Broadband transparent coating as well as preparation method and application thereof

Abstract

The invention discloses a broadband transparent coating as well as a preparation method and application thereof, and belongs to the technical field of material preparation. The coating sequentially comprises an ITO thin layer, a photonic crystal multilayer, an ITO thin layer, a dielectric-metal-dielectric type dielectric multilayer, an ITO thin layer and a SiO2 infrared emission layer from a substrate to the outside. The invention aims to provide the broadband transparent coating and the preparation method and application thereof, and the coating can effectively cover a broadband range from visible light to near-infrared light and protect threats of lasers with different wavelengths. The high transmittance of the coating in the visible light band is higher than 90%, the clear visual field of optical equipment is guaranteed, meanwhile, the high reflectivity of the coating in the near-infrared band and the far-infrared band is higher than 85%, and damage of laser to the equipment is effectively avoided.

Description

Technical Field

[0001] The invention belongs to the technical field of material preparation, and in particular relates to a broadband transparent coating and a preparation method and application thereof. Background Art

[0002] With the widespread application of laser technology in the fields of communication, detection, medical treatment and military, especially in military guidance, detection and weapon systems, laser threats have become a major challenge in modern warfare. Laser weapons, with their rapid response, energy concentration and high-precision strike characteristics, have become a key technical means to counter traditional weapons. However, this also puts higher requirements on the laser protection of target equipment.

[0003] At present, laser protection materials on the market are mainly divided into two types: absorption type and reflection type. Absorption type materials reduce laser hazards by converting laser energy into heat energy, but they are prone to thermal effects, resulting in material ablation failure, and have poor transparency, making them unsuitable for occasions that require high light transmittance. Reflective materials reflect lasers of specific bands through metal or multi-layer dielectric films, but strong reflectivity may cause light pollution, affect imaging quality, and most of them can only provide protection for a single band. The technical bottlenecks of traditional laser protective coatings are mainly reflected in band limitations, lack of transparency, and poor environmental stability. Therefore, the development of new laser protection materials to achieve wide-band protection, high transparency, and good environmental stability is of great significance to improving the laser protection capabilities of modern equipment. Summary of the invention

[0004] The present invention aims to provide a wide-band transparent coating and a preparation method and application thereof. The coating has high transmittance in the visible light band and high reflectivity in the near-infrared and other bands, thereby achieving the purpose of wide-band laser protection.

[0005] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:

[0006] A method for preparing a broadband stealth composite material comprises the following steps;

[0007] A wide-band transparent coating comprises, from a substrate outwards, an ITO thin layer, a photonic crystal multilayer, an ITO thin layer, a dielectric-metal-dielectric type dielectric multilayer, an ITO thin layer and a SiO2 infrared emitting layer.

[0008] Preferably, the photonic crystal multilayer consists of a three-layer photonic crystal structure; the photonic crystal structure consists of a TiO2 thin layer and a SiO2 thin layer.

[0009] The present invention also provides a method for preparing the broadband transparent coating, comprising the following steps:

[0010] S1. Select the optical lens substrate material and deposit a thin ITO layer on the substrate surface by magnetron sputtering;

[0011] S2, preparing a photonic crystal structure: coating the precursor on the ITO thin layer in step S1 by spin coating, annealing, depositing a TiO2 thin layer on the ITO thin layer, adjusting the pressure to 200 Pa, introducing SiH4 and O2, reacting at 50° C. for 60 min, and depositing a SiO2 thin layer on the TiO2 thin layer to obtain a photonic crystal structure;

[0012] S3, repeat step S2 three times to obtain a photonic crystal multilayer with a thickness less than 800 nm;

[0013] S4, repeating step S1, depositing an ITO thin layer on the photonic crystal multilayer in step S3;

[0014] S5, applying the precursor on the ITO thin layer of step S4 by spin coating, annealing, depositing a TiO2 thin layer on the ITO thin layer, depositing an Ag thin layer on the TiO2 thin layer by electron beam evaporation, and then applying the precursor on the Ag thin layer by spin coating, annealing, and depositing a TiO2 thin layer on the Ag thin layer to obtain a dielectric-metal-dielectric type dielectric multilayer;

[0015] S6, repeating step S1, depositing a thin ITO layer on the dielectric-metal-dielectric multilayer of step S5;

[0016] S7, adjusting the pressure to 200 Pa, introducing SiH4 and O2, reacting at 50°C for 60 min, depositing a SiO2 thin layer on the ITO thin layer in step S6 to obtain a SiO2 infrared emitting layer, annealing to obtain a wide-band transparent coating.

[0017] Preferably, in step S1, the specific conditions of the magnetron sputtering are: the magnetron sputtering target is ITO, the target-substrate distance is 5-10 cm, the substrate temperature is 200-300° C., and the gas atmosphere is Ar / O2=9 / 1.

[0018] Preferably, the ITO consists of 90% In2O3 and 10% SnO2.

[0019] Preferably, in step S1, the reaction equation for preparing the ITO thin layer by magnetron sputtering is: InCl3+SnCl4+H2+O2→ITO+HCl.

[0020] Preferably, in step S1, the thickness of the ITO thin layer is 150-250 nm.

[0021] Preferably, in step S2, the precursor is TiCl4 or TBT, the spin coating speed is 2000 rpm, the annealing temperature is 400°C, and the annealing time is 30 min.

[0022] Preferably, in step S2, the thickness of the TiO2 thin layer is 80-120 nm; the thickness of the SiO2 thin layer is 80-120 nm; and the thickness of the single-layer photonic crystal structure is 160-240 nm.

[0023] Preferably, in step S3, the photonic crystal multilayer thickness is less than 800 nm.

[0024] Preferably, in step S4, the thickness of the ITO thin layer is 150-250 nm.

[0025] Preferably, in step S5, the precursor is TiCl4 or TBT, the spin coating speed is 2000 rpm, the annealing temperature is 400°C, the annealing time is 30 min, and the electron beam evaporation parameters are specifically: temperature is 50-100°C, and evaporation rate is 0.5-1 nm / s.

[0026] Preferably, in step S5, the thickness of the TiO2 thin layer is 40-60 nm; the thickness of the Ag thin layer is 30-50 nm.

[0027] Preferably, in step S6, the thickness of the ITO thin layer is 150-250 nm.

[0028] Preferably, in step S7, the annealing temperature is 400° C. and the time is 1 hour.

[0029] Preferably, in step S7, the thickness of the SiO2 infrared emitting layer is 80-120 nm.

[0030] The present invention also provides an application of the broadband transparent coating or the broadband transparent coating prepared by the preparation method in laser protection.

[0031] Compared with the prior art, the present invention has the following advantages and technical effects:

[0032] The present invention discloses a wide-band transparent coating and its preparation method and application. The coating can effectively cover a wide band range from visible light to near infrared (400-3000nm) to protect against laser threats of different wavelengths. The coating achieves a high transmittance of more than 85% in the visible light band (400-700nm), ensuring a clear field of view for optical equipment. At the same time, it exhibits a high reflectivity of more than 90% in the near infrared and far infrared bands (700-3000nm), effectively avoiding damage to the equipment by laser.

[0033] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 This is a process flow chart for preparing a broadband transparent coating according to Example 1 of the present invention;

[0035] Figure 2 A schematic diagram of the structure of a broadband transparent coating provided in Example 1 of the present invention;

[0036] Figure 3 The transmittance, reflectance and absorptance spectra of the transparent coating material obtained in Example 1 of the present invention. DETAILED DESCRIPTION

[0037] The technical solution of the present invention is further described below through the accompanying drawings and embodiments.

[0038] Unless otherwise defined, technical or scientific terms used in the present invention shall have the common meanings understood by one having ordinary skills in the field to which the present invention belongs.

[0039] In the present invention, unless otherwise specified, other test materials and instruments and equipment are conventional test materials in the art and can be purchased through commercial channels.

[0040] Example 1

[0041] A wide-band transparent coating, which includes an ITO thin layer, a photonic crystal multilayer, an ITO thin layer, a dielectric-metal-dielectric type dielectric multilayer, an ITO thin layer and a SiO2 infrared emitting layer in order from a quartz glass optical lens substrate to the outside. Figure 2 As shown, an ITO thin layer is first deposited on the upper layer of the discretionary collective, and the upper layer of the thin layer is a photonic crystal structure composed of alternating SiO2 and TiO2. After the ITO thin layer is attached, a dielectric-metal-dielectric dielectric multilayer structure of TiO2-Ag-TiO2 is deposited, and after the ITO thin layer is deposited again, a SiO2 infrared emission layer is deposited on the outermost layer. The photonic crystal multilayer consists of three layers of photonic crystal structure; the photonic crystal structure consists of a TiO2 thin layer and a SiO2 thin layer.

[0042] A wide-band transparent coating, the preparation method of which comprises the following steps;

[0043] S1. Using quartz glass optical lens substrate material, magnetron sputtering is used, wherein the magnetron sputtering target is ITO (90% In2O3 and 10% SnO2), the target-substrate distance is 10 cm, the substrate temperature is 300°C, the gas atmosphere is Ar / O2=9 / 1, and a 200 nm thick ITO thin layer is deposited on the substrate surface;

[0044] S2, preparing a photonic crystal structure: TiCl4 is coated on the ITO thin layer in step S1 by spin coating at 2000 rpm, annealed at 400°C for 30 min, a TiO2 thin layer with a thickness of 100 nm is deposited on the ITO thin layer, the pressure is adjusted to 200 Pa, SiH4 and O2 are introduced, reacted at 50°C for 60 min, and a SiO2 thin layer with a thickness of 100 nm is deposited on the TiO2 thin layer, and finally a photonic crystal structure with a thickness of 200 nm is obtained;

[0045] S3, repeat step S2 three times to obtain a photonic crystal multilayer with a thickness of 600 nm;

[0046] S4, repeat step S1, and deposit a 200nm thick ITO thin layer on the photonic crystal multilayer in step S3;

[0047] S5, coating TiCl4 on the ITO thin layer of step S4 by spin coating at 2000 rpm, annealing at 400° C. for 30 min, depositing a 60 nm thick TiO2 thin layer on the ITO thin layer, using electron beam evaporation at a temperature of 100° C. and an evaporation rate of 0.5 nm / s, depositing a 50 nm thick Ag thin layer on the TiO2 thin layer, then coating TiCl4 on the Ag thin layer by spin coating at 2000 rpm, annealing at 400° C. for 30 min, and depositing a 60 nm thick TiO2 thin layer on the Ag thin layer to obtain a dielectric-metal-dielectric type dielectric multilayer;

[0048] S6, repeating step S1, depositing a 200 nm thick ITO thin layer on the dielectric-metal-dielectric type dielectric multilayer of step S5;

[0049] S7, adjust the pressure to 200 Pa, introduce SiH4 and O2, react at 50°C for 60 min, deposit a SiO2 thin layer on the ITO thin layer in step S6 to obtain a SiO2 infrared emission layer with a thickness of 80-120 nm, anneal at 400°C for 1 h to obtain a wide-band transparent coating.

[0050] Through infrared, ultraviolet spectrometer and other testing equipment, the transmittance, reflectivity and emissivity of the transparent coating material are obtained as the wavelength of the incident light changes. Figure 3 As shown. Figure 3 It can be seen that the material shows a high transmittance within 0.3-0.6μm, with the highest transmittance reaching 93%; at the same time, the material maintains excellent reflectivity (above 60%) in the mid- and near-infrared, with the highest reflectivity being 88%. This proves that the overall transparent coating material has excellent transparency in the visible light band and excellent reflective performance in the infrared band.

[0051] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solution of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solution to deviate from the spirit and scope of the technical solution of the present invention.

Claims

1. A broadband transparent coating, characterized in that: The coating comprises, from the substrate outwards, an ITO thin layer, a photonic crystal multilayer, an ITO thin layer, a dielectric-metal-dielectric type dielectric multilayer, an ITO thin layer and a SiO2 infrared emitting layer.

2. A broadband transparent coating according to claim 1, characterized in that: The photonic crystal multilayer is composed of three layers of photonic crystal structure; the photonic crystal structure is composed of a TiO2 thin layer and a SiO2 thin layer.

3. A method for preparing a broadband transparent coating as claimed in claim 1 or 2, characterized in that: The method comprises the following steps: S1. Select an optical lens substrate material and deposit an ITO thin layer on the substrate surface by magnetron sputtering; S2, preparing a photonic crystal structure: coating the precursor on the ITO thin layer in step S1 by spin coating, annealing, depositing a TiO2 thin layer on the ITO thin layer, adjusting the pressure to 200 Pa, introducing SiH4 and O2, reacting at 50° C. for 60 min, and depositing a SiO2 thin layer on the TiO2 thin layer to obtain a photonic crystal structure; S3, repeat step S2 three times to obtain a photonic crystal multilayer with a thickness less than 800 nm; S4, repeating step S1, depositing an ITO thin layer on the photonic crystal multilayer in step S3; S5, applying the precursor on the ITO thin layer of step S4 by spin coating, annealing, depositing a TiO2 thin layer on the ITO thin layer, depositing an Ag thin layer on the TiO2 thin layer by electron beam evaporation, and then applying the precursor on the Ag thin layer by spin coating, annealing, and depositing a TiO2 thin layer on the Ag thin layer to obtain a dielectric-metal-dielectric type dielectric multilayer; S6, repeating step S1, depositing a thin ITO layer on the dielectric-metal-dielectric multilayer of step S5; S7, adjusting the pressure to 200 Pa, introducing SiH4 and O2, reacting at 50°C for 60 min, depositing a SiO2 thin layer on the ITO thin layer in step S6 to obtain a SiO2 infrared emitting layer, annealing to obtain a wide-band transparent coating.

4. The preparation method according to claim 3, characterized in that: The specific conditions of the magnetron sputtering in step S1 are: the magnetron sputtering target is ITO, the target-substrate distance is 5-10 cm, the substrate temperature is 200-300° C., and the gas atmosphere is Ar / O2=9 / 1.

5. The preparation method according to claim 3, characterized in that: In step S2, the precursor is TiCl4 or TBT, the spin coating speed is 2000 rpm, the annealing temperature is 400°C, and the annealing time is 30 min.

6. The preparation method according to claim 3, characterized in that: In step S5, the precursor is TiCl4 or TBT, the spin coating speed is 2000 rpm, the annealing temperature is 400°C, the annealing time is 30 min, and the electron beam evaporation parameters are specifically: temperature is 50-100°C, and evaporation rate is 0.5-1 nm / s.

7. The preparation method according to claim 3, characterized in that: In step S7, the annealing temperature is 400° C. and the time is 1 hour.

8. Use of the broadband transparent coating according to claim 1 or 2 or the broadband transparent coating prepared by the preparation method according to any one of claims 3 to 7 in laser protection.

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