CN103022473A - Method for preparing gamma-Fe2O3 positive-pole material for lithium-ion battery - Google Patents

Method for preparing gamma-Fe2O3 positive-pole material for lithium-ion battery Download PDF

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CN103022473A
CN103022473A CN2013100087621A CN201310008762A CN103022473A CN 103022473 A CN103022473 A CN 103022473A CN 2013100087621 A CN2013100087621 A CN 2013100087621A CN 201310008762 A CN201310008762 A CN 201310008762A CN 103022473 A CN103022473 A CN 103022473A
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ion battery
lithium ion
magnetron sputtering
fe2o3
copper sheet
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CN103022473B (en
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李长明
孙柏
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Southwest University
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Southwest University
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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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a method for preparing a gamma-Fe2O3 positive-pole material for a lithium-ion battery. The method comprises the following steps of: (1) forming a target material through carrying out press-forming on gamma-Fe2O3 powder; (2) loading the press-formed gamma-Fe2O3 target material into a magnetron sputtering cavity; (3) taking a copper sheet as a substrate, and placing the copper sheet in the magnetron sputtering cavity; (4) filling the magnetron sputtering cavity with inert gas after the magnetron sputtering cavity is vacuumized, and depositing a gamma-Fe2O3 film on the copper sheet by using a magnetron sputtering method; and (5) annealing the copper sheet which is subjected to gamma-Fe2O3 film deposition at the temperature of 300-600 DEG C under vacuum conditions, and cooling to obtain the gamma-Fe2O3 positive-pole material for the lithium-ion battery. The gamma-Fe2O3 positive-pole material for the lithium-ion battery, prepared by the method, has good unique physical property in lithium ion transmission, and the good gamma-Fe2O3 crystalline degree is difficultly destructed by the lithium ion transmission, so that not only can the actual capacity of the battery be increased, but also the cyclic service life can be greatly prolonged.

Description

γ-Fe 2O 3The preparation method of lithium ion battery anode material
Technical field
The present invention relates to a kind of preparation method of lithium ion battery anode material, particularly a kind of γ-Fe 2O 3The preparation method of lithium ion battery anode material.
Background technology
Since Gaston Plante in 1859 proposed lead-sour battery concept, chemical power source circle was being explored new high-energy-density, the secondary cell that has extended cycle life always.Japan Sony Corporation took the lead in succeeding in developing and realized commercial lithium ion battery nineteen ninety, show wide application prospect and potential great economic benefit in many-sides such as portable electric appts, electric automobile, space technology, national defense industry, become rapidly the study hotspot of widely paying close attention in recent years.
One of key of exploitation lithium ion battery is to seek suitable anode material, makes battery have sufficiently high lithium embedded quantity and takes off the embedding invertibity with good lithium, with the high voltage that guarantees battery, large capacity and long circulation life.Material with carbon element is applied in commercial Li-ion batteries because having higher specific capacity, and shows good electrochemical behavior, but still has the low defective of theoretical capacity.Since P. Poizot etc. has reported with other transition metal oxides such as FeO, CoO, MoO, Cu 2Since the chemical property as the lithium rechargeable battery anode material such as O, other transition metal oxides and ferrite be ZnFe for example 2O 4, CoFe 2O 4Deng the focus that also becomes gradually research, and these material lists reveal higher specific discharge capacity.Yet the lithium ion battery success is used, and key is reversibly to embed the preparation of the anode material of removal lithium embedded ion.
Summary of the invention
In view of this, the invention provides a kind of γ-Fe 2O 3The preparation method of lithium ion battery anode material, the γ-Fe of preparation 2O 3Lithium ion battery anode material can realize that the high power capacity of battery discharges and recharges, and has extended cycle life.
γ-Fe of the present invention 2O 3The preparation method of lithium ion battery anode material may further comprise the steps:
1) with γ-Fe 2O 3Powder compaction becomes target;
2) with the γ-Fe that is pressed into 2O 3Target is packed in the magnetron sputtering cavity;
3) with copper sheet as substrate, put into the magnetron sputtering cavity;
4) after vacuumizing in the magnetron sputtering cavity, be filled with inert gas, utilize magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film;
5) will deposit γ-Fe 2O 3The copper sheet of film is 300 ~ 600 ℃ of annealing under vacuum condition, obtain γ-Fe after the cooling 2O 3Lithium ion battery anode material.
Further, in the described step 3), clean the oxide layer of removing the copper sheet surface with watery hydrochloric acid first, copper sheet will be put into the magnetron sputtering cavity again.
Further, in the described step 4), inert gas is argon gas, and air pressure is 1.0Pa, and deposition rate is 0.1 nm/s, and deposit thickness is 350nm.
Further, in the described step 5), vacuum degree is 5.0 * 10 -4Pa, annealing time are 1 hour.
Further, described γ-Fe 2O 3Powder prepares with coprecipitation.
Beneficial effect of the present invention is: the present invention utilizes method depositing gamma-Fe on copper sheet of magnetron sputtering 2O 3Film, and utilized the method for high-temperature vacuum annealing, Effective Raise γ-Fe 2O 3Crystallization degree, simultaneously at γ-Fe 2O 3The surface can form a large amount of holes, thereby makes its unique physical character with good transmission lithium ion, and the survivable γ-Fe of the transmission of lithium ion 2O 3Good crystallization degree, therefore with it as lithium ion battery anode material, not only can improve the actual capacity of battery, and can prolong widely service life cycle; γ-the Fe of the present invention's preparation 2O 3Lithium ion battery anode material can be realized long-life, the high power capacity of battery, can be used in the desirable lithium ion battery of various electronic devices.
Description of drawings
In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is described in further detail below in conjunction with accompanying drawing, wherein:
Fig. 1 is γ-Fe that embodiment 1, embodiment 2 and comparative example 1 prepare 2O 3The XRD figure of lithium ion battery anode material;
Fig. 2 is γ-Fe that embodiment 2 prepares 2O 3The XPS figure of lithium ion battery anode material;
Fig. 3 is γ-Fe that embodiment 1, embodiment 2 and comparative example 1 prepare 2O 3SEM plane and the sectional view of lithium ion battery anode material;
Fig. 4 is the CV curve of three button lithium ion batteries of embodiment 1, embodiment 2 and comparative example 1;
Fig. 5 is front ten charge and discharge cycles curves of three button lithium ion batteries of embodiment 1, embodiment 2 and comparative example 1;
Fig. 6 is first three time charge and discharge cycles curve of the button lithium ion battery of embodiment 2;
Fig. 7 is the capacity of button lithium ion battery under different discharge-rates---the cycle-index curve of embodiment 2;
Fig. 8 is the capacity of button lithium ion battery under same discharge-rate---the cycle-index curve of embodiment 2;
Fig. 9 is the capacity of three button lithium ion batteries under same discharge-rate---the cycle-index curve of embodiment 1, embodiment 2 and comparative example 1;
Figure 10 is the impedance curve of three button lithium ion batteries before discharging and recharging and after discharging and recharging of embodiment 1, embodiment 2 and comparative example 1.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.
Embodiment 1
γ-Fe of embodiment 1 2O 3The preparation method of lithium ion battery anode material may further comprise the steps:
1) prepares γ-Fe with conventional coprecipitation 2O 3Powder is with γ-Fe 2O 3Powder compaction becomes target;
2) with the γ-Fe that is pressed into 2O 3Target is packed in the magnetron sputtering cavity;
3) with copper sheet as substrate, clean to remove first the oxide layer on copper sheet surface with watery hydrochloric acid, copper sheet will be put into the magnetron sputtering cavity again;
4) be filled with argon gas after vacuumizing in the magnetron sputtering cavity, air pressure is 1.0Pa, utilizes magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film, deposition rate are 0.1 nm/s, and deposit thickness is 350 nm;
5) will deposit γ-Fe 2O 3The copper sheet of film is 5.0 * 10 in vacuum degree -4The lower 300 ℃ of annealing of the vacuum condition of Pa 1 hour obtain γ-Fe after the cooling 2O 3Lithium ion battery anode material.
Embodiment 2
γ-Fe of embodiment 2 2O 3The preparation method of lithium ion battery anode material may further comprise the steps:
1) prepares γ-Fe with conventional coprecipitation 2O 3Powder is with γ-Fe 2O 3Powder compaction becomes target;
2) with the γ-Fe that is pressed into 2O 3Target is packed in the magnetron sputtering cavity;
3) with copper sheet as substrate, clean to remove first the oxide layer on copper sheet surface with watery hydrochloric acid, copper sheet will be put into the magnetron sputtering cavity again;
4) be filled with argon gas after vacuumizing in the magnetron sputtering cavity, air pressure is 1.0Pa, utilizes magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film, deposition rate are 0.1 nm/s, and deposit thickness is 350 nm;
5) will deposit γ-Fe 2O 3The copper sheet of film is 5.0 * 10 in vacuum degree -4The lower 600 ℃ of annealing of the vacuum condition of Pa 1 hour obtain γ-Fe after the cooling 2O 3Lithium ion battery anode material.
Comparative example 1
γ-the Fe of comparative example 1 2O 3The preparation method of lithium ion battery anode material may further comprise the steps:
1) prepares γ-Fe with conventional coprecipitation 2O 3Powder is with γ-Fe 2O 3Powder compaction becomes target;
2) with the γ-Fe that is pressed into 2O 3Target is packed in the magnetron sputtering cavity;
3) with copper sheet as substrate, clean to remove first the oxide layer on copper sheet surface with watery hydrochloric acid, copper sheet will be put into the magnetron sputtering cavity again;
4) be filled with argon gas after vacuumizing in the magnetron sputtering cavity, air pressure is 1.0Pa, utilizes magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film, deposition rate are 0.1 nm/s, and deposit thickness is 350nm; Obtain γ-Fe 2O 3Lithium ion battery anode material.
Fig. 1 is γ-Fe that embodiment 1, embodiment 2 and comparative example 1 prepare 2O 3The XRD figure of lithium ion battery anode material as shown in Figure 1, can find out γ-Fe of embodiment 1 and embodiment 2 2O 3Passed through high annealing, Effective Raise γ-Fe 2O 3Crystallization degree.
Fig. 2 is γ-Fe that embodiment 2 prepares 2O 3The XPS figure of lithium ion battery anode material as shown in Figure 2, as known in the figure, through high annealing, does not have Fe 2+Occur with Fe, this sample that proves absolutely us only comprises Fe 3+
Fig. 3 is γ-Fe that embodiment 1, embodiment 2 and comparative example 1 prepare 2O 3SEM plane and the sectional view of lithium ion battery anode material, as shown in Figure 3, Fig. 3 (a) and (b) be the planar S EM figure of comparative example 1 wherein, Fig. 3 (c) and (d) be the planar S EM figure of embodiment 1, Fig. 3 (e) and (f) be the planar S EM figure of embodiment 2, Fig. 3 (γ) and (h) be γ-Fe 2O 3The sectional view of film.As seen from Figure 3, γ-Fe of embodiment 1 and embodiment 2 2O 3Passed through high-temperature vacuum annealing, at γ-Fe 2O 3The surface has formed a large amount of Micro porosities, and this hole has realized that sufficiently high lithium embedded quantity and good lithium take off the embedding invertibity.
γ-the Fe that respectively embodiment 1, embodiment 2 and comparative example 1 is prepared 2O 3Lithium ion battery anode material is as work electrode, and the lithium sheet is prepared into three button lithium ion batteries as to electrode.
Fig. 4 is the CV curve of three button lithium ion batteries, as shown in Figure 4, and γ-Fe that comparative example 1 and embodiment 1 are prepared 2O 3Only have a pair of redox peak, and two pairs of redox peaks have appearred in embodiment 2.
Fig. 5 is front ten charge and discharge cycles curves of three button lithium ion batteries, as shown in Figure 5, and γ-Fe that comparative example 1 and embodiment 1 are prepared 2O 3In front ten times discharged and recharged, capacity attenuation was serious, and the prepared γ-Fe of embodiment 2 2O 3In front ten times discharge and recharge, almost there is not capacity attenuation.
Fig. 6 is first three time charge and discharge cycles curve of the button lithium ion battery of embodiment 2, as shown in Figure 6, as known in the figure, γ-Fe that embodiment 2 is prepared 2O 3No matter be to discharge and recharge or high current density discharges and recharges at low current density, from for the second time circulation, its capacity has decay hardly, and discharge platform voltage approximately all is 1.0 V.
Fig. 7 is the capacity of button lithium ion battery under different discharge-rates---the cycle-index curve of embodiment 2, as shown in Figure 7, and γ-Fe that visible embodiment 2 is prepared 2O 3Under different discharge-rates, its capacity is all very stable.
Fig. 8 is the capacity of button lithium ion battery under same discharge-rate---the cycle-index curve of embodiment 2, as shown in Figure 8, and as seen, when little electric current discharges and recharges, its capacity constantly increases with charge and discharge cycles, and when high current charge-discharge, its cycle life is quite long.
Fig. 9 is the capacity of three button lithium ion batteries under same discharge-rate---cycle-index curve, as shown in Figure 9, as seen, γ-Fe that comparative example 1 is prepared 2O 3It is very serious to decay, and embodiment 1 is after charge and discharge cycles 600 times, and capacity is not decay almost, and the prepared γ-Fe of embodiment 2 2O 3Along with the increase that discharges and recharges number of times, capacity continues to rise.
Figure 10 be three button lithium ion batteries before discharging and recharging and the impedance curve after discharging and recharging, as shown in figure 10, can find out, before charge and discharge cycles, along with the rising of annealing temperature, its cloudy anti-corresponding increase.But after 500 times discharge and recharge, the γ-Fe of annealed processing 2O 3Impedance be far smaller than do not have annealing γ-Fe 2O 3Impedance.
Can prove that by above-mentioned experiment embodiment 1 and embodiment 2 are by magnetron sputtering deposition γ-Fe 2O 3The film then method of high-temperature vacuum annealing prepares γ-Fe 2O 3Lithium ion battery anode material, this anode material has good crystallization degree, simultaneously at γ-Fe 2O 3The surface has formed a large amount of holes, thereby has improved the actual capacity of battery, has prolonged the service life cycle of battery; And there is not the γ-Fe of annealed processing 2O 3Lithium ion battery anode material, all relatively relatively poor at the aspects such as service life cycle of the actual capacity of battery, battery.
Among the present invention, the magnetron sputtering technique parameter can be the magnetron sputtering plating parameter of routine, and deposit thickness can STOCHASTIC CONTROL; And the temperature of vacuum annealing need to be controlled between 300 ~ 600 ℃.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.

Claims (5)

1. γ-Fe 2O 3The preparation method of lithium ion battery anode material is characterized in that: may further comprise the steps:
1) with γ-Fe 2O 3Powder compaction becomes target;
2) with the γ-Fe that is pressed into 2O 3Target is packed in the magnetron sputtering cavity;
3) with copper sheet as substrate, put into the magnetron sputtering cavity;
4) after vacuumizing in the magnetron sputtering cavity, be filled with inert gas, utilize magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film;
5) will deposit γ-Fe 2O 3The copper sheet of film is 300 ~ 600 ℃ of annealing under vacuum condition, obtain γ-Fe after the cooling 2O 3Lithium ion battery anode material.
2. γ-Fe according to claim 1 2O 3The preparation method of lithium ion battery anode material is characterized in that: in the described step 3), clean the oxide layer of removing the copper sheet surface with watery hydrochloric acid first, copper sheet will be put into the magnetron sputtering cavity again.
3. γ-Fe according to claim 1 2O 3The preparation method of lithium ion battery anode material is characterized in that: in the described step 4), inert gas is argon gas, and air pressure is 1.0Pa, and deposition rate is 0.1 nm/s, and deposit thickness is 350 nm.
4. γ-Fe according to claim 1 2O 3The preparation method of lithium ion battery anode material is characterized in that: in the described step 5), vacuum degree is 5.0 * 10 -4Pa, annealing time are 1 hour.
5. according to claim 1 to the described γ-Fe of 4 any one 2O 3The preparation method of lithium ion battery anode material is characterized in that: described γ-Fe 2O 3Powder prepares with coprecipitation.
CN201310008762.1A 2013-01-10 2013-01-10 Method for preparing gamma-Fe2O3 positive-pole material for lithium-ion battery Expired - Fee Related CN103022473B (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN103199240A (en) * 2013-04-03 2013-07-10 西南大学 Preparation method of gamma-Fe2O3 sodium ion battery anode material
CN106784723A (en) * 2017-01-12 2017-05-31 青岛大学 One kind oxidation iron-based nano-complex electrode material and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103199240A (en) * 2013-04-03 2013-07-10 西南大学 Preparation method of gamma-Fe2O3 sodium ion battery anode material
CN103199240B (en) * 2013-04-03 2015-05-20 西南大学 Preparation method of gamma-Fe2O3 sodium ion battery anode material
CN106784723A (en) * 2017-01-12 2017-05-31 青岛大学 One kind oxidation iron-based nano-complex electrode material and preparation method thereof
CN106784723B (en) * 2017-01-12 2019-10-18 青岛大学 It is a kind of to aoxidize iron-based nano-complex electrode material and preparation method thereof

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