CN103165893A - Preparation method of zinc oxide nanometer fiber cathode material for lithium ion battery - Google Patents
Preparation method of zinc oxide nanometer fiber cathode material for lithium ion battery Download PDFInfo
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- CN103165893A CN103165893A CN2011104195024A CN201110419502A CN103165893A CN 103165893 A CN103165893 A CN 103165893A CN 2011104195024 A CN2011104195024 A CN 2011104195024A CN 201110419502 A CN201110419502 A CN 201110419502A CN 103165893 A CN103165893 A CN 103165893A
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- lithium ion
- zinc oxide
- ion battery
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- nanometer fiber
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
A zinc oxide nanometer fiber cathode material for lithium ion battery and a preparation method thereof belong to the technical fields of high polymer material and chemical power source. The zinc oxide nanometer fiber material for lithium ion battery provided by the invention has large specific surface area. The method first prepares composite nanometer fiber by electrospinning, and then the nanometer fiber is subjected to high-temperature calcination to obtain the zinc oxide nanometer fiber. The preparation process provided by the invention is simple and easy to control, and has low production cost. The cathode electrode material for lithium ion battery provided by the invention overcomes the disadvantages of zinc oxide nanorod prepared by other methods as cathode material for lithium ion battery, such as low first cycling efficiency, weak cycle stability and high-rate discharge ability. The invention provides a zinc oxide nanometer fiber cathode material for lithium ion battery and the preparation method thereof. The material has high initial discharge capacity and cycling stability, improves high power characteristic and high-rate discharge capacity of cathode material, and is suitable for development requirements of lithium ion power battery for electric vehicles.
Description
Technical field
The invention belongs to macromolecular material and technical field of chemical power, be specifically related to a kind of nanometer negative materials for Li-ion batteries and preparation method, particularly a kind of lithium ion battery zinc oxide nano fiber negative material and preparation method.
Background technology
In recent years, to have voltage high due to it for lithium-ions battery, volume and capacity ratio, specific discharge capacity are high, memory-less effect, little chemical property and the characteristics such as life-span length, safety nuisance free that wait excellence of self discharge, develop very soon, commercially obtained huge success, be widely used on numerous civilian and military fields such as mobile phone, notebook computer, video camera, digital camera, Mp3, PDA.Present commercial lithium-ions battery negative pole is all to adopt material with carbon element basically, as graphite, and carbon fiber, coke, and the RESEARCH OF PYROCARBON for preparing under inert atmosphere of various organic precursor, all these carbon all have reversible lithium storage ability to a certain degree.But also have some shortcomings aspect practical application: the theoretical specific capacity of graphite is 372mAh/g, only has 1/10th of lithium metal; Material with carbon element embedding lithium current potential is low, exists to separate out the potential safety hazard of Li dendrite; Because the surface nature of graphite is very inhomogeneous, be difficult to form even, fine and close solid electrolyte film (SEI film) at material surface when discharging first, cause first charge-discharge efficiency low, cycle performance is undesirable.To the raising day by day that battery performance requires, replace material with carbon element in the urgent need to seeking new negative material along with people.
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 topic.The lithium ion cell nano material is compared with the non-nano material, physics and chemistry character with many uniquenesses, the degree of depth that as large in specific area, lithium ion takes off embedding is little, the ion the evolving path is short, the electrode polarization degree is little during high current charge-discharge, reversible capacity is high, have extended cycle life etc.Lithium ion battery can significantly improve specific capacity and the rate charge-discharge performance of battery, is the important directions of lithium ion battery development of new generation.
Existing lithium ion battery zinc-oxide nano negative material and preparation method, as the article that is published in Electrochimica Acta " lithium ion battery zinc oxide nano rod negative material " is: utilize the hydro thermal method reaction, growing zinc oxide nanorod on the copper matrix is made lithium ion battery negative material.But, the zinc oxide nano rod negative material of the method preparation first cycle efficieny and cyclical stability poor; In addition, the zinc oxide nano rod poorly conductive of the method preparation causes the problems such as the high power characteristic of this negative material and fast charging and discharging ability.
Summary of the invention
The shortcoming such as low, the cyclical stability of cycle efficieny and fast charging and discharging ability first when the objective of the invention is to overcome above-mentioned zinc oxide nano rod as lithium ion battery negative material provides a kind of lithium ion battery with zinc oxide nano fiber negative material and preparation method; Require it to improve cycle efficieny and fast charging and discharging ability first, simultaneously the method processing cost is low, technique 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 to utilize electrostatic spinning technique to prepare PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane is then with made PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane carries out calcination processing in high temperature process furnances, obtain the zinc oxide nano fiber negative material.Concrete steps are as follows:
(1) taking a certain amount of polyacrylonitrile (PAN), to be dissolved in dimethyl formamide (DMF) preparation mass fraction be 8~12% DMF solution, then with PVP (PVP) by PAN/PVP=7: 3 add in mentioned solution, add at last zinc acetate ((CH
3COO)
2Zn), institute joins solution and uses magnetic stirrer 20~60min to complete swelling, then mixed solution is transferred in the 50ml conical flask, and is put into magnet rotor, regulates suitable rotating speed, at room temperature stirs 12~24 hours.
(2) 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 high temperature process furnances, be heated to 600~800 ℃ from room temperature in air atmosphere, heating rate is 0.5~5 ℃/min.
Owing to having adopted technique scheme, the present invention has following advantage and effect:
1. material of the present invention has improved high power characteristic and the fast charging and discharging ability of negative material, and has improved 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 as the lithium ion battery negative electrode material, has higher initial discharge capacity and cyclical stability.
Description of drawings
The scanning electron microscope diagram sheet of Fig. 1 zinc oxide nano fiber negative material.
First all charging and discharging curves of Fig. 2 zinc oxide nano fiber negative material.
The gained sample finds that through sem observation (seeing Fig. 1) sample is comprised of the inhomogeneous nanofiber of thickness, and the fibre diameter size is 180~300nm.The gained sample finds that through charge-discharge performance test (seeing Fig. 2) initial discharge capacity up to 1208mAh/g, illustrates that this porous material has application prospect preferably as lithium ion battery negative material.
Embodiment
3), (CH take PAN 1.4g, PVP 0.6g (PAN/PVP=7:
3COO)
2Then Zn 1.0g joins in 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 preparing 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 PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane.With above-mentioned PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane changes in high temperature process furnances, is heated to 600 ℃ from room temperature in air atmosphere, and 0.5 ℃/min of heating rate is cooled to room temperature after calcining finishes naturally.
Embodiment 2
3), (CH take PAN 1.4g, PVP 0.6g (PAN/PVP=7:
3COO)
2Then Zn 1.0g joins in 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 preparing 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 PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane.With above-mentioned PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane changes in high temperature process furnances, is heated to 600 ℃ from room temperature in air atmosphere, and 1.5 ℃/min of heating rate is cooled to room temperature after calcining finishes naturally.
Embodiment 3
3), (CH take PAN 1.4g, PVP 0.6g (PAN/PVP=7:
3COO)
2Then Zn 1.0g joins in 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 preparing 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 PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane.With above-mentioned PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane changes in high temperature process furnances, is heated to 700 ℃ from room temperature in air atmosphere, and 0.5 ℃/min of heating rate is cooled to room temperature after calcining finishes naturally.
Embodiment 4
3), (CH take PAN 1.4g, PVP 0.6g (PAN/PVP=7:
3COO)
2Then Zn 1.0g joins in 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 preparing 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 PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane.With above-mentioned PAN/PVP/ (CH
3COO)
2The Zn composite nano-fiber membrane changes in high temperature process furnances, is heated to 700 ℃ from room temperature in air atmosphere, and 1.0 ℃/min of heating rate is cooled to room temperature after calcining finishes naturally.
Claims (2)
1. the preparation method of a lithium ion battery use zinc oxide nano fiber negative material, is characterized in that, method of electrostatic spinning and high-temperature calcination comprise the following steps:
1) taking a certain amount of polyacrylonitrile (PAN), to be dissolved in dimethyl formamide (DMF) preparation mass fraction be 8~12% DMF solution, then with PVP (PVP) by PAN/PVP=7: 3 add in mentioned solution, add at last zinc acetate ((CH
3COO)
2Zn), institute joins solution and uses magnetic stirrer 20~60min to complete swelling, then mixed solution is transferred in the 50ml conical flask, and is put into magnet rotor, regulates suitable rotating speed, at room temperature stirs 12~24 hours.
2) with step 1) spinning solution of 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 high temperature process furnances, is heated to 600~800 ℃ from room temperature, and heating rate is 0.5~5 ℃/min.
2. a kind of lithium ion battery according to claim 1 with the preparation method of zinc oxide nano fiber negative material, is characterized in that: electrostatic spinning voltage, collection distance, spinning flow velocity and calcining heat.
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Cited By (14)
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CN103551588A (en) * | 2013-10-30 | 2014-02-05 | 常州大学 | Method for preparing metal nano fiber pipes on basis of single-channel electrospinning method |
CN103647048A (en) * | 2013-12-10 | 2014-03-19 | 北京理工大学 | Preparation method of high-rate lithium ion battery negative electrode material |
CN104347872A (en) * | 2013-07-30 | 2015-02-11 | 江南大学 | Preparation method of zinc ferrite nanofiber cathode material for lithium ion batteries |
CN104577108A (en) * | 2013-10-14 | 2015-04-29 | 江南大学 | Preparation method of lithium ion battery cathode material cobalt ferrite nanofibers |
CN104577109A (en) * | 2013-10-14 | 2015-04-29 | 江南大学 | Preparation method of copper sulfate nanofiber serving as negative material of lithium ion battery |
CN104701526A (en) * | 2013-12-05 | 2015-06-10 | 江南大学 | Nickel ferrite nano-fiber negative electrode material preparation method |
CN106159256A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | A kind of preparation method of magnesium ferrite nanofiber anode material |
CN106159211A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | A kind of preparation method of carbon/cobalt/Graphene composite nano fiber negative material |
CN106159210A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | The preparation method of lithium ion battery carbon/stannum/Graphene composite nano fiber |
CN106159248A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | A kind of preparation method of lithium ion battery Zinc vanadate nanofiber anode material |
CN109755528A (en) * | 2019-01-04 | 2019-05-14 | 中南大学 | A kind of preparation method and applications of manganese selenide/carbon fiber energy storage material |
CN109755527A (en) * | 2019-01-04 | 2019-05-14 | 中南大学 | A kind of preparation method and applications of zinc selenide/carbon fiber energy storage material |
CN110707294A (en) * | 2019-08-29 | 2020-01-17 | 北京化工大学 | Lithium-philic heteroatom and metal oxide co-doped three-dimensional fiber framework lithium battery cathode and preparation method thereof |
CN111740099A (en) * | 2020-07-06 | 2020-10-02 | 中国石油大学(华东) | Preparation method and application of high-dispersion metal oxide/carbon nanofiber composite material |
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CN101905974A (en) * | 2010-02-05 | 2010-12-08 | 西安理工大学 | Electrostatic spinning preparation method of ceramic nanometer composite fibers |
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Cited By (17)
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CN104347872A (en) * | 2013-07-30 | 2015-02-11 | 江南大学 | Preparation method of zinc ferrite nanofiber cathode material for lithium ion batteries |
CN104577108A (en) * | 2013-10-14 | 2015-04-29 | 江南大学 | Preparation method of lithium ion battery cathode material cobalt ferrite nanofibers |
CN104577109A (en) * | 2013-10-14 | 2015-04-29 | 江南大学 | Preparation method of copper sulfate nanofiber serving as negative material of lithium ion battery |
CN103551588A (en) * | 2013-10-30 | 2014-02-05 | 常州大学 | Method for preparing metal nano fiber pipes on basis of single-channel electrospinning method |
CN103551588B (en) * | 2013-10-30 | 2015-09-23 | 常州大学 | A kind of method preparing metal nano fibre pipe based on single channel electrical spinning method |
CN104701526A (en) * | 2013-12-05 | 2015-06-10 | 江南大学 | Nickel ferrite nano-fiber negative electrode material preparation method |
CN103647048A (en) * | 2013-12-10 | 2014-03-19 | 北京理工大学 | Preparation method of high-rate lithium ion battery negative electrode material |
CN103647048B (en) * | 2013-12-10 | 2015-10-14 | 北京理工大学 | Preparation method of high-rate lithium ion battery negative electrode material |
CN106159256A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | A kind of preparation method of magnesium ferrite nanofiber anode material |
CN106159211A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | A kind of preparation method of carbon/cobalt/Graphene composite nano fiber negative material |
CN106159210A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | The preparation method of lithium ion battery carbon/stannum/Graphene composite nano fiber |
CN106159248A (en) * | 2015-04-28 | 2016-11-23 | 江南大学 | A kind of preparation method of lithium ion battery Zinc vanadate nanofiber anode material |
CN109755528A (en) * | 2019-01-04 | 2019-05-14 | 中南大学 | A kind of preparation method and applications of manganese selenide/carbon fiber energy storage material |
CN109755527A (en) * | 2019-01-04 | 2019-05-14 | 中南大学 | A kind of preparation method and applications of zinc selenide/carbon fiber energy storage material |
CN109755527B (en) * | 2019-01-04 | 2021-06-04 | 中南大学 | Preparation method and application of zinc selenide/carbon fiber energy storage material |
CN110707294A (en) * | 2019-08-29 | 2020-01-17 | 北京化工大学 | Lithium-philic heteroatom and metal oxide co-doped three-dimensional fiber framework lithium battery cathode and preparation method thereof |
CN111740099A (en) * | 2020-07-06 | 2020-10-02 | 中国石油大学(华东) | Preparation method and application of high-dispersion metal oxide/carbon nanofiber composite material |
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Application publication date: 20130619 |