CN102074683A - Porous carbon nanofiber anode material for lithium ion battery and preparation method thereof - Google Patents
Porous carbon nanofiber anode material for lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The invention provides a porous carbon nanofiber anode material for a lithium ion battery and a preparation method thereof, belonging to the technical field of nanometer materials and chemical power sources. The material is a carbon nanofiber material with a porous structure, which is provided with larger specific surface. The preparation method comprises the following steps: firstly using an electrostatic spinning technology to prepare composite nanofiber; and then carrying out pre-oxidation and carbonization to obtain the porous carbon nanofiber. The preparation method is simple, is easy to control, and has the advantage of low production cost. The material taken as an electrode material for a lithium ion battery anode provided by the invention has higher initial discharge capacity and cyclical stability, thus improving the high power characteristics and the fast charge-discharge capacity of the anode material, and meeting development requirements on a lithium ion power battery for an electric vehicle.
Description
Technical field
The invention belongs to nano material and technical field of chemical power, be specifically related to a kind of lithium ion cell nano negative material and preparation method, particularly a kind of lithium ion battery porous carbon nanofiber negative material and preparation method.
Background technology
In recent years, lithium ion battery is with excellent properties such as its high-energy-density, long circulation life, the low self-discharge rate type energy storage system that is widely used rapidly.And,, the performance of the lithium ion battery of energy then has higher requirement to being provided for it along with the progress of electronics industry, electric automobile and aeronautical and space technology.(negative pole is material with carbon element, just very LiCoO to existing battery system
2) volumetric specific energy has been near its limiting value 500Wh/L (inside battery space availability ratio, electrode density and membrane thicknesses have reached the limit).Therefore will realize the breakthrough of lithium ion battery on energy density and power density, vital " bottleneck " problem is how to design and develop the novel electrode material.The negative material that commercial lithium ion battery adopted nearly all is carbon/graphite material the earliest, but because carbon/graphite material when discharging and recharging for the first time, can form passivating film on its surface, cause capacitance loss; And the current potential of the electrode potential of carbon and lithium is very approaching, and when over-charging of battery, lithium metal may be separated out in carbon electrodes, forms dendrite and causes safety problem and capacity reduces, thereby need research and development novel high-energy lithium ion battery negative material.
The design that develops into lithium ion battery material and the development of nanometer technology provide new thinking, and the electrode material of nano material as lithium ion battery become when previous important research project.The lithium ion cell nano material is compared with the non-nano material, physics and chemical property with many uniquenesses, the degree of depth big as specific area, that lithium ion takes off embedding is little, the ions diffusion path short, the electrode polarization degree is little during high current charge-discharge, reversible capacity is high, have extended cycle life etc.Therefore the carbon nano-fiber material is compared with the conventional carbon negative material as lithium ion battery negative material, had following advantage: (1) stock utilization height, storage lithium capacity height; (2) the electrode/electrolyte contact area is big, electronics and Li
+The path of ionic conduction is short, and power output improves; (3) lithium embeds and to take off in the embedding process bulk effect little, and cycle life improves.Therefore, the carbon nano-fiber material is used for specific capacity and the rate charge-discharge performance that lithium ion battery can significantly improve battery, is the important directions of lithium ion battery development of new generation.
Existing lithium ion battery negative material and preparation method, as publication number is that the patent of CN 1812168A " a kind of modified method for lithium ion cell negative electrode material " is: utilize chemical reaction, original flavor growing nano carbon fiber on the surface of existing negative material is made modified composite material.But the carbon nano-fiber diameter of this invention preparation is bigger and thickness is inhomogeneous, has caused reducing the cycle efficieny first and the cyclical stability of this negative material; In addition, carbon nano-fiber degree of graphitization of this invention preparation is low, and poorly conductive causes problems such as the high power characteristic of this negative material and fast charging and discharging ability.
Summary of the invention
Shortcoming such as low, cyclical stability of cycle efficieny and fast charging and discharging ability first when the objective of the invention is to overcome above-mentioned carbon nano-fiber as lithium ion battery negative material provides a kind of lithium ion battery with porous carbon nanofiber negative material and preparation method; Require it to improve cycle efficieny and fast charging and discharging ability first, this method processing cost is low simultaneously, technology is simple and easy to control, the cycle is short, energy-efficient, being convenient to further extension and producing.
The present invention adopt technical scheme be; at first utilize electrostatic spinning technique to prepare the PAN/PMMA composite nano-fiber membrane; with made PAN/PMMA composite nano-fiber membrane pre-oxidation, further high-temperature heat treatment under protective atmosphere obtains porous carbon nanofiber negative material at last then.Concrete steps are as follows:
(1) taking by weighing a certain amount of polyacrylonitrile (PAN), to be dissolved in dimethyl formamide (DMF) preparation mass fraction be 8～12% DMF solution, then polymethyl methacrylate (PMMA) is pressed PAN/PMMA=5: 5,7: 3, add in the above-mentioned solution at 9: 1,, then mixed solution is transferred in the 50ml conical flask to complete swelling with magnetic stirrer 20～60min, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 12～24 hours.
(2) above-mentioned solution is spun uniform nano fibrous membrane in electrostatic spinning apparatus, spinning condition: voltage is 10～20KV, and collecting distance is 8～20cm, and the spinning solution rate of flow of fluid is 0.3～2.0ml/h.
(3) spun nano fibrous membrane is changed in the high temperature process furnances, be heated to 230～280 ℃ from room temperature, 2～5 ℃/min of heating rate is then at 230～280 ℃ of following pre-oxidation 1～2h.
(4) above-mentioned pre-oxidation felt is carried out further carbonization in tube furnace, feed inert gas protection is provided, 0.5～2 ℃/min of heating rate, final temperature are 600～1000 ℃, are cooled to room temperature under inert gas shielding naturally.
Owing to adopted technique scheme, the present invention to have following advantage and effect:
1. material of the present invention has improved the high power characteristic and the fast charging and discharging ability of negative material, and has improved the cycle efficieny first and the cyclical stability of negative material.
2. preparation technology of the present invention is simple and easy to control, and production cost is low, is convenient to further extension and produces.
3. material of the present invention has higher initial discharge capacity and cyclical stability as the lithium ion battery negative electrode material, relatively is applicable to the demand for development of electric vehicle lithium-ion-power cell.
Description of drawings
The scanning electron microscope diagram sheet of Fig. 1 porous carbon nanofiber negative material.
The circulation volume curve of Fig. 2 porous carbon nanofiber negative material.
The gained sample is through the sem observation (see figure 1), and the discovery sample is made up of the uneven nanofiber of thickness, and the fibre diameter size is 100～600nm.The gained sample is through charge-discharge performance test (see figure 2), find circulation 30 times after reversible capacity still up to 425mAh/g, illustrate that this porous material has application promise in clinical practice as lithium ion battery negative material.
Embodiment
Embodiment 1
Take by weighing PAN 1.8g, PMMA 0.2g (PAN/PMMA=9: 1) respectively; PAN 1.4g, PMMA 0.6g (PAN/PMMA=7: 3); Each 1g of PAN, PMMA (PAN/PMMA=5: 5), join respectively then in 3 parts of 23ml DMF solution, with the extremely fully even swelling of glass bar stir about 20min.Again mixed solution is transferred in the 50ml conical flask, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 24 hours.The above-mentioned spinning solution of being prepared is inserted the self-control spinning equipment, at spinning voltage 10kV, collects apart from 8cm, and under the process conditions of solution extruded velocity 0.3ml/h, spinning 10 hours in vacuum drying chamber dry 2 hours subsequently, obtains the PAN/PMMA nano fibrous membrane.Above-mentioned PAN/PMMA nano fibrous membrane is changed in the high temperature process furnances, be heated to 230 ℃ from room temperature, 2 ℃/min of heating rate is then at 230 ℃ of following pre-oxidation 1h.Feed inert gas N
2Protection is provided, and 0.5 ℃/min of heating rate, final temperature are 600 ℃, are cooled to room temperature under inert gas shielding naturally.
Embodiment 2
Take by weighing PAN 1.8g, PMMA 0.2g (PAN/PMMA=9: 1) respectively; PAN 1.4g, PMMA 0.6g (PAN/PMMA=7: 3); Each 1g of PAN, PMMA (PAN/PMMA=5: 5), join respectively then in 3 parts of 23ml DMF solution, with the extremely fully even swelling of glass bar stir about 20min.Again mixed solution is transferred in the 50ml conical flask, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 24 hours.The above-mentioned spinning solution of being prepared is inserted the self-control spinning equipment, at spinning voltage 10kV, collects apart from 12cm, and under the process conditions of solution extruded velocity 0.5ml/h, spinning 10 hours in vacuum drying chamber dry 2 hours subsequently, obtains the PAN/PMMA nano fibrous membrane.Above-mentioned PAN/PMMA nano fibrous membrane is changed in the high temperature process furnances, be heated to 250 ℃ from room temperature, 2 ℃/min of heating rate is then at 250 ℃ of following pre-oxidation 1h.Feed inert gas N
2Protection is provided, and 1.5 ℃/min of heating rate, final temperature are 600 ℃, are cooled to room temperature under inert gas shielding naturally.
Embodiment 3
Take by weighing PAN 1.8g, PMMA 0.2g (PAN/PMMA=9: 1) respectively; PAN 1.4g, PMMA 0.6g (PAN/PMMA=7: 3); Each 1g of PAN, PMMA (PAN/PMMA=5: 5), join respectively then in 3 parts of 23ml DMF solution, with the extremely fully even swelling of glass bar stir about 20min.Again mixed solution is transferred in the 50ml conical flask, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 24 hours.The above-mentioned spinning solution of being prepared is inserted the self-control spinning equipment, at spinning voltage 12kV, collects apart from 15cm, and under the process conditions of solution extruded velocity 1.0ml/h, spinning 10 hours in vacuum drying chamber dry 2 hours subsequently, obtains the PAN/PMMA nano fibrous membrane.Above-mentioned PAN/PMMA nano fibrous membrane is changed in the high temperature process furnances, be heated to 250 ℃ from room temperature, 2 ℃/min of heating rate is then at 250 ℃ of following pre-oxidation 1h.Feed inert gas N
2Protection is provided, and 0.5 ℃/min of heating rate, final temperature are 800 ℃, are cooled to room temperature under inert gas shielding naturally.
Embodiment 4
Take by weighing PAN 1.8g, PMMA 0.2g (PAN/PMMA=9: 1) respectively; PAN 1.4g, PMMA 0.6g (PAN/PMMA=7: 3); Each 1g of PAN, PMMA (PAN/PMMA=5: 5), join respectively then in 3 parts of 23ml DMF solution, with the extremely fully even swelling of glass bar stir about 20min.Again mixed solution is transferred in the 50ml conical flask, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 24 hours.The above-mentioned spinning solution of being prepared is inserted the self-control spinning equipment, at spinning voltage 15kV, collects apart from 15cm, and under the process conditions of solution extruded velocity 1.0ml/h, spinning 10 hours in vacuum drying chamber dry 2 hours subsequently, obtains the PAN/PMMA nano fibrous membrane.Above-mentioned PAN/PMMA nano fibrous membrane is changed in the high temperature process furnances, be heated to 280 ℃ from room temperature, 5 ℃/min of heating rate is then at 280 ℃ of following pre-oxidation 1h.Feed inert gas N
2Protection is provided, and 1.0 ℃/min of heating rate, final temperature are 600 ℃, are cooled to room temperature under inert gas shielding naturally.
Take by weighing PAN 1.8g, PMMA 0.2g (PAN/PMMA=9: 1) respectively; PAN 1.4g, PMMA 0.6g (PAN/PMMA=7: 3); Each 1g of PAN, PMMA (PAN/PMMA=5: 5), join respectively then in 3 parts of 23ml DMF solution, with the extremely fully even swelling of glass bar stir about 20min.Again mixed solution is transferred in the 50ml conical flask, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 24 hours.The above-mentioned spinning solution of being prepared is inserted the self-control spinning equipment, at spinning voltage 20kV, collects apart from 20cm, and under the process conditions of solution extruded velocity 1.5ml/h, spinning 10 hours in vacuum drying chamber dry 2 hours subsequently, obtains the PAN/PMMA nano fibrous membrane.Above-mentioned PAN/PMMA nano fibrous membrane is changed in the high temperature process furnances, be heated to 250 ℃ from room temperature, 5 ℃/min of heating rate is then at 250 ℃ of following pre-oxidation 2h.Feed inert gas N
2Protection is provided, and 1.5 ℃/min of heating rate, final temperature are 800 ℃, are cooled to room temperature under inert gas shielding naturally.
Embodiment 6
Take by weighing PAN 1.8g, PMMA 0.2g (PAN/PMMA=9: 1) respectively; PAN 1.4g, PMMA 0.6g (PAN/PMMA=7: 3); Each 1g of PAN, PMMA (PAN/PMMA=5: 5), join respectively then in 3 parts of 23ml DMF solution, with the extremely fully even swelling of glass bar stir about 20min.Again mixed solution is transferred in the 50ml conical flask, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 24 hours.The above-mentioned spinning solution of being prepared is inserted the self-control spinning equipment, at spinning voltage 20kV, collects apart from 15cm, and under the process conditions of solution extruded velocity 2.0ml/h, spinning 10 hours in vacuum drying chamber dry 2 hours subsequently, obtains the PAN/PMMA nano fibrous membrane.Above-mentioned PAN/PMMA nano fibrous membrane is changed in the high temperature process furnances, be heated to 280 ℃ from room temperature, 2 ℃/min of heating rate is then at 280 ℃ of following pre-oxidation 2h.Feed inert gas N
2Protection is provided, and 2.0 ℃/min of heating rate, final temperature are 1000 ℃, are cooled to room temperature under inert gas shielding naturally.
Claims (2)
1. a lithium ion battery is characterized in that method of electrostatic spinning and pre-oxidation, carbonization may further comprise the steps with the preparation method of porous carbon nanofiber negative material:
1) taking by weighing a certain amount of polyacrylonitrile (PAN), to be dissolved in dimethyl formamide (DMF) preparation mass fraction be 8～12% DMF solution, then polymethyl methacrylate (PMMA) is pressed PAN/PMMA=5: 5,7: 3, add in the above-mentioned solution at 9: 1,, then mixed solution is transferred in the 50ml conical flask to complete swelling with magnetic stirrer 20～60min, and put into magnet rotor, regulate suitable rotating speed, at room temperature stirred 12～24 hours;
2) spinning solution with the step 1) preparation spins uniform nano fibrous membrane, spinning condition in electrostatic spinning apparatus: voltage is 10～20KV, and collecting distance is 8～20cm, and the spinning solution rate of flow of fluid is 0.3～2.0ml/h;
3) with step 2) spun nano fibrous membrane changes in the high temperature process furnances, is heated to 230～280 ℃ from room temperature, and 2～5 ℃/min of heating rate is then at 230～280 ℃ of following pre-oxidation 1～2h;
4) the pre-oxidation felt that step 3) is obtained carries out further carbonization in tube furnace, feed inert gas protection is provided, and 0.5～2 ℃/min of heating rate, final temperature are 600～1000 ℃, are cooled to room temperature under inert gas shielding naturally.
2. a kind of lithium ion battery according to claim 1 is characterized in that: the mist of inert nitrogen gas, argon gas, nitrogen and argon gas with the preparation method of porous carbon nanofiber negative material.
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Cited By (22)
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|---|---|---|---|---|
| CN102797111A (en) * | 2012-08-16 | 2012-11-28 | 黑龙江大学 | Method for preparing porous nitrogen-contained carbon fiber electrode material from melamine resin/polyvinyl alcohol aqueous solution through high-pressure static spinning technology |
| CN103093973A (en) * | 2013-02-07 | 2013-05-08 | 北京化工大学 | Prepared method of super capacitor materials |
| CN103311523A (en) * | 2013-06-04 | 2013-09-18 | 清华大学深圳研究生院 | Silicon-carbon composite material with nano micropores and preparation method as well as application thereof |
| CN103305965A (en) * | 2013-06-04 | 2013-09-18 | 清华大学深圳研究生院 | Silicon-carbon composite material with nano micropores and preparation method as well as application thereof |
| CN103855361A (en) * | 2014-03-28 | 2014-06-11 | 清华大学 | Method for preparing nitrogen-doped porous carbon nanofiber cloth |
| CN104342852A (en) * | 2014-10-27 | 2015-02-11 | 东华大学 | Preparation methods of porous carbon nanofiber felt and porous carbon nanofiber electrode |
| CN104466168A (en) * | 2014-12-09 | 2015-03-25 | 江苏科技大学 | Preparation method of cobaltosic oxide-carbon porous nanofiber and application of cobaltosic oxide-carbon porous nanofiber to preparation of lithium ion battery |
| CN104882588A (en) * | 2015-06-08 | 2015-09-02 | 中国工程物理研究院化工材料研究所 | Carbon fiber/carbon nanotube composite membrane as well as preparation method and application thereof |
| CN105322147A (en) * | 2015-09-28 | 2016-02-10 | 复旦大学 | Tungsten disulfide/carbon nanofiber/graphene composite material and preparation method thereof |
| CN105529448A (en) * | 2016-01-22 | 2016-04-27 | 西北工业大学 | Preparation method for flexible lithium ion battery cathode material |
| CN105552342A (en) * | 2016-02-18 | 2016-05-04 | 长春理工大学 | Flexible negative electrode with MnO2 attached onto carbon fiber of lithium ion battery and preparation method of flexible negative electrode |
| CN105914359A (en) * | 2016-06-28 | 2016-08-31 | 王行柱 | Preparation method of flexible positive electrode of foldable lithium battery |
| CN106450308A (en) * | 2016-09-09 | 2017-02-22 | 成都理工大学 | High-capacity mesoporous carbon nanofiber for lithium-ion battery and preparation method of high-capacity mesoporous carbon nanofiber |
| CN106480552A (en) * | 2016-09-28 | 2017-03-08 | 广州凯耀资产管理有限公司 | Graphene/carbon nano-porous fiber and preparation method and application |
| CN106549170A (en) * | 2016-12-07 | 2017-03-29 | 深圳大学 | A kind of porous carbon fiber for Proton Exchange Membrane Fuel Cells and preparation method thereof |
| CN109817974A (en) * | 2019-03-27 | 2019-05-28 | 山东理工大学 | A kind of sodium ion nickel manganese magnesium iron quaternary positive electrode and preparation method thereof |
| CN109904452A (en) * | 2019-02-21 | 2019-06-18 | 三峡大学 | The preparation method of sodium base Dual-ion cell based on carbon fiber negative electrode material |
| CN111180727A (en) * | 2020-02-17 | 2020-05-19 | 五邑大学 | Preparation method and application of flexible compact carbon nanofiber membrane |
| CN112271295A (en) * | 2020-11-11 | 2021-01-26 | 深圳职业技术学院 | Preparation method of negative electrode material without current collector of lithium ion battery |
| CN112993247A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | High-surface-capacity self-supporting hard carbon cathode and preparation and application thereof |
| CN113015617A (en) * | 2018-08-17 | 2021-06-22 | Cence公司 | Novel carbon nanofibers and method of making |
| CN113224292A (en) * | 2021-02-02 | 2021-08-06 | 江西理工大学 | High-performance lithium ion battery polyacrylonitrile carbon fiber negative electrode material and preparation method thereof |
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Application publication date: 20110525 |