide more storage lithium sites, and be advantageous to alleviate bulk effect, and more passages are provided for the infiltration of electrolyte.
The preparation method of the present invention is simple, and cost is low, and obtained specific capacity of negative electrode material of lithium ion battery is high, good cycling stability.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
The embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings.
Fig. 1 is the SEM figures of tin ash/N doping exfoliated-graphite composite in the embodiment of the present invention 1；
Fig. 2 is the TEM figures of tin ash/N doping exfoliated-graphite composite in the embodiment of the present invention 1；
Fig. 3 is the stable circulation linearity curve of tin ash/N doping exfoliated-graphite composite made from embodiment 1.
Embodiment
The invention provides a kind of preparation method of tin ash/N doping exfoliated-graphite composite, including following step
Suddenly：
A) Expandable graphite sheet, urea and stanniferous presoma are dispersed in absolute ethyl alcohol, stirred at 60~80 DEG C to nothing
Water-ethanol all volatilizees, and obtains persursor material；
B) under protective gas atmosphere, the persursor material is carbonized, obtains tin ash/N doping expansion
Graphite composite material.
The present invention preferably by Expandable graphite sheet by ultrasonic disperse in absolute ethyl alcohol, then under stirring add urine
Plain and stanniferous presoma, mixed solution is stirred into 20~40min to uniform, solution is then warming up to 60~80 DEG C, persistently stirred
Mix 1~6 hour, ethanol is all volatilized, obtain persursor material.
In the present invention, the Expandable graphite sheet is preferred buys from Qingdao graphite material Co., Ltd, the stanniferous forerunner
Body is preferably stannous chloride and/or stannic chloride, the mass ratio of the Expandable graphite sheet, urea and stanniferous presoma for (0.1~
1)：(1~10)：(5~40), more preferably 1：(5~10)：(5~10), most preferably 1：(7.5~10)：(5~10), specifically
, can be 1 in an embodiment of the present invention:10:7.5,1:7.5:5,1:7.5:10 or 1:8:10.
In the present invention, the time of the Expandable graphite sheet ultrasonic disperse is preferably 10~30min, more preferably 15~
25min, most preferably 20min；It is preferred that the mixed solution is warming up into 70~80 DEG C, stirs 2 hours, all waved to ethanol
Hair.In the step of above-mentioned three kinds of material mixings, involved stirring is preferably entered with 300~1000rpm mixing speed
OK.
The present invention is preferably shown in above-mentioned persursor material under nitrogen and/or argon gas atmosphere, with 1~10 DEG C/min speed
It is warming up to 500~600 DEG C to be carbonized, is carbonized 1~4 hour, obtains tin ash/N doping exfoliated-graphite composite.
In the present invention, the speed of the heating is preferably 2~8 DEG C/min, more preferably 4~7 DEG C/min, is most preferably
5~6 DEG C/min；The temperature of the carbonization is preferably 500~600 DEG C, and the time of the carbonization is preferably 2~3 hours.
Present invention also offers a kind of tin ash/N doping exfoliated-graphite composite, according to above-mentioned preparation method system
, in the tin ash/N doping exfoliated-graphite composite, the mass fraction of tin ash is preferably 30~80%, more
Preferably 40~70%, most preferably 50~60%；The particle diameter of the tin ash is preferably 5~50nm, more preferably 10~
40nm, most preferably 20~30nm；The content of the nitrogen is preferably 0.01-0.1%, and more preferably 0.05~0.06%.
The invention provides a kind of preparation method of tin ash/N doping exfoliated-graphite composite, including following step
Suddenly：A) Expandable graphite sheet, urea and stanniferous presoma are dispersed in absolute ethyl alcohol, stirred at 60~80 DEG C to absolute ethyl alcohol
All volatilizations, obtain persursor material；B) under protective gas atmosphere, the persursor material is carbonized, obtains two
Tin oxide/N doping exfoliated-graphite composite.Composite in the present invention includes N doping expanded graphite matrix and uniformly
The nano-stannic oxide particle being distributed in N doping expanded graphite sheet matrix.Nanoscale tin ash is uniformly embedded into nitrogen and mixed
In miscellaneous expanded graphite sheet matrix, N doping expanded graphite not only possesses good electric conductivity, and can suppress tin ash
Volumetric expansion of the grain in charge and discharge process, so as to the structure of stabilized electrodes.The N doping expanded graphite of laminated structure not only may be used
To provide more storage lithium sites, and be advantageous to alleviate bulk effect, and more passages are provided for the infiltration of electrolyte.
The preparation method of the present invention is simple, and cost is low, and obtained specific capacity of negative electrode material of lithium ion battery is high, good cycling stability.
In order to further illustrate the present invention, with reference to embodiments to a kind of tin ash/N doping provided by the invention
Expanded graphite composite wood and preparation method thereof is described in detail, but can not be understood as the limit to the scope of the present invention
It is fixed.
Embodiment 1
0.2g Expandable graphite sheets are added in 100mL absolute ethyl alcohols, 20min is ultrasonically treated, makes Expandable graphite sheet in nothing
Disperse in water-ethanol complete.2g urea is added, stirring is completely dissolved it.Then 1.5g stannous chloride dihydrates are added, are persistently stirred
Mix.After stannous chloride is completely dissolved, ethanol is volatilized completely after stirring 2h at 70 DEG C, obtain persursor material.It will obtain
Precursor product be placed in tube furnace, in an argon stream, with 5 DEG C/min heating rate, 600 DEG C of 2h that are carbonized and are incubated,
Obtain tin ash/N doping Expandable graphite sheet composite.
According to 8：1：1 ratio is cohesive by the tin ash prepared/N doping exfoliated-graphite composite, acetylene black
Agent (PVDF) is mixed, and is then added N- methyl arsenic pyrrolidone solvents and is stirred.The slurry of gained is coated on aluminium foil,
120 DEG C of vacuum drying 12h, obtain positive plate.Button cell assembling is carried out in full of argon gas glove box, using lithium piece as negative pole,
Polypropylene is barrier film, LiPF6For electrolyte.The battery assembled is subjected to electrochemical property test.
Fig. 1 is the SEM figures of tin ash/N doping exfoliated-graphite composite in the embodiment of the present invention 1, and Fig. 2 is this hair
The TEM figures of tin ash/N doping exfoliated-graphite composite in bright embodiment 1.The titanium dioxide sijna it can be seen from Fig. 1~2
Rice grain is uniformly embedded into N doping expanded graphite, forms tin ash/N doping exfoliated-graphite composite.
Fig. 3 is the stable circulation linearity curve of tin ash/N doping exfoliated-graphite composite made from embodiment 1,
The capability retention of 50 holdings 100% is circulated under 200mA/g current densities；100 98.3% capability retentions of holding of circulation.
Embodiment 2
0.2g Expandable graphite sheets are added in 100mL absolute ethyl alcohols, 20min is ultrasonically treated, makes Expandable graphite sheet in nothing
Disperse in water-ethanol complete.1.5g urea is added, stirring is completely dissolved it.Then 1.0g stannous chloride dihydrates are added, are continued
Stirring.After stannous chloride is completely dissolved, ethanol is volatilized completely after stirring 2h at 80 DEG C, obtain persursor material.It will obtain
The precursor product obtained is placed in tube furnace, and in an argon stream, with 5 DEG C/min heating rate, 500 DEG C of carbonizations are simultaneously incubated
2h, obtain tin ash/N doping Expandable graphite sheet composite.
According to 8：1：1 ratio is cohesive by the tin ash prepared/N doping exfoliated-graphite composite, acetylene black
Agent (PVDF) is mixed, and is then added N- methyl arsenic pyrrolidone solvents and is stirred.The slurry of gained is coated on aluminium foil,
120 DEG C of vacuum drying 12h, obtain positive plate.Button cell assembling is carried out in full of argon gas glove box, using lithium piece as negative pole,
Polypropylene is barrier film, LiPF6For electrolyte.The battery assembled is subjected to electrochemical property test.Tin ash/N doping is swollen
Swollen graphite composite material shows excellent cycling stability.
Embodiment 3
0.2g Expandable graphite sheets are added in 100mL absolute ethyl alcohols, 20min is ultrasonically treated, makes Expandable graphite sheet in nothing
Disperse in water-ethanol complete.1.5g urea is added, stirring is completely dissolved it.Then 2.0g butters of tin, lasting stirring are added.
After butter of tin is completely dissolved, ethanol is volatilized completely after stirring 2h at 70 DEG C, obtain persursor material.Before acquisition
Drive body product to be placed in tube furnace, in an argon stream, with 5 DEG C/min heating rate, 600 DEG C are carbonized and are incubated 2h, obtain
Tin ash/N doping Expandable graphite sheet composite.
According to 8：1：1 ratio is cohesive by the tin ash prepared/N doping exfoliated-graphite composite, acetylene black
Agent (PVDF) is mixed, and is then added N- methyl arsenic pyrrolidone solvents and is stirred.The slurry of gained is coated on aluminium foil,
120 DEG C of vacuum drying 12h, obtain positive plate.Button cell assembling is carried out in full of argon gas glove box, using lithium piece as negative pole,
Polypropylene is barrier film, LiPF6For electrolyte.The battery assembled is subjected to electrochemical property test.Tin ash/N doping is swollen
Swollen graphite composite material shows excellent cycling stability.
Embodiment 4
0.15g Expandable graphite sheets are added in 100mL absolute ethyl alcohols, 20min is ultrasonically treated, makes Expandable graphite sheet in nothing
Disperse in water-ethanol complete.1.2g urea is added, stirring is completely dissolved it.Then 1.5g butters of tin, lasting stirring are added.
After butter of tin is completely dissolved, ethanol is volatilized completely after stirring 2h at 70 DEG C, obtain persursor material.Before acquisition
Drive body product to be placed in tube furnace, in an argon stream, with 5 DEG C/min heating rate, 500 DEG C are carbonized and are incubated 2h, obtain
Tin ash/N doping Expandable graphite sheet composite.
According to 8：1：1 ratio is cohesive by the tin ash prepared/N doping exfoliated-graphite composite, acetylene black
Agent (PVDF) is mixed, and is then added N- methyl arsenic pyrrolidone solvents and is stirred.The slurry of gained is coated on aluminium foil,
120 DEG C of vacuum drying 12h, obtain positive plate.Button cell assembling is carried out in full of argon gas glove box, using lithium piece as negative pole,
Polypropylene is barrier film, LiPF6For electrolyte.The battery assembled is subjected to electrochemical property test.Tin ash/N doping is swollen
Swollen graphite composite material shows excellent cycling stability.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of tin ash/N doping exfoliated-graphite composite, comprises the following steps：
A) Expandable graphite sheet, urea and stanniferous presoma are dispersed in absolute ethyl alcohol, stirred at 60~80 DEG C to anhydrous second
Alcohol all volatilizees, and obtains persursor material；
B) under protective gas atmosphere, the persursor material is carbonized, obtains tin ash/N doping expanded graphite
Composite.
2. preparation method according to claim 1, it is characterised in that the stanniferous presoma stannous chloride and/or chlorination
Tin.
3. preparation method according to claim 1, it is characterised in that the Expandable graphite sheet, urea and stanniferous presoma
Mass ratio be (0.1~1)：(1~10)：(5~40).
4. preparation method according to claim 1, it is characterised in that the temperature of the carbonization is 500~600 DEG C；
The time of the carbonization is 1~4 hour.
5. preparation method according to claim 4, it is characterised in that the carburizing temperature, the liter are realized by heating
The speed of temperature is 1~10 DEG C/min.
A kind of 6. tin ash/N doping exfoliated-graphite composite, according to the preparation described in Claims 1 to 5 any one
Method is made.
7. tin ash according to claim 6/N doping exfoliated-graphite composite, it is characterised in that the dioxy
The mass fraction for changing tin ash in tin/N doping exfoliated-graphite composite is 30~80%.
8. tin ash according to claim 6/N doping exfoliated-graphite composite, it is characterised in that the dioxy
The particle diameter for changing tin ash in tin/N doping exfoliated-graphite composite is 5~50nm.
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Cited By (4)
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| CN108400312A (en) * | 2018-03-27 | 2018-08-14 | 广东工业大学 | A kind of nickel antimony alloy/N doping exfoliated-graphite composite and preparation method thereof |
| CN109546099A (en) * | 2018-10-16 | 2019-03-29 | 中航锂电（洛阳）有限公司 | A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery |
| CN111477842A (en) * | 2020-04-07 | 2020-07-31 | 山西大学 | Preparation device and preparation method of vertical structure electrode |
| CN114447305A (en) * | 2022-01-29 | 2022-05-06 | 辽宁中宏能源新材料股份有限公司 | Multi-element carbon-based rapid-charging negative electrode composite material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108400312A (en) * | 2018-03-27 | 2018-08-14 | 广东工业大学 | A kind of nickel antimony alloy/N doping exfoliated-graphite composite and preparation method thereof |
| CN108400312B (en) * | 2018-03-27 | 2021-03-16 | 广东工业大学 | Nickel-antimony alloy/nitrogen-doped expanded graphite composite material and preparation method thereof |
| CN109546099A (en) * | 2018-10-16 | 2019-03-29 | 中航锂电（洛阳）有限公司 | A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery |
| CN109546099B (en) * | 2018-10-16 | 2021-08-31 | 中航锂电（洛阳）有限公司 | Graphite composite negative electrode material, preparation method thereof and lithium ion battery |
| CN111477842A (en) * | 2020-04-07 | 2020-07-31 | 山西大学 | Preparation device and preparation method of vertical structure electrode |
| CN111477842B (en) * | 2020-04-07 | 2021-07-02 | 山西大学 | Preparation device and preparation method of vertical structure electrode |
| CN114447305A (en) * | 2022-01-29 | 2022-05-06 | 辽宁中宏能源新材料股份有限公司 | Multi-element carbon-based rapid-charging negative electrode composite material and preparation method thereof |
| CN114447305B (en) * | 2022-01-29 | 2023-08-08 | 辽宁中宏能源新材料股份有限公司 | Multi-carbon-based quick-charge anode composite material and preparation method thereof |
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