CN101349769A - Method for preparing ALON protection film for optical element - Google Patents
Method for preparing ALON protection film for optical element Download PDFInfo
- Publication number
- CN101349769A CN101349769A CNA2008102222133A CN200810222213A CN101349769A CN 101349769 A CN101349769 A CN 101349769A CN A2008102222133 A CNA2008102222133 A CN A2008102222133A CN 200810222213 A CN200810222213 A CN 200810222213A CN 101349769 A CN101349769 A CN 101349769A
- Authority
- CN
- China
- Prior art keywords
- gas
- alon
- optical element
- preparation
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a preparation method of AION protective films for optical elements, belonging to the film preparation technical field, which uses high-purity metal AI as target, Ar gas as working gas, N2 and O2 gas as reaction gas, uses reaction magnetic control splash technique to prepare AION films. The AION film has high transmittance and low absorption factor in wide waveband of 0.2 to 12um, high mechanical strength, rigidity, abrasion resistance, high chemical stability and corrosion resistance, which is suitable for the use as rigid protective film of military optical windows and the uses as moisture proof protective film and abrasion resistant film for general optical elements as prisms and lens.
Description
Technical field
The invention belongs to the film preparing technology field, particularly a kind of preparation method of ALON protection film for optical element.
Background technology
Material hardnesses such as ZnSe, ZnS, Ge are low; therefore optical element surface in working environment of being made by these materials is easily impaired and influence operate as normal; and the prism that the KCl plasma crystal is made, window etc. since in atmosphere deliquescence very easily, therefore all need be at the surface-coated diaphragm to guarantee normal use.
Desirable optical protection layer is visible except that having, near infrared, in infrared, the optical property such as the far infrared multiband is transparent, absorption coefficient is little, also should have physical strength height, hardness height, wear-resistant, chemical stability good, characteristics such as corrosion-resistant.DLC, Ge
1-xC
xFilm is the optical element diaphragm of using always, but since itself exist big such as stress, absorb big and drawbacks limit such as visible light wave range is opaque its range of application.
Al
2O
3Be a kind of optical thin film material commonly used, its physical strength height simultaneously, hardness height, stable chemical performance, as in mechanical industry often with Al
2O
3Film is as the instrument hard coat, but Al
2O
3Absorption coefficient at long wave band (8～12 μ m) is very big, so Al
2O
3Film generally only is used for 0.2～8 μ m.If the N atom can substitute for Al
2O
3Part of O atom in the structure, form AlON structure of the present invention, so along with the increase of N atom content, long wave absorbs and will significantly reduce, make the AlON film can be applied to 0.2～12 μ m broadband, but owing to the increase along with the N atom content, the film mechanical property also can descend gradually, therefore to adjust the O/N ratio according to request for utilization, reach the coupling of optical property and mechanical property.
Summary of the invention
The invention provides a kind of preparation method of ALON protection film for optical element, is target with high pure metal Al, and Ar gas is working gas, N
2Gas and O
2Gas is reacting gas, adopts reaction magnetocontrol sputtering technology to prepare the AlON film, it is characterized in that preparation process may further comprise the steps:
(1) the optical element substrate is placed on the chip bench, at first the vacuum chamber vacuum is evacuated to and is higher than 3 * 10
-3Pa is heated to room temperature～800C with matrix then;
(2) charge into Ar gas to vacuum chamber, keep vacuum at 0.1～0.5Pa, sputtering power 100～1000W cleaned 8-12 minute the bombardment of target surface;
(3) press N
2/ (N
2+ O
2)=0.05～0.95, (N
2+ O
2The proportional range of)/Ar=0.1～0.5 feeds Ar, N
2Gas and O
2The mixed gas of gas keeps sputtering power 50～300W, working vacuum 0.1～0.3Pa, and depositing Al ON film is until reaching required thickness;
(4) deposition is slowly reduced to room temperature with workpiece temperature, rate of temperature fall 30～100C/ hour after finishing in above-mentioned mixed gas.
Described magnetron sputtering technique is rf magnetron sputtering technology or magnetically controlled DC sputtering technology.
Thickness is by rate of sedimentation and sedimentation time control in the described magnetron sputtering technique deposition process.
The flow of described magnetron sputtering technique deposition process gas is controlled by mass-flow gas meter, and flow range is 5～200sccm.
Described optical element refers to optical system prism, lens and window, and its material comprises ZnS, ZnSe, Ge, Si, quartz glass, As
2S
3, KCl and CaF
2, it is shaped as plate shaped or spherical.
Described AlON diaphragm, the scope of N/ (N+O) atomic ratio is 5～95%, the long wave band absorptivity was little when wherein the N atom content was high, but mechanical property is relatively poor, better mechanical property when the O atom content is high, but the long wave band absorptivity is big, and through performance is relatively poor.。
Described AlON diaphragm is single face diaphragm or two-sided diaphragm.
Beneficial effect of the present invention is: the AlON film of preparation; in 0.2～12 μ m broadband scope, have high transmitance and low absorption coefficient; and physical strength height, hardness height, wear-resistant, chemical stability good, corrosion-resistant; be suitable for doing the hard coating of military optics window, also be suitable for doing the moisture-proof protective film of general optical element such as prism, lens etc. and the film that resistance to wears.
Description of drawings
Fig. 1 is the reaction magnetocontrol sputtering depositing device sketch of preparation AlON film.
Number in the figure:
The 1-AlON diaphragm; The 2-magnet arrangement; The 3-Al target; The 4-vacuum chamber; The 5-air intake opening; The 6-gas outlet; The 7-shielding power supply; The 8-chip bench; The 9-well heater; 10-optical element substrate.
Embodiment
The invention provides a kind of preparation method of ALON protection film for optical element, the present invention is described further below in conjunction with description of drawings and embodiment.
Fig. 1 is the reaction magnetocontrol sputtering depositing device sketch of preparation AlON film.Be provided with air intake opening 5 and gas outlet 6 in vacuum chamber 4 bottoms, vacuum chamber is provided with shielding power supply 7, be provided with chip bench 8 in vacuum chamber 4 inside, chip bench 8 inside are provided with well heater 9, chip bench 8 is used for placing optical element substrate 10, on chip bench 8, be provided with magnet arrangement 2, be fixed with Al target 3 on the magnet arrangement.
Embodiment 1:
(1) by the above-mentioned steps erecting equipment, optical element substrate 10 is placed on the chip bench 8, the material of optical element substrate 10 is KCl, at first vacuum chamber 4 vacuum is evacuated to be higher than 3 * 10
-3Pa adopts the resistance-type type of heating then, and optical element substrate 10 is heated to 200C;
(2) charge into Ar gas to vacuum chamber 4, keep vacuum, adopt rf magnetron sputtering technology at 0.2Pa, sputtering power 300W, 3 surface bombardments were cleaned 10 minutes to the Al target;
(3) press N
2/ (N
2+ O
2)=0.5, (N
2+ O
2The ratio of)/Ar=0.2 feeds Ar, N
2Gas and O
2The mixed gas of gas, working vacuum 0.2Pa adopts rf magnetron sputtering technology, keeps sputtering power 100W, and control rate of sedimentation and sedimentation time are at the thick plate AlON diaphragm 1 of the two-sided plating 100nm of optical base-substrate 10;
(4) deposition is slowly reduced to room temperature with workpiece temperature, rate of temperature fall 30C/ hour after finishing in above-mentioned mixed gas.
The flow of magnetron sputtering technique deposition process gas is controlled by mass-flow gas meter, and flow range is 5～200sccm.
The KCl optical element that is coated with the AlON diaphragm that makes is carried out Chinese People's Anti-Japanese Military and Political College's gas deliquescence test, and test findings shows at wet environment placed three months, and it is transparent that crystal still keeps, no deliquescence phenomenon.
Embodiment 2:
(1) by the above-mentioned steps erecting equipment, optical element substrate 10 is placed on the chip bench 8, the material of optical element substrate 10 is ZnSe, at first vacuum chamber 4 vacuum is evacuated to be higher than 3 * 10
-3Pa adopts the resistance-type type of heating then, and optical element substrate 10 is heated to 500C;
(2) charge into Ar gas to vacuum chamber 4, keep vacuum, adopt rf magnetron sputtering technology at 0.3Pa, sputtering power 100W, 3 surface bombardments were cleaned 10 minutes to the Al target;
(3) press N
2/ (N
2+ O
2)=0.6, (N
2+ O
2The ratio of)/Ar=0.2 feeds Ar, N
2Gas and O
2The mixed gas of gas, working vacuum 0.2Pa adopts rf magnetron sputtering technology, keeps sputtering power 200W, and control rate of sedimentation and sedimentation time are at the thick ball crown type AlON of the two-sided plating 800nm of optical base-substrate 10 diaphragm 1;
(4) deposition is slowly reduced to room temperature with workpiece temperature, rate of temperature fall 50C/ hour after finishing in above-mentioned mixed gas.
The flow of magnetron sputtering technique deposition process gas is controlled by mass-flow gas meter, and flow range is 5～200sccm.
The ZnSe optical element that is coated with the AlON diaphragm that makes is tested, in its optical absorption of 0.5～12 mu m waveband less than 3%; Adopt the nano-probe indentation method to test its microhardness greater than 20Gpa, the hardness of ZnSe matrix is about 2～3GPa.
Embodiment 3:
(1) by the above-mentioned steps erecting equipment, optical element substrate 10 is placed on the chip bench 8, the material of optical element substrate 10 is Ge, at first vacuum chamber 4 vacuum is evacuated to be higher than 3 * 10
-3Pa adopts the resistance-type type of heating then, and optical element substrate 10 is heated to 400C;
(2) charge into Ar gas to vacuum chamber 4, keep vacuum, adopt magnetically controlled DC sputtering technology at 0.1Pa, sputtering power 500W, 3 surface bombardments were cleaned 8 minutes to the Al target;
(3) press N
2/ (N
2+ O
2)=0.2, (N
2+ O
2The ratio of)/Ar=0.3 feeds Ar, N
2Gas and O
2The mixed gas of gas, working vacuum 0.2Pa adopts magnetically controlled DC sputtering technology, keeps sputtering power 50W, and control rate of sedimentation and sedimentation time are at the thick plate AlON diaphragm 1 of the two-sided plating 80nm of optical base-substrate 10;
(4) deposition is slowly reduced to room temperature with workpiece temperature, rate of temperature fall 70C/ hour after finishing in above-mentioned mixed gas.
The flow of magnetron sputtering technique deposition process gas is controlled by mass-flow gas meter, and flow range is 5～200sccm.
The Ge optical element that is coated with the AlON diaphragm that makes is tested, in its optical absorption of 3～12 mu m wavebands less than 3%; Adopt the nano-probe indentation method to test its microhardness greater than 20Gpa, the hardness of Ge matrix is about 10～12GPa.
Above-described embodiment is a preferable embodiment of the present invention, and those skilled in the art can make various modifications within the scope of the appended claims.
Claims (7)
1. the preparation method of an ALON protection film for optical element is a target with high pure metal Al, and Ar gas is working gas, N
2Gas and O
2Gas is reacting gas, adopts reaction magnetocontrol sputtering technology to prepare the AlON film, it is characterized in that preparation process may further comprise the steps:
(1) the optical element matrix is placed on the chip bench, at first the vacuum chamber vacuum is evacuated to and is higher than 3 * 10
-3Pa is heated to matrix room temperature～800 ℃ then;
(2) charge into Ar gas to vacuum chamber, keep vacuum at 0.1～0.5Pa, sputtering power 100～1000W cleaned 8-12 minute the bombardment of target surface;
(3) press N
2/ (N
2+ O
2)=0.05～0.95, (N
2+ O
2The proportional range of)/Ar=0.1～0.5 feeds Ar, N
2Gas and O
2The mixed gas of gas keeps sputtering power 50～300W, working vacuum 0.1～0.3Pa, depositing Al ON film;
(4) deposition is slowly reduced to room temperature with workpiece temperature, 30～100 ℃/hour of rate of temperature fall after finishing in above-mentioned mixed gas.
2. the preparation method of ALON protection film for optical element according to claim 1 is characterized in that, described magnetron sputtering technique is rf magnetron sputtering technology or magnetically controlled DC sputtering technology.
3. the preparation method of ALON protection film for optical element according to claim 1 is characterized in that, thickness is by rate of sedimentation and sedimentation time control in the described magnetron sputtering technique deposition process.
4. the preparation method of ALON protection film for optical element according to claim 1 is characterized in that, the flow of described magnetron sputtering technique deposition process gas is controlled by mass-flow gas meter, and flow range is 5～200sccm.
5. the preparation method of ALON protection film for optical element according to claim 1 is characterized in that, described optical element refers to optical system prism, lens and window, and its material comprises ZnS, ZnSe, Ge, Si, quartz glass, As
2S
3, KCl and CaF
2, it is shaped as plate shaped or spherical.
6. the preparation method of ALON protection film for optical element according to claim 1 is characterized in that, described AlON diaphragm, and the scope of N/ (N+O) atomic ratio is 5～95%.
7. the preparation method of ALON protection film for optical element according to claim 1 is characterized in that, described AlON diaphragm is single face diaphragm or two-sided diaphragm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102222133A CN101349769A (en) | 2008-09-11 | 2008-09-11 | Method for preparing ALON protection film for optical element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102222133A CN101349769A (en) | 2008-09-11 | 2008-09-11 | Method for preparing ALON protection film for optical element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101349769A true CN101349769A (en) | 2009-01-21 |
Family
ID=40268623
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008102222133A Pending CN101349769A (en) | 2008-09-11 | 2008-09-11 | Method for preparing ALON protection film for optical element |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101349769A (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433537A (en) * | 2010-09-29 | 2012-05-02 | 鸿富锦精密工业（深圳）有限公司 | Coated part and manufacturing method thereof |
| CN102650039A (en) * | 2011-02-28 | 2012-08-29 | 鸿富锦精密工业（深圳）有限公司 | Aluminum or aluminum alloy shell and method for producing same |
| CN102677007A (en) * | 2011-03-14 | 2012-09-19 | 鸿富锦精密工业（深圳）有限公司 | Aluminum or aluminum alloy shell and manufacturing method thereof |
| CN102676989A (en) * | 2011-03-11 | 2012-09-19 | 鸿富锦精密工业（深圳）有限公司 | Film coating part and preparation method thereof |
| US9079802B2 (en) | 2013-05-07 | 2015-07-14 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US9110230B2 (en) | 2013-05-07 | 2015-08-18 | Corning Incorporated | Scratch-resistant articles with retained optical properties |
| US9335444B2 (en) | 2014-05-12 | 2016-05-10 | Corning Incorporated | Durable and scratch-resistant anti-reflective articles |
| US9366784B2 (en) | 2013-05-07 | 2016-06-14 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US9684097B2 (en) | 2013-05-07 | 2017-06-20 | Corning Incorporated | Scratch-resistant articles with retained optical properties |
| US9703011B2 (en) | 2013-05-07 | 2017-07-11 | Corning Incorporated | Scratch-resistant articles with a gradient layer |
| US9790593B2 (en) | 2014-08-01 | 2017-10-17 | Corning Incorporated | Scratch-resistant materials and articles including the same |
| US10948629B2 (en) | 2018-08-17 | 2021-03-16 | Corning Incorporated | Inorganic oxide articles with thin, durable anti-reflective structures |
| US11002885B2 (en) | 2015-09-14 | 2021-05-11 | Corning Incorporated | Scratch-resistant anti-reflective articles |
| US11267973B2 (en) | 2014-05-12 | 2022-03-08 | Corning Incorporated | Durable anti-reflective articles |
| CN116161959A (en) * | 2022-12-07 | 2023-05-26 | 河南鎏溪科技有限公司 | Method for preparing wide-spectrum high-strength zinc sulfide optical material |
-
2008
- 2008-09-11 CN CNA2008102222133A patent/CN101349769A/en active Pending
Cited By (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433537A (en) * | 2010-09-29 | 2012-05-02 | 鸿富锦精密工业（深圳）有限公司 | Coated part and manufacturing method thereof |
| CN102650039A (en) * | 2011-02-28 | 2012-08-29 | 鸿富锦精密工业（深圳）有限公司 | Aluminum or aluminum alloy shell and method for producing same |
| CN102676989A (en) * | 2011-03-11 | 2012-09-19 | 鸿富锦精密工业（深圳）有限公司 | Film coating part and preparation method thereof |
| CN102677007A (en) * | 2011-03-14 | 2012-09-19 | 鸿富锦精密工业（深圳）有限公司 | Aluminum or aluminum alloy shell and manufacturing method thereof |
| US10444408B2 (en) | 2013-05-07 | 2019-10-15 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US9079802B2 (en) | 2013-05-07 | 2015-07-14 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US11714213B2 (en) | 2013-05-07 | 2023-08-01 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US9359261B2 (en) | 2013-05-07 | 2016-06-07 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US9366784B2 (en) | 2013-05-07 | 2016-06-14 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US9684097B2 (en) | 2013-05-07 | 2017-06-20 | Corning Incorporated | Scratch-resistant articles with retained optical properties |
| US9703011B2 (en) | 2013-05-07 | 2017-07-11 | Corning Incorporated | Scratch-resistant articles with a gradient layer |
| US11667565B2 (en) | 2013-05-07 | 2023-06-06 | Corning Incorporated | Scratch-resistant laminates with retained optical properties |
| US9110230B2 (en) | 2013-05-07 | 2015-08-18 | Corning Incorporated | Scratch-resistant articles with retained optical properties |
| US11231526B2 (en) | 2013-05-07 | 2022-01-25 | Corning Incorporated | Low-color scratch-resistant articles with a multilayer optical film |
| US11267973B2 (en) | 2014-05-12 | 2022-03-08 | Corning Incorporated | Durable anti-reflective articles |
| US9726786B2 (en) | 2014-05-12 | 2017-08-08 | Corning Incorporated | Durable and scratch-resistant anti-reflective articles |
| US9335444B2 (en) | 2014-05-12 | 2016-05-10 | Corning Incorporated | Durable and scratch-resistant anti-reflective articles |
| US10436945B2 (en) | 2014-05-12 | 2019-10-08 | Corning Incorporated | Durable and scratch-resistant anti-reflective articles |
| US10995404B2 (en) | 2014-08-01 | 2021-05-04 | Corning Incorporated | Scratch-resistant materials and articles including the same |
| US10837103B2 (en) | 2014-08-01 | 2020-11-17 | Corning Incorporated | Scratch-resistant materials and articles including the same |
| US9790593B2 (en) | 2014-08-01 | 2017-10-17 | Corning Incorporated | Scratch-resistant materials and articles including the same |
| US11698475B2 (en) | 2015-09-14 | 2023-07-11 | Corning Incorporated | Scratch-resistant anti-reflective articles |
| US11002885B2 (en) | 2015-09-14 | 2021-05-11 | Corning Incorporated | Scratch-resistant anti-reflective articles |
| US11567237B2 (en) | 2018-08-17 | 2023-01-31 | Corning Incorporated | Inorganic oxide articles with thin, durable anti-reflective structures |
| US10948629B2 (en) | 2018-08-17 | 2021-03-16 | Corning Incorporated | Inorganic oxide articles with thin, durable anti-reflective structures |
| US11906699B2 (en) | 2018-08-17 | 2024-02-20 | Corning Incorporated | Inorganic oxide articles with thin, durable anti reflective structures |
| CN116161959A (en) * | 2022-12-07 | 2023-05-26 | 河南鎏溪科技有限公司 | Method for preparing wide-spectrum high-strength zinc sulfide optical material |
| CN116161959B (en) * | 2022-12-07 | 2023-12-08 | 河南鎏溪科技有限公司 | Method for preparing wide-spectrum high-strength zinc sulfide optical material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101349769A (en) | Method for preparing ALON protection film for optical element | |
| Chen et al. | High-performance transparent barrier films of SiO x∕ SiN x stacks on flexible polymer substrates | |
| JP4033286B2 (en) | High refractive index dielectric film and manufacturing method thereof | |
| CN104977632A (en) | Hard anti-reflection coating layer and manufacture and use thereof | |
| CN100485082C (en) | Method for preparing ZnO:Al transparent conductive film by direct magnetic control co-sputtering method | |
| CN101660117B (en) | Solar selective absorbing coating and preparation method thereof | |
| CN101465172A (en) | Transparent conductive film with compound structure and preparation method thereof | |
| MXPA01002967A (en) | Heat-resistant reflecting layer, laminate formed of the reflecting layer, and liquid crystal display device having the reflecting layer or the laminate. | |
| CN113105214B (en) | Ceramic material with low infrared emissivity in middle and far infrared bands and preparation method and application thereof | |
| Guo et al. | Past achievements and future challenges in the development of infrared antireflective and protective coatings | |
| CN111443522A (en) | Light guide plate with reflection function, preparation method thereof and backlight module | |
| CN101058871A (en) | Method of preparing HfON protective film for optical element | |
| CN106222618B (en) | The preparation method of SnO2 doping ZnO sputtering target material | |
| CN106772730B (en) | A kind of durable multi-layer film material of high infrared reflection based on hafnium nitride | |
| CN113652640B (en) | Method for preparing nano composite phase vanadium oxide flexible film by sputtering and film | |
| CN105223634A (en) | The high low stress membrane and preparation method thereof thoroughly of a kind of 2.5-10um spectral coverage | |
| Panprom et al. | Growth of Ag/SnO2 thin film by DC magnetron sputtering deposition intended for low emissivity application | |
| CN1221016C (en) | Method for preparing low stress composite medium film of non-refrigeration infrared focal plane device | |
| CN103572238A (en) | Preparation method of double-frosted surface ZnO-based film | |
| Lai et al. | Effect of oxygen flow rate on the properties of SiOx films deposited by reactive magnetron sputtering | |
| Kim | Characterization of a crystallized ZnO/CuSn/ZnO multilayer film deposited with low temperature magnetron sputtering | |
| TWI700383B (en) | Composite metal oxide target and composite metal oxide film formed from the composite metal oxide target | |
| Tripathi et al. | Refractive index tailoring of morphology engineered SiO2 thin films by collimated glancing angle RF magnetron sputtering | |
| Mertin et al. | Coloured coatings for glazing of active solar thermal façades by reactive magnetron sputtering | |
| Zoubian et al. | Potential of TaOxNy thin films deposited by reactive sputtering as antireflective coatings: composition and optical properties |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090121 |