CN106159248A - A kind of preparation method of lithium ion battery Zinc vanadate nanofiber anode material - Google Patents
A kind of preparation method of lithium ion battery Zinc vanadate nanofiber anode material Download PDFInfo
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- CN106159248A CN106159248A CN201510213901.3A CN201510213901A CN106159248A CN 106159248 A CN106159248 A CN 106159248A CN 201510213901 A CN201510213901 A CN 201510213901A CN 106159248 A CN106159248 A CN 106159248A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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 preparation method of a kind of lithium ion battery Zinc vanadate nanofiber anode material, belongs to nano material and technical field of chemical power.Material of the present invention is a kind of lithium ion battery Zinc vanadate nano-fiber material, prepares PVP/C first with electrostatic spinning technique4H6ZnO4/C10H14O5V composite nano fiber, is then passed through high-temperature calcination and obtains Zinc vanadate nanofiber.Preparation method technique of the present invention is simple, production cost is low, with the Zinc vanadate nanofiber of the method gained, there is big specific surface area, shorter ion the evolving path, good structure and electrochemical stability, from cell negative electrode material, there is good development prospect as lithium.
Description
Technical field
The present invention relates to a kind of nanometer negative materials for Li-ion batteries and preparation method, particularly relate to a kind of lithium ion battery vanadic acid
Zinc nanofiber anode material and preparation method；Belong to nano material and technical field of chemical power.
Background technology
The storage of energy is the most all one of hot issue of concern, the most in the last few years between environment and the energy
Contradiction is increasingly sharpened.Mankind's weight on the road of device finding high-efficiency energy-storage does not rests.Compared with other energy storage devices, lithium from
Sub-battery has the advantage of environmental protection, memory-less effect etc., has the most been widely used in various portable electric appts.
Along with hybrid vehicle and the rise of electric automobile and development, people are to lithium ion battery specific capacity, service life and quickly
Charge-discharge performance is had higher requirement.But, the negative material that business-like lithium ion battery uses is mainly graphite, stone
The theoretical capacity of ink material is relatively low, only 372mAh/g, the most more and more can not meet the requirement of current height ratio capacity.Therefore
Develop novel have the lithium ion battery negative material that specific capacity is high, efficiency for charge-discharge is high, have extended cycle life have very must
The property wanted.
In recent years, there is substantial amounts of research to find that transition metal oxide has higher theoretical specific capacity, be that current graphite cathode is dived
Substitution material.Wherein, the metal composite oxide Zn of spinel-type2V2O7, its theoretical specific capacity is high, and raw material ring
Protect, cheap, stable cycle performance.Utilize electrostatic spinning technique can prepare nanofiber, owing to fibre diameter is little, ratio
The advantages such as surface area is big, are used in lithium ion battery and can effectively increase the evolving path of ion and the surface area of electric transmission,
And then improve reversible capacity and the cycle life of lithium ion battery.At present, electrostatic spinning technique is utilized to tie mutually with high-temperature calcination technology
Close, prepare Zn2V2O7Nanofiber is also used as the most not relevant document of lithium ion battery negative material and patent report.
Summary of the invention
For the deficiencies in the prior art, the problem to be solved in the present invention is the preparation of a kind of Zinc vanadate nanofiber for lithium battery
And application.
The technical solution used in the present invention is, uses the method for electrostatic spinning to prepare PVP/C4H6ZnO4/C10H14O5V composite Nano
Fiber, obtains Zinc vanadate nanofiber anode material through high-temperature calcination, specifically comprises the following steps that
(1) weigh a certain amount of PVP to be dissolved in ethanol, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.
(2) a certain amount of vanadyl acetylacetonate (C is weighed10H14O5And zinc acetate (C V)4H6ZnO4·2H2O) it is dissolved in DMF
In, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to forming homogeneous solution.
(3) solution in step (2) is slowly poured in the solution of step (1), continue to be stirred at room temperature 5～6 hours to uniformly.
(4) solution in step (3) is carried out spinning in electrostatic spinning apparatus, obtain PVP/C4H6ZnO4/C10H14O5V
Composite nano-fiber membrane, spinning voltage is 15～25kV, and receiving range is 10～20cm, and spinning speed is 0.3～1.0mL/h.
(5) composite nano-fiber membrane obtained in step (4) is put in tube furnace and calcine, from room temperature in air atmosphere
To 500 DEG C, keeping temperature 3～5h, heating rate is 0.5～2 DEG C/min, and calcining is naturally cooling to room temperature after terminating.
Owing to have employed technique scheme, the invention have the advantages that and effect:
(1) the preparation method technique of the present invention is simple, i.e. can get Zinc vanadate nanofiber through electrostatic spinning and calcining.
(2) the Zinc vanadate nanofiber negative pole that prepared by the present invention can give full play to nano-fiber material have big specific surface area,
The advantages such as shorter ion the evolving path and good structural stability, electrochemical stability is excellent, and therefore it can be new as one
The lithium ion battery negative material of type is used widely.
Accompanying drawing explanation
The scanning electron microscope image of Fig. 1 Zinc vanadate nanofiber.
The cycle performance figure of Fig. 2 Zinc vanadate nanofiber anode material.
Detailed description of the invention
Embodiment 1
Weigh PVP 3g to add in 8.5g ethanol solution, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.The vanadyl acetylacetonate and the 0.26315g bis-water zinc acetate that weigh 0.63685g are dissolved in simultaneously
In 8.5g DMF, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to uniformly.Treat both
After forming homogeneous solution, DMF solution is joined in ethanol solution, continue to be stirred at room temperature 5～6 hours to uniformly.Then,
In self-control electrostatic spinning apparatus, the spinning liquid prepared is carried out spinning, and spinning voltage is 15kV, and receiving range is 15cm,
Spinning speed is 0.5mL/h, obtains PVP/C4H6ZnO4/C10H14O5V composite nano-fiber membrane.The composite Nano that will obtain again
Fibrous membrane is put in tube furnace and is calcined, and from room temperature to 500 DEG C in air atmosphere, keeps 500 DEG C of 4h, and heating rate is 1 DEG C
/ min, calcining is naturally cooling to room temperature after terminating, i.e. obtains Zinc vanadate nanofiber.
Embodiment 2
Weigh PVP 3g to add in 8.5g ethanol solution, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.The vanadyl acetylacetonate and the 0.26315g bis-water zinc acetate that weigh 0.63685g are dissolved in simultaneously
In 8.5g DMF, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to uniformly.Treat both
After forming homogeneous solution, DMF solution is joined in ethanol solution, continue to be stirred at room temperature 5～6 hours to uniformly.Then,
In self-control electrostatic spinning apparatus, the spinning liquid prepared is carried out spinning, and spinning voltage is 20kV, and receiving range is 20cm,
Spinning speed is 0.5mL/h, obtains PVP/C4H6ZnO4/C10H14O5V composite nano-fiber membrane.The composite Nano that will obtain again
Fibrous membrane is put in tube furnace and is calcined, and from room temperature to 500 DEG C in air atmosphere, keeps 500 DEG C of 3h, and heating rate is
0.5 DEG C/min, calcining is naturally cooling to room temperature after terminating, and i.e. obtains Zinc vanadate nanofiber.
Embodiment 3
Weigh PVP 3g to add in 8.5g ethanol solution, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.The vanadyl acetylacetonate and the 0.26315g bis-water zinc acetate that weigh 0.63685g are dissolved in simultaneously
In 8.5g DMF, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to uniformly.Treat both
After forming homogeneous solution, DMF solution is joined in ethanol solution, continue to be stirred at room temperature 5～6 hours to uniformly.Then,
In self-control electrostatic spinning apparatus, the spinning liquid prepared is carried out spinning, and spinning voltage is 15kV, and receiving range is 20cm,
Spinning speed is 1mL/h, obtains PVP/C4H6ZnO4/C10H14O5V composite nano-fiber membrane.The composite Nano that will obtain again
Fibrous membrane is put in tube furnace and is calcined, and from room temperature to 500 DEG C in air atmosphere, keeps 500 DEG C of 5h, and heating rate is 2 DEG C
/ min, calcining is naturally cooling to room temperature after terminating, i.e. obtains Zinc vanadate nanofiber.
Embodiment 4
Weigh PVP 3g to add in 8.5g ethanol solution, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.The vanadyl acetylacetonate and the 0.26315g bis-water zinc acetate that weigh 0.63685g are dissolved in simultaneously
In 8.5g DMF, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to uniformly.Treat both
After forming homogeneous solution, DMF solution is joined in ethanol solution, continue to be stirred at room temperature 5～6 hours to uniformly.Then,
In self-control electrostatic spinning apparatus, the spinning liquid prepared is carried out spinning, and spinning voltage is 25kV, and receiving range is 15cm,
Spinning speed is 0.8mL/h, obtains PVP/C4H6ZnO4/C10H14O5V composite nano-fiber membrane.The composite Nano that will obtain again
Fibrous membrane is put in tube furnace and is calcined, and from room temperature to 500 DEG C in air atmosphere, keeps 500 DEG C of 2h, and heating rate is 1 DEG C
/ min, calcining is naturally cooling to room temperature after terminating, i.e. obtains Zinc vanadate nanofiber.
Embodiment 5
Weigh PVP 3g to add in 8.5g ethanol solution, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.The vanadyl acetylacetonate and the 0.26315g bis-water zinc acetate that weigh 0.63685g are dissolved in simultaneously
In 8.5g DMF, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to uniformly.Treat both
After forming homogeneous solution, DMF solution is joined in ethanol solution, continue to be stirred at room temperature 5～6 hours to uniformly.Then,
In self-control electrostatic spinning apparatus, the spinning liquid prepared is carried out spinning, and spinning voltage is 15kV, and receiving range is 20cm,
Spinning speed is 0.5mL/h, obtains PVP/C4H6ZnO4/C10H14O5V composite nano-fiber membrane.The composite Nano that will obtain again
Fibrous membrane is put in tube furnace and is calcined, and from room temperature to 500 DEG C in air atmosphere, keeps 500 DEG C of 4h, and heating rate is
0.5 DEG C/min, calcining is naturally cooling to room temperature after terminating, and i.e. obtains Zinc vanadate nanofiber.
Embodiment 6
Weigh PVP 3g to add in 8.5g ethanol solution, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.The vanadyl acetylacetonate and the 0.26315g bis-water zinc acetate that weigh 0.63685g are dissolved in simultaneously
In 8.5g DMF, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to uniformly.Treat both
After forming homogeneous solution, DMF solution is joined in ethanol solution, continue to be stirred at room temperature 5～6 hours to uniformly.Then,
In self-control electrostatic spinning apparatus, the spinning liquid prepared is carried out spinning, and spinning voltage is 18kV, and receiving range is 18cm,
Spinning speed is 1mL/h, obtains PVP/C4H6ZnO4/C10H14O5V composite nano-fiber membrane.The composite Nano that will obtain again
Fibrous membrane is put in tube furnace and is calcined, and from room temperature to 500 DEG C in air atmosphere, keeps 500 DEG C of 2h, and heating rate is 1 DEG C
/ min, calcining is naturally cooling to room temperature after terminating, i.e. obtains Zinc vanadate nanofiber.
Claims (3)
1. the lithium ion battery preparation method of Zinc vanadate nanofiber anode material, it is characterised in that use electrostatic spinning
Method prepare PVP/C4H6ZnO4/C10H14O5V composite nano fiber, obtains Zinc vanadate nanofiber negative pole through high-temperature calcination
Material, specifically comprises the following steps that
(1) weigh a certain amount of PVP to be dissolved in ethanol, put into stirrer, regulate suitable rotating speed, under room temperature, stir 12～24
Hour to uniformly, stand de-bubble.
(2) a certain amount of vanadyl acetylacetonate (C is weighed10H14O5And zinc acetate (C V)4H6ZnO4·2H2O) it is dissolved in DMF
In, put into stirrer equally, regulate suitable rotating speed, stir 12～24 hours under room temperature to forming homogeneous solution.
(3) solution in step (2) is slowly poured in the solution of step (1), continue to be stirred at room temperature 5～6 hours to uniformly.
(4) solution in step (3) is carried out spinning in electrostatic spinning apparatus, obtain PVP/C4H6ZnO4/C10H14O5V
Composite nano-fiber membrane, spinning voltage is 15～25kV, and receiving range is 10～20cm, and spinning speed is 0.3～1.0mL/h.
(5) composite nano-fiber membrane obtained in step (4) is put in tube furnace and calcine, from room temperature in air atmosphere
To 500 DEG C, keeping temperature 3～5h, heating rate is 0.5～2 DEG C/min, and calcining is naturally cooling to room temperature after terminating.
The preparation method of a kind of lithium ion battery zinc ferrite nanofiber anode material the most according to claim 1, its feature exists
In: the vanadic salts described in step (2) is vanadyl acetylacetonate；Zinc salt is zinc acetate.
The preparation method of a kind of lithium ion battery zinc ferrite nanofiber anode material the most according to claim 1, its feature exists
In: prepared Zinc vanadate nanofiber is used for lithium ion battery negative material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106941158A (en) * | 2017-03-21 | 2017-07-11 | 成都新柯力化工科技有限公司 | A kind of Zinc vanadate molybdenum trioxide nanosheet electrode material of lithium battery and preparation method |
| CN107162055A (en) * | 2017-05-23 | 2017-09-15 | 宁波大学 | A kind of preparation method of vanadium niobates nano wire |
| CN114335578A (en) * | 2022-01-06 | 2022-04-12 | 齐鲁工业大学 | Zinc vanadate electrocatalytic material and preparation method and application thereof |
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| US20090305135A1 (en) * | 2008-06-04 | 2009-12-10 | Jinjun Shi | Conductive nanocomposite-based electrodes for lithium batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107162055A (en) * | 2017-05-23 | 2017-09-15 | 宁波大学 | A kind of preparation method of vanadium niobates nano wire |
| CN114335578A (en) * | 2022-01-06 | 2022-04-12 | 齐鲁工业大学 | Zinc vanadate electrocatalytic material and preparation method and application thereof |
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Application publication date: 20161123 |