CN101339989A - Aluminum-tin alloy film for lithium ionic cell negative electrode and method for preparing the same - Google Patents
Aluminum-tin alloy film for lithium ionic cell negative electrode and method for preparing the same Download PDFInfo
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- CN101339989A CN101339989A CNA2008100286855A CN200810028685A CN101339989A CN 101339989 A CN101339989 A CN 101339989A CN A2008100286855 A CNA2008100286855 A CN A2008100286855A CN 200810028685 A CN200810028685 A CN 200810028685A CN 101339989 A CN101339989 A CN 101339989A
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- 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 provides a preparation method of a tin aluminum alloy membrane used in a lithium-ion battery cathode, which comprises the steps as follows: (1) a metal foil taken as a membrane electrode current collector is taken as a substrate for magnetron sputtering and the substrate is cleaned; (2) the air pressure of a sputtering chamber is adjusted to be 1.0*10<-3>Pa or above, and then is adjusted within the range of 0.1-10Pa after inert gas is introduced; (3) the tin aluminum alloy membrane is prepared by magnetron sputtering, the sputtering power is needed to be adjusted within the range of 10W-5kW, the sputtering type belongs to DC magnetron sputtering or RF magnetron sputtering, and the sputtering deposition time is controlled within the range of 10-60 minutes. The tin aluminum alloy membrane used in the lithium-ion battery cathode prepared by using the method is composed of the tin aluminum alloy of solid solution alloy material; the tin aluminum alloy comprises 25-75% of tin and the rest is aluminum. The preparation method has the advantages of simple process, low cost, high efficiency and no by-product; the prepared membrane electrode material has uniform crystal grain, and good crystallinity and mechanical property.
Description
Technical field
The present invention relates to the lithium ion battery negative material technology, particularly a kind of aluminum-tin alloy film for lithium ionic cell negative electrode and preparation method thereof.
Background technology
Lithium ion battery has become one of important novel energy of 21 century, is widely used in fields such as various portable type electronic products and electric tool, and is expected to one of energy resource supply that becomes following hybrid vehicle and pure electric automobile.Negative material is one of key factor of lithium ion battery combination property quality, though the commercialization carbon negative pole material has better cycle performance at present, but, far can not satisfy the demand of following high-capacity and long-life electronic equipment owing to its lower specific capacity (theoretical specific capacity 372mAh/g) and relatively poor multiplying power discharging property.
In recent years, metal and alloy type material are the new and effective storage cathode of lithium material systems of studying morely, wherein aluminium and Xi Yin its have the specific capacity more much higher (theoretical specific capacity be respectively 2234mAh/g, 994mAh/g) receives much concern than material with carbon element.In addition, aluminium alloy has that specific strength and specific stiffness height, high-temperature behavior are good, resistance to wear and advantage such as fatigue durability is good, thermal coefficient of expansion is low.Utilize the advantage of aluminium alloy to have very great help for the cycle performance that improves electrode used as lithium ion battery negative material.
Fine aluminium or pure tin are as lithium ion battery negative material the time, because the embedding of lithium ion is taken off and " intrusion " of electrolyte, electrode takes off in the process in the lithium embedding can produce very big change in volume, causes the mechanical disintegration of lithium active materials such as aluminium or tin, causes electrode avalanche efflorescence inefficacy gradually.At this shortcoming, present research mainly concentrates on composite oxides and two aspects of alloy material, and alloy material adopts the alloy material of active and nonactive element formation as lithium ion battery negative material, as tin-nickel alloy mostly.This class material lithium ion embed and the process of deviating from can form the material of active and inert matter structure, active material reacts with lithium provides energy, inert matter to serve as the cycle life that " buffer body " keeps the basic structure assurance electrode of electrode.Obviously, when introducing non-active material, though cycle performance has bigger improvement, the problem that exists its electrode capacity to reduce.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, propose a kind of aluminum-tin alloy film for lithium ionic cell negative electrode that when improving the electrode cycle performance, increases electrode capacity.
It is simple to another object of the present invention is to propose a kind of operating procedure, and cost is low, the efficient height, the above-mentioned aluminum-tin alloy film for lithium ionic cell negative electrode of preparation of no coupling product method.
Purpose of the present invention is achieved through the following technical solutions: a kind of aluminum-tin alloy film for lithium ionic cell negative electrode, constitute by the solid solution alloy material mock silver, and the content of tin is 25～75% in the described mock silver, is preferably 50%, all the other are aluminium; The thickness of aluminum-tin alloy film is preferably 100 μ m at 50～200 mu m ranges.
Above-mentioned aluminum-tin alloy film for lithium ionic cell negative electrode adopts the magnetron sputtering technique preparation, and concrete grammar comprises the steps:
(1) selects for use as the substrate of the metal forming of membrane electrode collector, and carry out substrate and clean as magnetron sputtering;
(2) regulate sputtering chamber air pressure to 1.0 * 10
-3Pa or more than, feed inert gas then and regulate air pressure in 0.1～10Pa scope;
(3) magnetron sputtering prepares aluminum-tin alloy film, regulates sputtering power deposit film in 10W～5KW scope, and sedimentation time was 10～60 minutes scopes.
The described metal forming as the membrane electrode collector of step (1) is Copper Foil, aluminium foil or other metal formings.
Clean to substrate in the step (1) is: the concentration that earlier substrate is placed metal cleaner (can select STC-M101 high-efficiency water-base metal cleaner for use) preparation is that 3～10% solution soaks, put into the deionized water soaking and washing again, then substrate is carried out putting on the sputtering chamber substrate pedestal after the drying, at last substrate surface is carried out backwash and handle; Remove the impurity such as micronic dust, greasy dirt of substrate surface.
The described inert gas of step (2) is argon gas or other inert gases, and the air pressure of regulating behind the described feeding inert gas is preferably 1Pa～3Pa.
The described magnetron sputtering type of step (3) can be magnetically controlled DC sputtering or rf magnetron sputtering.
Described magnetron sputtering concrete operations mode can be vertical sputter or cosputtering, and the target that vertical sputter is adopted is a mock silver target, and the mass percent of its aluminium is 25～75% (being preferably 50%); The target that cosputtering adopts is for being installed in two aluminium monomer target and tin monomer targets on the different target pedestals respectively.
Can make aluminum-tin alloy film for lithium ionic cell negative electrode of the present invention by said method.
The present invention has following advantage and effect with respect to prior art:
What (1) the present invention proposed prepares aluminum-tin alloy film for lithium ionic cell negative electrode increase electrode capacity when improving the electrode cycle performance with magnetron sputtering technique, with respect to the pure tin electrode of reporting in the document, electrode capacity can improve about 40%, and cycle performance also is greatly improved.Has the charge/discharge capacity height, the advantage of good cycle.
(2) mock silver of the present invention's proposition is a kind of solid solution alloy, with respect to existing general non-solid solution body alloy, can not exist because of material itself causes electrode capacity and reduce problem, and the alloy material of this process " solution strengthening " has good mechanical strength.
(3) aluminum-tin alloy film for lithium ionic cell negative electrode of the present invention's proposition adopts the magnetron sputtering technique preparation.With respect to existing alloy firm electrode preparation method, as preparation methods such as electrochemical deposition method, ball-milling method, high temperature solid-state methods, adopting magnetron sputtering to prepare thin-film electrode material, to have an operating procedure simple, cost is low, the efficient height, advantages such as no coupling product, the thin-film electrode material uniform crystal particles of preparing is tiny, degree of crystallinity and good mechanical properties.
Description of drawings
Fig. 1 is the X-ray diffractogram of aluminum-tin alloy film among the present invention.
Fig. 2 is the surface topography map of aluminum-tin alloy film among the present invention.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples, but the working of an invention mode is not limited thereto.
In following examples, work electrode is the square sheets after the membrane electrode for preparing is cut into 8mm * 8mm, to electrode is pour lithium slice, electrolyte is for containing 1M LiPF6/EC: DMC: EMC=1: 1: 1 solution, barrier film is microporous polypropylene membrane Celgard-2300, is assembled into CR2016 type button cell at last in being filled with the glove box of argon gas (water content and oxygen content all are lower than 1ppm).
Employed magnetic control sputtering system is the JGP560 type superelevation magnetic control sputtering system that Shenyang scientific instrument Co., Ltd of the Chinese Academy of Sciences produces.Monomer target and alloy target material that sputtering target material adopts Ou Lai (Shenzhen) sputtering target material Co., Ltd to produce.Blue electricity (Land) battery test system that the battery charging and discharging test macro adopts Wuhan Jin Nuo Electronics Co., Ltd. to produce.
Adopt the constant current charge-discharge test on the battery charging and discharging test macro, charging and discharging currents is 0.03mA, and the charging/discharging voltage scope is controlled between the 0-2.5V.
Embodiment 1
Employing is of a size of the pure Sn monomer of Φ 40mm * 3mm target (purity is 99.9%), and the interior initial gas pressure of sputtering chamber is 1.0 * 10 before the sputter
-4Pa.At room temperature, feed argon gas, make that the interior sputtering pressure of sputtering chamber is 3.0Pa.Regulating radio-frequency power supply power is 200W, the pure Sn film of deposition on Copper Foil, sedimentation time 10 minutes.
The membrane electrode of preparation is assembled into CR2016 type button cell by method noted earlier.Electro-chemical test shows, the initial charge capacity of the Sn membrane electrode that foundation magnetically controlled sputter method of the present invention is prepared is 660mAh/g, and discharge capacity is 570mAh/g, and 30 times circulation back capacity remains on 550mAh/g, capability retention is 83%, and efficiency for charge-discharge maintains 90%.
Prepared sample is carried out the X-ray diffraction material phase analysis, found that the tin thin film of rf magnetron sputtering preparation is a kind of polycrystalline.
Embodiment 2
Employing is of a size of the pure Sn monomer of Φ 40mm * 3mm target (purity is 99.9%), and the interior initial gas pressure of sputtering chamber is 1.0 * 10 before the sputter
-4Pa.At room temperature, feed argon gas, make that the interior sputtering pressure of sputtering chamber is 0.1Pa.Regulating DC power supply power is 10W, the pure Sn film of deposition on Copper Foil, sedimentation time 30 minutes.
The membrane electrode of preparation is assembled into CR2016 type button cell by method noted earlier.Electro-chemical test shows, the initial charge capacity of the Sn membrane electrode that foundation magnetically controlled sputter method of the present invention is prepared is 781mAh/g, and discharge capacity is 500Ah/g first, and 30 times circulation back capacity remains on 100mAh/g, capability retention is 13%, and efficiency for charge-discharge maintains 90%.
Embodiment 3
Employing is of a size of Φ 40mm * 3mm, element mass ratio Al: Sn=1: the interior initial gas pressure of sputtering chamber is 1.0 * 10 before 3 the AlSn alloy target material (purity is 99.95%), sputter
-4Pa.At room temperature, feed argon gas, make that the interior sputtering pressure of sputtering chamber is 3.0Pa.In room temperature, under the argon atmosphere condition, regulating radio-frequency power supply power is 200W, depositing Al Sn film on Copper Foil, sedimentation time 10 minutes.
The membrane electrode of preparation is assembled into CR2016 type button cell by method noted earlier.Electro-chemical test shows, the initial charge capacity of the AlSn alloy firm electrode that foundation magnetically controlled sputter method of the present invention is prepared is 905mAh/g, and discharge capacity is 698Ah/g, and 30 times circulation back capacity remains on 768mAh/g, capability retention is 85%, and efficiency for charge-discharge maintains 98%.
Prepared sample is carried out the X-ray diffraction material phase analysis, and the result can only obtain single S n and exist mutually, and the X ray energy spectrum then finds to have in the sample Al element to exist, and this explanation Al atom is dissolved among the Sn and with Sn and has formed solid solution alloy.The phase structure of mock silver as shown in Figure 1.This solid solution alloy has solved the capacity attenuation problem that general non-solid solution body alloy causes owing to inert matter, and has improved the cycle performance of electrode to a certain extent.Sample discharges and recharges preceding surface topography as shown in Figure 2, the sample uniform crystal particles, and adhesion is good.。
Embodiment 4
Employing is of a size of Φ 40mm * 3mm, element mass ratio Al: Sn=1: the interior initial gas pressure of sputtering chamber is 1.0 * 10 before 3 the AlSn alloy target material (purity is 99.95%), sputter
-4Pa.At room temperature, feed argon gas, make that the interior sputtering pressure of sputtering chamber is 0.1Pa.In room temperature, under the argon atmosphere condition, utilize dc magnetron sputtering method to regulate DC power supply power and be 2000W, on Copper Foil, be deposited as the AlSn film, sedimentation time 30 minutes.
The membrane electrode of preparation is assembled into CR2016 type button cell by method noted earlier.Electro-chemical test shows that the initial charge capacity of the AlSn alloy firm electrode that foundation magnetically controlled sputter method of the present invention is prepared is 1156mAh/g, and discharge capacity is 728Ah/g, and 30 times circulation back capacity remains on 878.5mAh/g, and capability retention is 76%.
Embodiment 5
Employing is of a size of Φ 40mm * 3mm, element mass ratio Al: Sn=1: the interior initial gas pressure of sputtering chamber is 1.0 * 10 before 1 the AlSn alloy target material (purity is 99.95%), sputter
-4Pa.At room temperature, feed argon gas, make that the interior sputtering pressure of sputtering chamber is 10Pa.In room temperature, under the argon atmosphere condition, utilize radio frequency magnetron sputtering method to regulate radio-frequency power supply power 1500W, on Copper Foil, be deposited as the AlSn alloy firm, sputtering time 60 minutes.
The membrane electrode of preparation is assembled into CR2016 type button cell by method noted earlier.Electro-chemical test shows that the initial charge capacity of the AlSn alloy firm electrode that foundation magnetically controlled sputter method of the present invention is prepared is 1523mAh/g, and discharge capacity is 931Ah/g, and 30 times circulation back capacity remains on 1218mAh/g, and capability retention is 80%.
Embodiment 6
Employing is of a size of Φ 40mm * 3mm, element mass ratio Al: Sn=1: the interior initial gas pressure of sputtering chamber is 1.0 * 10 before 1 the AlSn alloy target material (purity is 99.95%), sputter
-4Pa.At room temperature, feed argon gas, make that the interior sputtering pressure of sputtering chamber is 1Pa.In room temperature, under the argon atmosphere condition, utilize dc magnetron sputtering method to regulate radio-frequency power supply power 500W, on Copper Foil, be deposited as the AlSn film, sputtering time 60 minutes.
The membrane electrode of preparation is assembled into CR2016 type button cell by method noted earlier.Electro-chemical test shows that the initial charge capacity of the AlSn alloy firm electrode that foundation magnetically controlled sputter method of the present invention is prepared is 1638mAh/g, and discharge capacity is 987Ah/g, and 30 times circulation back capacity remains on 1392mAh/g, and capability retention is 85%.
Embodiment 7
Employing is of a size of Φ 40mm * 3mm, element mass ratio Al: Sn=1: the interior initial gas pressure of sputtering chamber is 1.0 * 10 before 1 the AlSn alloy target material (purity is 99.95%), sputter
-4Pa.At room temperature, feed argon gas, make that the interior sputtering pressure of sputtering chamber is 5Pa.In room temperature, under the argon atmosphere condition, utilize radio frequency magnetron sputtering method to regulate power 1000W, on Copper Foil, be deposited as the AlSn film, sputtering time 30 minutes.
The membrane electrode of preparation is assembled into CR2016 type button cell by method noted earlier.Electro-chemical test shows that the initial charge capacity of the AlSn alloy firm electrode that foundation magnetically controlled sputter method of the present invention is prepared is 1596mAh/g, and discharge capacity is 1023Ah/g, and 30 times circulation back capacity remains on 1420.4mAh/g, and capability retention is 89%.
The chemical property that the foregoing description is recorded is listed in the table below:
| The embodiment numbering | Target composition (Al: Sn) | Sputtering technology | Initial charge capacity mAh/g | Discharge capacity mAh/g first | 30 circulation volume mAh/ |
30 circulation volume conservation rate/% |
| 1 | Sn | Radio frequency, 200W, 3.0Pa, 10 minutes | 660 | 570 | 550 | 83 |
| 2 | Sn | Direct current, 10W, 0.1Pa, 30 minutes | 781 | 500 | 100 | 13 |
| 3 | AlSn (1∶3) | Radio frequency, 200W, 3.0Pa, 10 minutes | 905 | 698 | 768 | 85 |
| 4 | AlSn (1∶3) | Direct current, 2000W, 0.1Pa, 30 minutes | 1156 | 728 | 878.5 | 76 |
| 5 | AlSn (1∶1) | Radio frequency, 1500W, 10Pa, 60 minutes | 1523 | 931 | 1218 | 80 |
| 6 | AlSn (1∶1) | Radio frequency, 500W, 1Pa, 60 minutes | 1638 | 987 | 1392 | 85 |
| 7 | AlSn (3∶1) | Radio frequency, 1000W, 5Pa, 30 minutes | 1596 | 1023 | 1292 | 81 |
Comparing embodiment 1 and embodiment 3, under identical sputtering condition, the aluminium tin solid solution alloy membrane electrode that adopts alloy target material (containing 25wt%Al) to prepare has first charge-discharge capacity height, efficiency for charge-discharge height, advantages such as good cycle than pure Sn membrane electrode.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1, a kind of preparation method of aluminum-tin alloy film for lithium ionic cell negative electrode is characterized in that comprising the steps:
(1) selects for use as the substrate of the metal forming of membrane electrode collector, and carry out substrate and clean as magnetron sputtering;
(2) regulate sputtering chamber air pressure to 1.0 * 10
-3Pa or more than, feed inert gas then and regulate air pressure in 0.1～10Pa scope;
(3) magnetron sputtering prepares aluminum-tin alloy film, regulates sputtering power in 10W～5KW scope, and sedimentation time is in 10～60 minutes scopes.
2, the preparation method of aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 1 is characterized in that: the described metal forming as the membrane electrode collector of step (1) is Copper Foil or aluminium foil.
3, the preparation method of aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 1, it is characterized in that: in the step (3), described magnetron sputtering type is magnetically controlled DC sputtering or rf magnetron sputtering, the concrete operations mode is vertical sputter or cosputtering, and the target that vertical sputter is adopted is a mock silver target, and the mass percent of its aluminium is 25～75%; The target that cosputtering adopts is for being installed in two aluminium monomer target and tin monomer targets on the different target pedestals respectively.
4, the preparation method of aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 1 is characterized in that: the described inert gas of step (2) is an argon gas.
5, the preparation method of aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 1 is characterized in that: the air pressure of regulating behind the described feeding inert gas of step (2) is 3Pa.
6, the preparation method of aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 1 is characterized in that: the described sputtering power of step (3) is 10W～5KW scope.
7, the preparation method of aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 1, it is characterized in that: it is that the first concentration that places metal cleaner to prepare substrate is 3～10% solution immersion that substrate described in the step (1) is cleaned, put into the deionized water soaking and washing again, then substrate is carried out putting on the sputtering chamber substrate pedestal after the drying, at last substrate surface is carried out backwash and handle.
8, a kind of aluminum-tin alloy film for lithium ionic cell negative electrode by each described method preparation of claim 1～7, it is characterized in that: be made of the solid solution alloy material mock silver, the content of tin is 25～75% in the described mock silver, and all the other are aluminium.
9, aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 7 is characterized in that, the content of tin is 50% in the described aluminum-tin alloy film.
10, aluminum-tin alloy film for lithium ionic cell negative electrode according to claim 7 is characterized in that, described aluminum-tin alloy film thickness is 50～200 μ m.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074677A (en) * | 2010-12-16 | 2011-05-25 | 潘宇强 | Method for manufacturing mercury-free battery through magnetron sputtering of indium or tin on negative pole piece |
| CN102212789A (en) * | 2011-05-05 | 2011-10-12 | 电子科技大学 | Magnetron sputtering preparation method of tin titanium film cathode of lithium ion battery |
| CN103904300A (en) * | 2014-03-14 | 2014-07-02 | 南开大学 | Tin-based composite thin film material for lithium ion battery as well as preparation method and application of thin film material |
| CN106058152A (en) * | 2016-01-27 | 2016-10-26 | 万向A二三***有限公司 | Cu-doped SnOx negative electrode and preparation method thereof |
| CN110190240A (en) * | 2019-05-15 | 2019-08-30 | 桂林电子科技大学 | Compound oxidate for lithium film and the preparation method and application thereof |
| CN110380011A (en) * | 2019-08-08 | 2019-10-25 | 吉林大学 | Long-life hydrogen bearing alloy film/nickel foil combination electrode material integration system is standby |
| CN112159956A (en) * | 2020-08-31 | 2021-01-01 | 西安交通大学 | Island-shaped Al film with Cu foil as substrate and preparation method and application thereof |
| CN114824286A (en) * | 2022-05-09 | 2022-07-29 | 广东工业大学 | Al-V alloy film substrate material for sodium metal battery and preparation method and application thereof |
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2008
- 2008-06-10 CN CNA2008100286855A patent/CN101339989A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074677A (en) * | 2010-12-16 | 2011-05-25 | 潘宇强 | Method for manufacturing mercury-free battery through magnetron sputtering of indium or tin on negative pole piece |
| CN102212789A (en) * | 2011-05-05 | 2011-10-12 | 电子科技大学 | Magnetron sputtering preparation method of tin titanium film cathode of lithium ion battery |
| CN103904300A (en) * | 2014-03-14 | 2014-07-02 | 南开大学 | Tin-based composite thin film material for lithium ion battery as well as preparation method and application of thin film material |
| CN106058152A (en) * | 2016-01-27 | 2016-10-26 | 万向A二三***有限公司 | Cu-doped SnOx negative electrode and preparation method thereof |
| CN110190240A (en) * | 2019-05-15 | 2019-08-30 | 桂林电子科技大学 | Compound oxidate for lithium film and the preparation method and application thereof |
| CN110380011A (en) * | 2019-08-08 | 2019-10-25 | 吉林大学 | Long-life hydrogen bearing alloy film/nickel foil combination electrode material integration system is standby |
| CN112159956A (en) * | 2020-08-31 | 2021-01-01 | 西安交通大学 | Island-shaped Al film with Cu foil as substrate and preparation method and application thereof |
| CN114824286A (en) * | 2022-05-09 | 2022-07-29 | 广东工业大学 | Al-V alloy film substrate material for sodium metal battery and preparation method and application thereof |
| CN114824286B (en) * | 2022-05-09 | 2023-12-29 | 广东工业大学 | Al-V alloy film substrate material for sodium metal battery and preparation method and application thereof |
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Open date: 20090107 |