CN1949564A - Ferrous selenide cathode material for lithium cell and preparing process thereof - Google Patents
Ferrous selenide cathode material for lithium cell and preparing process thereof Download PDFInfo
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- CN1949564A CN1949564A CNA2006101175954A CN200610117595A CN1949564A CN 1949564 A CN1949564 A CN 1949564A CN A2006101175954 A CNA2006101175954 A CN A2006101175954A CN 200610117595 A CN200610117595 A CN 200610117595A CN 1949564 A CN1949564 A CN 1949564A
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- Prior art keywords
- film
- ferrous selenide
- substrate
- lithium battery
- fese
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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 invention belongs to electrochemical technical field, concretely relating to a Li ion battery cathode material and the preparing method thereof. And it is an FeSe film prepared by reactive pulse laser deposition. And the electrode made from the FeSe film has very good charging and discharging circulating reversibility and specific capacity kept at about 400 mAh/g, and the capacity of the electrode has no obvious attenuation after 100 charging-discharging cycles. And it has good chemical stability, high specific capacity, and simple preparing method, applied to Li batteries.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a class and be used for lithium battery cathode material and preparation method thereof.
Background technology
Serondary lithium 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.In order further to improve the performance of lithium battery, people study, seek better novel negative electrode and anode material of performance.In addition, along with the miniaturization of microelectronic component, the lithium battery that an urgent demand exploitation is complementary therewith, for example film lithium cell etc.
Summary of the invention
The objective of the invention is to propose well behaved cathode materials for lithium battery of a class and preparation method thereof.
The cathode materials for lithium battery that the present invention proposes is a kind of ferrous selenide (FeSe) material with tetragonal.Show that after deliberation this type of material has good electrochemical, can be used as the high-performance lithium battery cathode material.So far not about the report of ferrous selenide (FeSe) material as cathode materials for lithium battery.
The ferrous selenide as cathode materials for lithium battery (FeSe) that the present invention proposes is a form of film, is made up of nano particle, and particle diameter is 40-100nm, and the thickness of thin-film material is 0.4-1 μ m.
The invention allows for the preparation method of aforementioned cathode materials for lithium battery, specifically be described below:
Ferrous selenide (FeSe) film as cathode materials for lithium battery can adopt reactive pulsed laser deposition preparation, concrete steps are: compressing tablet after iron powder and the selenium powder ground and mixed is made the used target of pulsed laser deposition, wherein the amount of substance of selenium powder be iron powder 1-3 doubly, the 1064nm fundamental frequency that is produced by neodymium-doped yttrium pyralspite laser obtains the 355nm pulse laser behind frequency tripling, laser beam is through inciding after the lens focus on the above-mentioned target, the distance of target and substrate is 25-50mm, deposition obtains ferrous selenide (FeSe) film on substrate in argon gas atmosphere, substrate can adopt stainless steel substrates, platinized platinum or gold-plated monocrystalline silicon piece, substrate temperature are 150-250 ℃.The depositing of thin film time is required to determine by film thickness, is generally 0.3-1.0h.Film thickness can be measured by ESEM, and the weight of film is made difference according to substrate weight before and after the electronic balance weighing experiment and obtained.
Among the present invention, the crystal structure of ferrous selenide (FeSe) film is determined by x-ray diffractometer (Bruker D8 Advance).X-ray diffracting spectrum shows that ferrous selenide (FeSe) film that is made by pulse laser reactive deposition method is the polycrystalline tetragonal.Show that by ESEM (Philips XL30) mensuration be made up of nano particle ferrous selenide (FeSe) film that pulse laser reactive deposition method makes, their particle diameter is 40-100nm, and distribution of particles is even.
Among the present invention, ferrous selenide (FeSe) film can directly be made the lithium battery membrane electrode.
Among the present invention, the electrochemical property test of ferrous selenide (FeSe) membrane electrode adopts the battery system of being made up of three electrodes, and wherein, ferrous selenide (FeSe) film is used 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).Battery is assemblied in the drying box of applying argon gas and carries out.The experiment that discharges and recharges of battery is carried out on blue electricity (Land) battery test system.
Among the present invention, ferrous selenide (FeSe) membrane electrode that is made on metal substrates such as stainless steel substrates, platinized platinum by the pulse laser reactive deposition processes all has charge-discharge performance, discharge platform appear at 1.62 and 1.45V (with respect to Li
+/ Li), for the first time irreversible discharge capacity loss is less than 10%, at voltage range 1.0-3.0V and current density 5 μ A/cm
2The time, the specific capacity of ferrous selenide (FeSe) membrane electrode remains on 355～402mAh/g in preceding 100 circulations.
Above-mentioned performance shows that ferrous selenide (FeSe) is the novel cathode material of a class, can be applicable to lithium battery.
Description of drawings
Fig. 1 is the XRD spectra of ferrous selenide (FeSe) film.The diffraction maximum of stainless steel substrate represented in asterisk among the figure.
Embodiment
Further introduce the present invention below by specific embodiment.
Embodiment 1
Adopt reactive pulsed laser deposition to prepare ferrous selenide (FeSe) film, color is a grey.During preparation, in the hybrid target, the amount of substance of selenium powder is 1.5 times of iron powder, adopt stainless steel substrates as substrate, the distance of substrate and target is 40mm, substrate temperature is 200 ℃, and the fundamental frequency that is produced by the Nd:YAG laser produces the 355nm pulse laser through frequency tripling, on the hybrid target of laser beam through inciding iron powder and selenium powder after the lens focus.Energy density is 2Jcm
-2, sedimentation time is 0.5 hour.
X-ray diffraction is measured and is shown that the film of deposition is the ferrous selenide (FeSe) of polycrystalline tetragonal, contains a spot of Fe
7Se
8And FeSe
2(accompanying drawing 1).Show that by stereoscan photograph mensuration ferrous selenide (FeSe) film surface that is made by the pulse laser reactive deposition is a nano particle.
Electrochemical property test result to the ferrous selenide on the stainless steel substrate (FeSe) membrane electrode is as follows:
Ferrous selenide (FeSe) membrane electrode can be at 5 μ A/cm
2Carry out charge and discharge cycles under the charge-discharge velocity.In voltage range 1.0-3.0V, discharge capacity can reach 388mAh/g for the first time, and reversible capacity is 360mAh/g, tends towards stability through 15 circulation back discharge capacities, and 100 capacity that circulate remain on 396mAh/g.
Therefore, the ferrous selenide that deposits on stainless steel substrates (FeSe) film can be used as lithium battery cathode material.
Actual tests shows, in above-mentioned preparation process, in the proportion of the amount of described in front selenium powder and iron powder and under the described preparation condition, all can obtain the ferrous selenide thin-film material of polycrystalline tetragonal, and have described chemical property, can be as lithium battery cathode material.Here give an example no longer one by one.
Claims (2)
1, a kind of cathode materials for lithium battery is characterized in that the ferrous selenide material that has tetragonal for a kind of, and such material is a form of film, is made up of nano particle, and particle diameter is 40-100nm, and the thickness of film is 0.4-1 μ m.
2, a kind of preparation method of cathode materials for lithium battery as claimed in claim 1, it is characterized in that the ferrous selenide thin-film material adopts reactive pulsed laser deposition preparation, concrete steps are: compressing tablet after iron powder and the selenium powder ground and mixed is made the used target of pulsed laser deposition, wherein the amount of substance of selenium powder be iron powder 1-3 doubly, the 1064nm fundamental frequency that is produced by neodymium-doped yttrium pyralspite laser obtains the 355nm pulse laser behind frequency tripling, laser beam is through inciding after the lens focus on the above-mentioned target, the distance of target and substrate is 25-45mm, deposition obtains the ferrous selenide film on substrate in argon gas atmosphere, substrate adopts stainless steel substrates, platinized platinum or gold-plated monocrystalline silicon piece, substrate temperature are 150-250 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101175954A CN100423330C (en) | 2006-10-26 | 2006-10-26 | Ferrous selenide cathode material for lithium cell and preparing process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101175954A CN100423330C (en) | 2006-10-26 | 2006-10-26 | Ferrous selenide cathode material for lithium cell and preparing process thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1949564A true CN1949564A (en) | 2007-04-18 |
| CN100423330C CN100423330C (en) | 2008-10-01 |
Family
ID=38018993
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101175954A Expired - Fee Related CN100423330C (en) | 2006-10-26 | 2006-10-26 | Ferrous selenide cathode material for lithium cell and preparing process thereof |
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| CN (1) | CN100423330C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759162B (en) * | 2010-01-11 | 2011-10-12 | 中山大学 | Low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet |
| CN102556984A (en) * | 2010-12-07 | 2012-07-11 | 北京有色金属研究总院 | Novel method for organically synthesizing FeSe superconductor precursor powder |
| CN102593446A (en) * | 2012-02-22 | 2012-07-18 | 清华大学 | Method for preparing active electrode material of lithium ion battery |
| CN106848274A (en) * | 2017-03-09 | 2017-06-13 | 华中科技大学 | The preparation method and sodium-ion battery of a kind of Nanoscale Iron selenium compound |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57172661A (en) * | 1981-04-17 | 1982-10-23 | Toshiba Corp | Solid lithium battery |
| US4911996A (en) * | 1988-03-11 | 1990-03-27 | Eic Laboratories, Inc. | Electrochemical cell |
| JPH06275312A (en) * | 1993-03-22 | 1994-09-30 | Matsushita Electric Ind Co Ltd | Full solid lithium battery |
| CN100341172C (en) * | 2005-09-15 | 2007-10-03 | 复旦大学 | Film lithium ion battery using stannous selenide film as anode material and its preparation method |
-
2006
- 2006-10-26 CN CNB2006101175954A patent/CN100423330C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759162B (en) * | 2010-01-11 | 2011-10-12 | 中山大学 | Low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet |
| CN102556984A (en) * | 2010-12-07 | 2012-07-11 | 北京有色金属研究总院 | Novel method for organically synthesizing FeSe superconductor precursor powder |
| CN102556984B (en) * | 2010-12-07 | 2013-12-11 | 北京有色金属研究总院 | Novel method for organically synthesizing FeSe superconductor precursor powder |
| CN102593446A (en) * | 2012-02-22 | 2012-07-18 | 清华大学 | Method for preparing active electrode material of lithium ion battery |
| CN106848274A (en) * | 2017-03-09 | 2017-06-13 | 华中科技大学 | The preparation method and sodium-ion battery of a kind of Nanoscale Iron selenium compound |
| CN106848274B (en) * | 2017-03-09 | 2019-04-12 | 华中科技大学 | A kind of preparation method and sodium-ion battery of Nanoscale Iron selenium compound |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100423330C (en) | 2008-10-01 |
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Granted publication date: 20081001 Termination date: 20111026 |