CN116892006B - Large-caliber deep curved surface infrared window anti-reflection protection structure and preparation method thereof - Google Patents
Large-caliber deep curved surface infrared window anti-reflection protection structure and preparation method thereof Download PDFInfo
- Publication number
- CN116892006B CN116892006B CN202310840874.7A CN202310840874A CN116892006B CN 116892006 B CN116892006 B CN 116892006B CN 202310840874 A CN202310840874 A CN 202310840874A CN 116892006 B CN116892006 B CN 116892006B
- Authority
- CN
- China
- Prior art keywords
- layer
- step gradient
- dlc layer
- gradient stress
- stress dlc
- 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.)
- Active
Links
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 74
- 230000007704 transition Effects 0.000 claims abstract description 26
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims description 78
- 239000005083 Zinc sulfide Substances 0.000 claims description 48
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 48
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 48
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 34
- 238000001704 evaporation Methods 0.000 claims description 30
- 230000008020 evaporation Effects 0.000 claims description 30
- 230000008021 deposition Effects 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 23
- 229910052732 germanium Inorganic materials 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 17
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 16
- XASAPYQVQBKMIN-UHFFFAOYSA-K ytterbium(iii) fluoride Chemical compound F[Yb](F)F XASAPYQVQBKMIN-UHFFFAOYSA-K 0.000 claims description 16
- 238000010884 ion-beam technique Methods 0.000 claims description 15
- 230000001105 regulatory effect Effects 0.000 claims description 14
- 239000001273 butane Substances 0.000 claims description 13
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 13
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 13
- 238000005229 chemical vapour deposition Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 2
- 238000010894 electron beam technology Methods 0.000 description 16
- 238000000605 extraction Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- 238000001514 detection method Methods 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000004880 explosion Methods 0.000 description 6
- 238000005336 cracking Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000007740 vapor deposition Methods 0.000 description 5
- 238000005187 foaming Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004429 Calibre Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
- C23C16/306—AII BVI compounds, where A is Zn, Cd or Hg and B is S, Se or Te
-
- 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
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
Abstract
The invention belongs to the technical field of glass, and particularly discloses a large-caliber deep curved surface infrared window anti-reflection protection structure and a preparation method thereof. The invention provides a large-caliber deep curved surface infrared window anti-reflection protection structure, which comprises a substrate, wherein a transition matching layer and an anti-reflection film layer are correspondingly arranged on the upper surface and the lower surface of the substrate respectively, and a hard protection film layer is arranged on the matching transition layer; the hard protective film layer sequentially comprises a first step gradient stress DLC layer, a second step gradient stress DLC layer, a third step gradient stress DLC layer and a fourth step gradient stress DLC layer from the substrate to the outside. The anti-reflection protection structure of the large-caliber deep curved surface infrared window, which is reasonably designed, avoids the problem that the large-caliber deep curved surface infrared window is easy to burst or take off film when being coated or soaked in water for a long time, and can also improve the scratch resistance, the friction resistance and the high transmittance of the large-caliber deep curved surface infrared window anti-reflection protection structure and the adhesive force of the hard protection film layer and the substrate.
Description
Technical Field
The invention belongs to the technical field of glass, and particularly relates to a large-caliber deep curved surface infrared window anti-reflection protection structure and a preparation method thereof.
Background
With the development of high and new science and technology such as space satellite, space relay and remote control telemetry, and the like, the great application demands in the field of high-speed and ultra-high-speed flight platforms are continuously put forward, and infrared photoelectric equipment represented by an infrared imaging guide system is widely applied to various accurate guide platforms. The optical window of the infrared band is positioned at the front end of the system, is a key component for integrating the structure/function of the infrared detection imaging equipment, and is accelerated to develop in the direction of large size and complex molded surfaces in recent years.
The large-caliber deep curved surface infrared window surface has larger space orientation, and the microstructure and macroscopic characteristic of the film material prepared on the large-caliber deep curved surface infrared window surface have obvious space difference characteristics. On one hand, the spectral characteristics of the infrared window are affected, so that the sensitivity and accuracy of the infrared detection system are deteriorated; on the other hand, when the infrared optical protection film is used in a severe and complex environment, the weak area of the film layer is easy to damage and destroy and even fall off, and finally the whole optical window cannot be used normally. However, for the infrared window with a large caliber and a deep curved surface, the problems of film explosion or film falling out of the furnace or soaking water and the like can occur when the film is coated through a conventional process. Therefore, the problems that the adhesion and the wear resistance of the film on the large-caliber deep-curved-surface infrared window anti-reflection protection structure are poor and the film is easy to explode are solved.
Disclosure of Invention
In view of the above, the invention provides a large-caliber deep curved surface infrared window anti-reflection protection structure and a preparation method thereof, and the invention avoids the problem that the large-caliber deep curved surface infrared window is easy to burst or take off film when being coated or soaked in water for a long time by reasonably designing the large-caliber deep curved surface infrared window anti-reflection protection structure, and further improves the scratch resistance, friction resistance and high transmittance of the large-caliber deep curved surface infrared window anti-reflection protection structure and the adhesive force of a hard protection film and a substrate.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the invention provides a large-caliber deep curved surface infrared window anti-reflection protection structure, which comprises a substrate, wherein a transition matching layer and an anti-reflection film layer are correspondingly arranged on the upper surface and the lower surface of the substrate respectively, and a hard protection film layer is arranged on the matching transition layer;
the hard protective film layer sequentially comprises a first step gradient stress DLC layer, a second step gradient stress DLC layer, a third step gradient stress DLC layer and a fourth step gradient stress DLC layer from the substrate outwards;
the internal stress of the first step gradient stress DLC layer, the second step gradient stress DLC layer, the third step gradient stress DLC layer and the fourth step gradient stress DLC layer is gradually reduced from the substrate to the outside;
the inner layer stresses of the first step gradient stress DLC layer and the third step gradient stress DLC layer are higher than the inner layer stresses of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer.
Compared with the prior art, the large-caliber deep curved surface infrared window anti-reflection protection structure provided by the invention has the advantages that the transition matching layer and the hard protection film layer are attached to one side of the substrate, so that the scratch resistance and the friction resistance of the substrate can be improved; the inventor conducts a great deal of research, and the stress of the hard protective film layer is reduced by adjusting the structure of the hard protective film layer and limiting the in-layer stress variation trend of the first step gradient stress DLC layer, the second step gradient stress DLC layer, the third step gradient stress DLC layer and the fourth step gradient stress DLC layer, so that the problem of film explosion when coating films on a large-caliber deep curved surface infrared window is avoided; the introduction of the transition matching layer improves the adhesion between the substrate and the hard protective film layer, thereby improving the bonding strength between the hard protective film layer and the substrate and avoiding the rupture phenomenon; the transmittance of the large-caliber deep curved surface infrared window anti-reflection protection structure is further improved by preparing an anti-reflection film layer on the other side of the substrate.
The anti-reflection protection structure of the large-caliber deep curved surface infrared window is reasonably designed, so that the problem that the large-caliber deep curved surface infrared window is easy to burst or take off a film when being coated or soaked in water for a long time is avoided, and the scratch resistance, the friction resistance and the high transmittance of the anti-reflection protection structure of the large-caliber deep curved surface infrared window and the adhesive force of the hard protection film layer and the substrate can be improved.
Preferably, the internal stress of the first step gradient stress DLC layer and the third step gradient stress DLC layer is reduced from (3.0-3.2) GPa to (2.5-2.7) GPa; the internal stress of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer is reduced from (2.1-2.3) GPa to (1.6-1.8) GPa.
Preferably, the caliber of the substrate is more than or equal to 200mm, and the sagittal height is more than or equal to 25mm.
Preferably, the substrate is made of Si or Ge.
Preferably, the material of the transition matching layer is Si or Ge.
Preferably, the antireflection film layer sequentially comprises a first zinc sulfide layer, a germanium layer, a second zinc sulfide layer, a ytterbium fluoride layer and a third zinc sulfide layer from the substrate to the outside.
Preferably, the thickness of the first zinc sulfide layer is 330-350nm.
Preferably, the thickness of the germanium layer is 110-130nm.
Preferably, the thickness of the second zinc sulfide layer is 550-570nm.
Preferably, the thickness of the ytterbium fluoride layer is 1080-1100nm.
Preferably, the third zinc sulfide layer has a thickness of 160-180nm.
The transmittance of the infrared window with the large caliber and the deep curved surface is improved by the optimized antireflection film.
Preferably, the thickness of the first step gradient stress DLC layer is 320nm-370nm.
Preferably, the thickness of the second step-by-step graded stress DLC layer is 320nm-370nm.
Preferably, the thickness of the third step gradient stress DLC layer is 320nm-370nm.
Preferably, the thickness of the fourth step gradient stress DLC layer is 320nm-370nm.
The thickness of the preferable DLC layer avoids the problem that the infrared window with a large caliber and a deep curved surface is easy to burst or take off when being coated or soaked in water for a long time.
The invention also provides a preparation method of the large-caliber deep curved surface infrared window anti-reflection protection structure, which at least comprises the following steps:
s1, depositing a matching transition layer on one side of a substrate by an ion beam assisted evaporation deposition method;
s2, placing the substrate in a fixing device, and sequentially depositing a first step gradient stress DLC layer and a second step gradient stress DLC layer on the transition matching layer by a chemical vapor deposition method;
s3, horizontally rotating the fixing device in situ by 180 degrees, and sequentially depositing a third step gradient stress DLC layer and a fourth step gradient stress DLC layer on the second step gradient stress DLC layer by a chemical vapor deposition method;
and S4, sequentially depositing a first zinc sulfide layer, a germanium layer, a second zinc sulfide layer, a ytterbium fluoride layer and a third zinc sulfide layer on the other side of the substrate by an ion beam assisted evaporation deposition method to obtain the large-caliber deep curved surface infrared window anti-reflection protection structure.
It is further preferred that the substrate be soaked with absolute ethanol before coating and then scrubbed with a mixture of absolute ethanol and diethyl ether.
Further preferably, in S1, the conditions of the ion beam assisted vapor deposition method are: the electron beam extraction voltage is 8kV-10kV, the evaporation beam current is 200mA-300mA, and the evaporation rate is 0.1nm/s-0.2nm/s.
Preferably, in S2, the fixing device includes a middle concave portion and convex portions with two ends extending upward and inward, and the arc formed by extending the convex portions at the two ends has the same curvature radius as the upper surface of the substrate.
The preferred fixing device also ensures edge uniformity of the film produced, thereby avoiding problems of film tapping or film stripping during use.
Preferably, the initial radio frequency power of the first step-graded stress DLC layer is 190w-200w higher than the initial radio frequency power of the second step-graded stress DLC layer.
The radio frequency power difference value of the preferable first step gradient stress DLC layer and the second step gradient stress DLC layer can avoid the problem of film explosion.
Preferably, the initial radio frequency power of the third step-gradient stress DLC layer is 190w-200w higher than the initial radio frequency power of the fourth step-gradient stress DLC layer.
The radio frequency power difference value of the preferable third step gradient stress DLC layer and the fourth step gradient stress DLC layer can avoid the problem of film explosion.
Preferably, in S2 and S3, the depositing steps of the first step-graded stress DLC layer and the third step-graded stress DLC layer include: introducing 20-25 sccm argon and 10-18 sccm butane under vacuum condition, setting the initial radio frequency power to 1000-1100 w, and regulating the radio frequency power to 5-8 w every 1min, wherein the total deposition time is 15-20 min.
The preferable deposition step controls the stress of the first step gradient stress DLC layer and the third step gradient stress DLC layer to be step gradient, thereby reducing the integral stress of the film layer and further avoiding the problem of film explosion when coating films on the large-caliber deep curved infrared window.
Preferably, in S2 and S3, the depositing steps of the second step graded stress DLC layer and the fourth step graded stress DLC layer include: introducing 20-25 sccm argon and 10-18 sccm butane under vacuum condition, setting the initial radio frequency power to 800-900 w, regulating the radio frequency power to 5-8 w every 1min, and depositing for 20-25 min.
The preferable deposition step controls the stress of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer to be in step gradient, so that the integral stress of the film layer is reduced, and the problem of film explosion during film coating on the large-caliber deep curved infrared window is avoided.
Preferably, in S2 and S3, after the second step gradient stress DLC layer and the fourth step gradient stress DLC layer are deposited, cooling for 4h-5h along with the furnace.
The preferable furnace cooling time can reduce the stress of the film layer and avoid the film.
Preferably, in S4, the conditions of the ion beam assisted vapor deposition method are as follows: argon with the flow of 20-30 sccm is introduced into the ion source environment, and the beam current of the ion source is regulated to 40-60 mA.
Preferably, in S4, the conditions of the first zinc sulfide layer, the second zinc sulfide layer and the third zinc sulfide layer when deposited are: the deposition rate is 0.3nm/s-0.5nm/s, the evaporation beam current is 15mA-25mA, and the extraction pressure of the electron beam is 8kV-10kV.
Preferably, in S4, the conditions of the germanium layer during deposition are as follows: the deposition rate is 0.1nm/s-0.2nm/s, the evaporation beam current is 200mA-300mA, and the extraction pressure of the electron beam is 8kV-10kV.
Preferably, in S4, the conditions of the ytterbium fluoride layer during deposition are: the deposition rate is 0.3nm/s-0.5nm/s, the evaporation beam current is 60mA-80mA, and the extraction pressure of the electron beam is 8kV-10kV.
According to the invention, through the reasonably designed large-caliber deep-curved-surface infrared window anti-reflection protection structure, the problem that the large-caliber deep-curved-surface infrared window is easy to burst or take off film when being coated or soaked in water for a long time is avoided, and the scratch resistance, the friction resistance and the high transmittance of the large-caliber deep-curved-surface infrared window anti-reflection protection structure are further improved, and the adhesive force between the hard protection film layer and the substrate is further improved.
Drawings
FIG. 1 is a diagram showing an anti-reflection protection structure of a large-caliber deep curved surface infrared window according to embodiment 1 of the present invention;
FIGS. 2 (A) and 2 (B) are schematic diagrams of the loading of the substrate and the tray;
wherein 1 is a substrate, 2 is a fixing device with the same curvature radius as the upper surface of the substrate, and R is the curvature radius.
Detailed Description
The present invention will be described in further detail with reference to the following examples and drawings in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The embodiment provides a large-caliber deep curved surface infrared window anti-reflection protection structure, which comprises an anti-reflection film layer, a substrate, a transition matching layer and a hard protection film layer from bottom to top;
wherein, the substrate is made of Si, the caliber is more than or equal to 200mm, and the sagittal height is more than or equal to 25mm;
the antireflection film layer sequentially comprises a first zinc sulfide layer with the thickness of 330nm, a germanium layer with the thickness of 130nm, a second zinc sulfide layer with the thickness of 570nm, a ytterbium fluoride layer with the thickness of 1100nm and a third zinc sulfide layer with the thickness of 180nm from the substrate to the outside;
the matching transition layer is made of Si;
the hard protection film layer sequentially comprises a first step gradient stress DLC layer with the thickness of 370nm, a second step gradient stress DLC layer with the thickness of 370nm, a third step gradient stress DLC layer with the thickness of 370nm and a fourth step gradient stress DLC layer with the thickness of 370nm from the substrate to the outside, wherein the inner stresses of the first step gradient stress DLC layer and the third step gradient stress DLC layer are respectively reduced to 2.7GPa from 3.2GPa from the substrate to the outside, and the inner stresses of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer are respectively reduced to 1.8GPa from 2.3GPa from the substrate to the outside.
The preparation method of the large-caliber deep curved surface infrared window anti-reflection protection structure comprises the following steps:
s1, setting the electron beam extraction voltage as 10kV, the evaporation beam current as 200mA and the evaporation rate as 0.1nm/S, and depositing a matching transition layer on one side of a substrate by an ion beam assisted evaporation deposition method; wherein, the substrate is soaked by absolute ethyl alcohol before coating, and then is scrubbed by a mixture of absolute ethyl alcohol and diethyl ether;
s2, placing the substrate in a fixing device, and sequentially depositing a first step gradient stress DLC layer and a second step gradient stress DLC layer on the matched transition layer by a chemical vapor deposition method; the fixing device comprises a middle concave part and convex parts with two ends extending upwards and inwards, and an arc formed by extending the convex parts at the two ends has the same curvature radius as the upper surface of the substrate;
s3, horizontally rotating the fixing device in situ by 180 degrees, and sequentially depositing a third step gradient stress DLC layer and a fourth step gradient stress DLC layer on the second step gradient stress DLC layer by a chemical vapor deposition method;
s4, sequentially depositing a first zinc sulfide layer, a germanium layer, a second zinc sulfide layer, a ytterbium fluoride layer and a third zinc sulfide layer on the other side of the substrate by an ion beam assisted evaporation deposition method to obtain the large-caliber deep curved surface infrared window anti-reflection protection structure;
in S2 and S3, the depositing steps of the first step gradient stress DLC layer and the third step gradient stress DLC layer include: introducing 25sccm argon and 10sccm butane under vacuum condition, setting the initial radio frequency power to 1100w, regulating the radio frequency power to 8w every 1min, and depositing for 15min;
in S2 and S3, the steps of depositing the second step gradient stress DLC layer and the fourth step gradient stress DLC layer comprise the following steps: introducing 25sccm argon and 10sccm butane under vacuum condition, setting the initial radio frequency power to 900w, regulating the radio frequency power to 8w every 1min, and depositing for 20min;
s2 and S3, cooling for 4 hours along with a furnace after the deposition of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer is completed;
in S4, the conditions of the ion beam assisted vapor deposition method are: argon with the flow of 20sccm is introduced into the ion source environment, and the beam current of the ion source is regulated to be 60mA.
In S4, the conditions of the first zinc sulfide layer, the second zinc sulfide layer and the third zinc sulfide layer when deposited are: the deposition rate is 0.3nm/s, the evaporation beam current is 25mA, and the extraction pressure of the electron beam is 10kV;
in S4, the conditions of the germanium layer during deposition are: the deposition rate is 0.1nm/s, the evaporation beam current is 300mA, and the extraction pressure of the electron beam is 10kV;
in S4, the conditions of the ytterbium fluoride layer during deposition are: the deposition rate was 0.3nm/s, the evaporation beam current was 80mA, and the extraction pressure of the electron beam was 10kV.
Example 2
The embodiment provides a large-caliber deep curved surface infrared window anti-reflection protection structure, which comprises an anti-reflection film layer, a substrate, a matching transition layer and a hard protection film layer from bottom to top;
wherein the substrate is made of Ge, the caliber is more than or equal to 200mm, and the sagittal height is more than or equal to 25mm;
the antireflection film comprises a first zinc sulfide layer with the thickness of 350nm, a germanium layer with the thickness of 110nm, a second zinc sulfide layer with the thickness of 550nm, a ytterbium fluoride layer with the thickness of 1080nm and a third zinc sulfide layer with the thickness of 160nm from the substrate outwards in sequence;
the material of the matching transition layer is Ge;
the hard protection film layer sequentially comprises a first step gradient stress DLC layer with the thickness of 320nm, a second step gradient stress DLC layer with the thickness of 320nm, a third step gradient stress DLC layer with the thickness of 320nm and a fourth step gradient stress DLC layer with the thickness of 320nm from the substrate to the outside, wherein the internal stress of the first step gradient stress DLC layer and the third step gradient stress DLC layer is reduced to 2.5GPa from the substrate to the outside, and the internal stress of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer is reduced to 1.6GPa from the substrate to the outside from the substrate to the inside.
The preparation method of the large-caliber deep curved surface infrared window anti-reflection protection structure comprises the following steps:
s1, setting electron beam extraction voltage to be 8kV, setting evaporation beam current to be 300mA, setting evaporation rate to be 0.2nm/S, and depositing a matching transition layer on one side of a substrate by an ion beam assisted evaporation deposition method; wherein, the substrate is soaked by absolute ethyl alcohol before coating, and then is scrubbed by a mixture of absolute ethyl alcohol and diethyl ether;
s2, placing the substrate in a fixing device, and sequentially depositing a first step gradient stress DLC layer and a second step gradient stress DLC layer on the matched transition layer by a chemical vapor deposition method; the fixing device comprises a middle concave part and convex parts with two ends extending upwards and inwards, and an arc formed by extending the convex parts at the two ends has the same curvature radius as the upper surface of the substrate;
s3, horizontally rotating the fixing device in situ by 180 degrees, and sequentially depositing a third step gradient stress DLC layer and a fourth step gradient stress DLC layer on the second step gradient stress DLC layer by a chemical vapor deposition method;
s4, sequentially depositing a first zinc sulfide layer, a germanium layer, a second zinc sulfide layer, a ytterbium fluoride layer and a third zinc sulfide layer on the other side of the substrate by an ion beam assisted evaporation deposition method to obtain the large-caliber deep curved surface infrared window anti-reflection protection structure;
in S2 and S3, the depositing steps of the first step gradient stress DLC layer and the third step gradient stress DLC layer include: introducing 20sccm argon and 18sccm butane under vacuum condition, setting the initial radio frequency power to 1000w, regulating the radio frequency power to 5w every 1min, and depositing for 20min;
in S2 and S3, the steps of depositing the second step gradient stress DLC layer and the fourth step gradient stress DLC layer comprise the following steps: introducing 20sccm argon and 18sccm butane under vacuum condition, setting the initial radio frequency power to 800w, regulating the radio frequency power to 5w every 1min, and depositing for 25min;
s2 and S3, cooling for 5 hours along with a furnace after the deposition of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer is completed;
in S4, the conditions of the ion beam assisted vapor deposition method are: argon gas with the flow of 30sccm is introduced into the ion source environment, and the beam current of the ion source is regulated to 40mA.
In S4, the conditions of the first zinc sulfide layer, the second zinc sulfide layer and the third zinc sulfide layer when deposited are: the deposition rate is 0.5nm/s, the evaporation beam current is 15mA, and the extraction pressure of the electron beam is 8kV;
in S4, the conditions of the germanium layer during deposition are: the deposition rate is 0.2nm/s, the evaporation beam current is 200mA, and the extraction pressure of the electron beam is 8kV;
in S4, the conditions of the ytterbium fluoride layer during deposition are: the deposition rate was 0.5nm/s, the evaporation beam current was 60mA, and the extraction pressure of the electron beam was 8kV.
Example 3
The embodiment provides a large-caliber deep curved surface infrared window anti-reflection protection structure, which comprises an anti-reflection film layer, a substrate, a matching transition layer and a hard protection film layer from bottom to top;
wherein the substrate is made of Ge, the caliber is more than or equal to 200mm, and the sagittal height is more than or equal to 25mm;
the antireflection film layer sequentially comprises a first zinc sulfide layer with the thickness of 340nm, a germanium layer with the thickness of 120nm, a second zinc sulfide layer with the thickness of 560nm, a ytterbium fluoride layer with the thickness of 1090nm and a third zinc sulfide layer with the thickness of 170nm from the substrate to the outside;
the material of the matching transition layer is Ge;
the hard protection film layer sequentially comprises a first step gradient stress DLC layer with the thickness of 350nm, a second step gradient stress DLC layer with the thickness of 350nm, a third step gradient stress DLC layer with the thickness of 350nm and a fourth step gradient stress DLC layer with the thickness of 350nm from the substrate to the outside, wherein the internal stress of the first step gradient stress DLC layer and the third step gradient stress DLC layer is reduced to 2.6GPa from the substrate to the outside, and the internal stress of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer is reduced to 1.7GPa from the substrate to the outside from the 2.2GPa gradient.
The preparation method of the large-caliber deep curved surface infrared window anti-reflection protection structure comprises the following steps:
s1, setting the electron beam extraction voltage to be 9kV, setting the evaporation beam current to be 250mA, setting the evaporation rate to be 0.15nm/S, and depositing a matching transition layer on one side of a substrate by an ion beam assisted evaporation deposition method; wherein, the substrate is soaked by absolute ethyl alcohol before coating, and then is scrubbed by a mixture of absolute ethyl alcohol and diethyl ether;
s2, placing the substrate in a fixing device, and sequentially depositing a first step gradient stress DLC layer and a second step gradient stress DLC layer on the matched transition layer by a chemical vapor deposition method; the fixing device comprises a middle concave part and convex parts with two ends extending upwards and inwards, and an arc formed by extending the convex parts at the two ends has the same curvature radius as the upper surface of the substrate;
s3, horizontally rotating the fixing device in situ by 180 degrees, and sequentially depositing a third step gradient stress DLC layer and a fourth step gradient stress DLC layer on the second step gradient stress DLC layer by a chemical vapor deposition method;
s4, sequentially depositing a first zinc sulfide layer, a germanium layer, a second zinc sulfide layer, a ytterbium fluoride layer and a third zinc sulfide layer on the other side of the substrate by an ion beam assisted evaporation deposition method to obtain the large-caliber deep curved surface infrared window anti-reflection protection structure;
in S2 and S3, the depositing steps of the first step gradient stress DLC layer and the third step gradient stress DLC layer include: introducing 22sccm argon and 15sccm butane under vacuum condition, setting initial radio frequency power to 1050w, regulating the radio frequency power down to 6w every 1min, and depositing for 18min;
in S2 and S3, the steps of depositing the second step gradient stress DLC layer and the fourth step gradient stress DLC layer comprise the following steps: introducing 22sccm argon and 15sccm butane under vacuum condition, setting the initial radio frequency power to 860w, regulating the radio frequency power to 8w every 1min, and depositing for 22min;
s2 and S3, cooling for 4.5 hours along with a furnace after the deposition of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer is completed;
in S4, the conditions of the ion beam assisted vapor deposition method are: argon gas with the flow of 25sccm is introduced into the ion source environment, and the beam current of the ion source is regulated to be 50mA.
In S4, the conditions of the first zinc sulfide layer, the second zinc sulfide layer and the third zinc sulfide layer when deposited are: the deposition rate is 0.4nm/s, the evaporation beam current is 20mA, and the extraction pressure of the electron beam is 9kV;
in S4, the conditions of the germanium layer during deposition are: the deposition rate is 0.15nm/s, the evaporation beam current is 250mA, and the extraction pressure of the electron beam is 9kV;
in S4, the conditions of the ytterbium fluoride layer during deposition are: the deposition rate was 0.4nm/s, the evaporation beam current was 70mA, and the extraction pressure of the electron beam was 9kV.
Comparative example 1
This comparative example provides an infrared window anti-reflection protection structure of heavy-calibre deep curved surface, and this comparative example is different from example 1 in that: the stresses of the first DLC layer, the second DLC layer, the third DLC layer and the fourth DLC layer are 2.3GPa, 1.4GPa, 2.3GPa and 1.4GPa, respectively;
the preparation method of the first DLC layer, the second DLC layer, the third DLC layer and the fourth DLC layer comprises the following steps: the first and third DLC layers are deposited by the following steps: introducing 25sccm argon and 10sccm butane under vacuum condition, setting the radio frequency power to 900w, keeping the radio frequency power unchanged, and depositing for 20min; the second and fourth DLC layers are deposited by the following steps: introducing 25sccm argon and 10sccm butane under vacuum condition, setting the radio frequency power to 650w, keeping the radio frequency power unchanged, and depositing for 25min.
Other procedure was the same as in example 1.
Comparative example 2
This comparative example provides an infrared window anti-reflection protection structure of heavy-calibre deep curved surface, and this comparative example is different from example 1 in that: the first DLC layer, the second DLC layer, the third DLC layer and the fourth DLC layer are integrated, the internal stress is 2.3GPa, and the stress of each layer is the same.
The DLC layer is deposited by the following steps: introducing 25sccm argon and 10sccm butane under vacuum condition, setting the radio frequency power to 900w, keeping the radio frequency power unchanged, and depositing for 80min.
Other procedure was the same as in example 1.
Application example
The large-caliber deep curved surface infrared window anti-reflection protection structures prepared in the embodiment 1, the comparative example 1 and the comparative example 2 are tested according to the detection standard in GJB2485-95, and the specific test method and the specific test result are as follows:
(1) transmittance test
The transmittance test is carried out on the large-caliber deep curved surface infrared window anti-reflection protection structure prepared in the embodiment 1 at the wave band of 8-12 mu m, and the average transmittance is more than 90%;
(2) adhesion test
Firmly adhering the adhesive tape to the surface of the film layer by using a 3M adhesive tape with the peel strength of more than 2.74N/cm and rapidly pulling the adhesive tape for 10 times from the edge of the part to the vertical direction of the surface;
detection result: the film layers of example 1 were free of peeling and damage, and the film layers of comparative examples 1 and 2 were peeled to some extent.
(3) Soaking experiments
Soaking the parts in trichloroethylene, acetone and absolute ethanol for 10min, and wiping with cotton cloth;
detection result: the film layers of example 1 did not show defects such as peeling, cracking, foaming, etc., whereas the film layers of comparative examples 1 and 2 showed peeling;
the parts were fully immersed in 4.5% sodium chloride solution for 24 hours;
detection result: the film layer of example 1 did not show defects such as peeling, cracking, foaming, etc., whereas the film layers of comparative examples 1 and 2 showed large-area peeling, and corroded spots appeared on the film layer surface at the non-peeling positions;
completely soaking the parts in distilled water for 24 hours;
detection result: the film layers of example 1 did not show defects such as peeling, cracking, foaming, etc., while the film layers of comparative examples 1 and 2 showed edge-to-edge peeling.
(4) Friction experiment
The film layer is rubbed by a rubber friction head with the pressure of 9.8N for 40 times;
detection result: the film of example 1 had no scratch or other damage marks, whereas the films of comparative examples 1 and 2 had scratches and the partial film had small cracks.
(5) Experiment of temperature and damp-heat
High-low temperature experiment: placing the coated part into a high-low temperature test box, setting the heating and cooling speeds of the high-low temperature test box to be less than 2 ℃ per minute, and respectively keeping the temperature at-62 ℃ and 70 ℃ for 2 hours;
detection result: the film layer of example 1 has no peeling, foaming, cracking, stripping and other phenomena, while the film layers of comparative examples 1 and 2 have pinholes exposing the substrate, and the film layer at the edge has stripping phenomena;
damp-heat experiment: placing the coated part into a high-low temperature test box, setting the temperature to be 50 ℃ and the relative humidity to be 95%, and keeping the temperature for 24 hours;
detection result: the film of example 1 was free of peeling, blistering, cracking, peeling, etc., while the films of comparative examples 1 and 2 exhibited pinholes exposing the substrate and edge film curling.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (9)
1. The large-caliber deep curved surface infrared window anti-reflection protection structure is characterized by comprising a substrate, wherein a transition matching layer and an anti-reflection film layer are respectively and correspondingly arranged on the upper surface and the lower surface of the substrate, and a hard protection film layer is arranged on the matching transition layer;
the hard protective film layer sequentially comprises a first step gradient stress DLC layer, a second step gradient stress DLC layer, a third step gradient stress DLC layer and a fourth step gradient stress DLC layer from the substrate outwards;
the internal stress of the first step gradient stress DLC layer, the second step gradient stress DLC layer, the third step gradient stress DLC layer and the fourth step gradient stress DLC layer is gradually reduced from the substrate to the outside;
the inner stresses of the first step gradient stress DLC layer and the third step gradient stress DLC layer are higher than the inner stresses of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer;
the caliber of the substrate is more than or equal to 200mm, and the sagittal height is more than or equal to 25mm;
the internal stress of the first step gradient stress DLC layer and the third step gradient stress DLC layer is reduced from (3.0-3.2) GPa to (2.5-2.7) GPa; the internal stress of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer is reduced from (2.1-2.3) GPa to (1.6-1.8) GPa.
2. The large-caliber deep curved surface infrared window anti-reflection protection structure according to claim 1, wherein the substrate is made of Si or Ge; and/or
The material of the transition matching layer is Si or Ge; and/or
The antireflection film layer sequentially comprises a first zinc sulfide layer, a germanium layer, a second zinc sulfide layer, a ytterbium fluoride layer and a third zinc sulfide layer from the substrate to the outside.
3. The large caliber deep curved surface infrared window anti-reflection protection structure according to claim 2, wherein the thickness of the first zinc sulfide layer is 330-350nm; and/or
The thickness of the germanium layer is 110-130nm; and/or
The thickness of the second zinc sulfide layer is 550-570nm; and/or
The thickness of the ytterbium fluoride layer is 1080-1100nm; and/or
The thickness of the third zinc sulfide layer is 160-180nm.
4. The large-caliber deep curved surface infrared window anti-reflection protection structure according to claim 1, wherein the thickness of the first step gradient stress DLC layer is 320nm-370nm; and/or
The thickness of the second step gradient stress DLC layer is 320nm-370nm; and/or
The thickness of the third step gradient stress DLC layer is 320nm-370nm; and/or
The thickness of the fourth step gradient stress DLC layer is 320nm-370nm.
5. A method for preparing the large-caliber deep curved surface infrared window anti-reflection protection structure according to any one of claims 1 to 4, which is characterized by at least comprising the following steps:
s1, depositing a matching transition layer on one side of a substrate by an ion beam assisted evaporation deposition method;
s2, placing the substrate in a fixing device, and sequentially depositing a first step gradient stress DLC layer and a second step gradient stress DLC layer on the transition matching layer by a chemical vapor deposition method;
s3, horizontally rotating the fixing device in situ by 180 degrees, and sequentially depositing a third step gradient stress DLC layer and a fourth step gradient stress DLC layer on the second step gradient stress DLC layer by a chemical vapor deposition method;
and S4, sequentially depositing a first zinc sulfide layer, a germanium layer, a second zinc sulfide layer, a ytterbium fluoride layer and a third zinc sulfide layer on the other side of the substrate by an ion beam assisted evaporation deposition method to obtain the large-caliber deep curved surface infrared window anti-reflection protection structure.
6. The method for manufacturing an anti-reflection protection structure for a large-caliber deep curved surface infrared window according to claim 5, wherein in S2, the fixing device comprises a middle concave part and convex parts with two ends extending upwards and inwards, and an arc formed by the convex parts at the two ends in an extending way has the same curvature radius as the upper surface of the substrate; and/or
S2, the initial radio frequency power of the first step gradient stress DLC layer is 190w-200w higher than that of the second step gradient stress DLC layer; and/or
In S3, the initial radio frequency power of the third step gradient stress DLC layer is 190w-200w higher than that of the fourth step gradient stress DLC layer.
7. The method for preparing the large-caliber deep curved surface infrared window anti-reflection protection structure according to claim 6, wherein in S2 and S3, the steps of depositing the first step gradient stress DLC layer and the third step gradient stress DLC layer include: introducing 20-25 sccm argon and 10-18 sccm butane under vacuum condition, setting the initial radio frequency power to 1000-1100 w, and regulating the radio frequency power to 5-8 w every 1min, wherein the total deposition time is 15-20 min.
8. The method for preparing the large-caliber deep curved surface infrared window anti-reflection protection structure according to claim 6, wherein in S2 and S3, the depositing steps of the second step gradient stress DLC layer and the fourth step gradient stress DLC layer include: introducing 20-25 sccm argon and 10-18 sccm butane under vacuum condition, setting the initial radio frequency power to 800-900 w, regulating the radio frequency power to 5-8 w every 1min, and depositing for 20-25 min.
9. The method for preparing the large-caliber deep curved surface infrared window anti-reflection protection structure according to claim 5, wherein in S2 and S3, after the second step gradient stress DLC layer and the fourth step gradient stress DLC layer are deposited, cooling for 4h-5h along with a furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310840874.7A CN116892006B (en) | 2023-07-10 | 2023-07-10 | Large-caliber deep curved surface infrared window anti-reflection protection structure and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310840874.7A CN116892006B (en) | 2023-07-10 | 2023-07-10 | Large-caliber deep curved surface infrared window anti-reflection protection structure and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116892006A CN116892006A (en) | 2023-10-17 |
| CN116892006B true CN116892006B (en) | 2024-02-13 |
Family
ID=88311628
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310840874.7A Active CN116892006B (en) | 2023-07-10 | 2023-07-10 | Large-caliber deep curved surface infrared window anti-reflection protection structure and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116892006B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033653A (en) * | 1987-12-22 | 1989-07-05 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| JP2004010923A (en) * | 2002-06-04 | 2004-01-15 | Toyota Motor Corp | Sliding member and its production method |
| CN108754450A (en) * | 2018-07-03 | 2018-11-06 | 广东省新材料研究所 | A kind of low stress diamond-like multi-layer film and preparation method thereof |
| CN110106470A (en) * | 2019-04-28 | 2019-08-09 | 西安工业大学 | A kind of preparation method of low stress DLC film |
| CN113466972A (en) * | 2020-03-31 | 2021-10-01 | 华为技术有限公司 | Infrared anti-reflection lens and related assembly and equipment |
| CN113862613A (en) * | 2021-09-18 | 2021-12-31 | 美戈利(浙江)轨道交通研究院有限公司 | Amorphous gradient structure superhard DLC (diamond-like carbon) cutter coating and preparation method thereof and cutter |
| KR20230014330A (en) * | 2021-07-21 | 2023-01-30 | 대전대학교 산학협력단 | A stress control method of amorphous carbon layer |
-
2023
- 2023-07-10 CN CN202310840874.7A patent/CN116892006B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033653A (en) * | 1987-12-22 | 1989-07-05 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| JP2004010923A (en) * | 2002-06-04 | 2004-01-15 | Toyota Motor Corp | Sliding member and its production method |
| CN108754450A (en) * | 2018-07-03 | 2018-11-06 | 广东省新材料研究所 | A kind of low stress diamond-like multi-layer film and preparation method thereof |
| CN110106470A (en) * | 2019-04-28 | 2019-08-09 | 西安工业大学 | A kind of preparation method of low stress DLC film |
| CN113466972A (en) * | 2020-03-31 | 2021-10-01 | 华为技术有限公司 | Infrared anti-reflection lens and related assembly and equipment |
| KR20230014330A (en) * | 2021-07-21 | 2023-01-30 | 대전대학교 산학협력단 | A stress control method of amorphous carbon layer |
| CN113862613A (en) * | 2021-09-18 | 2021-12-31 | 美戈利(浙江)轨道交通研究院有限公司 | Amorphous gradient structure superhard DLC (diamond-like carbon) cutter coating and preparation method thereof and cutter |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116892006A (en) | 2023-10-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4869755A (en) | Encapsulation of a photovoltaic element | |
| US10473821B2 (en) | Optical member and its production method | |
| CN106199772B (en) | Radio wave transmissive multilayer optical coating | |
| CN1675059A (en) | Flexible electrically conductive film | |
| JPS63122533A (en) | Coating product and manufacture thereof | |
| EP0048542B2 (en) | Coating infra red transparent semiconductor material | |
| US5976684A (en) | Organic substrate provided with a light absorptive antireflection film and process for its production | |
| JP2006267561A (en) | Optical element and manufacturing method thereof | |
| US20170269263A1 (en) | Diamond coated antireflective window system and method | |
| CN116892006B (en) | Large-caliber deep curved surface infrared window anti-reflection protection structure and preparation method thereof | |
| US5674599A (en) | Deposited multi-layer device | |
| CN114019591B (en) | Optical element comprising anti-reflection protective film and preparation method thereof | |
| KR920002551B1 (en) | Antireflection film of optical parts made of synthetic resin | |
| US10705273B2 (en) | Multispectral interference coating with diamond-like carbon (DLC) film | |
| US7674417B2 (en) | Method of manufacturing window having at least one of radio wave stealth property and electromagnetic wave shield property, and window material having at least one of radio wave stealth property and electromagnetic wave shield property | |
| US20120263885A1 (en) | Method for the manufacture of a reflective layer system for back surface mirrors | |
| GB2082562A (en) | Coating germanium or silica with carbon | |
| CN112859208B (en) | Infrared window anti-reflection protective film | |
| CN210237752U (en) | High-temperature-resistant CO2Laser antireflection film | |
| CN110004408B (en) | High-temperature-resistant CO 2 Laser antireflection film and preparation method thereof | |
| CN114774847A (en) | Preparation method of low-stress protection anti-reflection film of large-size infrared optical element | |
| CN109576706A (en) | A kind of silicon base diamond-like protective film and preparation method thereof | |
| CN109932064B (en) | Infrared focal plane array detector with DLC protective film and preparation method thereof | |
| CN217239987U (en) | Semiconductor laser, anti-reflection film thereof and film coating device of semiconductor laser | |
| EP0581584A1 (en) | Antireflective plastic optical element and method for producing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |