CN106159210A - The preparation method of lithium ion battery carbon/stannum/Graphene composite nano fiber - Google Patents
The preparation method of lithium ion battery carbon/stannum/Graphene composite nano fiber Download PDFInfo
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- CN106159210A CN106159210A CN201510213903.2A CN201510213903A CN106159210A CN 106159210 A CN106159210 A CN 106159210A CN 201510213903 A CN201510213903 A CN 201510213903A CN 106159210 A CN106159210 A CN 106159210A
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- composite nano
- stannum
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses the preparation method of lithium ion battery carbon/stannum/Graphene composite nano fiber, belong to nano material and technical field of chemical power.The present invention is by being dissolved in N by polyacrylonitrile, stannous chloride, Graphene respectively, dinethylformamide, it is mixing uniformly to form spinning liquid, recycling electrostatic spinning technique prepares polyacrylonitrile/stannous chloride/Graphene composite nano-fiber membrane, is then passed through carbonization and obtains carbon/stannum/Graphene composite nano fiber negative material.Preparation technology of the present invention is simple, and production cost is low.Material prepared by the present invention is for lithium ion battery negative material, having the electrochemical properties of excellence, good cycle, multiplying power property is good, overcome tin base cathode material cycle performance difference shortcoming, can be used widely in portable equipment as a new generation's lithium ion battery negative material.
Description
Technical field
The present invention relates to a kind of preparation method for lithium ion battery negative material, particularly relate to electrostatic spinning and prepare carbon/stannum/graphite
The method of alkene composite nano fiber, belongs to nano material and technical field of chemical power.
Background technology
Current era, the concept of sustainable development increasingly becomes the common recognition of the mankind.Coal, oil, the big main energy sources of natural gas three
A large amount of uses of the Fossil fuel for representing, bring huge pressure to ecological environment.And along with the exhaustion day by day of resource,
The development and utilization of reproducible clean energy resource was particularly important in today.Lithium ion battery is owing to open-circuit voltage is high, specific capacity
Greatly, self-discharge rate is low, life-span length, memory-less effect etc. have advantage to become modern high performance and clean energy resource representative, extensively
Being applied on miniaturized electronics, especially at electric automobile, Aero-Space and military field also have preferable prospect.
At present, the negative material used in commercial lithium-ion batteries is mainly graphite material, and its theoretical specific capacity is only 372
MAh/g, can not meet people's demand to battery performance.Therefore exploitation and the industrialization of Novel ion cell negative electrode material should
With becoming an important topic.The theoretical specific capacity (990mAh/g) of metallic tin (Sn) negative material Yin Qigao and volume specific volume
Amount (7200mAh/cm3), it is nearly three times of traditional carbon negative pole material theoretical capacity, has become the main flow studied in the world and born
One of pole material.When stannum is as lithium ion battery negative material, during the embedding and deintercalation of lithium ion, change in volume is violent,
Material internal can produce stress, and the macro-mechanical performance of stannum itself can not be enough to resist the stress produced therefrom, thus leads
Cause material of main part is broken, efflorescence, so that the efficiency for charge-discharge of electrode is low, cycle performance is very poor.
Graphene has special construction and performance because of it, and its application in lithium ion battery electrode material have also been obtained extensive concern.
The Two-dimensional Carbon material of this monolayer carbon atomic thickness has broad theory specific surface area (2600m2/ g) and cellular void structure, thus
There is higher storage lithium ability.Additionally, the high electron mobility (15000cm of material itself2/ (V s)), prominent heat conductivility (3000
W/ (m K)), the mechanical property (stretch modulus 1.01TPa) of good chemical stability and excellence so that it is as combination electrode
The matrix of material has more outstanding advantage.
The developing into of electrostatic spinning technique is prepared new electrode materials and is provided new probability, utilizes electrostatic spinning to prepare and receives
Rice or micron-sized fibrous material.The appearance structure of its uniqueness of nanofiber and specific surface area are applied to lithium ion battery and demonstrate
Big advantage: electrode/electrolyte contact area is big, and the path of electronics and lithium ion conduction is short, output is high;Lithium deintercalation
During bulk effect little, cycle life improve.Therefore, nano-fiber material can significantly improve battery for lithium ion battery
Specific capacity and rate charge-discharge performance.At present, electrostatic spinning and high temperature cabonization technology is utilized to prepare carbon/stannum/Graphene composite Nano
Fiber is also seen for the relevant report of lithium ion battery negative material.
Summary of the invention
For the shortcoming and defect of prior art, the primary and foremost purpose of the present invention is to provide a kind of negative material for lithium ion battery
The preparation method of carbon/stannum/Graphene composite nano fiber.
The technical scheme is that with polyacrylonitrile (PAN), stannous chloride (SnCl2·2H2O), Graphene and N, N-diformazan
Base Methanamide (DMF) is raw material.First with electro-spinning for presoma PAN/SnCl2/ Graphene composite nano-fiber membrane, so
After obtained composite nano-fiber membrane is placed on carbonization in high temperature process furnances, just obtain carbon/stannum/Graphene composite nano fiber negative pole
Material.Specifically comprise the following steps that
(1) weighing a certain amount of PAN to be dissolved in DMF, preparation mass fraction is the solution of 8~15%, puts into stirrer,
Regulating suitable rotating speed, under room temperature, stirring stands de-bubble to uniformly in 12~24 hours.
(2) weighing a certain amount of stannous chloride and Graphene adds in above-mentioned (1) solution, put into stirrer equally, regulation is suitable
Work as rotating speed, stir 8~10 hours under room temperature to forming homogeneous solution.
(3) by the solution ultrasonic vibration 1 in step (2)~3 hours to uniformly.
(4) solution in step (3) is carried out spinning in electrostatic spinning apparatus, obtain PAN/SnCl2/ Graphene is compound to be received
Rice fibrous membrane, spinning voltage is 10~20kV, and receiving range is 10~20cm, and spinning speed is 0.2~2mL/h.
(5) composite nano-fiber membrane obtained in step (4) is put in tube furnace, in air atmosphere with heating rate be
1~10 DEG C/min, from room temperature to 200~300 DEG C, keeps temperature 2~5h.Heat up under nitrogen or argon atmosphere afterwards
Carrying out carbonization to 600~1000 DEG C, heating rate is 1~10 DEG C/min, insulation 2~5h after be cooled to room temperature, obtain carbon/stannum/
Graphene composite nano fiber.
Compared with prior art, the invention have the advantages that and effect:
(1) lithium ion battery negative material carbon/stannum of the present invention/Graphene composite nano fiber preparation technology is simple, production cost
Cheap, it is simple to expanding production further.
(2) carbon/stannum/Graphene composite nano fiber a diameter of 100~300 nanometer that prepared by the present invention, tin nanoparticles and graphite
Alkene is uniformly dispersed in fiber.Having the electrochemical properties of excellence, first charge-discharge efficiency is high, specific capacity height (, cyclicity
Can be good, there is good high-rate characteristics simultaneously.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope image of prepared carbon/stannum/Graphene composite nano fiber.
Fig. 2 is first all charging and discharging curves of prepared carbon/stannum/Graphene composite nano fiber.
Detailed description of the invention
Embodiment 1
The PAN weighing 3g is dissolved in 27g DMF, puts into stirrer, regulates suitable rotating speed, stirs 12~24 under room temperature
Hour to uniformly, preparing PAN mass fraction is the DMF solution of 10%.Weigh stannous chloride and the 0.15g graphite of 1.5g
Alkene adds in above-mentioned DMF solution, puts into stirrer equally, regulates suitable rotating speed, stirs 8~10 hours, ultrasonic shake under room temperature
Swing 1~3 hours to forming homogeneous solution.Use electrostatic spinning apparatus to carry out spinning, obtain PAN/SnCl2/ Graphene is compound to be received
Rice fibrous membrane, spinning voltage is 20kV, and receiving range is 20cm, and spinning speed is 1mL/h.The composite Nano fibre that will obtain
Dimension film is put in tube furnace, is 2 DEG C/min from room temperature to 250 DEG C with heating rate, keeps temperature 2h in air atmosphere.
Being warming up to 800 DEG C under nitrogen protection atmosphere afterwards and carry out carbonization, heating rate is 1 DEG C/min, is cooled to room after insulation 5h
Temperature, obtains carbon/stannum/Graphene composite nano fiber.
Embodiment 2
The PAN weighing 3g is dissolved in 27g DMF, puts into stirrer, regulates suitable rotating speed, stirs 12~24 under room temperature
Hour to uniformly, preparing PAN mass fraction is the DMF solution of 10%.Weigh stannous chloride and the 0.15g graphite of 1.5g
Alkene adds in above-mentioned DMF solution, puts into stirrer equally, regulates suitable rotating speed, stirs 8~10 hours, ultrasonic shake under room temperature
Swing 1~3 hours to forming homogeneous solution.Use electrostatic spinning apparatus to carry out spinning, obtain PAN/SnCl2/ Graphene is compound to be received
Rice fibrous membrane, spinning voltage is 15kV, and receiving range is 25cm, and spinning speed is 0.5mL/h.The composite Nano that will obtain
Fibrous membrane is put in tube furnace, is 4 DEG C/min from room temperature to 300 DEG C with heating rate, keeps temperature 2 in air atmosphere
h.Being warming up to 600 DEG C under nitrogen protection atmosphere afterwards and carry out carbonization, heating rate is 2 DEG C/min, lowers the temperature after insulation 5h
To room temperature, obtain carbon/stannum/Graphene composite nano fiber.
Embodiment 3
The PAN weighing 3g is dissolved in 27g DMF, puts into stirrer, regulates suitable rotating speed, stirs 12~24 under room temperature
Hour to uniformly, preparing PAN mass fraction is the DMF solution of 10%.Weigh stannous chloride and the 0.15g graphite of 1.5g
Alkene adds in above-mentioned DMF solution, puts into stirrer equally, regulates suitable rotating speed, stirs 8~10 hours, ultrasonic shake under room temperature
Swing 1~3 hours to forming homogeneous solution.Use electrostatic spinning apparatus to carry out spinning, obtain PAN/SnCl2/ Graphene is compound to be received
Rice fibrous membrane, spinning voltage is 18kV, and receiving range is 22cm, and spinning speed is 0.8mL/h.The composite Nano that will obtain
Fibrous membrane is put in tube furnace, is 5 DEG C/min from room temperature to 300 DEG C with heating rate, keeps temperature 3 in air atmosphere
h.Being warming up to 700 DEG C under nitrogen protection atmosphere afterwards and carry out carbonization, heating rate is 4 DEG C/min, lowers the temperature after insulation 5h
To room temperature, obtain carbon/stannum/Graphene composite nano fiber.
Embodiment 4
The PAN weighing 3g is dissolved in 27g DMF, puts into stirrer, regulates suitable rotating speed, stirs 12~24 under room temperature
Hour to uniformly, preparing PAN mass fraction is the DMF solution of 10%.Weigh stannous chloride and the 0.15g graphite of 1.5g
Alkene adds in above-mentioned DMF solution, puts into stirrer equally, regulates suitable rotating speed, stirs 8~10 hours, ultrasonic shake under room temperature
Swing 1~3 hours to forming homogeneous solution.Use electrostatic spinning apparatus to carry out spinning, obtain PAN/SnCl2/ Graphene is compound to be received
Rice fibrous membrane, spinning voltage is 22kV, and receiving range is 18cm, and spinning speed is 1.2mL/h.The composite Nano that will obtain
Fibrous membrane is put in tube furnace, is 8 DEG C/min from room temperature to 300 DEG C with heating rate, keeps temperature 2 in air atmosphere
h.Being warming up to 900 DEG C under nitrogen protection atmosphere afterwards and carry out carbonization, heating rate is 6 DEG C/min, lowers the temperature after insulation 5h
To room temperature, obtain carbon/stannum/Graphene composite nano fiber.
Embodiment 5
The PAN weighing 3g is dissolved in 27g DMF, puts into stirrer, regulates suitable rotating speed, stirs 12~24 under room temperature
Hour to uniformly, preparing PAN mass fraction is the DMF solution of 10%.Weigh stannous chloride and the 0.15g graphite of 1.5g
Alkene adds in above-mentioned DMF solution, puts into stirrer equally, regulates suitable rotating speed, stirs 8~10 hours, ultrasonic shake under room temperature
Swing 1~3 hours to forming homogeneous solution.Use electrostatic spinning apparatus to carry out spinning, obtain PAN/SnCl2/ Graphene is compound to be received
Rice fibrous membrane, spinning voltage is 25kV, and receiving range is 15cm, and spinning speed is 1.5mL/h.The composite Nano that will obtain
Fibrous membrane is put in tube furnace, is 10 DEG C/min from room temperature to 300 DEG C with heating rate, keeps temperature in air atmosphere
2h.Being warming up to 1000 DEG C under nitrogen protection atmosphere afterwards and carry out carbonization, heating rate is 8 DEG C/min, drops after insulation 5h
Warm to room temperature, obtain carbon/stannum/Graphene composite nano fiber.
Claims (4)
1. the preparation method of lithium ion battery carbon/stannum/Graphene composite nano fiber, it is characterised in that prepared by following concrete steps:
(1) weighing a certain amount of PAN to be dissolved in DMF, preparation mass fraction is the solution of 8~15%, puts into stirrer,
Regulating suitable rotating speed, under room temperature, stirring stands de-bubble to uniformly in 12~24 hours.
(2) weighing a certain amount of stannous chloride and Graphene adds in above-mentioned (1) solution, put into stirrer equally, regulation is suitable
Work as rotating speed, stir 8~10 hours under room temperature to forming homogeneous solution.
(3) by the solution ultrasonic vibration 1 in step (2)~3 hours to uniformly.
(4) solution in step (3) is carried out spinning in electrostatic spinning apparatus, obtain PAN/SnCl2/ Graphene is compound to be received
Rice fibrous membrane, spinning voltage is 10~20kV, and receiving range is 10~20cm, and spinning speed is 0.2~2mL/h.
(5) composite nano-fiber membrane obtained in step (4) is put in tube furnace, be 1~10 with heating rate in air atmosphere
DEG C/min from room temperature to 200~300 DEG C, keep temperature 2~5h.It is warming up under nitrogen or argon atmosphere afterwards
600~1000 DEG C carry out carbonization, and heating rate is 1~10 DEG C/min, be cooled to room temperature, obtain carbon/stannum/graphite after insulation 2~5h
Alkene composite nano fiber.
A kind of preparation side for lithium ion battery negative material carbon/stannum/Graphene composite nano fiber the most according to claim 1
Method, it is characterised in that described preparation method is method of electrostatic spinning and high-temperature calcination.
A kind of preparation side for lithium ion battery negative material carbon/stannum/Graphene composite nano fiber the most according to claim 1
Method, it is characterised in that: the spinning voltage described in step (4) is 16~20kV;Described receiving range is 10~20cm;
Described spinning speed is 0.2~2mL/h.
A kind of preparation side for lithium ion battery negative material carbon/stannum/Graphene composite nano fiber the most according to claim 1
Method, it is characterised in that: the carburizing temperature described in step (5) is 600~1000 DEG C;Described holding temperature 2~5h;Described
Heating rate be 1~10 DEG C/min.
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106784684A (en) * | 2016-12-21 | 2017-05-31 | 盐城工学院 | A kind of used as negative electrode of Li-ion battery flexible compound nano-fiber material and preparation method |
CN107170974A (en) * | 2017-05-26 | 2017-09-15 | 中南大学 | A kind of carbon coating MoSe2/ graphene electro spinning nano fiber and preparation method thereof |
CN108771981A (en) * | 2018-06-04 | 2018-11-09 | 郑州新世纪材料基因组工程研究院有限公司 | Graphene composite material and its preparation method and application, graphene-carbon nano-fiber film and preparation method thereof |
CN110061219A (en) * | 2019-04-28 | 2019-07-26 | 湘潭大学 | A kind of electrostatic spinning preparation method of self-supporting SnTe/C nanofiber |
CN110085836A (en) * | 2019-05-05 | 2019-08-02 | 青岛大学 | A kind of preparation method of three-dimensional hierarchical structure flexible electrode |
CN111321477A (en) * | 2018-12-17 | 2020-06-23 | 深圳先进技术研究院 | SnX2Nanofiber material, preparation method, negative electrode active material, negative electrode, secondary battery or capacitor and preparation method thereof |
CN111564619A (en) * | 2020-05-21 | 2020-08-21 | 宁波大学 | Preparation method of carbon-coated nano nickel lithium battery material |
CN111575835A (en) * | 2020-05-15 | 2020-08-25 | 江苏科技大学 | ZnSnO3-C composite nanofiber and preparation method thereof |
CN111785940A (en) * | 2020-06-28 | 2020-10-16 | 旌德君创科技发展有限公司 | Bipyridine tin sheet-shaped composite material and preparation method thereof |
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Cited By (13)
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CN106784684B (en) * | 2016-12-21 | 2019-11-12 | 盐城工学院 | A kind of negative electrode of lithium ion battery flexible compound nano-fiber material and preparation method |
CN106784684A (en) * | 2016-12-21 | 2017-05-31 | 盐城工学院 | A kind of used as negative electrode of Li-ion battery flexible compound nano-fiber material and preparation method |
CN107170974A (en) * | 2017-05-26 | 2017-09-15 | 中南大学 | A kind of carbon coating MoSe2/ graphene electro spinning nano fiber and preparation method thereof |
CN107170974B (en) * | 2017-05-26 | 2019-10-08 | 中南大学 | A kind of carbon coating MoSe2/ graphene electro spinning nano fiber and preparation method thereof |
CN108771981A (en) * | 2018-06-04 | 2018-11-09 | 郑州新世纪材料基因组工程研究院有限公司 | Graphene composite material and its preparation method and application, graphene-carbon nano-fiber film and preparation method thereof |
CN111321477A (en) * | 2018-12-17 | 2020-06-23 | 深圳先进技术研究院 | SnX2Nanofiber material, preparation method, negative electrode active material, negative electrode, secondary battery or capacitor and preparation method thereof |
CN110061219A (en) * | 2019-04-28 | 2019-07-26 | 湘潭大学 | A kind of electrostatic spinning preparation method of self-supporting SnTe/C nanofiber |
CN110085836A (en) * | 2019-05-05 | 2019-08-02 | 青岛大学 | A kind of preparation method of three-dimensional hierarchical structure flexible electrode |
CN111575835A (en) * | 2020-05-15 | 2020-08-25 | 江苏科技大学 | ZnSnO3-C composite nanofiber and preparation method thereof |
CN111575835B (en) * | 2020-05-15 | 2022-02-11 | 江苏科技大学 | ZnSnO3-C composite nanofiber and preparation method thereof |
CN111564619A (en) * | 2020-05-21 | 2020-08-21 | 宁波大学 | Preparation method of carbon-coated nano nickel lithium battery material |
CN111564619B (en) * | 2020-05-21 | 2022-06-24 | 宁波大学 | Preparation method of carbon-coated nano nickel lithium battery material |
CN111785940A (en) * | 2020-06-28 | 2020-10-16 | 旌德君创科技发展有限公司 | Bipyridine tin sheet-shaped composite material and preparation method thereof |
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Application publication date: 20161123 |