CN101872855B - V2ON cathode material for lithium ion cells and preparing method thereof - Google Patents
V2ON cathode material for lithium ion cells and preparing method thereof Download PDFInfo
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- CN101872855B CN101872855B CN201010202345A CN201010202345A CN101872855B CN 101872855 B CN101872855 B CN 101872855B CN 201010202345 A CN201010202345 A CN 201010202345A CN 201010202345 A CN201010202345 A CN 201010202345A CN 101872855 B CN101872855 B CN 101872855B
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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
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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
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Abstract
The invention belongs to the technical field of lithium ion thin film cells, in particular to a V2ON electrode material for lithium ion cells and a preparation method thereof. In the invention, a V2ON thin film is prepared by combining a direct current reactive sputtering process and a post annealing process, the particle size of the thin film is 100 to 200 nanometers, and the thickness of the thin film is 100 to 700 nanometers. The thin film, as an electrode material, has a reversible specific capacity up to 900mAh/g, and shows excellent electrochemical properties in repeated charging and discharging processes. The thin film electrode material has a high specific cavity and good circulating performance. The preparation method is simple. The material is suitable for manufacturing thin-film lithium cells.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to negative active core-shell material that can be used as lithium ion battery and preparation method thereof.The present invention combines dc reactive sputtering deposition and post growth annealing successfully to prepare V
2The ON film, its main feature is V
2The ON particle diameter is at 100~200nm, and thickness is at 100-700nm, and the preparation method is simple.This film has good electrochemical as the electrode material of lithium ion battery.
Background technology
Along with the develop rapidly of mobile electronic device in recent years, the miniaturization long-life Research of Power that is complementary with electronic product more and more comes into one's own, and lithium ion battery is because its volume is little, in light weight, and operating voltage is high, and energy density receives much concern greatly.In order to develop jumbo lithium ion battery, the selection of anode material is particularly important.At present, the most frequently used lithium ion battery negative material is a graphite, but its specific capacity has only about 350mAh/g, and this makes the energy density of entire cell be difficult to be greatly improved.Seek new ion cathode material lithium and become very urgent.
The present invention proposes to combine the V of dc reactive sputtering deposition and post growth annealing preparation
2The ON film cathode material is a kind of novel negative material with dianion structure, has the high-capacity electrode material of good charge-discharge performance.
Summary of the invention
The objective of the invention is to propose that a kind of impulse electricity performance is good, capacitance is high is used for negative material of lithium ion battery and preparation method thereof.
The negative material oxynitriding vanadium (V that is used for lithium ion battery that the present invention proposes
2ON) negative material, be a kind of be the oxynitriding vanadium (V that the particle of 100-200nm is formed by crystallite dimension
2ON) thin-film material, film thickness is at 100-700nm.Show that after deliberation this type of material has good electrochemical, can be used as the negative material of high performance lithium ion battery.So far not about this oxynitriding vanadium (V
2ON) material is as the report of lithium ion battery negative material.
The oxynitriding vanadium (V that the present invention proposes as lithium ion battery negative material
2ON) material is a form of film.
The present invention proposes to be used for the oxynitriding vanadium (V of lithium ion battery
2ON) preparation method of negative material, concrete steps are following:
As target, adopt the dc reactive sputtering method with high pure metal V earlier at N
2Deposition obtains V in the atmosphere
xN (1<x<2).Distance between target and the substrate is 5~8cm, and sputtering power is 40~60W, keeps air pressure 10 during sputter
-1~1Pa, sedimentation time are 10~40min.To deposit good VN sample then and insert and carry out annealing in process in the tube furnace, annealing temperature 450--550 ℃, annealing time 5~30min.
Among the present invention, oxynitriding vanadium (V
2ON) crystal structure of film is confirmed by transmission electron microscope (JEOL 2010).SEAD (SAED) shows that oxynitriding vanadium film obtained by this method is a face-centred cubic structure, and space group is Fm3m.
Among the present invention, oxynitriding vanadium (V
2ON) film can directly be processed the lithium ion cell film electrode.
Among the present invention, oxynitriding vanadium (V
2ON) electrochemical property test of film adopts the hull cell system that is made up of three electrodes.Wherein, oxynitriding vanadium film is as work electrode, and the high purity lithium sheet is used separately as to electrode and reference electrode.Electrolyte is 1M LiPF
6+ EC+DMC (V/V=1/1).Hull cell is assemblied in the drying box of applying argon gas and carries out.The experiment that discharges and recharges of hull cell is carried out on the Land battery test system.
Among the present invention, combine post growth annealing at stainless steel substrates by dc reactive sputtering, the oxynitriding vanadium (V that makes on the multiple substrate such as platinized platinum
2ON) membrane electrode all has charge-discharge performance, at voltage range 0.01~4.0V and current density 2 μ A/cm
2The time, the platform of exoelectrical reaction appears at 0.7V (with respect to Li/Li
+), for the second time discharge process with the first time discharge process compare, irreversible discharge capacity loss is 12.9%.The second later cyclic process of week has good invertibity, and average each circulation volume decay is merely.
Above-mentioned performance shows, is combined the oxynitriding vanadium (V of post growth annealing preparation by dc reactive sputtering
2ON) film is a kind of novel negative material, can be applicable to lithium ion battery.
Description of drawings
Fig. 1 is V
2The ON film be 2 μ A/cm in current density
2The time charging and discharging curve.
Fig. 2 is V
2The specific capacity variation diagram of preceding 50 circulations of ON film.
Embodiment
The invention is further illustrated by the following examples.
As target, adopt the dc reactive sputtering method with high pure metal V (99.99%) earlier at N
2Deposition obtains V in the atmosphere
xN (1<x<2).Distance between target and the substrate is 7cm, and sputtering power is 50W, keeps air pressure at 0.8Pa during sputter, and sedimentation time is 20min.To deposit good VN sample then inserts and carries out 500 ℃ of annealing 10min, cooling in the tube furnace.
The scanning electron microscopy characterization result shows that the grain diameter in the film is at 100~200nm, and film thickness is about 400nm.Show that by electronic diffraction mensuration this film crystal structure is a face-centered cubic, space group is Fm3m.With this film as work electrode, with the high purity lithium sheet as electrode is assembled into simulated battery.Wherein electrolyte is 1M LiPF
6+ EC+DMC (volume ratio of EC and DMC is 1/1), battery are assemblied in the drying box of applying argon gas and carry out.Discharging and recharging on the Land battery test system of battery carried out.The mixture film electrode has shown good electrochemical.The battery discharge platform is about 0.7V, and reversible capacity reaches 900mAh/g left and right sides (see figure 1), and the very little (see figure 2) of capacity attenuation.
Claims (2)
1. a negative material that is used for lithium ion battery is characterized in that being a kind of V
2The ON nano thin-film, the film particle diameter is between 100-200nm, and thickness is between 100-700nm.
2. the preparation method of the negative material of a lithium ion battery as claimed in claim 1 is characterized in that concrete steps are: as target, adopt the dc reactive sputtering method at N with high pure metal V
2Deposition obtains V in the atmosphere
xN, 1<x<2, target and substrate distance are 5~8cm, sputtering power is 40~60W, keeps air pressure 10 during sputter
-1~1Pa, sedimentation time are 10~40min; The V that then deposition is obtained
xThe N sample is inserted and is carried out annealing in process, annealing temperature 450--550 ℃, annealing time 5~30min in the tube furnace.
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Citations (2)
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CN101034741A (en) * | 2007-04-05 | 2007-09-12 | 复旦大学 | Zirconium adulterated lithium manganate anode film material and its making method |
CN101238582A (en) * | 2005-08-05 | 2008-08-06 | 夏普株式会社 | Variable resistor element and production method therefor and storage device provided with it |
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JP4849221B2 (en) * | 2006-04-25 | 2012-01-11 | 三菱マテリアル株式会社 | Surface coated cutting tool with excellent chipping resistance with hard coating layer in heavy cutting of difficult-to-cut materials |
FR2914653B1 (en) * | 2007-04-06 | 2009-05-22 | H E F Soc Par Actions Simplifi | TARGET OF CATHODIC OXYNITRIDE SPRAY |
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CN101238582A (en) * | 2005-08-05 | 2008-08-06 | 夏普株式会社 | Variable resistor element and production method therefor and storage device provided with it |
CN101034741A (en) * | 2007-04-05 | 2007-09-12 | 复旦大学 | Zirconium adulterated lithium manganate anode film material and its making method |
Non-Patent Citations (1)
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JP特开2007-290079A 2007.11.08 |
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