CN113529034A - Coating method of near-infrared conductive optical filter - Google Patents
Coating method of near-infrared conductive optical filter Download PDFInfo
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- CN113529034A CN113529034A CN202110708485.XA CN202110708485A CN113529034A CN 113529034 A CN113529034 A CN 113529034A CN 202110708485 A CN202110708485 A CN 202110708485A CN 113529034 A CN113529034 A CN 113529034A
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
-
- 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
- C23C14/0641—Nitrides
- C23C14/0652—Silicon nitride
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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
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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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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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/08—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of polarising materials
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Abstract
The invention relates to the technical field of optics, in particular to a coating method of a near-infrared conductive optical filter, which carries out the coating of a filter layer on the surface of one side of a substrate in a coating space; after the completion, cooling the filter layer and the coating space; and coating the ITO layer on the surface of one side of the filter layer in a coating space with a certain preset temperature, and introducing preset amounts of oxygen and hydrogen into the coating space in the coating process of the ITO layer. The invention has the advantages that: the prepared near-infrared conductive filter has high transmittance in an infrared band and low surface resistance; the coating method is controllable, has wide application range, is beneficial to industrial production and is suitable for popularization.
Description
Technical Field
The invention relates to the technical field of optics, in particular to a film coating method of a near-infrared conductive filter.
Background
With the accelerated development of artificial intelligence products, infrared filters are needed by enterprises of many intelligent products, and the infrared filters are widely applied, for example, the infrared filters can be applied to the fields of infrared detection, infrared induction, communication and the like. A conductive Indium Tin Oxide (ITO) layer is typically formed on the surface of the infrared filter by a vacuum sputtering process. In addition, the thickness of the ITO layer needs to be increased to reduce the sheet resistance thereof, so as to obtain a better conductive effect. However, an increase in the thickness of the ITO layer leads to a significant decrease in its transmittance.
Disclosure of Invention
The invention aims to provide a coating method of a near-infrared conductive filter according to the defects of the prior art, which can effectively reduce the surface resistance of an ITO layer and improve the service performance of the ITO layer while ensuring the transmittance of the filter.
The purpose of the invention is realized by the following technical scheme:
a coating method of a near-infrared conductive filter comprises a substrate, a filter layer and an ITO layer which are sequentially stacked, and is characterized in that: plating the filter layer in a film plating space; after the completion, cooling the filter layer and the coating space; and plating the ITO layer on the surface of one side of the filter layer in the film plating space at a preset temperature, and introducing preset amounts of oxygen and hydrogen into the film plating space in the process of plating the ITO layer.
The preset temperature of the coating space is below 100 ℃.
The preset temperature of the coating space is 45-100 ℃.
The ratio of the introduced volume flow of the oxygen to the introduced volume flow of the hydrogen is 3:1-15: 1.
The volume flow ratio of the introduced oxygen to the introduced hydrogen is 4:1-8: 1.
The filter layer comprises a hydrogenated silicon layer and a silicon dioxide layer which are sequentially and alternately plated on the substrate, and the ITO layer is plated on the surface of the outermost silicon dioxide layer.
And plating an AR layer on the other side surface of the substrate.
The AR layer is a silicon dioxide layer and a silicon nitride layer which are sequentially and alternately plated on the other side surface of the substrate.
And plating the filter layer and the ITO layer by adopting a sputtering coating process.
And bombarding an ITO target of the ITO layer by adopting plasma, wherein atoms of the ITO target form the ITO layer on the surface of the filter layer after passing through ICP.
The invention has the advantages that: the prepared near-infrared conductive filter has high transmittance in an infrared band and low surface resistance; the coating method is controllable, has wide application range, is beneficial to industrial production and is suitable for popularization.
Drawings
FIG. 1 is a process flow diagram of one embodiment of the present invention;
FIG. 2 is a process parameter diagram according to an embodiment of the present invention;
fig. 3 is a transmittance test chart of the near-infrared conductive filter manufactured by the present invention.
Detailed Description
The features of the present invention and other related features are described in further detail below by way of example in conjunction with the following drawings to facilitate understanding by those skilled in the art:
example (b): the method for coating the near-infrared conductive filter in the embodiment is used for coating the near-infrared conductive filter. The near-infrared conductive optical filter comprises a glass substrate, wherein a filter layer formed by alternately coating a hydrogenated silicon layer and a silicon dioxide layer is coated on the surface of one side of the glass substrate, an ITO (indium tin oxide) layer is coated on the filter layer, and an AR layer formed by alternately coating a silicon dioxide layer and silicon nitride is coated on the surface of the other side of the glass substrate.
Based on the near-infrared conductive filter, as shown in fig. 1, the coating method in this embodiment includes the following steps:
1) by adopting a sputtering coating process, a plurality of hydrogenated silicon layers and a plurality of silicon dioxide layers are sequentially and alternately coated on the surface of one side of a glass substrate in a coating cavity (coating space) of coating equipment capable of executing the sputtering coating process to form the optical filter. The hydrogenated silicon layer and the silicon dioxide layer combine to form a filter layer to filter visible light other than in the near infrared wavelength range. The innermost layer of the filter layer, which is in contact with the glass substrate, is a hydrogenated silicon layer, and the outermost layer of the filter layer is a silicon dioxide layer; the respective numbers of layers (the total number of layers of the filter layer) of the hydrogenated silicon layer and the silicon dioxide layer and the respective film thicknesses (the total thickness of the filter layer) can be designed according to the actual filtering requirements.
2) And taking the glass substrate coated with the filter layer out of the coating cavity of the coating machine for cooling, and simultaneously cooling the coating cavity to a preset temperature below 100 ℃. The cooling operation may be natural cooling by allowing it to be in an atmospheric environment, or accelerated cooling by a cooling device. Preferably, the plating chamber can be cooled to 45-100 ℃, so as to further improve the effect of the plating process performed subsequently. Further preferably, the coating chamber may be cooled to 65 ℃.
3) And placing the cooled glass substrate with the plated filter layer in a film coating cavity cooled to a preset temperature to plate an ITO (indium tin oxide) layer, wherein the ITO layer is plated on a silicon dioxide layer serving as the outermost layer of the filter layer. When the ITO layer is plated, hydrogen and hydrogen with the volume flow ratio of 3:1-15:1 are introduced into the film plating cavity, so that the surface resistance of the ITO layer is effectively reduced while the transmittance is ensured, and the service performance of the ITO layer is improved. Preferably, the ratio of the flow volume of the oxygen to the flow volume of the hydrogen is 4:1 to 8:1, so as to further improve the reaction effect. Further preferably, the ratio of the flow volume of oxygen to the flow volume of hydrogen is 6: 1.
Specifically, in the ITO layer plating process, a certain amount of oxygen is introduced to inhibit the decomposition of the ITO material in the plating process, so that the reduction of the transmittance caused by the generation of dark low-valence oxides by the ITO material is avoided; meanwhile, the introduced hydrogen can reduce the indium oxide in the ITO layer into indium, so that the surface resistance is reduced, and the influence of the lighter color of the indium on the transmittance is smaller. Meanwhile, the film coating cavity is cooled to be below 100 ℃, so that the decomposition of ITO at high temperature and the reoxidation of indium reduced by hydrogen can be avoided.
In practice, if the amount of hydrogen introduced is too large, the metal indium in the ITO material is likely to be excessively substituted, resulting in a decrease in transmittance. If the oxygen is introduced in too much amount, the surface resistance is increased; if the amount of oxygen introduced is small, the transmittance is reduced. Therefore, in the embodiment, the three process steps of cooling, introducing hydrogen and oxygen are organically combined, so that the surface resistance of the ITO layer is greatly reduced while the transmittance of the near-infrared conductive filter is ensured.
4) After the ITO layer is plated, the AR layers formed by alternately plating the silicon dioxide layer and the silicon nitride layer are sequentially and alternately plated on the other side surface of the glass substrate. The transmittance can be further improved by plating the AR layer; meanwhile, the surface resistance of the ITO layer can be further reduced through the plating of the AR layer. Wherein, the innermost layer of the AR layer contacting with the glass substrate is a silicon dioxide layer, and the outermost layer of the AR layer is a silicon nitride layer; the number of the silicon dioxide layer and the silicon nitride layer (the total number of the AR layers) and the thickness of the film (the total thickness of the AR layers) can be designed according to the actual filtering requirements.
The actual production of the near-infrared conductive filter is carried out by using the film coating method of the steps 1) to 4) and corresponding tests are carried out, specifically as follows:
the production of the near-infrared conductive filter is performed according to the process parameters shown in fig. 2, wherein one side surface of the near-infrared conductive filter provided with the ITO layer is a surface a, and the other side surface of the near-infrared conductive filter is a surface B.
Firstly, a plating process of the surface A of the near-infrared conductive optical filter:
1) cleaning: and placing the glass substrate in a vacuum coating chamber for ICP cleaning, wherein the ICP power is 0.5-4KW, and the cleaning time is 30-300 s.
2) Plating an optical filter: plating 5-100nm silicon dioxide (SiO) on the surface of the cleaned glass substrate2) Introducing argon into the silicon target material, wherein the flow of the argon is as follows: the target is bombarded by the generated argon ions with the temperature of 100-. Sputtering silicon atoms under the action of a magnetic field, wherein the generated silicon atoms pass through ICP, the ICP power is 0.5-5KW, the oxygen flow is 100-500sccm, the argon flow is 10-500sccm, and oxygen and argon are introduced into the ICP to generate oxygen ions and argon ions to act on the silicon atoms to generate silicon dioxide. Then plating 1-100nm of silicon hydride with ICP power of0.5-5KW, hydrogen flow rate of 1-100sccm, argon flow rate of 100-500sccm, and introducing hydrogen and argon into ICP to generate argon ions and hydrogen ions to act on silicon atoms to generate silicon hydride. Then, the silicon hydride with the thickness of 10-500nm and the silicon dioxide with the thickness of 10-300nm are plated alternately.
3) And (3) cooling: taking out the glass substrate coated with the optical filter, and placing the glass substrate in an atmospheric state to allow the surface temperature of the glass substrate to reach normal temperature.
4) And (3) plating an ITO layer: placing the glass substrate with the coated optical filter in a vacuum coating chamber to coat an ITO layer of 10-1000nm, and introducing argon into an ITO target, wherein the flow of the argon is as follows: 100-. ITO atoms are sputtered under the action of a magnetic field, the ICP power is 0.5-5KW after ICP, and the argon flow is as follows: 100-: 1-50sccm, hydrogen flow rate: 0.1-50sccm, argon gas flow of 10-500sccm, and ions generated after oxygen, argon gas and hydrogen gas are introduced into ICP act on ITO atoms to generate an ITO layer on the optical filter.
Secondly, coating the film on the B surface of the near-infrared conductive optical filter:
1) cleaning: and placing the glass substrate in a vacuum coating chamber for ICP cleaning, wherein the ICP power is 0.5-4KW, and the cleaning time is 30-300 s.
2) AR coating (AR layer): plating 5-100nm silicon dioxide on the surface of the cleaned glass substrate, introducing argon into the silicon target material, wherein the flow of the argon is as follows: bombarding the target by using 100-1800sccm generated argon ions, sputtering silicon atoms under the action of a magnetic field, enabling the generated silicon atoms to pass through ICP, wherein the ICP power is 0.5-5KW, the oxygen flow is 100-500sccm, the argon flow is 10-500sccm, and oxygen and argon are introduced into the ICP to generate oxygen ions and argon ions to act on the silicon atoms to generate silicon dioxide. Then, 5-100nm silicon nitride is plated, ICP power is 0.5-5KW, nitrogen flow is 100-500sccm, argon flow is 100-500sccm, and nitrogen and argon are introduced into ICP to generate oxygen ions and argon ions to act on silicon atoms to generate silicon nitride. Then, the silicon nitride with the thickness of 10-500nm and the silicon dioxide with the thickness of 10-300nm are plated alternately.
The performance test result of the near-infrared conductive filter prepared by the coating method is as follows:
as shown in fig. 3, the near infrared conductive filter has an extremely high transmittance in the near infrared wavelength range.
When the optical filter and the ITO layer are plated in the same furnace, the surface resistance is 36 omega/cm2Left and right.
When the step 2) and the step 3) of the plating method in the present embodiment are sequentially performed, the sheet resistance of the ITO layer can be reduced to 26 Ω/cm2Left and right; if step 2) is not executed, that is, the optical filter and the coating cavity are not cooled, the sheet resistance of the ITO layer is higher by about 4 Ω/cm than when the temperature is lower than 100 ℃.
When step 4) of the plating method in the present embodiment is further performed in cooperation with step 2) and step 3), the sheet resistance of the ITO layer is from 26 Ω/cm2The left and right can be further reduced to 20 omega/cm2Left and right.
The test result shows that the film coating method in the embodiment can ensure the transmittance of the near-infrared conductive filter, greatly reduce the sheet resistance of the ITO layer and improve the service performance of the ITO layer.
In the embodiment, in specific implementation: in addition to the filter layer and the AR layer made of specific materials in this embodiment, a film layer made of other materials and having a filtering function or an anti-reflection function may be used instead, but the characteristics of the ITO layer and the implementation process thereof should be matched when the film layer is selected, so as to avoid adverse effects.
Although the conception and the embodiments of the present invention have been described in detail with reference to the drawings, those skilled in the art will recognize that various changes and modifications can be made therein without departing from the scope of the appended claims, and therefore, they are not to be considered repeated herein.
Claims (10)
1. A coating method of a near-infrared conductive filter comprises a substrate, a filter layer and an ITO layer which are sequentially stacked, and is characterized in that: plating the filter layer on one side surface of the substrate in a film plating space; after the completion, cooling the filter layer and the coating space; and plating the ITO layer on the surface of one side of the filter layer in the film plating space at a preset temperature, and introducing preset amounts of oxygen and hydrogen into the film plating space in the process of plating the ITO layer.
2. The method according to claim 1, wherein: the preset temperature of the coating space is below 100 ℃.
3. The method according to claim 2, wherein: the preset temperature of the coating space is 45-100 ℃.
4. The method according to claim 1, wherein: the ratio of the introduced volume flow of the oxygen to the introduced volume flow of the hydrogen is 3:1-15: 1.
5. The method according to claim 4, wherein: the volume flow ratio of the introduced oxygen to the introduced hydrogen is 4:1-8: 1.
6. The method according to claim 1, wherein: the filter layer comprises a hydrogenated silicon layer and a silicon dioxide layer which are sequentially and alternately plated on the substrate, and the ITO layer is plated on the surface of the outermost silicon dioxide layer.
7. The method according to claim 1, wherein: and plating an AR layer on the other side surface of the substrate.
8. The method according to claim 7, wherein: the AR layer is a silicon dioxide layer and a silicon nitride layer which are sequentially and alternately plated on the other side surface of the substrate.
9. The method according to claim 1, wherein: and plating the filter layer and the ITO layer by adopting a sputtering coating process.
10. The method according to claim 9, wherein: and bombarding an ITO target of the ITO layer by adopting plasma, wherein atoms of the ITO target form the ITO layer on the surface of the filter layer after passing through ICP.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110708485.XA CN113529034A (en) | 2021-06-25 | 2021-06-25 | Coating method of near-infrared conductive optical filter |
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| CN202110708485.XA CN113529034A (en) | 2021-06-25 | 2021-06-25 | Coating method of near-infrared conductive optical filter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI813161B (en) * | 2022-01-28 | 2023-08-21 | 光洋應用材料科技股份有限公司 | Indium-tin-oxide film, preparation method thereof and light absorption element comprising the same |
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|---|---|---|---|---|
| JPH0254755A (en) * | 1988-08-19 | 1990-02-23 | Ulvac Corp | Manufacture of transparent conductive film |
| US20110192716A1 (en) * | 2010-02-11 | 2011-08-11 | Applied Materials, Inc. | Method for producing an ito layer and sputtering system |
| US20150293284A1 (en) * | 2012-12-28 | 2015-10-15 | Asahi Glass Company, Limited | Near infrared cutoff filter |
| CN108873135A (en) * | 2018-08-06 | 2018-11-23 | 信阳舜宇光学有限公司 | A kind of near-infrared narrow band filter and infrared imaging system |
| CN110218988A (en) * | 2019-06-10 | 2019-09-10 | 浙江水晶光电科技股份有限公司 | AR membrane preparation device, AR membrane preparation method and AR film |
-
2021
- 2021-06-25 CN CN202110708485.XA patent/CN113529034A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0254755A (en) * | 1988-08-19 | 1990-02-23 | Ulvac Corp | Manufacture of transparent conductive film |
| US20110192716A1 (en) * | 2010-02-11 | 2011-08-11 | Applied Materials, Inc. | Method for producing an ito layer and sputtering system |
| US20150293284A1 (en) * | 2012-12-28 | 2015-10-15 | Asahi Glass Company, Limited | Near infrared cutoff filter |
| CN108873135A (en) * | 2018-08-06 | 2018-11-23 | 信阳舜宇光学有限公司 | A kind of near-infrared narrow band filter and infrared imaging system |
| CN110218988A (en) * | 2019-06-10 | 2019-09-10 | 浙江水晶光电科技股份有限公司 | AR membrane preparation device, AR membrane preparation method and AR film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI813161B (en) * | 2022-01-28 | 2023-08-21 | 光洋應用材料科技股份有限公司 | Indium-tin-oxide film, preparation method thereof and light absorption element comprising the same |
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