阅读说明：本技术 近红外滤光片及其制备方法和滤光设备 (Near-infrared filter, preparation method thereof and filtering equipment ) 是由 周群飞 朱斌 于 2018-07-26 设计创作，主要内容包括：本发明涉及光学器件技术领域,具体而言,提供了一种近红外滤光片及其制备方法和滤光设备。本发明提供的近红外滤光片,包括玻璃基体和设于玻璃基体一侧表面的滤光层,滤光层包括依次交替设置的SiO<Sub>2</Sub>膜层与SiH膜层,其中,SiO<Sub>2</Sub>膜层与玻璃基体接触,SiO<Sub>2</Sub>膜层与SiH膜层的层数之和为20-40层,滤光层的厚度为3000-4500nm。该近红外滤光片,SiH膜层为高折射率薄膜,SiO<Sub>2</Sub>膜层为低折射率薄膜,两种薄膜交替堆叠得到的滤光层用于近红外滤光片的制备,使得近红外滤光片起到有效地滤光作用。本发明提供上述近红外滤光片的制备方法,该方法操作简单,成本低,不需要的特殊的设备和工艺条件,适合工业化和自动化生产。(The invention relates to the technical field of optical devices, and particularly provides a near-infrared optical filter, a preparation method thereof and optical filtering equipment. The near-infrared filter provided by the invention comprises a glass substrate and a filter layer arranged on the surface of one side of the glass substrate, wherein the filter layer comprises SiO (silicon dioxide) layers which are alternately arranged in sequence 2 A film layer and an SiH film layer, wherein, SiO 2 Film layer in contact with glass substrate, SiO 2 The sum of the number of layers of the film layer and the SiH film layer is 20-40 layers, and the thickness of the filter layer is 3000-4500 nm. In the near infrared filter, the SiH film layer is a high refractive index film, SiO 2 The film layer is a low refractive index film, and the filter layer obtained by alternately stacking the two films is used for preparing the near-infrared filter, so that the near-infrared filter has an effective filtering effect. The preparation method of the near-infrared filter is simple to operate, low in cost, free of special equipment and process conditions and suitable for industrial and automatic production.)

1. The near-infrared filter is characterized by comprising a glass substrate and a filter layer arranged on the surface of one side of the glass substrate; the filter layer comprises SiO alternately arranged in sequence₂Film layer and SiH film layer, the SiO₂The film layer is in contact with the glass substrate;

The SiO₂The sum of the number of the layers of the film layer and the SiH film layer is 20-40 layers, and the thickness of the filter layer is 3000-4500 nm.

2. The near-infrared filter according to claim 1, wherein the SiO is present in an amount of less than one₂The sum of the number of layers of the film layer and the SiH film layer is 20-35 layers, preferably 20-30 layers.

3. the near-infrared filter according to claim 1, wherein the SiO is present in an amount of less than one₂The sum of the thicknesses of all the layers of the film layer is 2500-3500nm, and the sum of the thicknesses of all the layers of the SiH film layer is 500-1000 nm.

4. The near-infrared filter according to claim 1, wherein the SiO is present in an amount of less than one₂The thickness of each layer of the film layer is 10-400nm, and the thickness of each layer of the SiH film layer is 10-100 nm.

5. A near-infrared filter according to any one of claims 1 to 4, wherein the glass substrate is sapphire glass.

6. A method for manufacturing a near-infrared filter as defined in any one of claims 1 to 5, wherein SiO is alternately formed on the surface of the glass substrate in sequence₂A membrane layer and an SiH membrane layer.

7. The production method according to claim 6, wherein SiO is alternately deposited on the surface of the glass substrate in sequence by a sputtering process₂A membrane layer and an SiH membrane layer.

8. The method according to claim 7, wherein in the sputtering process, Si is used as a target material, and oxygen and hydrogen are sequentially and alternately introduced as reaction gases to sequentially and alternately deposit SiO on the surface of the glass substrate₂a membrane layer and an SiH membrane layer.

9. Method for the production according to claim 8, characterized in that SiO is deposited₂The sputtering technological parameters of the film layer comprise: vacuum degree of 6.0X 10^-3-10×10^-3Pa, target power 6-12KW, inert gas flow rate 45-65sccm, ICP power 2-6KW, oxygen flow rate 260-;

Preferably, the sputtering process parameters for depositing the SiH film layer include: vacuum degree of 6.0X 10^-3-10×10^-3pa, target power 6-12KW, inert gas flow rate 45-65sccm, ICP power 2-6KW, and hydrogen flow rate 380-.

10. a light filtering device comprising the near-infrared filter according to any one of claims 1 to 5 or the near-infrared filter obtained by the production method according to any one of claims 6 to 9.

Technical Field

The invention relates to the technical field of optical devices, in particular to a near-infrared optical filter, a preparation method thereof and optical filtering equipment.

Background

The near-infrared optical filter plays an important role in aerospace meteorology, natural disasters, resource general survey, remote sensing systems, infrared cameras and a plurality of military products. From the perspective of optical coating, the near-infrared filter is an optical device that has high transmittance for a specific wavelength band and high cutoff for another characteristic wavelength band. The near-infrared filter has extremely high requirements on the thickness, firmness and optical performance of each film layer. However, the existing near-infrared filters have few varieties, high preparation difficulty, low product yield, high cost, poor filtering effect and the like, which are technical problems to be solved.

the existing near-infrared filter mainly uses common glass (refractive index is 1.52) as a matrix, and adopts Ge and Ta₂O₅、TiO₂、Si、SiO、SiO₂The scheme of material combination is used as a filter layer to prepare the near-infrared filter, the filter has high absorptivity to near-infrared band light, and particularly, more than 80 layers of material layers in the filter layer need to be prepared to achieve a good light filtering effect. Therefore, the preparation process and difficulty of the filter layer are increased, the material cost and the thickness of the optical filter are increased, and the quality and the yield of the optical filter are difficult to guarantee.

In view of the above, the present invention is particularly proposed.

Disclosure of Invention

The first objective of the present invention is to provide a near-infrared filter, so as to alleviate the technical problems in the prior art that the thickness of the near-infrared filter is thick, the filtering effect is poor, the yield is low, the number of stacked layers of materials is large, and the preparation difficulty and the cost are high.

The second objective of the present invention is to provide a method for preparing the near-infrared filter, so as to alleviate the technical problems in the prior art that the yield of the production process of the near-infrared filter is low, the cost is high, and the prepared near-infrared filter has a poor filtering effect.

The third purpose of the present invention is to provide a light filtering device, which alleviates the lack of a light filtering device with good light filtering effect and low cost in the prior art.

In order to achieve the above purpose of the present invention, the following technical solutions are adopted:

A near-infrared filter comprises a glass substrate and a filter layer arranged on the surface of one side of the glass substrate;

The filter layer comprises SiO alternately arranged in sequence₂Film layer and SiH film layer, the SiO₂The film layer is in contact with the glass substrate;

The SiO₂The sum of the number of the layers of the film layer and the SiH film layer is 20-40 layers, and the thickness of the filter layer is 3000-4500 nm.

Further, the SiO₂The sum of the number of layers of the film layer and the SiH film layer is 20-35 layers, preferably 20-30 layers.

Further, the SiO₂the sum of the thicknesses of all the layers of the film layer is 2500-3500nm, and the sum of the thicknesses of all the layers of the SiH film layer is 500-1000 nm.

Further, the SiO₂The thickness of each layer of the film layer is 10-400nm, and the thickness of each layer of the SiH film layer is 10-100 nm.

Further, the glass substrate is sapphire glass.

The preparation method of the near-infrared optical filter comprises the steps of sequentially and alternately preparing SiO on the surface of the glass substrate₂A membrane layer and an SiH membrane layer.

Further, SiO is sequentially and alternately deposited on the surface of the glass substrate by utilizing a sputtering process₂A membrane layer and an SiH membrane layer.

Further, in the sputtering process, Si is used as a target material, oxygen and hydrogen are sequentially and alternately introduced to serve as reaction gases, and SiO is sequentially and alternately deposited on the surface of the glass substrate₂A membrane layer and an SiH membrane layer.

Further, SiO is deposited₂The sputtering technological parameters of the film layer comprise: vacuum degree of 6.0X 10^-3-10×10^-3Pa, target power 6-12KW, inert gas flow rate 45-65sccm, ICP power 2-6KW, oxygen flow rate 260-;

Further, the sputtering process parameters for depositing the SiH film layer include: vacuum degree of 6.0X 10^-3-10×10^-3Pa, target power 6-12KW, inert gas flow rate 45-65sccm, ICP power 2-6KW, and hydrogen flow rate 380-.

A light filtering device comprises the near-infrared filter or the near-infrared filter obtained by the preparation method.

Compared with the prior art, the invention has the beneficial effects that:

The invention provides a near-infrared filter, which comprises glassThe glass substrate and the filter layer arranged on one side surface of the glass substrate are arranged, and the filter layer comprises SiO (silicon dioxide) layers which are alternately arranged in sequence₂A film layer and an SiH film layer, wherein, SiO₂Film layer in contact with glass substrate, SiO₂The total number of layers of the film layer and the SiH film layer is 20-40 layers, and the thickness of the filter layer is 3000-4500 nm. In the near infrared filter, the SiH film layer is a high-refractive-index film, namely SiO₂The film layer is a low refractive index film, and SiO with specific number of layers and specific thickness is alternately stacked₂the composite layer of the film layer and the SiH film layer is used as a filter layer of the near-infrared filter, and light rays in each wave band are continuously reflected, refracted, transmitted and absorbed through the filter layer, so that the near-infrared filter has extremely small absorption on the light rays in the near-infrared wave band, the light rays in other wave bands are effectively transmitted through the near-infrared filter, and the light rays in other wave bands are effectively cut off, so that the near-infrared filter has an effective filtering effect. Specifically, the transmittance of the near-infrared filter for light with wavelength bands of 1530-1570nm can reach more than 92%, the transmittance for light with wavelength bands of 330-1400nm can reach less than 2%, and the near-infrared filter can completely absorb light with wavelength bands of 300-700nm, thereby effectively playing a role in filtering. The near infrared filter is thin and SiO₂The total number of layers of the film layer and the SiH film layer is small, the preparation process is simplified, the raw material consumption is greatly reduced, the production cost is greatly reduced, the yield of the product is improved, the yield of the product can reach 90%, meanwhile, the firmness of the filter layer and the glass substrate is high, the stability of the near-infrared filter is good, and the near-infrared filter can be applied to various scenes.

The preparation method of the near-infrared filter provided by the invention is simple to operate, low in cost, free of special equipment and process conditions and suitable for industrial and automatic production.

The invention finally provides a light filtering device which comprises the near-infrared light filter or the near-infrared light filter prepared by the preparation method. The filtering device has the performance advantages of the near-infrared filter.

Drawings

FIG. 1 is a chart of spectral detection of a near-infrared filter of example 4 in a test example of the present invention.

Detailed Description

Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.

The invention provides a near-infrared filter, which comprises a glass substrate and a filter layer arranged on the surface of one side of the glass substrate;

The filter layer comprises SiO alternately arranged in sequence₂Film and SiH film, SiO₂The film layer is contacted with the glass substrate;

SiO₂The sum of the number of layers of the film layer and the SiH film layer is 20-40 layers, and the thickness of the filter layer is 3000-4500 nm.

In the near infrared filter, the SiH film layer is a high-refractive-index film, namely SiO₂The film layer is a low refractive index film, and SiO with specific number of layers and specific thickness is alternately stacked₂The composite layer of the film layer and the SiH film layer is used as a filter layer of the near-infrared filter, and light rays in each wave band are continuously reflected, refracted, transmitted and absorbed through the filter layer, so that the near-infrared filter has extremely small absorption on the light rays in the near-infrared wave band, the light rays in other wave bands are effectively transmitted through the near-infrared filter, and the light rays in other wave bands are effectively cut off, so that the near-infrared filter has an effective filtering effect. In the invention, the thickness of the filter layer is 3000 + 4500nm, the SiH film layer and the SiO film layer₂When the sum of the number of the film layers is more than 20, the filtering effect of the near-infrared filter can be ensured. In a certain range, SiH film layer and SiO₂The larger the sum of the number of layers of the film layer is, the better the filtering effect of the near-infrared filter is, but the thickness of the filter layer is also large and exceeds a certain value, so that the filtering effect is not obviously improved, and the production cost is also increased unnecessarily. Therefore, while ensuring the light filtering effect, if the thickness of the filter layer and the SiH film layer and SiO are reduced₂The total number of layers of the film layer can greatly reduce the production cost. Specifically, the transmittance of the near-infrared filter for light in 1530-1570nm band can reach more than 92%, while the transmittance for light in 330-1400nm band can reach less than 2%, and meanwhile, the near-infrared filter can completely absorb light in 300-700nm band,Effectively playing a role of filtering light. The near infrared filter is thin and SiO₂The total number of layers of the film layer and the SiH film layer is small, the preparation process is simplified, the raw material consumption is greatly reduced, the production cost is greatly reduced, the yield of products is improved, meanwhile, the firmness of the filter layer and the glass substrate is high, the stability of the near-infrared filter is good, and the filter can be applied to various scenes.

In the present invention, the SiH film layer and SiO film layer₂The total number of layers of film is typically, but not limited to, 20, 21, 23, 25, 27, 29, 31, 33, 35, 37, 39, or 40; the thickness of the filter layer is typically, but not limited to, 3000nm, 3100nm, 3200nm, 3300nm, 3400nm, 3500nm, 3600nm, 3700nm, 3800nm, 3900nm, 4000nm, 4100nm, 4200nm, 4300nm, 4400nm, or 4500 nm.

Is different from the traditional infrared filter adopting Ge and Ta₂O₅、TiO₂、Si、SiO、SiO₂The invention adopts SiH and SiO₂The combined superposition method reduces the thickness of the near-infrared filter layer and simplifies the preparation process, and has the characteristics of low cost and simple preparation.

In some embodiments of the present invention, the glass substrate may be ordinary glass, tempered glass, quartz glass, sapphire glass, or the like. The chemical composition of the ordinary glass is Na₂SiO₃、CaSiO₃、SiO₂Or Na₂O·CaO·6SiO₂And the main component is silicate double salt which is amorphous solid with a random structure. The composition of the toughened glass is the same as that of the common glass, but the toughened glass is the prestressed glass obtained by reprocessing the common glass. Quartz glass is glass prepared from pure quartz, SiO₂The content is more than 99.5 percent, the thermal expansion coefficient is low, the high temperature resistance is high, the chemical stability is good, and the ultraviolet light and the infrared light are transmitted. Sapphire glass generally refers to artificially synthesized sapphire, which is a general name of corundum with other colors besides red sapphire in corundum, and the main component of the sapphire is alumina (Al)₂O₃) The sapphire glass has high temperature resistance, good heat conduction and high hardnessIt is infrared transparent and has high chemical stability.

In some preferred embodiments, the glass substrate is sapphire glass. In the embodiment of the invention, when the sapphire glass is used as the substrate, the light absorption rate of the sapphire glass to the near-infrared band is smaller, and the sapphire glass is matched with the filter layer to play a more effective role in filtering light. Meanwhile, the sapphire glass and the filter layer are combined more tightly, the surface is compact, the firmness is high, the stability is good, and the cost is low.

In a preferred embodiment of the present invention, the SiH film layer is formed with SiO₂The sum of the number of layers of the film layers is 20 to 35 layers, preferably 20 to 30 layers. In the preferred embodiment of the present invention, the SiH film layer and the SiO film layer of the near infrared filter₂The total number of the film layers is greatly reduced, the thickness of the filter layer is also greatly reduced, and even 20-35 layers, even 20-30 layers can completely achieve excellent filtering effect, thereby greatly reducing the production cost.

in a preferred embodiment of the invention, SiO₂The sum of the thicknesses of the layers is 2500-3500nm, and the sum of the thicknesses of the layers of the SiH film is 500-1000 nm. By the reaction of SiO₂The sum of the thicknesses of the film layers and the sum of the thicknesses of the SiH film layers are optimized and limited, and the two film layers are matched with each other to achieve the purpose of filtering light well. SiO 2₂The numerical value of the sum of the thicknesses of all the layers of the film layer and the sum of the thicknesses of all the layers of the SiH film layer is too low, so that the cut-off effect of the formed filter layer on light in other wave bands can be reduced; SiO 2₂The sum of the thicknesses of the layers of the film layer and the sum of the thicknesses of the layers of the SiH film layer are too large, and the transmittance of the filter layer to near-infrared band light may decrease. SiO 2₂The sum of the thicknesses of the layers of the film layer is typically, but not limited to, 2500nm, 2600nm, 2700nm, 2800nm, 2900nm, 3000nm, 3100nm, 3200nm, 3300nm, 3400nm, or 3500 nm; the sum of the thicknesses of the layers of the SiH film layer is typically, but not limited to, 500nm, 600nm, 700nm, 800nm, 900nm, or 1000 nm.

In a preferred embodiment of the invention, SiO₂The thickness of each layer of the film layer is 10-400nm, and the thickness of each layer of the SiH film layer is 10-100 nm. Mixing SiO₂The thickness of each of the film layer and the SiH film layer is preferably definedWithin a certain range, SiO can be ensured₂The thickness between each layer of rete is even relatively, and the thickness between each layer of SiH rete is even relatively, and then improves the stop action to near infrared band light's transmittance and other wave band light. SiO 2₂The thickness of the film layer is typically, but not limited to, 10nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, or 400 nm; the thickness of the SiH film layer is typically, but not limited to, 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, or 100 nm.

The invention also provides a preparation method of the near-infrared filter, which is characterized in that SiO is sequentially and alternately prepared on the surface of the glass substrate₂A membrane layer and an SiH membrane layer. The method has the advantages of simple operation, low cost, no need of special equipment and process conditions, and suitability for industrial and automatic production.

In a preferred embodiment of the present invention, SiO is alternately deposited on the surface of the glass substrate by a sputtering process₂A membrane layer and an SiH membrane layer.

In a preferred embodiment of the present invention, in the sputtering process, Si is used as a target material, and SiO is sequentially and alternately deposited on the surface of the glass substrate by sequentially and alternately introducing oxygen and hydrogen as reaction gases₂A membrane layer and an SiH membrane layer. Sputtering Si target material on the surface of the glass substrate by a sputtering process, forming a silicon film on the glass substrate by the Si target material, and reacting the silicon film with oxygen to generate SiO₂And (3) reacting the silicon film with hydrogen to generate an SiH film, and repeating the reaction for multiple times to obtain the near-infrared filter. The sputtering process makes the Si target material contact and react with oxygen or hydrogen more fully to form SiO on the surface of the glass substrate₂The film layer or the SiH film layer is more uniformly distributed, and the rate of forming the filter layer at each position on the surface of the glass substrate is also the same.

In a preferred embodiment of the invention, SiO is deposited₂The sputtering technological parameters of the film layer comprise: vacuum degree of 6.0X 10^-3-10×10^-3Pa, target power 6-12KW, inert gas flow rate 45-65sccm, ICP power 2-6KW, oxygen flow rate 260-.

ICP (inductively coupled plasma) is a method of generating current by electromagnetic induction with a time-varying magnetic fieldA plasma source as an energy source. ICP plasmatizes oxygen to obtain active oxygen which reacts with Si target material to generate SiO₂And (5) film layer.

the vacuum is typically, but not limited to, 6.0X 10^-3Pa、7.0×10^-3Pa、8.0×10^-3Pa、9.0×10^-3Pa or 10.0X 10^-3pa; the target power is typically, but not limited to, 6KW, 7KW, 8KW, 9KW, 10KW, 11KW or 12 KW; the inert gas flow rate is typically, but not limited to, 45sccm, 50sccm, 55sccm, 60sccm, or 65 sccm; ICP power is typically, but not limited to, 2KW, 3KW, 4KW, 5KW or 6 KW; the oxygen flow rate is typically, but not limited to, 260sccm, 270sccm, 280sccm, 290sccm, or 300 sccm.

Under the vacuum condition, the Si target is sputtered on the glass substrate at the flow rate of 45-65sccm by the inert gas, and oxygen is input at the flow rate of 260-300sccm, so that the Si target is deposited on the substrate to form a silicon film and reacts with the oxygen to form SiO₂And (5) film layer. SiO 2₂The film layer has a thickness forming rate of 0.6-0.8 nm/s. By controlling SiO₂The rate of film thickness formation can be calculated as SiO₂The generation time of the film layer is convenient for SiO₂And the film layers and the SiH film layers are alternately prepared, so that automatic management is realized.

In a preferred embodiment of the present invention, the sputtering process parameters for depositing the SiH film layer include: vacuum degree of 6.0X 10^-3-10×10^-3Pa, target power 6-12KW, inert gas flow rate 45-65sccm, ICP power 2-6KW, and hydrogen flow rate 380-. The vacuum is typically, but not limited to, 6.0X 10^-3Pa、7.0×10^-3Pa、8.0×10^-3Pa、9.0×10^-3Pa or 10.0X 10^-3Pa; the target power is typically, but not limited to, 6KW, 7KW, 8KW, 9KW, 10KW, 11KW or 12 KW; the inert gas flow rate is typically, but not limited to, 45sccm, 50sccm, 55sccm, 60sccm, or 65 sccm; ICP power is typically, but not limited to, 2KW, 3KW, 4KW, 5KW or 6 KW; the oxygen flow rate is typically, but not limited to, 380sccm, 390sccm, 400sccm, 410sccm, or 420 sccm.

Under vacuum condition, the flow rate of inert gas is 45-65sccm to make Si targetSputtering the material on a glass substrate, inputting oxygen at 380-₂and (5) film layer. SiO 2₂The film layer has a thickness forming rate of 0.3-0.4 nm/s. The generation time of the SiH film can be calculated by controlling the thickness forming rate of the SiH film, so that the SiH film and the SiO film can be conveniently formed₂and the film layers are alternately prepared, so that automatic management is realized.

in a preferred embodiment of the invention, the inert gas is argon.

The invention finally provides a light filtering device which comprises the near-infrared light filter or the near-infrared light filter obtained by the preparation method. The filter device has the performance advantages of the near-infrared filter and is low in cost. The filtering device may be, but is not limited to, an infrared gas analyzer, an infrared detector, an infrared printer, an infrared thermometer, an infrared camera, an infrared induction toilet, etc.

In order to facilitate a further understanding of the present invention, the technical solutions of the present invention will now be described in detail with reference to the preferred embodiments.