CN112342506A - Preparation method of low-stress low-absorption oxide film - Google Patents
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000010408 film Substances 0.000 claims abstract description 105
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 87
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000001659 ion-beam spectroscopy Methods 0.000 claims abstract description 27
- 238000000151 deposition Methods 0.000 claims abstract description 24
- 230000008021 deposition Effects 0.000 claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 16
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 9
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 54
- 229910052906 cristobalite Inorganic materials 0.000 claims description 54
- 229910052682 stishovite Inorganic materials 0.000 claims description 54
- 229910052905 tridymite Inorganic materials 0.000 claims description 54
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 24
- 239000001301 oxygen Substances 0.000 claims description 24
- 229910052760 oxygen Inorganic materials 0.000 claims description 24
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 11
- 239000010409 thin film Substances 0.000 claims description 10
- 238000004364 calculation method Methods 0.000 claims description 9
- 239000013077 target material Substances 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000005350 fused silica glass Substances 0.000 claims description 8
- 238000000411 transmission spectrum Methods 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 230000008033 biological extinction Effects 0.000 claims description 5
- 239000002019 doping agent Substances 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000012788 optical film Substances 0.000 abstract description 5
- 238000001228 spectrum Methods 0.000 abstract description 5
- 238000005477 sputtering target Methods 0.000 abstract 1
- 238000009501 film coating Methods 0.000 description 5
- 239000007888 film coating Substances 0.000 description 4
- 238000010884 ion-beam technique Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/3442—Applying energy to the substrate during sputtering using an ion beam
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
- C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
- C23C14/547—Controlling the film thickness or evaporation rate using measurement on deposited material using optical methods
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Abstract
The invention belongs to the technical field of optical films, and discloses a preparation method of a low-stress low-absorption oxide film, which adopts a dual-ion beam sputtering deposition technology, takes a tantalum target and a silicon dioxide target as sputtering targets, and can realize Ta with stress of-120 MPa and absorption loss of 8ppm by selecting proper dual-ion beam sputtering preparation process parameters2O5Film and SiO with stress of-80 MPa and absorption loss of 4ppm2And (3) preparing a film. The result shows that the method of the invention can obtain the oxide film with low stress and low absorption, and has important significance for designing and preparing the high-performance wide-spectrum multilayer film.
Description
Technical Field
The invention belongs to the technical field of optical films, relates to a preparation method of a low-stress low-absorption oxide film, and particularly relates to a double-ion thin filmBeamlet sputtering of Ta2O5And SiO2A method for preparing a film.
Background
With the development of modern large scientific devices and aerospace optoelectronic devices, higher and higher requirements are put on optical systems, the working spectrum band is changed from single wavelength to wide spectrum band, and the requirements on optical thin film elements are also developed from single wavelength to wide spectrum band. Due to the requirement of wide-spectrum optical performance, the number and thickness of the film layers are increased, high film stress is caused, and the problems of the ultra-poor surface shape and the falling off of the film layers of the optical film are caused, so that the problems of the ultra-poor surface shape and the falling off of the film layers of the optical film are core problems in the design and the manufacture of optical film elements.
With the demand of low-loss laser film preparation, the ion beam sputtering deposition technology is rapidly developed, and becomes the preferred scheme of the current high-performance laser film preparation mode. However, the stress of the ion beam sputtering deposited film is much larger than that of films prepared by other deposition methods, and therefore, how to reduce the stress of the ion beam sputtering film becomes a hot spot of current research. At present, the residual stress of the film is basically controlled by adjusting the deposition temperature, the oxygen partial pressure and other process parameters. Leplan et al studied SiO2The relationship between the film stress and the substrate temperature and the oxygen partial pressure during film coating, and the change relationship of the film stress along with time is researched. He found that the stress in the film can be controlled by adjusting the substrate temperature and the oxygen partial pressure during the coating, and the intrinsic stress in the film has a strong relationship with the density of the film. Liuhuasong and other systems research the ion beam sputtering process to prepare SiO2The correlation between the stress of the film and the technological parameters (substrate temperature, ion beam pressure, ion beam current and oxygen flow) shows that the low-stress SiO is prepared2The film should be selected to have a low substrate temperature and a high oxygen flow. The method prepares Ta by changing the process conditions of the beam pressure, the oxygen charging amount, the substrate temperature and the like of an ion source and adopting ion beam sputtering2O5、SiO2And Ta2O5/SiO2The high-reflection film is tested and analyzed for the stress characteristic, and the result is obtainedThe stress change rule of the film under different process conditions. But no report is found about a method for reducing the stress of an ion beam sputtered film by adopting a high beam voltage low current auxiliary mode.
In summary, the ion beam sputtering film stress is reduced by adjusting the preparation process parameters, and the reduction of the film stress by using the high beam voltage low current ion beam auxiliary process is not reported.
Disclosure of Invention
Objects of the invention
The purpose of the invention is: the preparation method of the low-stress low-absorption oxide film by ion beam sputtering is realized by adopting a double-ion beam sputtering deposition technology and changing the process parameters of a 12cm auxiliary ion source.
(II) technical scheme
In order to solve the above technical problems, the present invention provides a method for preparing a low-stress low-absorption oxide thin film, comprising the following steps:
s1: selecting a tantalum target and a silicon dioxide target as ion beam sputtering deposition target materials;
selecting tantalum target and silicon dioxide target as ion beam sputtering deposition target material, selecting fused quartz, silicon substrate as Ta2O5And SiO2Deposition substrate for thin films.
S2: preparing Ta on different substrates by adopting a dual-ion beam sputtering deposition technology and selecting different preparation process parameters2O5And SiO2A film;
the vacuum degree of the vacuum chamber body of the selected coating film is mx 10-6Torr, m is more than or equal to 1 and less than or equal to 50, and the working parameters of the main ion source are as follows: operating voltage of U1,900V≤U1Less than or equal to 1500V and working current I1,300mA≤ I1Less than or equal to 900 mA; auxiliary ion source operating parameters: operating voltage of U2,300V≤U2Less than or equal to 1500V and working current I2,100mA≤I2The flow rate of oxygen is less than or equal to 400mA, the flow rate of oxygen is X, the flow rate of X is less than or equal to 0sccm and less than or equal to 20sccm, the flow rate of argon is Y, and the flow rate of Y is less than or equal to 0sccm and less than or equal to 20 sccm; selecting different preparation process parameters from the molten quartz,Ta is prepared on a substrate of silicon and the like2O5And SiO2A film.
S3: measuring Ta with a spectrophotometer2O5And SiO2Calculating the visible light-near infrared band transmission spectrum of the film sample, and calculating Ta based on the inversion method of the transmission spectrum2O5And SiO2The refractive index and extinction coefficient of the film;
s4: measuring Ta by photothermal deflection2O5And SiO2Absorption loss of the film;
and measuring the absorption loss of the Ta2O5 and SiO2 films by adopting a weak absorption measuring instrument based on a photothermal deflection method.
S5: ta is obtained by adopting a stress calculation method based on Stoney formula2O5And SiO2Stress of the film;
measuring the surface shapes of the single-sided quartz substrate before and after coating by adopting a white light interferometer, and obtaining Ta by adopting a stress calculation method based on Stoney formula2O5And SiO2Stress of the film.
S6: obtaining low stress and low absorption Ta2O5And SiO2A film.
(III) advantageous effects
The preparation method of the low-stress low-absorption oxide film provided by the technical scheme realizes the preparation of the low-stress low-absorption oxide film by adopting a dual-ion beam sputtering deposition technology and changing the process parameters of the auxiliary ion source. The method has universality for preparing oxide films by different ion beam sputtering deposition technologies.
Drawings
FIG. 1 ion beam sputtering technique for preparing Ta2O5And SiO2The working schematic diagram of the film.
Ta on the quartz substrate of FIG. 22O5And SiO2Visible-near infrared transmittance curve of the film.
FIG. 3Ta2O5And SiO2The refractive index of the film.
FIG. 4Ta2O5And SiO2The thin film absorbs the loss amplitude plot.
FIG. 5Ta2O5Front and back surface patterns of the film coating.
FIG. 6SiO2-1 front and back surface patterns of film coating.
Detailed Description
In order to make the objects, contents and advantages of the present invention clearer, the following detailed description of the embodiments of the present invention will be made in conjunction with the accompanying drawings and examples.
The preparation method of the low-stress low-absorption oxide film comprises the following steps:
s1: selecting a tantalum target and a silicon dioxide target as ion beam sputtering deposition target materials;
selecting tantalum target and silicon dioxide target as ion beam sputtering deposition target material, selecting fused quartz, silicon substrate as Ta2O5And SiO2Deposition substrate for thin films.
S2: preparing Ta on different substrates by adopting a dual-ion beam sputtering deposition technology and selecting different preparation process parameters2O5And SiO2A film;
the vacuum degree of the vacuum chamber body of the selected coating film is mx 10-6Torr, m is more than or equal to 1 and less than or equal to 50, and the working parameters of the main ion source are as follows: operating voltage of U1,900V≤U1Less than or equal to 1500V and working current I1,300mA≤ I1Less than or equal to 900 mA; auxiliary ion source operating parameters: operating voltage of U2,300V≤U2Less than or equal to 1500V and working current I2,100mA≤I2The flow rate of oxygen is less than or equal to 400mA, the flow rate of oxygen is X, the flow rate of X is less than or equal to 0sccm and less than or equal to 20sccm, the flow rate of argon is Y, and the flow rate of Y is less than or equal to 0sccm and less than or equal to 20 sccm; selecting different preparation process parameters to prepare Ta on fused quartz, silicon and other substrates2O5And SiO2A film.
S3: measuring Ta with a spectrophotometer2O5And SiO2Calculating the visible light-near infrared band transmission spectrum of the film sample, and calculating Ta based on the inversion method of the transmission spectrum2O5And SiO2The refractive index and extinction coefficient of the film;
s4: measuring Ta by photothermal deflection2O5And SiO2Absorption loss of the film;
adopt weak absorption measuring instrument based on photothermal deflection method to measure Ta2O5And SiO2Absorption loss of the film.
S5: ta is obtained by adopting a stress calculation method based on Stoney formula2O5And SiO2Stress of the film;
measuring the surface shapes of the single-sided quartz substrate before and after coating by adopting a white light interferometer, and obtaining Ta by adopting a stress calculation method based on Stoney formula2O5And SiO2Stress of the film.
S6: obtaining low stress and low absorption Ta2O5And SiO2A film.
Examples of the invention
The following ion beam sputtering technique is used to prepare Ta2O5And SiO2The film is taken as an example, and the specific steps are as follows:
firstly, selecting a tantalum target and a silicon dioxide target as ion beam sputtering deposition target materials, and selecting a fused quartz substrate as Ta2O5And SiO2Deposition substrate for thin films.
Ta is prepared by adopting a double-ion-beam sputtering deposition technology2O5And SiO2The working diagram of the film is shown in figure 1. The vacuum degree of the vacuum chamber body of the selected coating film is 8 multiplied by 10-6Torr,Ta2O5The main ion source process parameters of the film are as follows: the working voltage is 1200V, and the working current is 600 mA. Ta2O5The auxiliary ion source process parameters of the film are as follows: 1) ta2O5-1 film: the working voltage is 1200V, the working current is 300mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 2) ta2O5-2 film: the working voltage is 600V, the working current is 300mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 3) ta2O5-3 film: the working voltage is 1200V, the working current is 150mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm.
SiO2Film dominant ionThe source operating parameters are: the working voltage is 1200V, and the working current is 600 mA. SiO22The working parameters of the film auxiliary ion source are as follows: 1) SiO22-1 film: the working voltage is 1200V, the working current is 200mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 2) SiO22-2 film: the working voltage is 600V, the working current is 200mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 3) SiO22-3 film: the working voltage is 1200V, the working current is 100mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm.
Measuring Ta on a fused silica substrate using a spectrophotometer2O5And SiO2Visible-near infrared transmittance curve of film, wherein Ta2O5-1 and SiO2The-1 film transmittance curve is shown in FIG. 2. Calculating Ta by adopting spectral inversion calculation method based on transmission spectrum2O5And SiO2Refractive index and extinction coefficient of the film. Ta2O5-1 and SiO2-1 the refractive index profile of the film is shown in FIG. 3, with an extinction coefficient of substantially 0 at wavelengths from 320nm to 2600 nm.
Adopt weak absorption measuring apparatu based on light and heat deflection technique, test Ta2O5And SiO2Absorption loss of film, Ta2O5-1 and SiO2-1 film amplitude diagram shown in FIG. 4, Ta2O5Absorption loss of-1 film was 8ppm, SiO2The absorption loss of the-1 film was 4 ppm.
Adopting a white light interferometer to measure the surface shapes of the single-sided quartz substrate before and after coating, wherein Ta2O5FIG. 5 shows front and rear surface patterns of-1 thin film coating, SiO2FIG. 6 shows the front and rear surface patterns of the film coating film of-1. Ta is obtained by adopting a stress calculation method based on Stoney formula2O5And SiO2The stress of the film was-120 MPa and-80 MPa, respectively.
Adopts ion beam sputtering deposition technology to realize low-stress low-absorption Ta2O5And SiO2And (3) preparing a film.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a low-stress low-absorption oxide film is characterized by comprising the following steps:
s1: selecting a tantalum target and a silicon dioxide target as ion beam sputtering deposition target materials;
s2: preparing Ta on different substrates by adopting a dual-ion beam sputtering deposition technology and selecting different preparation process parameters2O5And SiO2A film;
s3: measuring Ta with a spectrophotometer2O5And SiO2Calculating the visible light-near infrared band transmission spectrum of the film sample, and calculating Ta based on the inversion method of the transmission spectrum2O5And SiO2The refractive index and extinction coefficient of the film;
s4: measuring Ta by photothermal deflection2O5And SiO2Absorption loss of the film;
s5: ta is obtained by adopting a stress calculation method based on Stoney formula2O5And SiO2Stress of the film;
s6: obtaining low stress and low absorption Ta2O5And SiO2A film.
2. The method according to claim 1, wherein in step S1, the tantalum target and the silicon dioxide target are selected as target materials for ion beam sputter deposition, and the fused silica and the silicon are selected as target materials for Ta deposition2O5And SiO2Deposition substrate for thin films.
3. The method according to claim 2, wherein in step S2, the vacuum degree of the vacuum chamber is m x 10-6Torr, m is more than or equal to 1 and less than or equal to 50, and the working parameters of the main ion source are as follows:operating voltage of U1,900V≤U1Less than or equal to 1500V and working current I1,300mA≤I1Less than or equal to 900 mA; auxiliary ion source operating parameters: operating voltage of U2,300V≤U2Less than or equal to 1500V and working current I2,100mA≤I2The flow rate of oxygen is less than or equal to 400mA, the flow rate of oxygen is X, the flow rate of X is less than or equal to 0sccm and less than or equal to 20sccm, the flow rate of argon is Y, and the flow rate of Y is less than or equal to 0sccm and less than or equal to 20 sccm; selecting different preparation process parameters to prepare Ta on fused quartz and silicon substrate2O5And SiO2A film.
4. The method for preparing a low-stress and low-absorption oxide thin film according to claim 3, wherein in step S4, Ta is measured by using a weak absorption measuring instrument based on a photothermal deflection method2O5And SiO2Absorption loss of the film.
5. The method according to claim 4, wherein in step S5, the surface shapes of the single-sided quartz substrate before and after coating are measured by a white light interferometer, and Ta is obtained by a stress calculation method based on Stoney' S formula2O5And SiO2Stress of the film.
6. The method according to claim 5, wherein in step S1, the tantalum target and the silicon dioxide target are selected as target materials for ion beam sputter deposition, and the fused silica substrate is selected as Ta2O5And SiO2Deposition substrate for thin films.
7. The method according to claim 6, wherein in step S2, the vacuum degree of the vacuum chamber is 8 x 10-6Torr。
8. The method according to claim 7, wherein in step S2, Ta2O5The main ion source process parameters of the film are as follows: the working voltage is 1200V, and the working current is 600 mA; ta2O5The auxiliary ion source process parameters of the film are as follows: 1) ta2O5-1 film: the working voltage is 1200V, the working current is 300mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 2) ta2O5-2 film: the working voltage is 600V, the working current is 300mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 3) ta2O5-3 film: the working voltage is 1200V, the working current is 150mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm.
9. The method according to claim 8, wherein in step S2, SiO is used as the material2The working parameters of the film main ion source are as follows: the working voltage is 1200V, and the working current is 600 mA. SiO22The working parameters of the film auxiliary ion source are as follows: 1) SiO22-1 film: the working voltage is 1200V, the working current is 200mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 2) SiO22-2 film: the working voltage is 600V, the working current is 200mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm; 3) SiO22-3 film: the working voltage is 1200V, the working current is 100mA, the oxygen flow is 12sccm, and the argon flow is 5 sccm.
10. The method according to claim 9, wherein in step S4, Ta is used as the dopant2O5Absorption loss of the film was 8ppm, SiO2The absorption loss of the film was 4 ppm; in the step S5, Ta is obtained based on the stress calculation method of the Stoney formula2O5And SiO2The stress of the film was-120 MPa and-80 MPa, respectively.
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CN114075651A (en) * | 2021-11-16 | 2022-02-22 | 宁波江丰电子材料股份有限公司 | Tantalum-silicon dioxide sputtering target material and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050205998A1 (en) * | 2002-10-22 | 2005-09-22 | Asahi Glass Company Limited | Multilayer film-coated substrate and process for its production |
CN104480428A (en) * | 2014-12-02 | 2015-04-01 | 中国航天科工集团第三研究院第八三五八研究所 | Method for regulating and controlling ion beam sputtered silicon dioxide optical membrane stress |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050205998A1 (en) * | 2002-10-22 | 2005-09-22 | Asahi Glass Company Limited | Multilayer film-coated substrate and process for its production |
CN104480428A (en) * | 2014-12-02 | 2015-04-01 | 中国航天科工集团第三研究院第八三五八研究所 | Method for regulating and controlling ion beam sputtered silicon dioxide optical membrane stress |
Non-Patent Citations (2)
Title |
---|
申林: "氧化物激光薄膜的离子束溅射制备技术", 《强激光与粒子束》 * |
袁文佳: "离子束溅射制备Nb2O5、Ta2O5和SiO2薄膜的光学、力学特性和微结构", 《光学学报》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114075651A (en) * | 2021-11-16 | 2022-02-22 | 宁波江丰电子材料股份有限公司 | Tantalum-silicon dioxide sputtering target material and preparation method thereof |
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