CN103199240A - Preparation method of gamma-Fe2O3 sodium ion battery anode material - Google Patents

Preparation method of gamma-Fe2O3 sodium ion battery anode material Download PDF

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CN103199240A
CN103199240A CN2013101147530A CN201310114753A CN103199240A CN 103199240 A CN103199240 A CN 103199240A CN 2013101147530 A CN2013101147530 A CN 2013101147530A CN 201310114753 A CN201310114753 A CN 201310114753A CN 103199240 A CN103199240 A CN 103199240A
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sodium
ion battery
anode material
gamma
magnetron sputtering
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CN103199240B (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
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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 discloses a preparation method of a gamma-Fe2O3 sodium ion battery anode material. The preparation method comprises the following steps of: 1) pressing gamma-Fe2O3 powder to form a target material; 2) loading the gamma-Fe2O3 target material formed by pressing into a magnetron sputtering cavity; 3) placing a substrate into the magnetron sputtering cavity; 4) performing vacuum pumping on the magnetron sputtering cavity, then filling inert gas, and depositing a gamma-Fe2O3 thin film on the substrate by utilizing a magnetron sputtering method; and 5) annealing the substrate with the deposited gamma-Fe2O3 thin film at the temperature of 300-700 DEG C under vacuum conditions, and cooling to obtain the gamma-Fe2O3 sodium ion battery anode material. The gamma-Fe2O3 sodium ion battery anode material prepared by the preparation method disclosed by the invention has a good unique physical property of transmitting sodium ions; and furthermore, the transmission of the sodium ions is less prone to damaging the good crystallization degree of gamma-Fe2O3, thus the actual capacity of a battery can be improved and the cycle life can be also greatly prolonged.

Description

γ-Fe 2O 3The preparation method of sodium-ion battery anode material
Technical field
The present invention relates to a kind of preparation method of sodium-ion battery anode material, particularly a kind of γ-Fe 2O 3The preparation method of sodium-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 the research focus of widely paying close attention in recent years rapidly.
At present, the large-scale development of lithium ion battery is subjected to the restriction of lithium resource, and the lithium battery safety issue is also not basic solution technically.In the process of storage battery maximization from now on, the material cost proportion increases, and is subjected to the restriction of resource more.Tokyo Electric Power and N Γ K company cooperative development sodium-sulphur battery are as energy-storage battery, and the implementation phase beginning to enter commercialization in 2002, by in October, 2005 statistics, annual output sodium-sulphur battery amount has surpassed 100MW, begins simultaneously to overseas output.
Sodium-ion battery not only is beneficial to environmental protection, has more economy.The sodium ion radius is bigger, and to compare Coulomb attraction little with lithium ion, and ligand solvent easily breaks away from, and diffusion velocity is fast, and sode cell high speed charge-discharge performance can be better.
One of key of exploitation sodium-ion battery is to seek suitable anode material, makes battery have sufficiently high sodium embedded quantity and takes off the embedding invertibity with good sodium, with the high voltage that guarantees battery, big capacity and long circulation life.
Summary of the invention
In view of this, the invention provides a kind of γ-Fe 2O 3The preparation method of sodium-ion battery anode material, the γ-Fe of preparation 2O 3The sodium-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 sodium-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) substrate is put into the magnetron sputtering cavity;
4) after vacuumizing in the magnetron sputtering cavity, charge into inert gas, utilize magnetron sputtering method depositing gamma-Fe on substrate 2O 3Film;
5) will deposit γ-Fe 2O 3The substrate of film is 300 ~ 700 ℃ of annealing under vacuum condition, obtain γ-Fe after the cooling 2O 3The sodium-ion battery anode material.
Further, in the described step 1), γ-Fe 2O 3Powder prepares with coprecipitation.
Further, in the described step 3), substrate is copper sheet, cleans the oxide layer of removing the copper sheet surface with watery hydrochloric acid earlier, and 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 3.0Pa, and deposition rate is 0.08 nm/s, and deposit thickness is 350 nm.
Further, in the described step 5), vacuum degree is 8.0 * 10 -5Pa, annealing temperature is 600 ℃, annealing time is 1 hour.
Beneficial effect of the present invention is: the present invention utilizes method depositing gamma-Fe on substrate of magnetron sputtering 2O 3Film, and the method for having utilized high-temperature vacuum to anneal have effectively improved 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 sodium ion, and the survivable γ-Fe of the transmission of sodium ion 2O 3Good crystallization degree, therefore with it as the sodium-ion battery anode material, not only can improve the actual capacity of battery, and can prolong widely and recycle the life-span; γ-the Fe of the present invention's preparation 2O 3The sodium-ion battery anode material can be realized long-life, the high power capacity of battery, can be used in the desirable sodium-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, comparative example 2 prepare 2O 3The XRD figure of sodium-ion battery anode material;
γ-Fe that Fig. 2 prepares for embodiment 2 2O 3The XPS figure of sodium-ion battery anode material;
Fig. 3 is γ-Fe that embodiment 1, embodiment 2 and comparative example 1, comparative example 2 prepare 2O 3SEM plane and the sectional view of sodium-ion battery anode material;
Fig. 4 is the CV curve of four button sodium-ion batteries of embodiment 1, embodiment 2 and comparative example 1, comparative example 2;
Fig. 5 is first three time charge and discharge cycles curve of four button sodium-ion batteries of embodiment 1, embodiment 2 and comparative example 1, comparative example 2;
Fig. 6 is the capacity of four button sodium-ion batteries under different discharge-rates---the cycle-index curve of embodiment 1, embodiment 2 and comparative example 1, comparative example 2;
Fig. 7 is the capacity of four button sodium-ion batteries under same discharge-rate---the cycle-index curve of embodiment 1, embodiment 2 and comparative example 1, comparative example 2;
Fig. 8 is the impedance curve of four button sodium-ion batteries of embodiment 1, embodiment 2 and comparative example 1, comparative example 2.
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 sodium-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, earlier clean the oxide layer of removing the copper sheet surface with watery hydrochloric acid, copper sheet will be put into the magnetron sputtering cavity again;
4) charge into argon gas after vacuumizing in the magnetron sputtering cavity, air pressure is 3.0Pa, utilizes magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film, deposition rate are 0.08 nm/s, and deposit thickness is 350 nm;
5) will deposit γ-Fe 2O 3The copper sheet of film is 8.0 * 10 in vacuum degree -5The following 400 ℃ of annealing of the vacuum condition of Pa 1 hour obtain γ-Fe after the cooling 2O 3The sodium-ion battery anode material.
Embodiment 2
γ-Fe of embodiment 2 2O 3The preparation method of sodium-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, earlier clean the oxide layer of removing the copper sheet surface with watery hydrochloric acid, copper sheet will be put into the magnetron sputtering cavity again;
4) charge into argon gas after vacuumizing in the magnetron sputtering cavity, air pressure is 3.0Pa, utilizes magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film, deposition rate are 0.08 nm/s, and deposit thickness is 350 nm;
5) will deposit γ-Fe 2O 3The copper sheet of film is 8.0 * 10 in vacuum degree -5The following 600 ℃ of annealing of the vacuum condition of Pa 1 hour obtain γ-Fe after the cooling 2O 3The sodium-ion battery anode material.
Comparative example 1
γ-the Fe of comparative example 1 2O 3The preparation method of sodium-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, earlier clean the oxide layer of removing the copper sheet surface with watery hydrochloric acid, copper sheet will be put into the magnetron sputtering cavity again;
4) charge into argon gas after vacuumizing in the magnetron sputtering cavity, air pressure is 3.0Pa, utilizes magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film, deposition rate are 0.08 nm/s, and deposit thickness is 350 nm, obtains γ-Fe 2O 3The sodium-ion battery anode material.
Comparative example 2
γ-the Fe of comparative example 2 2O 3The preparation method of sodium-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, earlier clean the oxide layer of removing the copper sheet surface with watery hydrochloric acid, copper sheet will be put into the magnetron sputtering cavity again;
4) charge into argon gas after vacuumizing in the magnetron sputtering cavity, air pressure is 3.0Pa, utilizes magnetron sputtering method depositing gamma-Fe on copper sheet 2O 3Film, deposition rate are 0.08 nm/s, and deposit thickness is 350 nm;
5) will deposit γ-Fe 2O 3The copper sheet of film is 8.0 * 10 in vacuum degree -5The following 200 ℃ of annealing of the vacuum condition of Pa 1 hour obtain γ-Fe after the cooling 2O 3The sodium-ion battery anode material.
Fig. 1 is γ-Fe that embodiment 1, embodiment 2 and comparative example 1, comparative example 2 prepare 2O 3The XRD of sodium-ion battery anode material figure, as shown in Figure 1, γ-Fe of embodiment 1 and embodiment 2 as can be seen 2O 3Pass through the high annealing more than 300 ℃, effectively improved γ-Fe 2O 3Crystallization degree.
γ-Fe that Fig. 2 prepares for embodiment 2 2O 3The XPS figure of sodium-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+, be pure γ-Fe 2O 3
Fig. 3 is γ-Fe that embodiment 1, embodiment 2 and comparative example 1, comparative example 2 prepare 2O 3SEM plane and the sectional view of sodium-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 comparative example 2, Fig. 3 (e) and (f) be the planar S EM figure of embodiment 1, Fig. 3 (γ) and (h) be the planar S EM figure of embodiment 2, Fig. 3 (i) and (j) 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 the high-temperature vacuum annealing more than 300 ℃, at γ-Fe 2O 3The surface has formed a large amount of microcosmic holes, and this hole has realized that sufficiently high sodium embedded quantity and good sodium take off the embedding invertibity.
γ-Fe that embodiment 1, embodiment 2 and comparative example 1, comparative example 2 are prepared respectively 2O 3The sodium-ion battery anode material is as work electrode, and the sodium sheet is as to electrode, is dissolved in that concentration is the NaCF of 1M in the tetraethyleneglycol dimethyl ether 3SO 3As electrolyte, be prepared into four CR2025 type button sodium-ion batteries.
Fig. 4 is the CV curve of four button sodium-ion batteries, and as shown in Figure 4, along with the raising of annealing temperature, its oxidation peak is more sharp-pointed.
Fig. 5 is first three time charge and discharge cycles curve of four button sodium-ion batteries, and as shown in Figure 5, as known in the figure, its discharge platform voltage approximately all is 0.3V.
Fig. 6 is the capacity of four button sodium-ion batteries under different discharge-rates---cycle-index curve, as shown in Figure 6, and γ-Fe that visible embodiment 1 and embodiment 2 are prepared 2O 3Under different discharge-rates, its capacity is all higher.
Fig. 7 is the capacity of four button sodium-ion batteries under same discharge-rate---cycle-index curve, as shown in Figure 7, as seen, γ-Fe that comparative example 1 and comparative example 2 are prepared 2O 3It is very serious to decay, γ-Fe that embodiment 1 is prepared 2O 3After charge and discharge cycles 100 times, capacity attenuation 15%, and the prepared γ-Fe of embodiment 2 2O 3Capacity is not decay almost.
Fig. 8 is the impedance curve of four button sodium-ion batteries, as shown in Figure 8, as can be seen, along with the rising of annealing temperature, its cloudy anti-corresponding increase.
Can prove that by above-mentioned experiment embodiment 1 and embodiment 2 are by magnetron sputtering deposition γ-Fe 2O 3The film method that high-temperature vacuum is annealed more than 300 ℃ then prepares γ-Fe 2O 3The sodium-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 life-span that recycles of battery; And do not have annealed processing and be lower than the γ-Fe of 300 ℃ of vacuum annealings 2O 3The sodium-ion battery anode material, the actual capacity of battery, battery to recycle aspects such as life-span all relatively poor relatively.Therefore, among the present invention, the temperature of vacuum annealing need be controlled between 300 ~ 700 ℃, and most preferred annealing temperature is 600 ℃, and the vacuum degree of wherein annealing also can adjust according to the performance of instrument.
Among the present invention, the magnetron sputtering technique parameter can be the magnetron sputtering plating parameter of routine, and equipment of other preparation film also can be used for the present invention certainly, and deposit thickness can STOCHASTIC CONTROL; Substrate is not limited to copper sheet, and other sheet metal or conductive film also can be used for the present invention, but annealing conditions can be adjusted according to material therefor and substrate properties; γ-Fe 2O 3Powder is not limited to the coprecipitation preparation, also can prepare γ-Fe with other method 2O 3Powder.
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 sodium-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) substrate is put into the magnetron sputtering cavity;
4) after vacuumizing in the magnetron sputtering cavity, charge into inert gas, utilize magnetron sputtering method depositing gamma-Fe on substrate 2O 3Film;
5) will deposit γ-Fe 2O 3The substrate of film is 300 ~ 700 ℃ of annealing under vacuum condition, obtain γ-Fe after the cooling 2O 3The sodium-ion battery anode material.
2. γ-Fe according to claim 1 2O 3The preparation method of sodium-ion battery anode material is characterized in that: in the described step 1), and γ-Fe 2O 3Powder prepares with coprecipitation.
3. γ-Fe according to claim 1 2O 3The preparation method of sodium-ion battery anode material is characterized in that: in the described step 3), substrate is copper sheet, cleans the oxide layer of removing the copper sheet surface with watery hydrochloric acid earlier, and copper sheet will be put into the magnetron sputtering cavity again.
4. γ-Fe according to claim 1 2O 3The preparation method of sodium-ion battery anode material is characterized in that: in the described step 4), inert gas is argon gas, and air pressure is 3.0Pa, and deposition rate is 0.08 nm/s, and deposit thickness is 350 nm.
5. γ-Fe according to claim 1 2O 3The preparation method of sodium-ion battery anode material is characterized in that: in the described step 5), vacuum degree is 8.0 * 10 -5Pa, annealing temperature is 600 ℃, annealing time is 1 hour.
CN201310114753.0A 2013-04-03 2013-04-03 Preparation method of gamma-Fe2O3 sodium ion battery anode material Expired - Fee Related CN103199240B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103400975A (en) * 2013-08-13 2013-11-20 西南大学 Preparation method of Cu2O secondary battery anode material
CN110212188A (en) * 2019-06-14 2019-09-06 陕西科技大学 A kind of carbon makees the metal iron oxide and its preparation method and application of skeletal support growth
CN114824235A (en) * 2022-06-06 2022-07-29 河南固锂电技术有限公司 Multilayer sodium-ion battery positive electrode material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1630126A (en) * 2004-10-11 2005-06-22 湘潭大学 sodium ion battery and method for manufacturing the same
CN103022473A (en) * 2013-01-10 2013-04-03 西南大学 Method for preparing gamma-Fe2O3 positive-pole material for lithium-ion battery

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CN1630126A (en) * 2004-10-11 2005-06-22 湘潭大学 sodium ion battery and method for manufacturing the same
CN103022473A (en) * 2013-01-10 2013-04-03 西南大学 Method for preparing gamma-Fe2O3 positive-pole material for lithium-ion battery

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103400975A (en) * 2013-08-13 2013-11-20 西南大学 Preparation method of Cu2O secondary battery anode material
CN103400975B (en) * 2013-08-13 2015-10-14 西南大学 Cu 2the preparation method of O secondary cell anode material
CN110212188A (en) * 2019-06-14 2019-09-06 陕西科技大学 A kind of carbon makees the metal iron oxide and its preparation method and application of skeletal support growth
CN114824235A (en) * 2022-06-06 2022-07-29 河南固锂电技术有限公司 Multilayer sodium-ion battery positive electrode material and preparation method thereof
CN114824235B (en) * 2022-06-06 2023-03-24 河南固锂电技术有限公司 Multilayer sodium-ion battery positive electrode material and preparation method thereof

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