CN111962023B - Spectrum selective reflecting film and preparation method thereof - Google Patents

Spectrum selective reflecting film and preparation method thereof Download PDF

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CN111962023B
CN111962023B CN202010855565.3A CN202010855565A CN111962023B CN 111962023 B CN111962023 B CN 111962023B CN 202010855565 A CN202010855565 A CN 202010855565A CN 111962023 B CN111962023 B CN 111962023B
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layer
film
infrared
visible light
gas
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CN111962023A (en
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王成龙
王锐东
李东锴
王天鹏
王良璧
马军
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Lanzhou Jiaotong University
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Abstract

The invention relates to a spectrum selective reflecting film and a preparation method thereof, which consists of a buffer layer, an infrared reflecting layer and a visible light antireflection layer; the buffer layer is made of hard Al 2 O 3 Or Si 3 N 4 One of (1); the infrared reflecting layer is made of AZO or Si 3 N 4 Or ITO; the visible light antireflection layer is made of hard SiO 2 Or Si 3 N 4 One kind of (1). The buffer layer and the infrared reflecting layer are sequentially manufactured on one surface of the light-transmitting substrate, the visible light antireflection layer is respectively manufactured on the infrared reflecting layer and the other surface of the light-transmitting substrate, or the infrared reflecting layer and the buffer layer are sequentially manufactured on one surface of the light-transmitting substrate, and the visible light antireflection layer is respectively manufactured on the buffer layer and the other surface of the light-transmitting substrate. The film is used on the surface of the glass cover plate of the linear Fresnel condenser, can increase the utilization rate of solar heat energy, improves the optical efficiency, effectively reduces the heat loss, and provides great support for the operation of the system.

Description

Spectrum selective reflecting film and preparation method thereof
Technical Field
The invention belongs to the technical field of solar photo-thermal spectrum selective membranes, and particularly belongs to the field of linear Fresnel type light condensation and heat collection of spectrum selective reflecting membranes.
Background
The Low emissivity (Low-E film) is a film which has high reflectance to infrared rays with a wavelength range of 2.5-40 μm and high transmittance to a visible light region. According to the structure of the film system, the low-radiation film is mainly divided into two main systems: one type is a transparent conductive oxide thin film (TCO) based on undoped or doped wide bandgap semiconductors; the other is a composite film based on a dielectric/metal/dielectric "sandwich" multilayer structure. A dielectric/metal/dielectric (D/M/D) -based multi-layer composite film having a "sandwich" structure has become one of the most widely used low-emissivity films in the world, and has more excellent low-emissivity characteristics than a TCO film. The basic structure is shown in fig. 1. The metal layer is a functional layer, and Au, Ag, Al, Cu and the like are adopted, and Ag is the most common. Ag is exposed to air and is easily corroded. Therefore, dielectric layers must be added on both sides of the silver film for protection. The dielectric layer in contact with the glass substrate serves as a transition layer between the metal layer and the glass to enhance the adhesion between the metal layer and the glass. The dielectric layer (cover film) in contact with the air is mainly used to protect the metal layer. The metal-based low-emissivity glass can be divided into single-silver and double-silver (three-silver) low-emissivity film systems. The double silver film system structure has a higher reflectance in the far infrared region than the single silver film system structure, but has a lower transmittance than the conventional single silver film system. The emissivity of a typical Low-E glass currently in use is shown in table 1.
Figure DEST_PATH_IMAGE001
In the Low-E film layer structure, a metal Ag layer plays a role in high infrared reflection (Low thermal emission ratio), and the thicker the Ag layer is, the higher the infrared reflectivity is, the lower the emission ratio is (-0.1), and meanwhile, the lower the visible light transmittance is (about 60%). The Low-E film layer prepared by the existing process is suitable for building energy-saving glass with Low requirement on visible light transmittance, but is limited in application in fields with high requirement on visible light transmittance (more than 85%), such as visible light windows. Researchers replace silver films with aluminum-doped zinc oxide (AZO) and tin-doped indium oxide (ITO) double-layer films (AZO/ITO) to achieve Low-E film performance, and the emissivity of the AZO/ITO is 0.07 and the average visible light transmittance is 80% under experimental conditions. The result proves that the replacement of the Ag film by aluminum-doped zinc oxide (AZO) and tin-doped indium oxide (ITO) is a technical means for solving the problem of low visible light transmittance of the film prepared by the prior art. But the visible light transmittance is still low.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a spectral selective reflection film. And its preparation process is also disclosed.
The technical scheme of the invention is as follows: a spectrum selective reflecting film comprises a buffer layer, an infrared reflecting layer and a visible light antireflection layer; the buffer layer is made of hard Al 2 O 3 Or Si 3 N 4 One of (1); the infrared reflecting layer is made of Al: ZnO or Si 3 N 4 Or ITO; the visible light antireflection layer is made of hard SiO 2 Or Si 3 N 4 To (3) is provided.
The preparation method of the spectrum selective reflecting film comprises the following steps: the buffer layer and the infrared reflecting layer are sequentially manufactured on one surface of the light-transmitting substrate, the visible light antireflection layer is respectively manufactured on the infrared reflecting layer and the other surface of the light-transmitting substrate, or the infrared reflecting layer and the buffer layer are sequentially manufactured on one surface of the light-transmitting substrate, and the visible light antireflection layer is respectively manufactured on the buffer layer and the other surface of the light-transmitting substrate.
The light-transmitting substrate is high borosilicate glass.
It is preferable that: the buffer layer is made of hard Al 2 O 3 The infrared reflecting layer is AZO, and the visible light antireflection layer is hard SiO 2 。
Wherein the hard Al 2 O 3 The preparation method comprises the following steps: vacuum evaporation thermal oxidation method, using aluminum sheet with purity of 99.99% as evaporation raw material, washing with deionized water, placing in a thermal evaporation dry pan, and vacuum-evaporating at background of 1 × 10 -4 Pa～4×10 -4 Depositing an aluminum film with the thickness of 30-50nm on a glass substrate by thermal evaporation under the condition of Pa; introducing oxygen into the vacuum evaporation chamber with the vacuum degree of 100-500Pa, closing the vacuum-pumping system, and raising the temperature in the chamber to 500 ℃ in a couple heating modeKeeping for 7-9 h, and generating an aluminum oxide film with the visible light transmittance of more than 95% on the surface of the glass substrate;
AZO (aluminum doped zinc oxide, 2wt% Al doped in ZnO) 2 O 3 ) The preparation method of the film adopts magnetron sputtering, and the preparation process comprises the steps of placing an AZO target on a target base, and adjusting the Ar gas flow to ensure that the pressure is 0.3 multiplied by 10 -2 Pa～0.8×10 -2 Pa; adjusting the sputtering power to be 100W, controlling the sputtering time to be 20 min, and obtaining the required AZO film as an infrared high-reflection (low-radiation film system) dielectric layer, wherein the infrared reflectivity is more than 91 percent, and the infrared radiance is less than 0.1;
hard SiO 2 The preparation method comprises the following steps: prepared by adopting a medium-frequency magnetron sputtering coating method, adopts 99.99 percent of polycrystalline silicon as a target material, and vacuumizes the background to 1 multiplied by 10 -4 Pa～9×10 -4 After Pa, introducing Ar gas and oxygen gas, wherein the gas flow ratio is 2:1, the target voltage is maintained at 300-400V, and the deposition thickness is 80-100 nm.
It is preferable that: the buffer layer is made of Si 3 N 4 The infrared reflecting layer is made of ITO, and the visible light reflecting layer is made of hard SiO 2 。
Wherein Si is 3 N 4 The preparation method comprises the following steps: microwave enhanced chemical vapor deposition (PECVD) using SiH with volume fraction of 5% 4 （Ar：SiH 4 =19: 1) and high purity N 2 As a gas source, wherein nitrogen is introduced into the discharge chamber to participate in microwave plasma discharge, the gas flow is 10-80 sccm, silane gas is introduced into the downstream area of the plasma, the gas flow is 5-50 sccm, and the silane gas and N ions act on the substrate to deposit and form Si 3 N 4 The temperature in the deposition process is 350 ℃, the microwave power is 500-700W, the roughness of the silicon nitride film is 1.3-1.5nm, the thickness of the prepared film is 50-300nm, and the refractive index is 2.0;
the preparation method of the ITO comprises the following steps: preparing ITO film by radio-frequency magnetron sputtering method, using high-purity Ar as working gas and high-purity O 2 As a reaction gas, the target material is ITO (In) 2 O 3 And SnO 2 The mass fraction ratio is 9: 1), the purity is 99.99 percent, and the background vacuum degree is 4.0×10 -4 Pa, the substrate temperature is 200 ℃ during film coating, the radio frequency power is 130-150W, the pressure in the vacuum chamber is 1-2Pa during sputtering, the flow ratio of argon to oxygen is 99:1, and the sputtered ITO film is 1-1.5 mu m; the infrared reflectivity is more than 91 percent, and the infrared radiance is less than 0.1;
hard SiO 2 The preparation method comprises the following steps: prepared by adopting a medium-frequency magnetron sputtering coating method, adopts 99.99 percent of polycrystalline silicon as a target material, and vacuumizes the background to 1 multiplied by 10 -4 Pa～9×10 -4 After Pa, introducing Ar gas and oxygen gas, wherein the gas flow ratio is 2:1, the target voltage is maintained at 300-400V, and the deposition thickness is 80-100 nm.
The invention has the beneficial effects that: the buffer layer, the infrared reflecting layer and the visible light antireflection layer are coordinated and act together, when sunlight directly irradiates the surface of the glass, one part of light is reflected, the other part of light penetrates through the surface of the glass, the thickness of the spectrum selective reflecting film is 280 nm-2.5 mu m, and the visible light transmittance reaches over 90% under the thickness, so that the high transmittance of the light is ensured, and meanwhile, the buffer layer, the infrared reflecting layer and the visible light antireflection layer have high reflectance and low infrared heat emission ratio (0-0.1) for infrared light larger than 2.5 mu m. If the film is used on the surface of the glass cover plate at the opening of the linear Fresnel type condenser, the utilization rate of solar heat energy can be increased, the optical efficiency is improved, and the heat loss is effectively reduced.
Drawings
FIG. 1 is a basic structure of a low emissivity glass;
FIG. 2 is a schematic structural view of example 1;
FIG. 3 is a schematic structural view of example 2.
Detailed Description
Example 1
The buffer layer is made of hard Al 2 O 3 The infrared reflecting layer is AZO, and the visible light reflecting layer is hard SiO 2 ，
Hard Al 2 O 3 The preparation method comprises the following steps: vacuum evaporation thermal oxidation method, using aluminum sheet with purity of 99.99% as evaporation raw material, washing with deionized water, placing in a thermal evaporation dry pan, and vacuum evaporating at backgroundAbout 3X 10 -4 Depositing an aluminum film with the thickness of 30-50nm on a glass substrate by thermal evaporation under the condition of Pa; introducing oxygen into a vacuum evaporation chamber with the vacuum degree of 350Pa, closing a vacuum pumping system, raising the temperature in the chamber to 500 ℃ in a galvanic couple heating mode, keeping the temperature for 8 hours, and generating an aluminum oxide film with the visible light transmittance of over 95 percent on the surface of the glass substrate;
AZO (aluminum doped zinc oxide, 2wt% Al doped in ZnO) 2 O 3 ) The preparation method of the film adopts magnetron sputtering, and the preparation process comprises the steps of placing an AZO target on a target base, and adjusting the Ar gas flow to ensure that the pressure is 0.5 multiplied by 10 -2 Pa; adjusting the sputtering power to be 100W, controlling the sputtering time to be 20 min, and obtaining the required AZO film as an infrared high-reflection (low-radiation film system) dielectric layer, wherein the infrared reflectivity is 91 percent, and the infrared radiance is 0.09;
hard SiO 2 The preparation method comprises the following steps: prepared by adopting a medium-frequency magnetron sputtering coating method, adopts 99.99 percent of polycrystalline silicon as a target material, and vacuumizes the background to 3 multiplied by 10 -4 And after Pa, introducing Ar gas and oxygen gas at a gas flow ratio of 2:1, maintaining the target voltage at 350V, and depositing the film to a thickness of 90 nm.
The infrared reflectivity of the spectrum selective reflection film is 91% and the visible light transmissivity is 90% through tests.
Example 2
The spectral selective reflection film and the buffer layer are made of Si 3 N 4 The infrared reflecting layer is made of ITO, and the visible light reflecting layer is made of hard SiO 2 ，
Wherein Si is 3 N 4 The preparation method comprises the following steps: microwave enhanced chemical vapor deposition (PECVD) using SiH with volume fraction of 5% 4 （Ar：SiH 4 =19: 1) and high purity N 2 As a gas source, wherein nitrogen is introduced into the discharge chamber to participate in microwave plasma discharge, the gas flow is 10-80 sccm, silane gas is introduced into the downstream area of the plasma, the gas flow is 5-50 sccm, and the silane gas and N ions act on the substrate to deposit and form Si 3 N 4 The temperature in the deposition process is 350 ℃ of the substrate temperature, the microwave power is 600W, and the roughness of the silicon nitride filmThe degree is 1.3-1.5nm, the thickness of the prepared film is 200nm, and the refractive index is 2.0;
the preparation method of the ITO comprises the following steps: preparing ITO film by radio-frequency magnetron sputtering method, using high-purity Ar as working gas and high-purity O 2 As a reaction gas, the target material is ITO (In) 2 O 3 And SnO 2 The mass fraction ratio is 9: 1), the purity is 99.99 percent, and the background vacuum degree is 4.0 multiplied by 10 -4 Pa, the substrate temperature in coating is 200 ℃, the radio frequency power is 150W, the pressure in the vacuum chamber body is 1.5Pa in sputtering, the flow ratio of argon to oxygen is 99:1, and the ITO film is sputtered to be 1.3 mu m; the infrared reflectivity is 90%, and the infrared radiance is 0.1;
hard SiO 2 The preparation method comprises the following steps: prepared by adopting a medium-frequency magnetron sputtering coating method, adopts 99.99 percent of polycrystalline silicon as a target material, and vacuumizes the background to 3 multiplied by 10 -4 And after Pa, introducing Ar gas and oxygen gas at a gas flow ratio of 2:1, maintaining the target voltage at 350V, and depositing to a thickness of 100 nm.
The infrared reflectivity of the spectrum selective reflection film is 90% and the visible light transmissivity is 91% through tests.
The medium prepared by the method can enable the buffer layer, the infrared reflecting layer and the visible light antireflection layer to coordinate and act together, when sunlight directly irradiates on the surface of glass, a small part of visible light is reflected, most of the visible light penetrates through the surface of the glass, the thickness of the spectrum selective reflecting film is 280 nm-2.5 mu m, the light transmittance reaches over 90% under the thickness, and the reflectivity of a middle infrared band reaches 90%, so that the high light transmittance is ensured.

Claims (1)

1. A spectral selective reflection film for improving infrared reflectivity is characterized in that: the infrared reflection film comprises a buffer layer, an infrared reflection layer and a visible light antireflection layer;
the buffer layer is made of Si 3 N 4 The infrared reflecting layer is made of ITO, and the visible light reflecting layer is made of hard SiO 2 ；
Sequentially manufacturing a buffer layer and an infrared reflecting layer on one surface of a light-transmitting substrate, and respectively manufacturing an antireflection layer of visible light on the infrared reflecting layer and the other surface of the light-transmitting substrate, or sequentially manufacturing the infrared reflecting layer and the buffer layer on one surface of the light-transmitting substrate, and respectively manufacturing the antireflection layer of visible light on the buffer layer and the other surface of the light-transmitting substrate;
the light-transmitting substrate is high borosilicate glass;
Si 3 N 4 the preparation method comprises the following steps: microwave enhanced Chemical Vapor Deposition (CVD) with SiH of 5% by volume 4 And high purity N 2 As a gas source, wherein nitrogen is introduced into the discharge chamber to participate in microwave plasma discharge, the gas flow is 10-80 sccm, silane gas is introduced into the downstream area of the plasma, the gas flow is 5-50 sccm, and the silane gas and N ions act on the substrate to deposit and form Si 3 N 4 The temperature in the deposition process is 350 ℃, the microwave power is 500-700W, the roughness of the silicon nitride film is 1.3-1.5nm, the thickness of the prepared film is 50-300nm, and the refractive index is 2.0;
the preparation method of the ITO comprises the following steps: preparing ITO film by radio frequency magnetron sputtering method, using high-purity Ar as working gas and high-purity O 2 As reaction gas, the target material is ITO oxide ceramic target with the purity of 99.99 percent and the background vacuum degree of 4.0 multiplied by 10 -4 Pa, the substrate temperature is 200 ℃ during film coating, the radio frequency power is 130-150W, the pressure in the vacuum chamber is 1-2Pa during sputtering, the flow ratio of argon to oxygen is 99:1, and the sputtered ITO film is 1-1.5 mu m; the infrared reflectivity is more than 90 percent, and the infrared radiance is less than 0.1;
hard SiO 2 The preparation method comprises the following steps: prepared by adopting a medium-frequency magnetron sputtering coating method, adopts 99.99 percent of polycrystalline silicon as a target material, and vacuumizes the background to 1 multiplied by 10 -4 Pa～9×10 -4 After Pa, introducing Ar gas and oxygen gas, wherein the gas flow ratio is 2:1, the target voltage is maintained at 300-400V, and the deposition thickness is 80-100 nm.
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