CN102409293A - Preparation method of alumina film - Google Patents
Preparation method of alumina film Download PDFInfo
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- CN102409293A CN102409293A CN2011103963746A CN201110396374A CN102409293A CN 102409293 A CN102409293 A CN 102409293A CN 2011103963746 A CN2011103963746 A CN 2011103963746A CN 201110396374 A CN201110396374 A CN 201110396374A CN 102409293 A CN102409293 A CN 102409293A
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Abstract
The invention relates to a preparation method of an alumina film and belongs to the technical field of surface engineering. The method comprises the following steps: putting a flexible polymer film base in a vacuum chamber, and vacuumizing the vacuum chamber till pressure in the vacuum chamber is less than or equal to 2.0*10<-3> Pa; carrying out argon ion bombardment on the base with an ion source, thereby improving the adhesion of a plated film layer, wherein the flow of argon is 15sccm, the discharge voltage of an ion beam is 280V, and the current of the ion beam is 1A; and depositing an alumina film by using an oxygen ion beam aided impulse reaction magnetron sputtering technology, wherein a target source is an aluminum target. In the preparation process, the base is always maintained at room temperature, thus the damage of high temperature to the flexible polymer film base can be avoided; and the rapid deposition of the high-quality alumina film can be realized on the flexible polymer base.
Description
Technical field
The present invention relates to a kind of preparation method of aluminum oxide film, belong to field of surface engineering technique.
Background technology
Al
2O
3Film is a kind of important function thin-film material; Since have that higher dielectric constant, high heat conductance, radioresistance injury reinforcing ability are strong, alkali resistant iontophoretic injection ability is strong and in very wide wavelength region physics, the chemical property of many excellences such as transparent, it is had a wide range of applications in various fields such as microelectronic device, electroluminescent device, fiber waveguide device and corrosion-resistant coatings.
Al
2O
3The preparation method of film has a variety of, as: magnetron sputtering, ion beam assisted depositing (IBAD), pulsed laser deposition (PLD), electro beam physics vapour deposition, chemical vapor deposition (CVD), ald (ALD) and sol-gel (Sol-Gel) etc.The pulse reaction magnetron sputtering be because of can keeping the homogeneity of film in the big area scope, and can solve preparation deielectric-coating such as Al effectively
2O
3Discharge effect during film becomes the focus of research.But the pulse reaction magnetically controlled sputter method prepares Al
2O
3Receive the influence of hysteresis phenomenon during film, do not heat and target is in the Al that can't obtain complete stoichiometric ratio under the situation of metallic state in substrate
2O
3Film is only adopting substrate heating (more than 500 ℃) or under the situation that target is poisoned, is being coated with pure Al
2O
3Film can't be realized low temperature, the fast deposition of film, and this has limited the preparation and the application of compound film in the flexible polymer substrate.Ion beam assisted deposition can be under low underlayer temperature the synthetic compound film, prepared film has characteristics such as film substrate bond strength height, density of film are big, all is widely used aspect preparing at structural membrane material and film material with function.In traditional I BAD method, the auxiliary electron-beam evaporation method of Ar ion is generally adopted in the preparation of sull.The sedimentation rate of this method is low, thin film composition is restive.Therefore, be badly in need of a kind of new preparation method of exploitation, reduce depositing temperature, improve sedimentation rate.
Summary of the invention
The objective of the invention is that high poisoning causes the low problem of sedimentation rate with metal targets in order to overcome in the prior art deposited aluminum oxide thin film temperature; And a kind of high quality aluminum oxide thin film low temperature, quick method of preparation of realizing be provided; Substrate that this method is selected for use can be applied to flexible polymer film, expands the range of application of aluminum oxide film greatly.
A kind of preparation method of aluminum oxide film said method comprising the steps of:
(1) the flexible polymer film substrate is placed in the Vakuumkammer, Vakuumkammer is evacuated to pressure in the Vakuumkammer≤2.0 * 10
-3Pa;
(2) with ion source argon ion bombardment is carried out in substrate and handle, improve the sticking power that is coated with rete; Wherein argon flow amount is 15sccm, and the ionic fluid sparking voltage is 280V, and ion beam current is 1A;
(3) adopt oxygen ion beam satellite pulse reaction magnetocontrol sputtering deposition techniques aluminum oxide film, the target source is the aluminium target, and processing parameter is following:
The working gas argon flow amount is 8～15sccm;
Ion source carrier of oxygen integration amount is 86%～89%;
Operating air pressure 0.3～0.5Pa;
Ion source voltage 300～500V;
Ion beam current 0.85～1A;
Al target sputtering power 400～600W;
Sputter pulse-repetition 20～25KHz;
Wherein, said argon gas and oxygen are that purity is 99.99% high-purity gas.
Preferred said substrate is that thickness is 25～125 microns a polyimide film.
Beneficial effect
The present invention is through oxygen ion beam satellite pulse reaction magnetocontrol sputtering technology; Can utilize high chemically reactive of oxonium ion and ionic kinetic energy to surface adsorption, dissociate and the enhancing of diffusion and reduce depositing temperature; Solve the target intoxicating phenomenon simultaneously and improve sedimentation rate, and then reach the low temperature of aluminum oxide film, preparation fast.Substrate keeps room temperature always in the deposition process, has avoided the infringement of high temperature to the flexible polymer film substrate.Can in the flexible polymer substrate, realize the fast deposition of high quality aluminum oxide film, be equipped with corresponding flexible substrate winding apparatus, can realize big area serialization deposition.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is carried out detailed explanation.
Embodiment
A kind of preparation method of aluminum oxide film said method comprising the steps of:
(1) 50 μ m are thick Kapton substrate is placed in the Vakuumkammer, Vakuumkammer is evacuated to pressure is 2.0 * 10 in the Vakuumkammer
-3Pa;
(2) with ion source argon ion bombardment is carried out in substrate and handle, improve the sticking power that is coated with rete; Wherein argon flow amount is 15sccm, and the ionic fluid sparking voltage is 280V, and ion beam current is 1A;
(3) adopt oxygen ion beam satellite pulse reaction magnetocontrol sputtering deposition techniques aluminum oxide film, process and processing parameter are following:
The metallic aluminium target purity that sputter is used is 99.99%; Target is a long strip shape, and area is 560mm * 80mm, and the distance between target and the substrate is 100mm; The sputter working gas is the argon gas and the oxygen of purity 99.99%; The oxygen volume accounts for 86%～89%, and shielding power supply is the pulse power that U.S. AE PLC produces, the highest 5kW of output rating.The oxygen argon mixture gas feeds in the ion source, and the oxonium ion of generation makes aluminium oxidation in substrate of sputter prepare aluminum oxide film.
Metallic aluminium target as sputter working gas argon gas leads to the magnetic controlling target surface through aluminum pipe, and using mass flowmeter to regulate argon flow amount is 8～15sccm, opens the pulse shielding power supply, and voltage is applied between metal A l target and the Vakuumkammer.The oxygen argon mixture gas that feeds in the ion source is controlled through mass flowmeter, and oxonium ion makes the metallics oxidation of sputter, and argon ion is used for further improving film quality to the bombardment of film, improves its performance, realizes being coated with of high quality aluminum oxide film.Substrate all is in the nature temperature rising state in the film deposition process, not heating in addition.
The condition of a comparatively preferred treatment technology is following in this step: ion source voltage 300V, ion beam current 0.85A, ion source oxygen component 86%, magnetic controlling target sputtering power 600V, operating air pressure 0.45Pa.Other pulse reaction magnetron sputtering parameter is: argon flow amount 15sccm, pulse-repetition 25kHz, positive pulse amplitude 300V, positive pulse width 1 μ s.Deposition 30min, prepared membrane structure is fine and close, meets stoichiometric ratio, and sedimentation rate has reached 72.4nm/min.
In sum, more than being merely preferred embodiment of the present invention, is not to be used to limit protection scope of the present invention.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the preparation method of an aluminum oxide film is characterized in that: said method comprising the steps of:
(1) the flexible polymer film substrate is placed in the Vakuumkammer, Vakuumkammer is evacuated to pressure in the Vakuumkammer≤2.0 * 10
-3Pa;
(2) with ion source argon ion bombardment being carried out in substrate handles; Wherein argon flow amount is 15sccm, and the ionic fluid sparking voltage is 280V, and ion beam current is 1A;
(3) adopt oxygen ion beam satellite pulse reaction magnetocontrol sputtering deposition techniques aluminum oxide film, the target source is the aluminium target, and processing parameter is following:
The working gas argon flow amount is 8～15sccm;
Ion source carrier of oxygen integration amount is 86%～89%;
Operating air pressure 0.3～0.5Pa;
Ion source voltage 300～500V;
Ion beam current 0.85～1A;
Al target sputtering power 400～600W;
Sputter pulse-repetition 20～25KHz;
Wherein, said argon gas and oxygen are that purity is 99.99% high-purity gas.
2. the preparation method of a kind of aluminum oxide film according to claim 1, it is characterized in that: said substrate is that thickness is 25～125 microns a polyimide film.
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|---|---|---|---|
| CN2011103963746A CN102409293A (en) | 2011-12-04 | 2011-12-04 | Preparation method of alumina film |
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|---|---|---|---|
| CN2011103963746A CN102409293A (en) | 2011-12-04 | 2011-12-04 | Preparation method of alumina film |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104183203A (en) * | 2014-08-07 | 2014-12-03 | 北京空间飞行器总体设计部 | Instrument identifier for deep space probe |
| CN104561900A (en) * | 2014-12-16 | 2015-04-29 | 兰州空间技术物理研究所 | Method for preparing low-absorption rate silicon oxide film |
| CN104962873A (en) * | 2015-07-17 | 2015-10-07 | 广东工业大学 | Method for preparing polycrystalline aluminum oxide hard coating |
| WO2016037590A1 (en) * | 2014-09-12 | 2016-03-17 | Hong Kong Baptist University | Sapphire thin film coated flexible substrate |
| CN108603288A (en) * | 2015-11-16 | 2018-09-28 | 库伯斯股份有限公司 | The method for producing aluminium oxide and/or aluminium nitride |
| CN111621756A (en) * | 2020-03-27 | 2020-09-04 | 中国科学院力学研究所 | Method for preparing crystalline transparent alumina film by room temperature sputtering |
| CN111996502A (en) * | 2020-08-31 | 2020-11-27 | 中国科学院上海光学精密机械研究所 | Nickel-chromium alloy surface coating structure and preparation method thereof |
| US11028471B2 (en) | 2011-12-23 | 2021-06-08 | Hkbu R&D Licensing Limited | Sapphire thin film coated substrate |
| CN113025959A (en) * | 2021-03-07 | 2021-06-25 | 中国航空制造技术研究院 | Method for preparing hafnium oxide-based ferroelectric film at low temperature by ion beam assisted magnetron sputtering deposition |
| CN113322442A (en) * | 2021-06-03 | 2021-08-31 | 哈尔滨工业大学 | Preparation method of gamma-aluminum oxide film with excellent atomic oxygen resistance |
| CN114177783A (en) * | 2021-10-22 | 2022-03-15 | 广东电网有限责任公司广州供电局 | Filter membrane for transformer oil and preparation method |
| CN115142033A (en) * | 2022-05-06 | 2022-10-04 | 北京大学深圳研究生院 | Non-stoichiometric alumina material and preparation method thereof |
| US11535926B2 (en) | 2011-12-23 | 2022-12-27 | Hkbu R&D Licensing Limited | Sapphire thin film coated substrate |
| US11713503B2 (en) | 2011-12-23 | 2023-08-01 | Hong Kong Baptist University | Sapphire coated substrate with a flexible, anti-scratch and multi-layer coating |
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2011
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Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11535926B2 (en) | 2011-12-23 | 2022-12-27 | Hkbu R&D Licensing Limited | Sapphire thin film coated substrate |
| US11028471B2 (en) | 2011-12-23 | 2021-06-08 | Hkbu R&D Licensing Limited | Sapphire thin film coated substrate |
| US11713503B2 (en) | 2011-12-23 | 2023-08-01 | Hong Kong Baptist University | Sapphire coated substrate with a flexible, anti-scratch and multi-layer coating |
| CN104183203A (en) * | 2014-08-07 | 2014-12-03 | 北京空间飞行器总体设计部 | Instrument identifier for deep space probe |
| CN104183203B (en) * | 2014-08-07 | 2015-06-10 | 北京空间飞行器总体设计部 | Instrument identifier for deep space probe |
| WO2016037590A1 (en) * | 2014-09-12 | 2016-03-17 | Hong Kong Baptist University | Sapphire thin film coated flexible substrate |
| TWI574840B (en) * | 2014-09-12 | 2017-03-21 | 香港浸會大學 | Sapphire thin film coated flexible substrate |
| CN107109623A (en) * | 2014-09-12 | 2017-08-29 | 香港浸会大学 | The flexible substrate coated through sapphire thin film |
| CN107109623B (en) * | 2014-09-12 | 2019-02-15 | 香港浸会大学 | The flexible substrate coated through sapphire thin film |
| CN104561900A (en) * | 2014-12-16 | 2015-04-29 | 兰州空间技术物理研究所 | Method for preparing low-absorption rate silicon oxide film |
| CN104962873A (en) * | 2015-07-17 | 2015-10-07 | 广东工业大学 | Method for preparing polycrystalline aluminum oxide hard coating |
| CN108603288B (en) * | 2015-11-16 | 2020-01-14 | 库伯斯股份有限公司 | Method for producing aluminum oxide and/or aluminum nitride |
| CN108603288A (en) * | 2015-11-16 | 2018-09-28 | 库伯斯股份有限公司 | The method for producing aluminium oxide and/or aluminium nitride |
| CN111621756A (en) * | 2020-03-27 | 2020-09-04 | 中国科学院力学研究所 | Method for preparing crystalline transparent alumina film by room temperature sputtering |
| CN111621756B (en) * | 2020-03-27 | 2021-12-24 | 中国科学院力学研究所 | Method for preparing crystalline transparent alumina film by room temperature sputtering |
| CN111996502B (en) * | 2020-08-31 | 2022-09-02 | 中国科学院上海光学精密机械研究所 | Nickel-chromium alloy surface coating structure and preparation method thereof |
| CN111996502A (en) * | 2020-08-31 | 2020-11-27 | 中国科学院上海光学精密机械研究所 | Nickel-chromium alloy surface coating structure and preparation method thereof |
| CN113025959A (en) * | 2021-03-07 | 2021-06-25 | 中国航空制造技术研究院 | Method for preparing hafnium oxide-based ferroelectric film at low temperature by ion beam assisted magnetron sputtering deposition |
| CN113322442A (en) * | 2021-06-03 | 2021-08-31 | 哈尔滨工业大学 | Preparation method of gamma-aluminum oxide film with excellent atomic oxygen resistance |
| CN114177783A (en) * | 2021-10-22 | 2022-03-15 | 广东电网有限责任公司广州供电局 | Filter membrane for transformer oil and preparation method |
| CN115142033A (en) * | 2022-05-06 | 2022-10-04 | 北京大学深圳研究生院 | Non-stoichiometric alumina material and preparation method thereof |
| CN115142033B (en) * | 2022-05-06 | 2024-06-11 | 北京大学深圳研究生院 | Non-stoichiometric alumina material and preparation method thereof |
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Application publication date: 20120411 |