Preparation method of zinc selenide-based antireflection film system with wavelength of 1064nm and high reflectivity at wave band of 7.7-10.5 [mu] m

Abstract

The invention discloses a preparation method of a 1064nm-wavelength high-reflectivity 7.7-10.5 mu m waveband antireflection film system with a zinc selenide substrate. The preparation method comprises the following steps: S1, cleaning an accompanying plating sheet and a product of the zinc selenide substrate serving as a lens before plating, and preparing a film material; s2, putting the lens into a tool clamp, hanging the tool clamp into a cavity of a coating machine, vacuumizing and baking, and pre-melting a film material; s3, ion source cleaning; and S4, plating a first YbF3 film layer, a second ZnSe film layer, a third YbF3 film layer, a fourth ZnSe film layer, a fifth YbF3 film layer, a sixth ZnSe film layer, a seventh YbF3 film layer, an eighth ZnSe film layer, a ninth YbF3 film layer, a tenth ZnSe film layer, an eleventh YbF3 film layer, a twelfth ZnSe film layer, a thirteenth YbF3 film layer, a fourteenth ZnSe film layer and a fifteenth YbF3 film layer on the first surface of the lens under a vacuum condition. The sixteenth ZnSe film layer, the seventeenth YbF3 film layer and the eighteenth ZnSe film layer are subjected to ion source assisted deposition; s5, keeping at constant temperature after plating; s6, cooling and part taking; and S7, the step S1 to the step S6 are repeated, and the second face is plated.

Description

Technical Field

[0001] The present invention relates to the field of infrared coating technology, and more specifically to a method for preparing a zinc selenide substrate 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system. Background Art

[0002] In the field of modern optics and infrared technology, with the growing demand for high-performance optical films, how to achieve high reflection at a specific wavelength while maintaining high transmittance over a wide wavelength range has always been a hot topic and a difficult point in research. As an excellent infrared transmission material, zinc selenide has important implications for the design of infrared optical systems by improving its reflective performance at specific wavelengths. Summary of the invention

[0003] In view of the problems existing in the background technology, an object of the present disclosure is to provide a method for preparing a zinc selenide substrate 1064nm wavelength high reflective 7.7-10.5μm band anti-reflection film system, which can be used to achieve high reflectivity at 1064nm wavelength and high transmittance in the 7.7-10.5μm band.

[0004] One purpose of the present disclosure is to provide a method for preparing a zinc selenide substrate 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system, which can meet the GJB2485A-2019 acceptance.

[0005] Therefore, a method for preparing a 1064nm wavelength high-reflection 7.7-10.5μm band anti-reflection film system on a zinc selenide substrate comprises the following steps: S1, before plating, cleaning and YbF 3 , ZnSe two kinds of film material preparation work; S2, cleaned lens into the fixture, put the fixture with lens into the chamber of the coating machine, vacuum baking and film material pre-melting; S3, ion source cleaning lens; S4, under vacuum conditions, the first layer of YbF is plated on the first surface of the lens in turn 3 film layer, the second ZnSe film layer, the third YbF 3 film layer, the fourth ZnSe film layer, the fifth YbF 3 film layer, the sixth ZnSe film layer, the seventh YbF 3 film layer, the eighth ZnSe film layer, the ninth YbF 3 film layer, the tenth ZnSe film layer, the eleventh YbF 3 film layer, the twelfth ZnSe film layer, the thirteenth YbF 3 film layer, the fourteenth ZnSe film layer, the fifteenth YbF 3 film layer, the sixteenth ZnSe film layer, the seventeenth YbF 3The eighteen layers of the lens are deposited using an ion source to assist deposition; S5, maintaining a constant temperature after plating; S6, cooling and removing the lens; S7, repeating steps S1 to S6 to perform film coating on the second side of the lens.

[0006] The beneficial effects of the present disclosure are as follows.

[0007] In the method for preparing a highly reflective 7.7-10.5 μm band anti-reflection film system on a zinc selenide substrate at a wavelength of 1064 nm according to the present disclosure, the same film system structure is formed on both sides of the lens through steps S1 to S7. As verified by the test process described later, it can be used to achieve high reflectivity at a wavelength of 1064 nm and high transmittance in the 7.7-10.5 μm band. For example, the reflectivity at a wavelength of 1064 nm exceeds 99%, and the average transmittance in the 7.7-10.5 μm band exceeds 98.5%.

[0008] In the preparation method of the zinc selenide substrate 1064nm wavelength high reflection 7.7-10.5μm band anti-reflection film system according to the present disclosure, by using YbF 3 , ZnSe two kinds of film materials, YbF 3 The first to eighteenth layers are formed alternately with ZnSe on each surface, and the first to eighteenth layers are all deposited using an ion source to assist in deposition, which can meet the acceptance of GJB2485A-2019. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] Figure 1 It is a schematic structural diagram of a method for preparing a 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system on a zinc selenide substrate according to the present disclosure.

[0010] Figure 2 It is a reflectivity curve at 1064nm wavelength of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 1, which is plated on both sides of the accompanying plate.

[0011] Figure 3 It is a transmittance curve of the 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system of Example 1 in the 7.7-10.5μm band with zinc selenide substrate plated on both sides.

[0012] Figure 4 This is a reflectivity curve at 1064nm of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 2, which is plated on both sides of the accompanying plate.

[0013] Figure 5It is a transmittance curve diagram of the 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system of Example 2 in the 7.7-10.5μm band with zinc selenide substrate plated on both sides.

[0014] Figure 6 This is a reflectivity curve at 1064nm of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 3, which is plated on both sides of the accompanying plate.

[0015] Figure 7 It is a transmittance curve diagram of the 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system of Example 3 in the 7.7-10.5μm band with zinc selenide substrate plated on both sides.

[0016] Figure 8 This is a reflectivity curve of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 1 coated on both sides of the accompanying coating sheet at a wavelength of 1064nm.

[0017] Fig. 9 It is a transmittance curve of the 7.7-10.5 μm band antireflection film system of the 1064 nm wavelength high-reflection 7.7-10.5 μm band of the accompanying coating sheet of Example 1, which is plated on both sides of the zinc selenide substrate.

[0018] Fig.10 This is a reflectivity curve of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 2, which is plated on both sides of the accompanying plate.

[0019] Fig.11 It is a transmittance curve of the 7.7-10.5 μm band of the accompanying plate of Example 2, which is coated with a zinc selenide substrate with a 1064 nm wavelength high-reflection 7.7-10.5 μm band anti-reflection film on both sides.

[0020] Fig.12 This is a reflectivity curve of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 3, which is plated on both sides of the accompanying plate.

[0021] Fig.13 It is a transmittance curve of the 7.7-10.5 μm band of the 1064 nm wavelength high-reflective 7.7-10.5 μm band anti-reflection film system of the accompanying coating sheet of Example 3, which is plated on both sides of the zinc selenide substrate. DETAILED DESCRIPTION

[0022] It will be understood that the disclosed embodiments are merely examples of the present disclosure, which may be implemented in various forms, and therefore, the specific details disclosed herein should not be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one of ordinary skill in the art to implement the present disclosure in various ways.

[0023] [Preparation method of zinc selenide substrate 1064nm wavelength high reflection 7.7-10.5μm band anti-reflection film system]

[0024] Reference Figure 1 The preparation method of the high-reflection 7.7-10.5 μm band antireflection film system on a zinc selenide substrate with a wavelength of 1064 nm comprises the following steps:

[0025] S1, before plating, the accompanying plated sheet and products of the zinc selenide substrate used as the lens are cleaned and YbF 3 , ZnSe two kinds of film material preparation work;

[0026] S2, the cleaned lens is placed in a fixture, and the fixture with the lens is hung in the cavity of the coating machine for vacuum baking and pre-melting of the film material;

[0027] S3, ion source cleaning lens;

[0028] S4, the first layer of YbF is deposited on the first surface of the lens in a vacuum condition 3 film layer, the second ZnSe film layer, the third YbF 3 film layer, the fourth ZnSe film layer, the fifth YbF 3 film layer, the sixth ZnSe film layer, the seventh YbF 3 film layer, the eighth ZnSe film layer, the ninth YbF 3 film layer, the tenth ZnSe film layer, the eleventh YbF 3 film layer, the twelfth ZnSe film layer, the thirteenth YbF 3 film layer, the fourteenth ZnSe film layer, the fifteenth YbF 3 film layer, the sixteenth ZnSe film layer, the seventeenth YbF 3 The film layer, the eighteenth ZnSe film layer, and the eighteen film layers are all deposited using an ion source to assist deposition;

[0029] S5, constant temperature maintenance after plating;

[0030] S6, cooling and picking up;

[0031] S7, repeating steps S1 to S6 to perform film coating on the second surface of the lens.

[0032] In the method for preparing a highly reflective 7.7-10.5 μm band anti-reflection film system on a zinc selenide substrate at a wavelength of 1064 nm according to the present disclosure, the same film system structure is formed on both sides of the lens through steps S1 to S7. As verified by the test process described later, it can be used to achieve high reflectivity at a wavelength of 1064 nm and high transmittance in the 7.7-10.5 μm band. For example, the reflectivity at a wavelength of 1064 nm exceeds 99%, and the average transmittance in the 7.7-10.5 μm band exceeds 98.5%.

[0033] In the preparation method of the zinc selenide substrate 1064nm wavelength high reflection 7.7-10.5μm band anti-reflection film system according to the present disclosure, by using YbF 3 , ZnSe two kinds of film materials, YbF 3 The first to eighteenth layers are formed alternately with ZnSe on each surface, and the first to eighteenth layers are all deposited using an ion source to assist in deposition, which can meet the acceptance of GJB2485A-2019.

[0034] The cleaning in step S1 is beneficial to improving the surface state of the first and second surfaces of the lens, removing surface contaminants, ensuring cleanliness before coating, ensuring that there will be no interference from impurities during coating, and helping to improve the bonding performance between the film system structure on each surface and the corresponding surface of the lens, and improving the flatness of the film layer. For example, in step S1, the cleaning is performed by ultrasonic cleaning and manual wiping. For example, the thickness of the accompanying coating sheet is 1.0 mm.

[0035] The baking in step S2 prepares the temperature for pre-melting the film material. Pre-melting the film material can release the gas in the film material and remove the impurities in the film material to ensure the purity of the film material, thereby reducing the adverse factors that affect the quality of the film layer during the film coating process in step S4. In addition, baking also heats the lens. In one example, in step S2, the temperature of the chamber of the coating machine is set to 150°C; when the vacuum reaches (3.0-5.0)×10 -3 The film material is pre-melted at Pa. After the pre-melting of the film material is completed, the temperature of the cavity of the coating machine reaches 150°C and is kept constant for 15-20 minutes.

[0036] The ion source cleaning in step S3 uses ion bombardment to clean the surface microstructure of the lens, which can eliminate the oxide layer on the surface of the lens, making the surface of the lens cleaner and conducive to the firm adhesion and growth of the film layer. In one example, in step S3, when the vacuum degree reaches (1.0-2.0)×10 -3 Pa, start the ion source of the vacuum coating machine, and set the ion cleaning parameters of the ion source as follows: neutralization current 0.6A, neutralization gas flow rate 8sccm, anode voltage 220V, anode current 2A, argon flow rate in neutralization gas 100%, and cleaning time 250-350s.

[0037] In one example, in step S4, during the coating process, argon gas is filled into the chamber of the coating machine and evacuated to form a flowing vacuum, ensuring that the vacuum degree of the coating is maintained at (4.5-5.5)×10 -3 Pa, and maintain the coating temperature at 150°C.

[0038] In one example, in step S4, the evaporation mode of the film material is: YbF 3 Both Zn and ZnSe were evaporated using resistance heating.

[0039] In one example, in step S4, the deposition rate of the film material is: 3 The deposition rate of the film is The deposition rate of ZnSe film is

[0040] In one example, in step S4,

[0041] First layer YbF 3 The film thickness is 145.93±3nm.

[0042] The thickness of the second ZnSe film is 373.9±3nm.

[0043] The third layer YbF 3 The film thickness is 150.25±3nm.

[0044] The thickness of the fourth ZnSe film layer is 119.45±3nm.

[0045] Fifth layer YbF 3 The film thickness is 197.36±3nm.

[0046] The thickness of the sixth ZnSe film layer is 323.64±3nm.

[0047] The seventh layer YbF 3 The film thickness is 896.02±3nm.

[0048] The thickness of the eighth ZnSe film layer is 144±3nm.

[0049] Ninth floor YbF 3 The film thickness is 146.54±3nm.

[0050] The thickness of the tenth ZnSe film layer is 351.85±3nm.

[0051] 11th floor YbF 3 The film thickness is 216.78±3nm.

[0052] The thickness of the twelfth ZnSe film layer is 93.85±3nm.

[0053] Thirteenth floor YbF 3 The film thickness is 212.11±3nm.

[0054] The thickness of the fourteenth ZnSe film layer is 372.01±3nm.

[0055] The fifteenth floor YbF 3 The film thickness is 84.41±3nm.

[0056] The thickness of the sixteenth ZnSe film layer is 602.75±3nm.

[0057] The seventeenth floor YbF 3 The film thickness is 1318.9±3nm.

[0058] The thickness of the eighteenth ZnSe film layer is 95.35±3nm;

[0059] 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. After the ion source is cleaned, the crystal controller controls the corresponding operation of the new crystal oscillator pieces among the multiple crystal oscillator pieces, and the crystal oscillator frequency is not less than 6MHz.

[0060] In one example, in step S4, YbF is plated 3 The ion source parameters for the film layer are: neutralization current 0.6A, neutralization gas flow rate 8sccm, anode voltage 130V, anode current 1.3A, argon flow rate in the neutralization gas is 30%, and oxygen flow rate in the neutralization gas is 70%; the ion source parameters for plating the ZnSe film layer are: neutralization current 0.5A, neutralization gas flow rate 8sccm, anode voltage 100V, anode current 1A, and argon flow rate in the neutralization gas is 100%.

[0061] In one example, in step S5, after plating is completed, the chamber is kept at a constant temperature of 150°C for 5-15 minutes.

[0062] In one example, in step S6, the door is opened to take out the items when the temperature drops below 100°C.

[0063] [test]

[0064] Example 1

[0065] The preparation method of the zinc selenide substrate 1064nm wavelength high-reflection 7.7-10.5μm band anti-reflection film system of Example 1 adopts the following steps:

[0066] S1, before plating, ultrasonic cleaning and YbF 3 , ZnSe two kinds of film material preparation work, the thickness of the accompanying plating sheet is 1.0mm;

[0067] S2, the cleaned lens is placed in the fixture, and the fixture with the lens is hung in the cavity of the coating machine, vacuum baking and pre-melting of the film material. The coating machine is a vacuum coating machine with a Hall ion source with a neutralizer manufactured and sold by Chengdu Xiwoke Vacuum Technology Co., Ltd. The Hall ion source with a neutralizer is purchased from Boton Optoelectronics Technology Co., Ltd. The temperature of the cavity of the coating machine is set to 150°C. When the vacuum reaches 4.0×10 -3 The film material is pre-melted at Pa. After the pre-melting of the film material is completed, the temperature of the cavity of the coating machine reaches 150°C and is kept constant for 20 minutes.

[0068] S3, ion source cleaning lens, when the vacuum reaches 1.5×10 -3 Pa, start the ion source of the vacuum coating machine, and set the ion cleaning parameters of the ion source as follows: neutralization current 0.6A, neutralization gas flow rate 8sccm, anode voltage 220V, anode current 2A, argon flow rate in neutralization gas 100%, and cleaning time 300s;

[0069] S4, the first layer of YbF is deposited on the first surface of the lens in a vacuum condition 3 film layer, the second ZnSe film layer, the third YbF 3 film layer, the fourth ZnSe film layer, the fifth YbF 3 film layer, the sixth ZnSe film layer, the seventh YbF 3 film layer, the eighth ZnSe film layer, the ninth YbF 3 film layer, the tenth ZnSe film layer, the eleventh YbF 3 film layer, the twelfth ZnSe film layer, the thirteenth YbF 3 film layer, the fourteenth ZnSe film layer, the fifteenth YbF 3 film layer, the sixteenth ZnSe film layer, the seventeenth YbF 3 The film layer, the eighteenth ZnSe film layer, and the eighteen film layers are all deposited using an ion source to assist deposition;

[0070] Among them, in step S4,

[0071] During coating, argon gas is filled into the chamber of the coating machine and evacuated to form a flowing vacuum to ensure that the vacuum degree of the coating is maintained at 5.0×10 -3 Pa, and maintain the coating temperature at 150°C;

[0072] Yb 3 Both the ZnSe film and the ZnSe film are evaporated using resistance heating.

[0073] Yb 3 The deposition rate of the film is The deposition rate of ZnSe film is

[0074] First layer YbF 3 The film thickness is 145.93nm.

[0075] The thickness of the second ZnSe film is 373.9nm.

[0076] The third layer YbF 3 The film thickness is 150.25nm.

[0077] The thickness of the fourth ZnSe film layer is 119.45nm.

[0078] Fifth layer YbF 3 The film thickness is 197.36nm.

[0079] The thickness of the sixth ZnSe film layer is 323.64nm.

[0080] The seventh layer YbF 3 The film thickness is 896.02nm.

[0081] The thickness of the eighth ZnSe film layer is 144nm.

[0082] Ninth floor YbF 3 The film thickness is 146.54nm.

[0083] The thickness of the tenth ZnSe film layer is 351.85nm.

[0084] 11th floor YbF 3 The film thickness is 216.78nm.

[0085] The thickness of the twelfth ZnSe film layer is 93.85nm.

[0086] Thirteenth floor YbF 3 The film thickness is 212.11nm.

[0087] The thickness of the fourteenth ZnSe film layer is 372.01nm.

[0088] The fifteenth floor YbF 3 The film thickness is 84.41nm.

[0089] The thickness of the sixteenth ZnSe film layer is 602.75nm.

[0090] The seventeenth floor YbF 3 The film thickness is 1318.9nm.

[0091] The thickness of the eighteenth ZnSe film layer is 95.35 nm;

[0092] YbF plated 3 The ion source parameters during the film layer were: neutralization current 0.6A, neutralization gas flow rate 8sccm, anode voltage 130V, anode current 1.3A, argon flow rate in neutralization gas 30%, oxygen flow rate in neutralization gas 70%;

[0093] The ion source parameters when depositing the ZnSe film layer are: neutralization current 0.5A, neutralization gas flow rate 8sccm, anode voltage 100V, anode current 1A, and argon gas flow rate in the neutralization gas is 100%;

[0094] The crystal oscillator method uses the corresponding crystal oscillator of the multiple crystal oscillators of the crystal controller to monitor the film thickness. After the ion source is cleaned, the crystal controller controls the corresponding operation of the new crystal oscillator among the multiple crystal oscillators.

[0095] The crystal frequency is 6MHz;

[0096] S5, after plating is completed, the cavity is kept at a constant temperature of 150°C for 10 minutes;

[0097] S6, wait until the temperature drops below 100°C and then open the door to take out the items;

[0098] S7, repeating steps S1 to S6 to perform film coating on the second surface of the lens.

[0099] Example 2

[0100] Except for the vacuum degree of 3.0×10 -3 Pa, the vacuum degree involved in step S3 is 1.0×10 -3 Pa, the vacuum degree of step S4 was maintained at 4.50×10 -3 Except that the constant temperature of step S5 is 5 min, the rest is the same as that of embodiment 1.

[0101] Example 3

[0102] Except for the vacuum degree of 5.0×10 -3 Pa, the vacuum degree involved in step S3 is 2.0×10 -3 Pa, the vacuum degree of step S4 was maintained at 5.5×10 -3 Except that the constant temperature of step S5 is 15 min, the rest is the same as that of embodiment 1.

[0103] Comparative Example 1

[0104] Except that in step S4, the eighteen film layers are not deposited using an ion source, the rest is the same as in Example 1.

[0105] Comparative Example 2

[0106] In addition to preparing Y in step S1 2 O 3 Film material, the first layer in step S4 is Y with a film thickness of 20nm 2 O 3 Film layer, Y 2 O 3 The film layer is evaporated by electron beam heating, 2 O 3 The deposition rate of the film is Using ion source to assist deposition and plating Y 2 O 3 The ion source parameters during the film layer are: neutralization current 0.5A, neutralization gas flow rate 8sccm, anode voltage 180V, anode current 1.8A, argon flow rate in neutralization gas is 20%, oxygen flow rate in neutralization gas is 80%, and the coating temperature is maintained at 180°C. The rest is the same as Example 1.

[0107] Comparative Example 3

[0108] Except for the eighteenth layer of YbF with a thickness of 95.35 nm in step S4, 3 Except for the film layer, the rest is the same as in Example 1.

[0109] In accordance with GJB2485A-2019, the following tests were performed on both sides of Examples 1-3 and Comparative Examples 1-3 after coating.

[0110] Water bubble test: Take tap water to conduct a water bubble test for 2 hours to observe whether the film layer on each surface falls off from the accompanying plating sheet and whether the film layer on each surface is cracked.

[0111] Salt spray test: neutral salt spray test for 48 hours, observe whether the film layer on each side of the accompanying plating sheet falls off, observe whether the film layer on each side of the accompanying plating sheet cracks.

[0112] Adhesion test: After the blister or salt spray test with tap water is completed, stick 3M tape on each side of the PCB by hand and pull the tape in the direction opposite to the sticking end to observe whether the film layer is pulled up.

[0113] The blister test and the tape adhesion test can be used to determine whether the film adhesion on both sides of the plating sheet is good.

[0114] Thermal shock test: In a high and low temperature box, perform thermal shock test in the range of -40℃ to 85℃ for 24 hours to observe whether the film layers on each side of the accompanying plating sheet fall off or crack.

[0115] Constant temperature and humidity test: In a constant temperature and humidity chamber, at 50°C and 95% relative humidity for 48 hours, observe whether the film layers on each side of the accompanying plating sheet fall off or crack.

[0116] Low temperature test: In a low temperature box, at -40℃ for 48h, observe whether the film layers on each side of the accompanying plating sheet fall off, and observe whether the film layers on each side of the accompanying plating sheet crack.

[0117] High temperature test: In a high temperature box, at 85℃ for 48h, observe whether the film layers on each side of the accompanying plating sheet fall off, and observe whether the film layers on each side of the accompanying plating sheet crack.

[0118] Figure 2 It is a reflectivity curve at 1064nm wavelength of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 1, which is plated on both sides of the accompanying plate. Figure 3 It is a transmittance curve of the 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system of Example 1 in the 7.7-10.5μm band with zinc selenide substrate plated on both sides.

[0119] Figure 4 This is a reflectivity curve at 1064nm of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 2, which is plated on both sides of the accompanying plate. Figure 5 It is a transmittance curve diagram of the 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system of Example 2 in the 7.7-10.5μm band with zinc selenide substrate plated on both sides.

[0120] Figure 6 This is a reflectivity curve at 1064nm of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 3, which is plated on both sides of the accompanying plate. Figure 7 It is a transmittance curve diagram of the 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system of Example 3 in the 7.7-10.5μm band with zinc selenide substrate plated on both sides.

[0121] Figure 8 This is a reflectivity curve of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 1 coated on both sides of the accompanying coating sheet at a wavelength of 1064nm. Fig. 9 It is a transmittance curve of the 7.7-10.5 μm band antireflection film system of the 1064 nm wavelength high-reflection 7.7-10.5 μm band of the accompanying coating sheet of Example 1, which is plated on both sides of the zinc selenide substrate.

[0122] Fig.10 This is a reflectivity curve of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 2, which is plated on both sides of the accompanying plate. Fig.11It is a transmittance curve of the 7.7-10.5 μm band of the accompanying plate of Example 2, which is coated with a zinc selenide substrate with a 1064 nm wavelength high-reflection 7.7-10.5 μm band anti-reflection film on both sides.

[0123] Fig.12 This is a reflectivity curve of the 1064nm wavelength high-reflective 7.7m-10.5μm band anti-reflection film system of Example 3, which is plated on both sides of the accompanying plate. Fig.13 It is a transmittance curve of the 7.7-10.5 μm band of the 1064 nm wavelength high-reflective 7.7-10.5 μm band anti-reflection film system of the accompanying coating sheet of Example 3, which is plated on both sides of the zinc selenide substrate.

[0124] Table 1 shows the reflectivity (at a wavelength of 1064 nm), average transmittance (at a wavelength of 7.7-10.5 μm) of Examples 1-3 and Comparative Examples 1-3, and the results of various tests.

[0125] Table 1 Reflectivity, average transmittance and various test results of Examples 1-3 and Comparative Examples 1-3

[0126]

[0127]

[0128] As can be seen from Examples 1-3, the reflectivity of Examples 1-3 at a wavelength of 1064nm is more than 99%, the average transmittance in the 7.7-10.5μm band is more than 98.5%, and the blister test, salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, low temperature test, and high temperature test are all passed.

[0129] The plating on both sides of Comparative Example 1 did not use ion source assisted deposition. The reflectivity of Comparative Example 1 at a wavelength of 1064nm exceeded 99%, and the average transmittance in the 7.7-10.5μm band exceeded 98.5%, but the blister test failed. The remaining salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, low temperature test, and high temperature test were no longer tested.

[0130] Comparative Example 2: Y 2 O 3 The film material is used as the base, and the reflectivity of Comparative Example 2 at a wavelength of 1064nm is lower than 99%, and the average transmittance in the 7.7-10.5μm band is lower than 98%. It passes the blister test, salt spray test, adhesion test, hot and cold shock test, constant temperature and humidity test, low temperature test, and high temperature test.

[0131] The eighteenth layer of Comparative Example 3 is YbF with a film thickness of 95.35 nm. 3For the film layer, the reflectivity of comparative example 3 at a wavelength of 1064nm exceeds 99%, and the average transmittance in the 7.7-10.5μm band exceeds 98.5%. It passes the blister test, adhesion test, and hot and cold shock test, but fails the constant temperature and humidity test. The salt spray test, low temperature test, and high temperature test are no longer tested.

[0132] 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 zinc selenide substrate 1064nm wavelength high-reflection 7.7-10.5μm band anti-reflection film system, characterized in that: Includes steps: S1, before plating, clean the accompanying plating sheet and products of the zinc selenide substrate as the lens and prepare the two film materials of YbF3 and ZnSe; S2, the cleaned lens is placed in a fixture, and the fixture with the lens is hung in the cavity of the coating machine for vacuum baking and pre-melting of the film material; S3, ion source cleaning lens; S4, under vacuum conditions, sequentially depositing a first YbF3 film layer, a second ZnSe film layer, a third YbF3 film layer, a fourth ZnSe film layer, a fifth YbF3 film layer, a sixth ZnSe film layer, a seventh YbF3 film layer, an eighth ZnSe film layer, a ninth YbF3 film layer, a tenth ZnSe film layer, an eleventh YbF3 film layer, a twelfth ZnSe film layer, a thirteenth YbF3 film layer, a fourteenth ZnSe film layer, a fifteenth YbF3 film layer, a sixteenth ZnSe film layer, a seventeenth YbF3 film layer, and an eighteenth ZnSe film layer on the first surface of the lens, wherein all eighteen film layers are deposited using an ion source assisted deposition; S5, constant temperature maintenance after plating; S6, cooling and picking up; S7, repeating steps S1 to S6 to perform film coating on the second surface of the lens.

2. The method for preparing a zinc selenide substrate 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system according to claim 1, characterized in that: In step S1, Cleaning is done by ultrasonic cleaning and manual wiping; The thickness of the accompanying plating sheet is 1.0 mm.

3. The method for preparing a 1064nm wavelength high-reflective 7.7-10.5μm band anti-reflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S2, The temperature of the coating machine chamber is set to 150°C; When the vacuum reaches (3.0-5.0)×10 -3 The film material is pre-melted at Pa. After the pre-melting of the film material is completed, the temperature of the cavity of the coating machine reaches 150°C and is kept constant for 15-20 minutes.

4. The method for preparing a 1064nm wavelength high-reflective 7.7-10.5μm band antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S3, When the vacuum degree reaches (1.0-2.0)×10 -3 Pa, start the ion source of the vacuum coating machine, The ion cleaning parameters of the ion source were set as follows: neutralization current 0.6 A, neutralization gas flow rate 8 sccm, anode voltage 220 V, anode current 2 A, argon flow rate in neutralization gas 100%, and cleaning time 250-350 s.

5. The method for preparing a 1064nm wavelength high-reflective 7.7-10.5μm band antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S4, During coating, argon gas is filled into the cavity of the coating machine and evacuated to form a flowing vacuum to ensure that the vacuum degree of the coating is maintained at (4.5-5.5)×10 -3 Pa, and maintain the coating temperature at 150°C.

6. The method for preparing a 1064nm wavelength high-reflective 7.7-10.5μm band antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S4, The evaporation mode of the film material is: both the YbF3 film layer and the ZnSe film layer are evaporated using resistance heating.

7. The method for preparing a 1064 nm wavelength high-reflective 7.7-10.5 μm band antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S4, The deposition rate of the film material is: The deposition rate of the YbF3 film layer is The deposition rate of ZnSe film is 8. The method for preparing a 1064 nm wavelength high-reflective 7.7-10.5 μm band antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S4, The thickness of the first YbF3 film is 145.93±3nm. The thickness of the second ZnSe film is 373.9±3nm. The thickness of the third YbF3 film is 150.25±3nm. The thickness of the fourth ZnSe film layer is 119.45±3nm. The thickness of the fifth YbF3 film is 197.36±3nm. The thickness of the sixth ZnSe film layer is 323.64±3nm. The thickness of the seventh YbF3 film is 896.02±3nm. The thickness of the eighth ZnSe film layer is 144±3nm. The thickness of the ninth YbF3 film layer is 146.54±3nm. The thickness of the tenth ZnSe film layer is 351.85±3nm. The thickness of the eleventh YbF3 film layer is 216.78±3nm. The thickness of the twelfth ZnSe film layer is 93.85±3nm. The thickness of the thirteenth YbF3 film layer is 212.11±3nm. The thickness of the fourteenth ZnSe film layer is 372.01±3nm. The thickness of the fifteenth YbF3 film layer is 84.41±3nm. The thickness of the sixteenth ZnSe film layer is 602.75±3nm. The thickness of the seventeenth YbF3 film layer is 1318.9±3nm. The thickness of the eighteenth ZnSe film layer is 95.35±3nm; 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. After the ion source is cleaned, the crystal controller controls the corresponding operation of the new crystal oscillator pieces among the multiple crystal oscillator pieces, and the crystal oscillator frequency is not less than 6MHz.

9. The method for preparing a 1064 nm wavelength high-reflective 7.7-10.5 μm band antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S4, The ion source parameters when depositing the YbF3 film layer are: neutralization current 0.6A, neutralization gas flow rate 8sccm, anode voltage 130V, anode current 1.3A, argon flow rate in neutralization gas 30%, oxygen flow rate in neutralization gas 70%; The ion source parameters when depositing the ZnSe film layer are: neutralization current 0.5A, neutralization gas flow rate 8sccm, anode voltage 100V, anode current 1A, and argon gas flow rate in the neutralization gas is 100%.

10. The method for preparing a 1064 nm wavelength high-reflective 7.7-10.5 μm band antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S5, after the plating is completed, the cavity is kept at a constant temperature of 150°C for 10 minutes; In step S6, the door is opened to take out the items when the temperature drops below 100°C.

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