CN102522556A - Nano-grade cathode material used in lithium ion battery, and preparation method thereof - Google Patents

Nano-grade cathode material used in lithium ion battery, and preparation method thereof Download PDF

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Publication number
CN102522556A
CN102522556A CN2011104341961A CN201110434196A CN102522556A CN 102522556 A CN102522556 A CN 102522556A CN 2011104341961 A CN2011104341961 A CN 2011104341961A CN 201110434196 A CN201110434196 A CN 201110434196A CN 102522556 A CN102522556 A CN 102522556A
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China
Prior art keywords
lithium ion
nano
stannous oxalate
ion battery
preparation
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CN2011104341961A
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Chinese (zh)
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任钦琪
傅正文
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Fudan University
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Fudan University
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Priority to CN2011104341961A priority Critical patent/CN102522556A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention belongs to the technical field of electrochemistry, and specifically relates to a nano-grade cathode material used in a lithium ion battery, and a preparation method thereof. The nano-grade cathode material is film-mode amorphous stannous oxalate (SnC2O4), and is prepared through a magnetron sputtering deposition method. With an electrode manufactured by using the film, a traditional perception that the type of material has no electrochemical property is out-broken. It is proofed that the material has good charge/discharge performance and circulation reversibility. Therefore, the material can be used as a cathode material for the lithium ion battery. Reversible specific capacity of the amorphous stannous oxalate (SnC2O4) nano-grade material film electrode is 504.5mAh/g. The amorphous stannous oxalate (SnC2O4) nano-grade electrode material has good stability, high specific capacity, low polarization of a charge/discharge platform, and simple preparation method. The material is suitable for lithium ion batteries.

Description

A kind of nanometer negative material that is used for lithium ion battery and preparation method thereof
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to one type and be used for negative material of lithium ion battery and preparation method thereof.
Background technology
Lithium ion battery is the vital power supply of notebook computer, camera, mobile phone and other Communication Equipment, and might be used for automobile and other vehicles as green energy resource.At present commercially available lithium ion battery is mainly by the carbon back negative material, and liquid organic electrolyte is formed with the transition metal oxide positive electrode that contains lithium.In order further to improve the performance of lithium ion battery, people study, seek than the better novel negative material of carbon back negative material performance.In addition, along with the miniaturization of microelectronic component, the lithium-ion film cell that an urgent demand exploitation is complementary therewith.
Summary of the invention
The objective of the invention is to propose one type and possess negative pole nano material of electro-chemical activity and well behaved lithium ion battery and preparation method thereof.
The negative pole nano material that is used for lithium ion battery that the present invention proposes is that (molecular formula is SnC to a kind of novel amorphous state stannous oxalate 2O 4) nano film material.Do not find stannous oxalate (SnC before this 2O 4) material possesses electro-chemical activity, yet the amorphous state stannous oxalate (SnC that comes out through this The project 2O 4) broken through traditional cognition, quilt is confirmed has good electrochemical, can be used as the negative material of high performance lithium ion battery.Do not have about amorphous state stannous oxalate (SnC up to now 2O 4) nano material is as the report of lithium ion battery negative material.
The amorphous state stannous oxalate (SnC that the present invention proposes as lithium ion battery negative material 2O 4) nano material is form of film, and possesses good electrochemical activity.
The present invention's proposition is used for the preparation method of the nanometer negative material of lithium ion battery, adopts the preparation of laser splash sedimentation, and concrete steps are: the stannous oxalate powder is ground the back compressing tablet process the used target of magnetron sputtering deposition.Target and substrate distance are 3~5cm, and vacuum degree is 10 in the sputtering chamber -1~10 -2Pa,, (carry out under 1~100Pa) atmosphere, sedimentation time is 0.5~2 hour to sputter at Ar.
Among the present invention, amorphous state stannous oxalate (SnC 2O 4) material of nano material film is made up of X-ray photoelectron spectroscopic analysis appearance (XPS), X-ray diffractometer and Raman spectrum and confirms.X-ray diffractometer (XRD) and Raman spectrum show the stannous oxalate (SnC that is made by the laser splash sedimentation 2O 4) nano material film is the SnC of amorphous state 2O 4
Among the present invention, amorphous state SnC 2O 4Nano material film can directly be processed the lithium ion cell film electrode.
Among the present invention, amorphous state SnC 2O 4The electrochemical property test of nano material film electrode adopts the hull cell system that is made up of three electrodes.Wherein, amorphous state SnC 2O 4Nano thin-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 blue electricity (Land) hull cell test macro.
Among the present invention, the amorphous state stannous oxalate (SnC that on substrates such as stainless steel substrates, makes by the laser splash sedimentation 2O 4) the nano material film electrode possesses charge-discharge performance, at voltage range 0.01~3.0V and current density 2 μ A/cm 2The time, the platform of exoelectrical reaction appears at 1.2V and 0.6V (with respect to Li/Li +), for the second time discharge process with the first time discharge process compare, irreversible discharge capacity loss is 17.86%.The second later cyclic process of week has good invertibity, and average each circulation volume decay is merely 8.6%.
Above-mentioned performance shows, amorphous state stannous oxalate (SnC 2O 4) nano material can be used as a kind of novel negative material and be applied to lithium ion battery.
Description of drawings
Fig. 1 is embodiment 1 amorphous state stannous oxalate (SnC 2O 4) the cycle charge-discharge spectrogram of nano material film.
Fig. 2 is embodiment 1 amorphous state stannous oxalate (SnC 2O 4) the Raman analysis spectrogram of nano material film.
Embodiment
Further specify the present invention through embodiment below.
Embodiment: adopt the laser splash sedimentation to prepare amorphous state stannous oxalate nano material (SnC 2O 4) during film, the stannous oxalate powder is ground the back compressing tablet process the used target of magnetron sputtering deposition.Target and substrate distance are 3~5cm, and vacuum degree is 10 in the sputtering chamber -1~10 -2Pa, (carry out under 1~100Pa) atmosphere, sedimentation time is 0.5~2 hour to sputter at Ar.
The Raman spectrogram is measured the amorphous state stannous oxalate (SnC that shows deposition 2O 4) material of nano material film forms (accompanying drawing 2).
To the amorphous state stannous oxalate (SnC on the stainless steel substrate 2O 4) the electrochemical property test result (accompanying drawing 1) as follows of nano material film electrode:
Amorphous state stannous oxalate (SnC 2O 4) the nano material film electrode can be at 2 μ A/cm 2Carry out charge and discharge cycles under the charge-discharge velocity.In voltage range 0.01-3.0V, discharge capacity can reach 504.5mAh/g for the first time, and reversible capacity is about 414.1mAh/g.
Therefore, the amorphous state stannous oxalate (SnC that on stainless steel substrates, deposits 2O 4) nano material film can be used as the negative material of lithium-ion film cell.

Claims (2)

1. lithium ion cell nano negative material, this is characterised in that and is a kind of amorphous state stannous oxalate nano film material that this amorphous state stannous oxalate molecular formula is SnC 2O 4
2. the preparation method of a lithium ion cell nano negative material as claimed in claim 1; It is characterized in that this nanometer negative material adopts the magnetron sputtering technique preparation, concrete steps are: the stannous oxalate powder is ground the back compressing tablet process the used target of magnetron sputtering deposition; Target and substrate distance are 3~5cm, and vacuum degree is 10 in the sputtering chamber -1~10 -2Pa sputters under the Ar atmosphere and carries out, and Ar is 1~100Pa, and sedimentation time is 0.5~2 hour.
CN2011104341961A 2011-12-22 2011-12-22 Nano-grade cathode material used in lithium ion battery, and preparation method thereof Pending CN102522556A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103811730A (en) * 2012-11-09 2014-05-21 万向电动汽车有限公司 High-capacity lithium ion battery composite negative electrode material and preparation method thereof
CN109306551A (en) * 2018-07-18 2019-02-05 湘潭大学 A kind of boron doped titanic oxide nanofiber and preparation method thereof and application as lithium ion battery negative material

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1848484A (en) * 2005-04-05 2006-10-18 河南科技大学 Method for producing tin-based oxide thin film positive pole

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1848484A (en) * 2005-04-05 2006-10-18 河南科技大学 Method for producing tin-based oxide thin film positive pole

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
QIN-QI REN等: "A new electrochemical reaction mechanism of tin pyrophosphate thin film with lithium", 《JOURNAL OF POWER SOURCES》, vol. 199, 17 October 2011 (2011-10-17), pages 336 - 340 *
R. ALCÁNTARA等: "Tin oxalate as precursor of tin dioxide and electrode materials for lithium-ion batteries", 《JOURNAL OF SOLID STATE ELECTROCHEMISTRY》, vol. 6, no. 1, 16 May 2001 (2001-05-16), pages 55 - 62 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103811730A (en) * 2012-11-09 2014-05-21 万向电动汽车有限公司 High-capacity lithium ion battery composite negative electrode material and preparation method thereof
CN103811730B (en) * 2012-11-09 2016-08-03 万向电动汽车有限公司 A kind of composite negative pole material of high-capacity lithium ion cell and preparation method thereof
CN109306551A (en) * 2018-07-18 2019-02-05 湘潭大学 A kind of boron doped titanic oxide nanofiber and preparation method thereof and application as lithium ion battery negative material

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Application publication date: 20120627