Preparation method for plating 8-12 [mu] m DLC + AR film on zinc selenide substrate

Abstract

The invention discloses a preparation method for plating a DLC + AR film of 8-12 microns on a zinc selenide substrate. The preparation method comprises the steps of plating a DLC film layer and plating an AR film. The plating of the DLC film layer comprises the following steps of: cleaning a plating accompanying sheet serving as a zinc selenide substrate of the lens and a convex surface of a lens product; placing a tool clamp, and hanging the tool clamp into the cavity; vacuumizing and heating, and cleaning with an ion source; the convex surface is plated with 251 nm Ge / 211 nm ZnS / 667.6 nm Ge; cooling, and taking out the tool clamp and the lens; inspecting the smoothness; placing the accompanying plating sheet and a product with qualified smoothness in a carbon film machine; vacuumizing, and cleaning with an RF ion source; plating DLC (Diamond Like Carbon); cooling and taking out the lens. The plating of the AR film comprises the following steps: cleaning a surface corresponding to the concave surface of the lens; placing a tool clamp, and hanging the tool clamp into the cavity; vacuumizing, heating the cavity, and cleaning the ion source; plating 41.5 nm Ge / 1443 nm ZnSe / 1484 nm YbF3 / 65 nm ZnS on a concave surface, carrying out electron beam evaporation on Ge, carrying out resistance heating evaporation on ZnSe, YbF3 and ZnS, and carrying out ion source assisted deposition; cooling, and taking out the tool clamp together with the lens.

Description

Technical Field

[0001] The present disclosure relates to the field of optical coating, and more specifically to a preparation method of coating an 8-12 μm DLC+AR film on a zinc selenide substrate. Background Art

[0002] Zinc selenide (ZnSe) is a very good infrared material with a wide light transmission range, low absorption of infrared wavelengths, and can transmit visible light. It is a high-quality material for making infrared lenses, windows, output coupling mirrors and beam expanders. It can transmit from 0.5μm to 19μm and has good imaging and thermal shock properties. Zinc selenide lenses used as windows need to have the ability to operate normally for a long time in harsh environments, such as high-speed flight in the atmosphere, resistance to friction from foreign objects, resistance to rain immersion and corrosion in rainy and humid weather, etc. Diamond-like carbon film solves these problems well, but the adhesion of DLC film directly plated on zinc selenide substrate is poor. Summary of the invention

[0003] In view of the problems existing in the background technology, an object of the present invention is to provide a method for preparing an 8-12μm DLC+AR film coated on a zinc selenide substrate, wherein the prepared zinc selenide substrate together with the film system on both sides can achieve an average transmittance in the 8-12μm band greater than 92.5%.

[0004] Another object of the present disclosure is to provide a method for preparing an 8-12μm DLC+AR film plated on a zinc selenide substrate, wherein the prepared zinc selenide substrate accompanying coating sheet together with the film system on both sides can pass blister test, salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, constant temperature and humidity test, friction resistance test, low temperature test and high temperature test, so as to meet the requirements of being used as a window sheet in various environments and meet the requirements of the application end.

[0005] Therefore, a method for preparing a 8-12 μm DLC+AR film plated on a zinc selenide substrate comprises the following steps:

[0006] S1, coating a DLC film layer, including sub-steps:

[0007] S10, for the ZnSe substrate used as the lens and the lens products that need to be plated

[0008] Clean the surface corresponding to the convex surface of the DLC film layer;

[0009] S11, placing the cleaned lens into a fixture with the convex surface facing downward, and hanging the fixture with the lens placed into the cavity of the vacuum coating machine, and setting the temperature of the cavity to 130°C;

[0010] S12, the vacuum coating machine is started, vacuumed and heated, and the temperature of the cavity reaches the set temperature of the cavity and is kept constant for 2 hours. After that, the vacuum degree reaches 1.5×10 -3 When Pa, the Hall ion source of the vacuum coating machine was turned on for cleaning. The cleaning time was 6 min. The anode voltage of the Hall ion source was 220 V, the anode current was 1.2-1.5 A, the neutralization current was 1.3-1.5 A, the neutralization gas flow rate was 10 sccm, and the argon gas flow rate accounted for 100%;

[0011] S13, vacuum degree reaches 1.0×10 -3 When the temperature is 0.504°C, a dielectric layer consisting of 251nmGe / 211nmZnS / 667.6nmGe is deposited on the convex surface of the lens in sequence, wherein the numbers with nm before Ge and ZnS are the thicknesses of the corresponding film layers, the Ge film layer is evaporated by electron beam, the ZnS film layer is evaporated by resistance heating, the deposition rate of the Ge film layer is 0.4nm / s, the deposition rate of the ZnS film layer is 0.6nm / s, and each film layer of the dielectric layer is deposited by ion source assisted deposition and is deposited at the set temperature of the chamber;

[0012] S14, after the dielectric layer is plated, the cavity is naturally cooled to below 80°C, and the fixture and the lens are taken out;

[0013] S15, remove the lens coated with the dielectric layer from the fixture and check the smoothness of the dielectric layer of the product;

[0014] S16, placing the accompanying plating sheet and the product that has passed the surface finish inspection on the bottom plate of the carbon film machine with the dielectric layer facing upward;

[0015] S17, carbon film machine vacuum reaches 1.2×10 -3 Pa, the carbon film machine starts to clean the RF ion source, the cleaning time is 3min, the argon flow rate of the RF ion source is 20sccm and the power is 600-700W;

[0016] S18, carbon film machine vacuum reaches 8.0×10 -4 Pa started to deposit the DLC film, the methane gas flow rate was 160 sccm, the argon gas flow rate was 10 sccm, the RF power was 1000 W, the deposition time was 3800 s, and the thickness of the DLC film was 1200 nm;

[0017] S19, after the DLC film is coated, the carbon film machine is cooled for 50-60 minutes, and the door is opened to take out the lens; S2, AR film coating, including sub-steps:

[0018] S21, for the ZnSe substrate with DLC coating on the convex surface as the lens

[0019] Clean the surface of the plated sheet and lens products corresponding to the concave surface of the lens;

[0020] S22, placing the cleaned lens into a fixture with the concave surface facing downward, and hanging the fixture with the lens placed into the cavity of the vacuum coating machine, and setting the temperature of the cavity to 130°C;

[0021] S23, vacuum coating machine starts, vacuumizes and heats the cavity, and the vacuum degree reaches 1.5×10 -3 Pa and the temperature of the chamber reaches the set temperature, turn on the Hall ion source of the vacuum coating machine for cleaning. The cleaning time is 6 minutes. The anode voltage of the Hall ion source is 220V, the anode current is 1.2-1.5A, the neutralization current is 1.3-1.5A, the neutralization gas flow rate is 10sccm, and the argon gas flow rate accounts for 100%;

[0022] S24, vacuum degree reaches 1.0×10 -3 Pa, 41.

[0023] AR film composed of 5nmGe / 1443nmZnSe / 1484nmYbF3 / 65nmZnS, where the numbers with nm before Ge, ZnSe, YbF3 and ZnS are the thickness of the corresponding film layers. The Ge film layer is evaporated by electron beam, and the ZnSe film layer, YbF3 film layer and ZnS film layer are evaporated by resistance heating. The deposition rate of the Ge film layer is 0.4nm / s, and the deposition rate of the ZnSe film layer is 0.

[0024] 8nm / s, the deposition rate of the YbF3 film is 0.6nm / s, and the deposition rate of the ZnS film is 0.

[0025] 8nm / s, each film layer of the AR film is deposited using ion source assisted deposition and at the set temperature of the chamber;

[0026] S25, after the AR film is coated, the cavity is naturally cooled to below 80°C, and the fixture and the lens are taken out.

[0027] The beneficial effects of the present disclosure are as follows: In the preparation method of coating 8-12 μm DLC+AR film on zinc selenide substrate according to the present disclosure, through step S1 and step S2, by coating Sub (zinc selenide substrate) / Ge / ZnS / Ge / DLC / AIR (air) film system on the convex surface of the lens of zinc selenide substrate (i.e., coating DLC) and coating Sub (zinc selenide substrate) / Ge / ZnSe / YbF3 / ZnS / AIR (air) film system on the concave surface of the lens of zinc selenide substrate (i.e. AR film), as verified by the test process, the zinc selenide-based accompanying film together with the film system on both sides can not only achieve an average transmittance of more than 92.5% (specifically 92.8%) in the 8-12μm band, but also pass the blister test, salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, constant temperature and humidity test, friction resistance test (moderate friction test), low temperature test and high temperature test, so as to meet the use of window films in various environments and meet the requirements of the application end. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic structural diagram of a zinc selenide substrate and film systems on both sides prepared according to the preparation method of coating 8-12 μm DLC+AR film on a zinc selenide substrate disclosed in the present invention.

[0029] Figure 2 It is a transmittance curve of the accompanying coating sheet of Example 1 together with the DLC+AR films on both sides in the 8-12 μm band. DETAILED DESCRIPTION

[0030] The accompanying drawings show embodiments of the present disclosure, and it will be understood that the disclosed embodiments are merely examples of the present disclosure, and the present disclosure can be implemented in various forms. Therefore, the specific details disclosed herein should not be interpreted as limiting, but merely as the basis for the claims and as a representative basis for teaching ordinary technicians in the field to implement the present disclosure in various ways.

[0031] [Preparation method of 8-12μm DLC+AR film coated on zinc selenide substrate]

[0032] Reference Figure 1 According to the present invention, the method for preparing a 8-12 μm DLC+AR film on a zinc selenide substrate includes the following steps:

[0033] S1, coating a DLC film layer, including sub-steps:

[0034] S10, for the ZnSe substrate used as the lens and the lens products that need to be plated

[0035] Clean the surface corresponding to the convex surface of the DLC film layer;

[0036] S11, placing the cleaned lens into a fixture with the convex surface facing downward, and hanging the fixture with the lens placed into the cavity of the vacuum coating machine, and setting the temperature of the cavity to 130°C;

[0037] S12, the vacuum coating machine is started, vacuumed and heated, and the temperature of the cavity reaches the set temperature of the cavity and is kept constant for 2 hours. After that, the vacuum degree reaches 1.5×10 -3 When Pa, the Hall ion source of the vacuum coating machine was turned on for cleaning. The cleaning time was 6 min. The anode voltage of the Hall ion source was 220 V, the anode current was 1.2-1.5 A, the neutralization current was 1.3-1.5 A, the neutralization gas flow rate was 10 sccm, and the argon gas flow rate accounted for 100%;

[0038] S13, vacuum degree reaches 1.0×10 -3 When the lens is 1.50 mm thick, a dielectric layer consisting of 251 nm Ge / 211 nm ZnS / 667.6 nm Ge is deposited on the convex surface of the lens in sequence, wherein the numbers in front of Ge and ZnS are the thicknesses of the corresponding film layers. The Ge film layer is evaporated by electron beam, and the ZnS film layer is evaporated by resistance heating. The deposition rate of the Ge film layer is 0.4 nm / s, and the deposition rate of the ZnS film layer is 0.6 nm / s. Each film layer of the dielectric layer is deposited by ion source assistance and at the set temperature of the chamber.

[0039] Deposition under the degree;

[0040] S14, after the dielectric layer is plated, the cavity is naturally cooled to below 80°C, and the fixture and the lens are taken out;

[0041] S15, remove the lens coated with the dielectric layer from the fixture and check the smoothness of the dielectric layer of the product;

[0042] S16, placing the accompanying plating sheet and the product that has passed the surface finish inspection on the bottom plate of the carbon film machine with the dielectric layer facing upward;

[0043] S17, carbon film machine vacuum reaches 1.2×10 -3 Pa, the carbon film machine starts to clean the RF ion source, the cleaning time is 3min, the argon flow rate of the RF ion source is 20sccm and the power is 600-700W;

[0044] S18, carbon film machine vacuum reaches 8.0×10 -4 Pa started to deposit the DLC film, the methane gas flow rate was 160 sccm, the argon gas flow rate was 10 sccm, the RF power was 1000 W, the deposition time was 3800 s, and the thickness of the DLC film was 1200 nm;

[0045] S19, after the DLC film is coated, the carbon film machine is cooled for 50-60 minutes, and the door is opened to take out the lens; S2, AR film coating, including sub-steps:

[0046] S21, cleaning the accompanying plated sheet of the zinc selenide substrate with the DLC film layer coated on the convex surface of the lens and the surface of the lens product corresponding to the concave surface of the lens;

[0048] S22, placing the cleaned lens into a fixture with the concave surface facing downward, and hanging the fixture with the lens placed into the cavity of the vacuum coating machine, and setting the temperature of the cavity to 130°C;

[0050] S23, vacuum coating machine starts, vacuumizes and heats the cavity, and the vacuum degree reaches 1.5×10 -3 Pa and the temperature of the chamber reaches the set temperature, turn on the Hall ion source of the vacuum coating machine for cleaning. The cleaning time is 6 minutes. The anode voltage of the Hall ion source is 220V, the anode current is 1.2-1.5A, the neutralization current is 1.3-1.5A, the neutralization gas flow rate is 10sccm, and the argon gas flow rate accounts for 100%;

[0052] S24, vacuum degree reaches 1.0×10 -3 When the temperature is 0.5040°C, an AR film composed of 41.5nmGe / 1443nmZnSe / 1484nmYbF3 / 65nmZnS is deposited on the concave surface of the lens in sequence, wherein the numbers with nm before Ge, ZnSe, YbF3 and ZnS are the thicknesses of the corresponding film layers, the Ge film layer is evaporated by electron beam, the ZnSe film layer, the YbF3 film layer and the ZnS film layer are evaporated by resistance heating, the deposition rate of the Ge film layer is 0.4nm / s, the deposition rate of the ZnSe film layer is 0.8nm / s, the deposition rate of the YbF3 film layer is 0.6nm / s, and the deposition rate of the ZnS film layer is 0.8nm / s, and each film layer of the AR film is deposited by ion source assisted deposition and is deposited at the set temperature of the chamber;

[0057] S25, after the AR film is coated, the cavity is naturally cooled to below 80°C, and the fixture and the lens are taken out.

[0058] In the preparation method of 8-12 μm DLC+AR film coated on a zinc selenide substrate according to the present disclosure, through step S1 and step S2, by coating the convex surface of the lens of the zinc selenide substrate with Sub (zinc selenide substrate) / Ge / ZnS / Ge / DLC / AIR (air) film system (i.e., coating DLC) and coating the concave surface of the lens of the zinc selenide substrate with Sub (zinc selenide substrate) / Ge / ZnSe / YbF3 / ZnS / AIR (air) film system (i.e., AR film), as verified by the test process, the accompanying plate of the zinc selenide substrate together with the film systems on both sides can not only achieve an average transmittance of more than 92.5% (specifically 92.8%) in the 8-12 μm band, but also pass the blister test, salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, constant temperature and humidity test, friction resistance test (moderate friction test), low temperature test and high temperature test, so as to meet the use of the window sheet in various environments and meet the requirements of the application end.

[0059] The cleaning of sub-step S10 and sub-step S21 is beneficial to improving the surface state of the corresponding surface of the film layer of the coating film system of the lens, and is helpful to improve the bonding performance between the film system on the corresponding surface and the corresponding surface of the lens. For example, in sub-step S10 and sub-step S21, ultrasonic cleaning is used for cleaning. Specifically, ultrasonic cleaning uses aluminum oxide polishing liquid polishing and then ultrasonic pure water cleaning. For example, the aluminum oxide polishing liquid uses a 0.1μm model polycrystalline diamond liquid of Nanjing Henry Precision Optics Co., Ltd. In step S10, for example, the accompanying plating sheet is a round sheet, and the thickness of the accompanying plating sheet is 2mm.

[0060] The temperature setting of the vacuum coating machine in sub-step S11 and sub-step S22 heats the lens through the cavity of the coating machine, which helps the growth of the film layer from the lens and reduces the film layer growth stress. In step S11 and sub-step S22, for example, the vacuum coating is Siwork ZZS-1350.

[0061] The ion source cleaning in sub-steps S12, S17 and S23 will separate the impurities and oil molecules adsorbed on the surface of the corresponding surface of the lens from the substrate surface, thereby greatly improving the interface state, which is helpful to improve the bonding performance between the film layer and the corresponding surface of the lens. At the same time, cleaning by the ion source can heat the corresponding surface of the lens, which is helpful for the growth of the film layer from the lens and reduces the growth stress of the film layer. In step S12 and sub-step S23, specifically, the anode current of the Hall ion source is 1.2A and the neutralization current is 1.5A. Specifically, in sub-step S17, the power of the RF ion source is 650W.

[0062] In sub-step S13, sub-step S18 and sub-step 24, for example, the crystal oscillator method is used to monitor the film thickness using the corresponding crystal oscillator pieces of the multiple crystal oscillator pieces of the crystal controller, the crystal controller controls the corresponding operation of the new crystal oscillator piece among the multiple crystal oscillator pieces, and the crystal oscillator frequency is not less than 5.99 MHz.

[0063] In sub-step S13, in one example, a Hall ion source is used as the ion source, and when the Ge film is deposited, the ion source parameters are: the neutralization current is 1.0A, the neutralization gas flow rate is 8sccm, the anode voltage is 150V, the anode current is 1.3A, and the argon gas flow rate accounts for 100%; when the ZnS film is deposited, the ion source parameters are: the neutralization current is 0.5A, the neutralization gas flow rate is 8sccm, the anode voltage is 100V, the anode current is 1.0A, and the argon gas flow rate accounts for 100%.

[0064] In sub-step 24, the ion source adopts a Hall ion source. When the Ge film is plated, the ion source parameters are: neutralization current is 1.5A, neutralization gas flow rate is 8sccm, anode voltage is 160V, anode current is 1.6A, and argon gas flow rate is 100%; when the ZnSe film is plated, the ion source parameters are: neutralization current is 0.6A, neutralization gas flow rate is 8sccm, anode voltage is 100V, anode current is 1.2A, and argon gas flow rate is 100%. When the YbF3 film is deposited, the ion source parameters are: the neutralization current is 0.6A, the neutralization gas flow rate is 8sccm, the anode voltage is 130V, the anode current is 1.3A, and the argon gas flow rate accounts for 100%; when the ZnS film is deposited, the ion source parameters are: the neutralization current is 0.6A, the neutralization gas flow rate is 8sccm, the anode voltage is 100V, the anode current is 1.2A, and the argon gas flow rate accounts for 100%.

[0065] In sub-step S15, for example, the smoothness of the dielectric layer of the product is detected as no dots, scratches or marks on the surface of the dielectric layer of the product are found by naked eyes.

[0066] In sub-step S16, for example, the carbon film machine is a Seawork HLWT700-VII.

[0067] After sub-step S25 is completed, in one example, the transmittance of the accompanying plate together with the films plated on both sides in the 8-12 μm band is greater than 92.5% on average.

[0068] After sub-step S25 is completed, in one example, the accompanying plating sheet together with the films on both sides pass the blister test, salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, friction resistance test, low temperature test and high temperature test.

[0069] [test]

[0070] Example 1

[0071] The preparation method of the zinc selenide substrate plated with 8-12 μm DLC+AR film of Example 1 adopts the following steps:

[0072] S1, coating the DLC film layer using the following sub-steps:

[0073] S10, cleaning the accompanying plating sheet of the zinc selenide substrate of the lens and the surface of the lens product corresponding to the convex surface to be plated with the DLC film layer, wherein the cleaning adopts ultrasonic cleaning, the ultrasonic cleaning adopts alumina polishing liquid polishing, and then ultrasonic pure water cleaning, the alumina polishing liquid adopts 0.1μm polycrystalline diamond liquid of Nanjing Henry Precision Optics Co., Ltd., the accompanying plating sheet is a round sheet, and the thickness of the accompanying plating sheet is 2mm;

[0074] S11, put the cleaned lens into the fixture with the convex surface facing downward, and hang the fixture with the lens into the cavity of the vacuum coating machine. The temperature of the cavity is set to 130°C. The vacuum coating machine is Siwork ZZS-1350;

[0075] S12, the vacuum coating machine is started, vacuumed and heated, and the temperature of the cavity reaches the set temperature of the cavity and is kept constant for 2 hours. After that, the vacuum degree reaches 1.5×10 -3 When Pa, the Hall ion source of the vacuum coating machine was turned on for cleaning. The cleaning time was 6 min. The anode voltage of the Hall ion source was 220 V, the anode current was 1.2 A, the neutralization current was 1.5 A, the neutralization gas flow rate was 10 sccm, and the argon gas flow rate accounted for 100%;

[0076] S13, vacuum degree reaches 1.0×10 -3 When the temperature is 0.504°C, a dielectric layer consisting of 251nmGe / 211nmZnS / 667.6nmGe is deposited on the convex surface of the lens in sequence, wherein the numbers with nm before Ge and ZnS are the thicknesses of the corresponding film layers. The Ge film layer is evaporated by electron beam, and the ZnS film layer is evaporated by resistance heating. The deposition rate of the Ge film layer is 0.4nm / s, and the deposition rate of the ZnS film layer is 0.6nm / s. Each film layer of the dielectric layer is deposited by ion source assisted deposition and is deposited at the set temperature of the chamber.

[0077] In sub-step S13,

[0078] The ion source adopts Hall ion source.

[0079] When depositing the Ge film layer, the ion source parameters are: neutralization current is 1.0A, neutralization gas flow rate is 8sccm, anode voltage is 150V, anode current is 1.3A, and argon gas flow rate is 100%;

[0080] When the ZnS film is plated, the ion source parameters are: neutralization current is 0.5A, neutralization gas flow rate is 8sccm, anode voltage is 100V, anode current is 1.0A, and argon gas flow rate is 100%; in sub-step S13,

[0081] The crystal oscillator method uses the corresponding crystal oscillator of multiple crystal oscillators of the crystal controller to monitor the film thickness. The crystal controller controls the corresponding operation of the new crystal oscillator among the multiple crystal oscillators.

[0082] The crystal frequency is not less than 5.99MHz;

[0083] S14, after the dielectric layer is plated, the cavity is naturally cooled to 80°C, and the fixture and the lens are taken out;

[0084] S15, removing the lens coated with the dielectric layer from the fixture, and inspecting the smoothness of the dielectric layer of the product. The smoothness of the dielectric layer of the product is inspected to be that no dots, scratches or marks are found on the surface of the dielectric layer of the product by naked eyes;

[0085] S16, placing the accompanying plating sheet and the qualified products after the finish inspection with the dielectric layer upward on the bottom plate of the carbon film machine, the carbon film machine is the West Work HLWT700-VII;

[0086] S17, carbon film machine vacuum reaches 1.2×10 -3 At Pa, the carbon film machine starts to clean the RF ion source, the cleaning time is 3 min, the argon flow rate of the RF ion source is 20 sccm and the power is 650 W;

[0087] S18, carbon film machine vacuum reaches 8.0×10 -4 Pa starts to plate the DLC film layer, the methane gas flow rate is 160sccm, the argon gas flow rate is 10sccm, the RF power is 1000W, the deposition time is 3800s, and the thickness of the DLC film layer is 1200nm. In sub-step S18, the film thickness is monitored by using a crystal oscillator method using a corresponding crystal oscillator of a plurality of crystal oscillators of a crystal controller, the crystal controller controls a new crystal oscillator of the plurality of crystal oscillators to work accordingly, and the crystal oscillator frequency is not less than 5.99MHz;

[0088] S19, after the DLC film is coated, the carbon film machine is cooled for 55 minutes, and the door is opened to take out the lens; S2, the AR film is coated using the following sub-steps:

[0089] S21, cleaning the accompanying plated sheet of the zinc selenide substrate with the DLC film layer on the convex surface of the lens and the surface of the lens product corresponding to the concave surface of the lens, wherein the cleaning is carried out by ultrasonic cleaning, and the ultrasonic cleaning is polished by aluminum oxide polishing liquid, and then ultrasonic pure water cleaning, and the aluminum oxide polishing liquid is a 0.1 μm polycrystalline diamond liquid of Nanjing Henry Precision Optics Co., Ltd.;

[0091] S22, placing the cleaned lens into a fixture with the concave surface facing downward, and hanging the fixture with the lens into the cavity of the vacuum coating machine. The temperature of the cavity is set to 130°C. The vacuum coating machine is Siwork ZZS-1350;

[0093] S23, vacuum coating machine starts, vacuumizes and heats the cavity, and the vacuum degree reaches 1.5×10 -3 When the temperature of the chamber reaches the set temperature, the Hall ion source of the vacuum coating machine is turned on for cleaning. The cleaning time is 6 minutes. The anode voltage of the Hall ion source is 220V, the anode current is 1.2A, the neutralization current is 1.5A, the neutralization gas flow rate is 10sccm, and the argon gas flow rate accounts for 100%;

[0096] S24, vacuum degree reaches 1.0×10 -3 When the temperature is 0.5000 ℃ and the tungsten oxide layer is 0.0440 ℃, the deposition rate of the Ge film is 0.4nm / s, the deposition rate of the ZnSe film is 0.8nm / s, the deposition rate of the YbF3 film is 0.6nm / s, and the deposition rate of the ZnS film is 0.8nm / s. Each film layer of the AR film is deposited by ion source assisted deposition and is deposited at the set temperature of the chamber.

[0100] In sub-step 24,

[0101] The ion source adopts Hall ion source.

[0102] When depositing the Ge film layer, the ion source parameters are: neutralization current is 1.5A, neutralization gas flow rate is 8sccm, anode voltage is 160V, anode current is 1.6A, and argon gas flow rate is 100%;

[0103] When depositing the ZnSe film, the ion source parameters are: neutralization current of 0.6A, neutralization gas flow of 8sccm, anode voltage of 100V, anode current of 1.2A, and argon gas flow ratio of 100%;

[0104] When depositing the YbF3 film, the ion source parameters are: neutralization current of 0.6A, neutralization gas flow of 8sccm, anode voltage of 130V, anode current of 1.3A, and argon gas flow ratio of 100%;

[0105] When depositing the ZnS film, the ion source parameters are: neutralization current of 0.6 A, neutralization gas flow of 8 sccm, anode voltage of 100 V, anode current of 1.2 A, and argon gas flow ratio of 100%;

[0106] In sub-step 24,

[0107] The crystal oscillator method is used to monitor the film thickness by using a corresponding crystal oscillator of a plurality of crystal oscillators of a crystal controller, the crystal controller controls a new crystal oscillator of the plurality of crystal oscillators to work correspondingly, and the crystal oscillator frequency is not less than 5.99 MHz;

[0108] S25, after the AR film is coated, the cavity is naturally cooled to 80°C, and the fixture and the lens are taken out.

[0109] Figure 2 The transmittance curve of the accompanying plate of Example 1 together with the DLC+AR films on both sides in the 8-12 μm band. Figure 2 It can be seen that the transmittance of the accompanying coating sheet of Example 1 together with the films on both sides in the 8-12 μm band is 92.8% (ie greater than 92.5%) on average.

[0110] The accompanying plating sheet of Example 1 and the films on both sides were tested as follows.

[0111] Water bubble test: Take tap water to carry out water bubble test for 2 hours, no film system on each side of the accompanying plating sheet is found to fall off from the accompanying plating sheet, and no film system on each side is found to be cracked.

[0112] Salt spray test: After 48 hours of neutral salt spray test, no film peeling or cracking on the surfaces of the accompanying plating sheets was found.

[0113] Adhesion test: Use hand to stick 3M tape on each side of the plating sheet and pull the tape in the direction opposite to the sticking end. The film layer is not pulled up.

[0114] Thermal shock test: In a high and low temperature box, thermal shock was carried out in the range of -40℃ to 85℃ for 24 hours. No film falling off or cracking of the film on each surface of the accompanying plating sheet was found.

[0115] Constant temperature and humidity test: In a constant temperature and humidity chamber, at 50°C and 95% relative humidity for 48 hours, no film peeling or cracking of the film on each surface of the accompanying plating sheet was found.

[0116] Friction test (moderate friction test): Wrap the rubber friction head of the friction machine with degreased cloth, apply a pressure of 4.9N on the film surface of the accompanying plating sheet for 50 times (25 back and forth), and no scratches or damage were found on the film surface of each side of the accompanying plating sheet.

[0117] Low temperature test: in a low temperature box, at -40℃ for 48h, no film peeling or cracking of the film on each side of the accompanying plating sheet was found.

[0118] High temperature test: in a high temperature box, at 85℃ for 48h, no film peeling or cracking of the film on each side of the accompanying plating sheet was found.

[0119] That is, the accompanying plating sheet of Example 1 and the film systems on both sides all passed the above eight tests.

[0120] The above detailed description is used to describe multiple exemplary embodiments, but this document is not intended to be limited to the explicitly disclosed combinations. Therefore, unless otherwise stated, the various features disclosed herein can be combined together to form multiple additional combinations that are not shown for the sake of simplicity.

Claims

1. A method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate, characterized in that: Includes steps: S1, coating a DLC film layer, including sub-steps: S10, cleaning the accompanying plated sheet as the zinc selenide substrate of the lens and the surface of the lens product corresponding to the convex surface on which the DLC film layer needs to be plated; S11, placing the cleaned lens into a fixture with the convex surface facing downward, and hanging the fixture with the lens placed into the cavity of the vacuum coating machine, and setting the temperature of the cavity to 130°C; S12, the vacuum coating machine is started, vacuumed and heated, and the temperature of the cavity reaches the set temperature of the cavity and is kept constant for 2 hours. After that, the vacuum degree reaches 1.5×10 -3 When Pa, the Hall ion source of the vacuum coating machine was turned on for cleaning. The cleaning time was 6 min. The anode voltage of the Hall ion source was 220 V, the anode current was 1.2-1.5 A, the neutralization current was 1.3-1.5 A, the neutralization gas flow rate was 10 sccm, and the argon gas flow rate accounted for 100%; S13, vacuum degree reaches 1.0×10 -3 When the temperature is 0.504°C, a dielectric layer consisting of 251nmGe / 211nmZnS / 667.6nmGe is deposited on the convex surface of the lens in sequence, wherein the numbers with nm before Ge and ZnS are the thicknesses of the corresponding film layers, the Ge film layer is evaporated by electron beam, the ZnS film layer is evaporated by resistance heating, the deposition rate of the Ge film layer is 0.4nm / s, the deposition rate of the ZnS film layer is 0.6nm / s, and each film layer of the dielectric layer is deposited by ion source assisted deposition and is deposited at the set temperature of the chamber; S14, after the dielectric layer is plated, the cavity is naturally cooled to below 80°C, and the fixture and the lens are taken out; S15, remove the lens coated with the dielectric layer from the fixture and check the smoothness of the dielectric layer of the product; S16, placing the accompanying plating sheet and the product that has passed the surface finish inspection on the bottom plate of the carbon film machine with the dielectric layer facing upward; S17, carbon film machine vacuum reaches 1.2×10 -3 Pa, the carbon film machine starts to clean the RF ion source, the cleaning time is 3min, the argon flow rate of the RF ion source is 20sccm and the power is 600-700W; S18, carbon film machine vacuum reaches 8.0×10 -4 Pa started to deposit the DLC film, the methane gas flow rate was 160 sccm, the argon gas flow rate was 10 sccm, the RF power was 1000 W, the deposition time was 3800 s, and the thickness of the DLC film was 1200 nm; S19, after the DLC film is deposited, the carbon film machine is cooled for 50-60 minutes, and the door is opened to take out the lens; S2, coating an AR film, including sub-steps: S21, cleaning the accompanying plated sheet of the zinc selenide substrate with the DLC film layer coated on the convex surface of the lens and the surface of the lens product corresponding to the concave surface of the lens; S22, put the cleaned lens into the fixture with the concave surface facing downward. The fixture with the lens is hung into the chamber of the vacuum coating machine, and the temperature of the chamber is set to 130°C; S23, vacuum coating machine starts, vacuumizes and heats the cavity, and the vacuum degree reaches 1.5×10 -3 Pa and the temperature of the chamber reaches the set temperature, turn on the Hall ion source of the vacuum coating machine for cleaning. The cleaning time is 6 minutes. The anode voltage of the Hall ion source is 220V, the anode current is 1.2-1.5A, the neutralization current is 1.3-1.5A, and the neutralization gas flow rate is 10sccm. The argon flow rate accounts for 100%; S24, vacuum degree reaches 1.0×10 -3 Pa, 41. AR film composed of 5nmGe / 1443nmZnSe / 1484nmYbF3 / 65nmZnS, among which, The numbers in nm before Ge, ZnSe, YbF3 and ZnS are the thickness of the corresponding film layers. The Ge film layer was evaporated by electron beam, and the ZnSe film layer, YbF3 film layer and ZnS film layer were evaporated by resistance heating. The deposition rate of the Ge film layer was 0.4nm / s, and the deposition rate of the ZnSe film layer was 0. 8nm / s, the deposition rate of the YbF3 film is 0.6nm / s, and the deposition rate of the ZnS film is 0. 8nm / s, each film layer of the AR film is deposited using ion source assisted deposition and at the set temperature of the chamber; S25, after the AR film is coated, the cavity is naturally cooled to below 80°C, and the fixture and the lens are taken out.

2. The method for preparing a 8-12 μm DLC+AR film by coating a zinc selenide substrate according to claim 1, characterized in that: In sub-step S10 and sub-step S21 , ultrasonic cleaning is used for cleaning.

3. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 2, characterized in that: Ultrasonic cleaning uses aluminum oxide polishing liquid for polishing, followed by ultrasonic pure water cleaning. The alumina polishing liquid adopts the 0.1μm polycrystalline diamond liquid produced by Nanjing Henry Precision Optics Co., Ltd.

4. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 1, characterized in that: In step S10, the accompanying plating sheet is a round sheet, and the thickness of the accompanying plating sheet is 2 mm; and / or In step S11 and sub-step S22, the vacuum coating machine is a Siwork ZZS-1350; and / or In step S12 and sub-step S23, the anode current of the Hall ion source is 1.2A and the neutralization current is 1.5A.

5. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 1, characterized in that: In sub-step S13, sub-step S18 and sub-step 24, The crystal oscillator method is used to monitor the film thickness using the corresponding crystal oscillator pieces of the multiple crystal oscillator pieces of the crystal controller. The crystal controller controls the corresponding operation of a new crystal oscillator piece among the multiple crystal oscillator pieces, and the crystal oscillator frequency is not less than 5.99 MHz.

6. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 1, characterized in that: In sub-step S13, The ion source adopts Hall ion source. When depositing the Ge film layer, the ion source parameters are: neutralization current is 1.0A, neutralization gas flow rate is 8sccm, anode voltage is 150V, anode current is 1.3A, and argon gas flow rate is 100%; When depositing the ZnS film layer, the ion source parameters are: neutralization current of 0.5 A, neutralization gas flow rate of 8 sccm, anode voltage of 100 V, anode current of 1.0 A, and argon gas flow rate of 100%.

7. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 1, characterized in that: In sub-step 24, The ion source adopts Hall ion source. When depositing the Ge film layer, the ion source parameters are: neutralization current is 1.5A, neutralization gas flow rate is 8sccm, anode voltage is 160V, anode current is 1.6A, and argon gas flow rate is 100%; When depositing the ZnSe film, the ion source parameters are: neutralization current of 0.6A, neutralization gas flow of 8sccm, anode voltage of 100V, anode current of 1.2A, and argon gas flow ratio of 100%; When depositing the YbF3 film, the ion source parameters are: neutralization current of 0.6A, neutralization gas flow of 8sccm, anode voltage of 130V, anode current of 1.3A, and argon gas flow ratio of 100%; When depositing the ZnS film, the ion source parameters are: neutralization current of 0.6 A, neutralization gas flow of 8 sccm, anode voltage of 100 V, anode current of 1.2 A, and argon gas flow ratio of 100%.

8. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 1, characterized in that: In sub-step S15, the smoothness of the dielectric layer of the product is detected as follows: no spots, scratches or marks are found on the surface of the dielectric layer of the product by naked eyes.

9. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 1, characterized in that: In sub-step S16, the carbon film machine is a Siwork HLWT700-VII; and / or In sub-step S17, the power of the RF ion source is 650W.

10. The method for preparing a 8-12 μm DLC+AR film by plating a zinc selenide substrate according to claim 1, characterized in that: After sub-step S25 is completed, the transmittance of the accompanying plated sheet and the films plated on both sides in the 8-12 μm band is greater than 92.5% on average; After sub-step S25 is completed, the accompanying plating sheet together with the films on both sides pass the blister test, salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, friction resistance test, low temperature test and high temperature test.

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