Preparation method of 1064nm infrared antireflection film system on zinc selenide substrate

Abstract

A method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate includes the following steps: S1, cleaning the surface of the zinc selenide substrate, the thickness of the zinc selenide substrate being 0.9-1.5mm; S2, placing the cleaned zinc selenide substrate into a fixture and hanging it into the cavity of a vacuum coating machine, the temperature of the cavity being set to 150℃; S3, starting the vacuum coating machine and evacuating the vacuum, the vacuum degree reaching 1×10⁻⁶. ‑3 S1. Turn on the ion source for cleaning. The cleaning time is 6 minutes. The ion source anode voltage is 220V, the anode current is 1.2-1.5A, and the emitter current is 1.3-1.5A. S2. Maintain the aforementioned vacuum level and deposit a ZnS film on one side of the zinc selenide substrate at a deposition rate of 0.8nm / s and a film thickness of 336nm±5nm. S3. Deposit a YbF3 film at a deposition rate of 0.6nm / s and a film thickness of 360nm±5nm. S4. Deposit another ZnS film at a deposition rate of 0.8nm / s and a film thickness of 314nm±5nm. S5. Deposit another YbF3 film at a deposition rate of 0.6nm / s and a film thickness of 189nm±5nm. S6. Repeat steps S4 to S7. S9. After the deposition is completed, wait for the vacuum chamber to cool and remove the film.

Description

Technical Field

[0001] The present disclosure relates to the infrared field, and more specifically to a method for preparing a 1064nm infrared anti-reflection film system on a zinc selenide substrate. Background Art

[0002] Zinc selenide (ZnSe) is a very good infrared material with a wide light transmittance range from 0.5μm to 19μm. Because zinc selenide has an extremely low absorption coefficient in the 1064nm band and has good imaging and thermal shock properties, it is often used as protective lenses and windows for lasers.

[0003] In order to improve the performance of zinc selenide in the 1064nm band, it is necessary to coat the surface of zinc selenide with an infrared anti-reflection film to increase the transmittance and reduce the reflectivity. Summary of the invention

[0004] In view of the problems existing in the background technology, the purpose of the present invention is to provide a method for preparing a 1064nm infrared anti-reflection film system on a zinc selenide substrate, which can prepare a zinc selenide-based infrared anti-reflection film system suitable for the 1064nm band, with a transmittance of more than 99%, a reflectivity of less than 0.3%, and good adhesion of the film layer.

[0005] Thus, a method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate comprises the following steps: S1, cleaning the surface of the zinc selenide substrate, wherein the thickness of the zinc selenide substrate is 0.9-1.5 mm; S2, placing the cleaned zinc selenide substrate into a fixture, and hanging the fixture with the zinc selenide substrate in the cavity of a vacuum coating machine, wherein the temperature of the cavity is set to 150°C; S3, starting the vacuum coating machine to evacuate the surface, and the vacuum degree reaches 1×10 -3Pa, open the ion source of the vacuum coating machine for cleaning, the cleaning time is 6 minutes, the anode voltage of the ion source is 220V, the anode current is 1.2-1.5A, and the emitter current is 1.3-1.5A; S4, maintain the above-mentioned vacuum degree, evaporate ZnS film on one side of the zinc selenide substrate, the deposition rate of ZnS film is 0.8nm / s, and the film thickness is controlled to be 336nm±5nm; S5, evaporate YbF3 film on the plated ZnS film, the deposition rate of YbF3 film is 0.6nm / s, and the film thickness is controlled to be 360nm±5nm; S6, evaporate another Zn on the plated YbF3 film S film layer, the deposition rate of the other ZnS film layer is 0.8nm / s, and the film thickness is controlled to be 314nm±5nm; S7, another YbF3 film layer is evaporated on the plated another ZnS film layer, the deposition rate of the other YbF3 film layer is 0.6nm / s, and the film thickness is controlled to be 189nm±5nm; S8, repeat steps S4 to S7, and evaporate a ZnS film layer, a YbF3 film layer, a ZnS film layer and a YbF3 film layer in sequence on the opposite side of the zinc selenide substrate; S9, after the plating is completed, wait for the vacuum chamber to cool to below 90°C and take out the zinc selenide substrate with the ZnS film layer and the YbF3 film layer plated on both sides.

[0006] The beneficial effects of the present disclosure are as follows: the zinc selenide substrate with ZnS film layer and YbF3 film layer plated on both sides prepared by the method for preparing a 1064nm infrared anti-reflection film system for a zinc selenide substrate according to the present disclosure is used as an optical part as a whole (that is, the ZnS film layer and YbF3 film layer (four layers on each side) plated on both sides of the zinc selenide substrate constitute an infrared anti-reflection film system), which is suitable for the 1064nm band, has a transmittance of more than 99%, a reflectivity of less than 0.3%, and good adhesion of the film layer. BRIEF DESCRIPTION OF THE DRAWINGS

[0007] Figure 1 It is a schematic structural diagram of ZnS layers and YbF3 film layers plated on both sides of a zinc selenide substrate prepared according to the method for preparing a 1064nm infrared anti-reflection film system for a zinc selenide substrate disclosed in the present invention.

[0008] Figure 2 It is a curve diagram of the transmittance of the ZnS layer and the YbF3 film layer plated on both sides of the zinc selenide substrate of Example 1.

[0009] Figure 3 It is a curve diagram of the reflectivity of the ZnS layer and the YbF3 film layer plated on both sides of the zinc selenide substrate of Example 1. DETAILED DESCRIPTION

[0010] 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.

[0011] [Preparation method of 1064nm infrared antireflection film system on zinc selenide substrate]

[0012] The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate disclosed in the present invention comprises the following steps:

[0013] S1, cleaning the surface of the zinc selenide substrate, the thickness of the zinc selenide substrate is 0.9-1.5 mm;

[0014] S2, placing the cleaned zinc selenide substrate into a fixture, and hanging the fixture with the zinc selenide substrate in the cavity of the vacuum coating machine, and setting the temperature of the cavity to 150°C;

[0015] S3, vacuum coating machine starts to evacuate, and the vacuum degree reaches 1×10 -3 Pa, open the ion source of the vacuum coating machine for cleaning, the cleaning time is 6 minutes, the anode voltage of the ion source is 220V, the anode current is 1.2-1.5A, and the emitter current is 1.3-1.5A;

[0016] S4, maintaining the aforementioned vacuum degree, evaporating a ZnS film layer on one side of the zinc selenide substrate, the deposition rate of the ZnS film layer is 0.8 nm / s, and the film thickness is controlled to be 336 nm±5 nm;

[0017] S5, evaporating a YbF3 film layer on the plated ZnS film layer, the deposition rate of the YbF3 film layer is 0.6nm / s, and the film thickness is controlled to be 360nm±5nm;

[0018] S6, evaporating another ZnS film layer on the plated YbF3 film layer, wherein the deposition rate of the another ZnS film layer is 0.8 nm / s, and the film thickness is controlled to be 314 nm±5 nm;

[0019] S7, evaporating another YbF3 film layer on the plated another ZnS film layer, the deposition rate of the another YbF3 film layer is 0.6nm / s, and the film thickness is controlled to be 189nm±5nm;

[0020] S8, repeating steps S4 to S7, sequentially evaporating a ZnS film layer, a YbF3 film layer, a ZnS film layer, and a YbF3 film layer on the opposite side of the zinc selenide substrate;

[0021] S9, after the plating is completed, wait for the vacuum chamber to cool down to below 90°C and take out the zinc selenide substrate with ZnS layer and YbF3 film layer plated on both sides.

[0022] The zinc selenide substrate with ZnS film layer and YbF3 film layer plated on both sides prepared by the method for preparing a 1064nm infrared anti-reflection film system on a zinc selenide substrate disclosed in the present invention is used as an optical part as a whole (that is, the ZnS film layer and YbF3 film layer (four layers on each side) plated on both sides of the zinc selenide substrate constitute an infrared anti-reflection film system), which is suitable for the 1064nm band, has a transmittance of more than 99%, a reflectivity of less than 0.3%, and good adhesion of the film layer.

[0023] It should be noted that the infrared antireflection films on both sides of the zinc selenide substrate obtained by repeating steps S4 to S7 in step S8 are identical.

[0024] In step S1, the surface of the zinc selenide substrate is cleaned, which is beneficial to improving the bonding effect between the two sides of the zinc selenide substrate and the ZnS film layer. For example, the surface of the zinc selenide substrate is cleaned by ultrasonic or hand wiping.

[0025] In step S1 , preferably, the thickness of the zinc selenide substrate is 1.0 mm.

[0026] In step S2, by setting the temperature of the chamber to 150°C, the surface of the zinc selenide substrate can be heated, which is conducive to the growth of the film layer (such as the ZnS film layer) on both sides of the zinc selenide substrate and reduces the film layer growth stress. The vacuum coating machine of step S2 can be any suitable commercially available equipment, such as the resistance evaporation coating machine manufactured and sold by Chengdu Xiwok Vacuum Technology Co., Ltd.

[0027] In step S3, an ion source is used for cleaning. The bombardment and sputtering of ions will cause the impurities, oil molecules, and oxides adsorbed on the surface of the zinc selenide substrate to separate from the substrate surface, thereby greatly improving the interface state, which is conducive to improving the bonding performance between the ZnS film layer and the zinc selenide substrate. At the same time, the surface of the zinc selenide substrate can be heated by bombarding the surface of the zinc selenide substrate with ions, which is conducive to the growth of the ZnS film layer and reduces the growth stress of the ZnS film layer. The ion source can be any suitable type, such as Ar.

[0028] In step S3 , the ion source may be a Hall ion source.

[0029] In one example, in step S3, the anode current is 1.2A and the emitter current is 1.5A.

[0030] In one example, in step S4 , the film thickness is controlled to be 336 nm.

[0031] In one example, in step S5 , the film thickness is controlled to be 360 ​​nm.

[0032] In one example, in step S6 , the film thickness is controlled to be 314 nm.

[0033] In one example, in step S7 , the film thickness is controlled to be 189 nm.

[0034] In one example, in steps S4 to S7 , the evaporation is performed using resistance heating.

[0035] [test]

[0036] Example 1

[0037] The preparation method of a 1064nm infrared antireflection film system on a zinc selenide substrate comprises the following steps:

[0038] S1, cleaning the surface of the zinc selenide substrate, the thickness of the zinc selenide substrate is 1.0 mm;

[0039] S2, placing the cleaned zinc selenide substrate into a fixture, and hanging the fixture with the zinc selenide substrate in place into the cavity of a vacuum coating machine, the temperature of the cavity is set to 150° C. The vacuum coating machine is a resistance evaporation coating machine manufactured and sold by Chengdu Siwork Vacuum Technology Co., Ltd.;

[0040] S3, vacuum coating machine starts to evacuate, and the vacuum degree reaches 1×10 -3 Pa, open the ion source of the vacuum coating machine for cleaning, the cleaning time is 6 minutes, the anode voltage of the ion source is 220V, the anode current is 1.2A, the emitter current is 1.5A, and the ion source is a Hall ion source;

[0041] S4, maintaining the aforementioned vacuum degree, evaporating a ZnS film layer on one side of the zinc selenide substrate, the deposition rate of the ZnS film layer is 0.8 nm / s, and the film thickness is controlled to be 336 nm;

[0042] S5, evaporating a YbF3 film layer on the plated ZnS film layer, the deposition rate of the YbF3 film layer is 0.6nm / s, and the film thickness is controlled to be 360nm;

[0043] S6, evaporating another ZnS film layer on the plated YbF3 film layer, wherein the deposition rate of the another ZnS film layer is 0.8 nm / s, and the film thickness is controlled to be 314 nm;

[0044] S7, evaporating another YbF3 film layer on the plated another ZnS film layer, the deposition rate of the another YbF3 film layer is 0.6nm / s, and the film thickness is controlled to be 189nm;

[0045] S8, repeating steps S4 to S7, sequentially evaporating a ZnS film layer, a YbF3 film layer, a ZnS film layer and a YbF3 film layer on the opposite side of the zinc selenide substrate;

[0046] S9, after the plating is completed, wait for the vacuum chamber to cool down to below 90°C and take out the zinc selenide substrate with ZnS layer and YbF3 film layer plated on both sides.

[0047] The zinc selenide substrate prepared in Example 1 with ZnS film and YbF3 film coated on both sides is used as an optical component as a whole, and the structure is as follows Figure 1 As shown schematically, Figure 2 The graph shows the transmittance of the entire infrared antireflection film system composed of the zinc selenide substrate prepared in Example 1 together with the ZnS film layer and the YbF3 film layer on both sides, Figure 3 The graph shows the reflectivity of the entire infrared anti-reflection film system composed of the zinc selenide substrate prepared in Example 1 together with the ZnS layer and the YbF3 film layer on both sides.

[0048] from Figure 2 It can be seen that in the 1064nm band, the transmittance can reach more than 99% and the reflectivity is below 0.3%.

[0049] The zinc selenide substrate prepared in Example 1, together with the ZnS film layer and the YbF3 film layer on both sides, was subjected to a blister test taken from tap water for 12 hours. It was found that the ZnS film layer and the YbF3 film layer on both sides of the zinc selenide substrate did not fall off from the zinc selenide substrate, nor was it found that the ZnS film layer and the YbF3 film layer on both sides of the zinc selenide substrate were cracked. After the blister test taken from tap water was completed, 3M tape was pasted on the YbF3 film layer on one side by hand and the tape was pulled in the direction opposite to the pasting end. The four film layers on one side of the zinc selenide substrate were not pulled up. The same tape pulling experiment was performed on the other side of the zinc selenide substrate. As a result, the four film layers on the other side of the zinc selenide substrate were not pulled up. The blister test and the tape pulling experiment indicate that the film layers constituting the infrared anti-reflection film system on both sides of the zinc selenide substrate have good adhesion.

[0050] 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 1064nm infrared antireflection film system on a zinc selenide substrate, characterized in that: Includes steps: S1, cleaning the surface of the zinc selenide substrate, the thickness of the zinc selenide substrate is 0.9-1.5 mm; S2, placing the cleaned zinc selenide substrate into a fixture, and hanging the fixture with the zinc selenide substrate in the cavity of the vacuum coating machine, and setting the temperature of the cavity to 150°C; S3, vacuum coating machine starts to evacuate, and the vacuum degree reaches 1×10 -3 Pa, open the ion source of the vacuum coating machine for cleaning, the cleaning time is 6 minutes, the anode voltage of the ion source is 220V, the anode current is 1.2-1.5A, and the emitter current is 1.3-1.5A; S4, maintaining the aforementioned vacuum degree, evaporating a ZnS film layer on one side of the zinc selenide substrate, the deposition rate of the ZnS film layer is 0.8 nm / s, and the film thickness is controlled to be 336 nm±5 nm; S5, evaporating a YbF3 film layer on the plated ZnS film layer, the deposition rate of the YbF3 film layer is 0.6nm / s, and the film thickness is controlled to be 360nm±5nm; S6, evaporating another ZnS film layer on the plated YbF3 film layer, wherein the deposition rate of the another ZnS film layer is 0.8 nm / s, and the film thickness is controlled to be 314 nm±5 nm; S7, evaporating another YbF3 film layer on the plated another ZnS film layer, the deposition rate of the another YbF3 film layer is 0.6nm / s, and the film thickness is controlled to be 189nm±5nm; S8, repeating steps S4 to S7, sequentially evaporating a ZnS film layer, a YbF3 film layer, a ZnS film layer, and a YbF3 film layer on the opposite side of the zinc selenide substrate; S9, after the plating is completed, wait for the vacuum chamber to cool to below 90°C and take out the zinc selenide substrate with ZnS film and YbF3 film on both sides; In the 1064nm band, the transmittance can reach over 99% and the reflectivity is below 0.3%.

2. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S1 , the thickness of the zinc selenide substrate is 1.0 mm.

3. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S1, the surface of the zinc selenide substrate is cleaned by ultrasonic wave or hand wiping.

4. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S3, the anode current is 1.2A and the emitter current is 1.5A.

5. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S3, the ion source is a Hall ion source.

6. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S4, the film thickness is controlled to be 336 nm.

7. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S5, the film thickness is controlled to be 360 ​​nm.

8. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S6, the film thickness is controlled to 314 nm.

9. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S7, the film thickness is controlled to 189 nm.

10. The method for preparing a 1064nm infrared antireflection film system on a zinc selenide substrate according to claim 1, characterized in that: In step S4 to step S7, the evaporation is performed by resistance heating.

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